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Grain Oriented Electrical Steel Sheet

Abstract: A grain-oriented electrical steel sheet pertaining to the present invention has a grooved steel sheet surface, the average projection height of surface projections extending in the longitudinal direction of the grooves being more than 5 µm and no more than 10 µm, and, when the surface projections are viewed in a cross section that includes the longitudinal direction of the grooves and the direction of a normal to the steel sheet surface, the total length in the groove longitudinal direction of a portion having a height that is at least 50% of the height of a peak appearing in an outline of the surface projections being at least 30% of the overall length in the groove longitudinal direction of the surface projections.

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Patent Information

Application #
Filing Date
29 July 2020
Publication Number
38/2020
Publication Type
INA
Invention Field
METALLURGY
Status
Email
mahua.ray@remfry.com
Parent Application
Patent Number
Legal Status
Grant Date
2023-12-14
Renewal Date

Applicants

NIPPON STEEL CORPORATION
6-1, Marunouchi 2-chome, Chiyoda-ku, Tokyo 1008071

Inventors

1. ARAI Satoshi
c/o NIPPON STEEL & SUMITOMO METAL CORPORATION, 6-1, Marunouchi 2-chome, Chiyoda-ku, Tokyo 1008071
2. HAMAMURA Hideyuki
c/o NIPPON STEEL & SUMITOMO METAL CORPORATION, 6-1, Marunouchi 2-chome, Chiyoda-ku, Tokyo 1008071
3. OKUMURA Shunsuke
c/o NIPPON STEEL & SUMITOMO METAL CORPORATION, 6-1, Marunouchi 2-chome, Chiyoda-ku, Tokyo 1008071
4. SUGIYAMA Kimihiko
c/o NIPPON STEEL & SUMITOMO METAL CORPORATION, 6-1, Marunouchi 2-chome, Chiyoda-ku, Tokyo 1008071

Specification

Title of invention: grain-oriented electrical steel sheet
Technical field
[0001]
The present invention relates to grain-oriented electrical steel sheets.
The present application claims priority based on Japanese Patent Application No. 2018-021104 filed in Japan on February 8, 2018, the contents of which are incorporated herein by reference.
Background technology
[0002]
Generally, a grain-oriented electrical steel sheet is a steel sheet in which the orientations of crystal grains in the steel sheet are highly integrated in the {110} <001> orientation and the easy-to-magnetize axes are aligned in the longitudinal direction. An electromagnetic steel sheet having the property of having little iron loss and excellent magnetism because the axes that are easily magnetized are aligned in the longitudinal direction.
This grain-oriented electrical steel sheet has a structure in which a plurality of magnetic domains (striped magnetic domains) whose magnetization is oriented in the rolling direction are arranged with a domain wall in between, and most of these domain walls are 180 ° domain walls and are directional. Electrical steel sheets are easily magnetized in the rolling direction. Therefore, the magnetic flux density is high and the iron loss is low at a relatively small constant magnetization force.
Therefore, grain-oriented electrical steel sheets are very excellent as iron core materials for transformers.
W17 / 50 [W / kg] is generally used as an index of iron loss. W17 / 50 is a value of iron loss generated in the grain-oriented electrical steel sheet when AC-excited so that the maximum magnetic flux density becomes 1.7 T at a frequency of 50 Hz. If the W17 / 50 is made smaller, a more efficient transformer can be manufactured.
When the grain-oriented electrical steel sheet is subjected to strains substantially perpendicular to the rolling direction (conveying direction) and at regular intervals (fixed intervals), the iron loss is further reduced. In this case, a reflux type magnetic domain whose magnetization is orthogonal to the rolling direction is formed by local strain, and the domain wall spacing of the substantially rectangular striped magnetic domain becomes narrower due to the energy increment there (the width of the striped magnetic domain becomes narrower). Become smaller). Since the iron loss (W17 / 50) has a positive correlation with the distance between the 180 ° domain walls, the iron loss is reduced by this principle. By the way, the method of reducing the iron loss of the grain-oriented electrical steel sheet utilizing this local strain is the strain-removing annealing (for about 2 hours at 800 ° C.) carried out in order to eliminate the deterioration of the iron loss due to the processing strain of the wound steel core. Annealing) loses its effect. As a method in which the effect of reducing iron loss is not lost even when strain relief annealing is performed, a method of introducing a periodic groove in a direction intersecting the rolling direction is generally used.
[0003]
For the purpose of reducing the iron loss of the iron core, for example, Patent Document 1 discloses that the iron loss is improved by introducing linear flaws in the grain-oriented electrical steel sheet before finish annealing.
Further, Patent Document 2 discloses that by irradiating a continuous wave laser beam having a limited wavelength, a groove is formed on the surface of an electromagnetic steel sheet with high power efficiency to reduce iron loss.
[0004]
Here, the prior art of the method of forming a groove will be described. In the method by electrolytic etching, for example, a resist film having linear holes is printed on the surface of a cold-rolled plate by gravure printing, grooves are formed by electrolytic etching, and then the resist film is removed. In this method, the process becomes complicated, the manufacturing cost becomes high, and the processing speed is limited.
[0005]
In the method using a mechanical tooth mold press, since the electromagnetic steel sheet is a very hard steel sheet containing about 3% Si, the tooth mold is likely to be worn and damaged. When the tooth mold is worn, the groove depth varies, so that the iron loss improving effect becomes non-uniform.
[0006]
The laser irradiation method (referred to as the laser method) has an advantage that high-speed grooving can be performed by a focused laser beam having a high power density. Further, since the laser method is non-contact processing, stable and uniform grooving can be performed by controlling the laser power or the like.
[0007]
Further, conventionally, a CO 2 laser that can easily obtain a relatively high power is used as a laser light source, but the wavelength of the CO 2 laser is in the 9 to 11 μm band, and the laser light of this wavelength is a processing point. It is largely absorbed by the metal vapor and plasma generated at (processing position). Therefore, the power of the laser beam reaching the surface of the steel sheet is reduced, and the processing efficiency is lowered. Furthermore, plasma or metal vapor that has been heated and expanded by absorbing laser light acts as a secondary heat source and melts the periphery of the end (shoulder) of the groove, so that the amount of melting increases and the shape of the groove (for example, , Increase in molten protrusions) worsens.
Prior art literature
Patent documents
[0008]
Patent Document 1: Japanese Patent Application Laid-Open No. 59-197520
Patent Document 2: Japanese Patent No. 5234222
Outline of the invention
Problems to be solved by the invention
[0009]
The groove-introduced SRA magnetic domain control technology of the conventional machining or electrolytic etching as described above does not have a sufficient effect of reducing the iron loss of the grain-oriented electrical steel sheet, and further improvement of the iron loss is required.
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a grain-oriented electrical steel sheet capable of reducing iron loss in an iron core.
Means for solving the problem
[0010]
The present invention employs the following means in order to solve the above problems and achieve the object.
That is, the directional electromagnetic steel sheet according to one aspect of the present invention is a directional electromagnetic steel sheet having a steel plate surface provided with grooves, and is a region extending from the groove width direction end portion of the groove toward the outside in the groove width direction. In the method, the surface protrusions protruding from the surface of the steel plate extend along the groove longitudinal direction of the groove, and the average protrusion height of the surface protrusions is more than 5 μm and 10 μm or less, and the method of the groove longitudinal direction and the steel plate surface. When the surface protrusion is viewed in a cross section including the linear direction, the total length in the groove longitudinal direction of the portion having a height of 50% or more of the height of the peak point appearing on the contour line of the surface protrusion is the surface. The length is 30% or more with respect to the total length of the protrusion in the longitudinal direction of the groove.
Effect of the invention
[0011]
According to the above aspect of the present invention, a magnetic domain control effect equal to or greater than the groove introduction type magnetic domain control effect can be obtained by the linear elastic stress due to the protrusions of the grain-oriented electrical steel sheet when laminating the grain-oriented electrical steel sheet in the iron core production. Therefore, the iron loss of the iron core can be reduced.
A brief description of the drawing
[0012]
FIG. 1 is a plan view schematically showing an example of a groove pattern provided on the surface of a grain-oriented electrical steel sheet according to an embodiment of the present invention.
[Fig. 2] Fig. 2 is a schematic view of a groove and surface protrusions existing around the groove in a cross section orthogonal to the longitudinal direction of the groove.
FIG. 3 is a schematic view of surface protrusions existing in the peripheral portion of the groove in a cross section including the groove longitudinal direction and the normal direction of the steel plate surface.
FIG. 4 is a schematic view showing an example of a manufacturing apparatus including a laser light source and a laser beam irradiating apparatus used in the present embodiment.
Mode for carrying out the invention
[0013]
 Hereinafter, the grain-oriented electrical steel sheet according to the embodiment of the present invention will be described in detail with reference to the drawings.
The grain-oriented electrical steel sheet according to the present embodiment (hereinafter, abbreviated as the grain-oriented electrical steel sheet) is a grain-oriented electrical steel sheet having a grooved steel sheet surface. In this electrical steel sheet, surface protrusions protruding from the surface of the steel sheet extend along the groove longitudinal direction of the groove in a region extending from the end of the groove in the groove width direction toward the outside in the groove width direction. The average protrusion height of the surface protrusions is more than 5 μm and 10 μm or less.
Further, in this electromagnetic steel plate, a portion having a height of 50% or more of the height of the peak point appearing on the contour line of the surface protrusion when the surface protrusion is viewed in the cross section including the groove longitudinal direction and the normal direction of the steel plate surface. The total length of the surface protrusion in the groove longitudinal direction is 30% or more of the total length of the surface protrusion in the groove longitudinal direction.
[0014]
 In the following explanation, the terms such as "parallel", "vertical", "identical", and "right angle" and the values ​​of length and angle, which specify the shape and geometric conditions and their degrees, are strictly referred to. It is interpreted to include the range in which similar functions can be expected, without being bound by any meaning.
[0015]
 In groove formation by laser beam irradiation, the laser beam is absorbed on the surface of the steel sheet, the metal (base iron) of the steel sheet melts and fine molten droplets scatter, or the base iron on the surface of the steel sheet heated to the boiling point evaporates. Grooves are formed. The melt on the surface of the steel sheet is scattered by the pressure of high-temperature metal vapor or plasma at the processing point (laser beam irradiation point). On the other hand, when a large amount of melt is generated or when the pressure is low, the melt cannot be completely scattered, and the melt adheres to the peripheral portion of the formed groove to generate surface protrusions (projections, molten protrusions, etc.). ..
 In the laser groove formation test using a CO 2 pulse laser (large irradiation diameter), 20 μm or more rising from the surface of the steel sheet in the region extending outward in the groove width direction from the end in the groove width direction (periphery of the groove). Surface protrusions (protrusions, molten protrusions, etc.) with a height of about 40% are generated, and about 40% of iron loss deterioration is seen in magnetic measurement (pressurized Epstein measurement) in which a compressive force is applied to the surface of the steel sheet, leading to practical use. There wasn't.
 In the laser groove forming technology using a continuous irradiation laser (small irradiation diameter), the groove width of the groove formed on the surface of the steel sheet is small, so that the generation of protrusions at the focal position can be almost suppressed, but the steel sheet When the distance between the surface and the laser irradiation device fluctuates and the defocus state is reached, the generation of protrusions on the surface of the steel sheet becomes remarkable.
 In the groove-introduced SRA magnetic domain control technology for lasers, when the laser is out of focus, the protrusions that are raised from the surface of the steel sheet at the periphery of the grooves become large. This protrusion may cause an interlayer short circuit, an increase in core loss due to stress acting during the formation of a laminated iron core, a decrease in the laminated space factor, and the like.
 Further, in the SRA magnetic domain control by laser groove formation, if the protrusions in the peripheral portion of the groove due to laser groove formation are too large, iron loss deterioration is caused by local elastic deformation in the electromagnetic steel sheet due to the steel plate surface compressive force during iron core lamination. It is thought that it will occur.
 On the other hand, the present inventors have the same as the strain-introduced laser magnetic domain control in the grain-oriented electrical steel sheet when the morphology of the surface protrusions formed in the peripheral portion of the groove satisfies the following two conditions. It was found that a linear elastic strain was introduced and the iron loss could be further reduced.
(Condition 1) The average protrusion height of the surface protrusions is more than 5 μm and 10 μm or less.
(Condition 2) Groove length of a portion having a height of 50% or more of the height of the peak point appearing on the contour line of the surface protrusion when the surface protrusion is viewed in the cross section including the groove longitudinal direction and the normal direction of the steel plate surface. The total length in the direction is 30% or more of the total length in the groove longitudinal direction of the surface protrusion.
 Hereinafter, each configuration of the electrical steel sheet will be described.
[0016]
 (1) Basic Structure of the
 Main Electromagnetic Steel Sheet The main electromagnetic steel sheet has a mother steel sheet, and may have a coating film on the surface of the mother steel sheet, if necessary. Examples of the coating include a glass coating and a tension insulating coating.
[0017]
 The mother steel sheet is a steel sheet in which the orientation of the crystal grains in the mother steel plate is highly integrated in the {110} <001> orientation, and has excellent magnetic properties in the rolling direction.
 The chemical composition of the grain steel sheet is not particularly limited, and can be appropriately selected and used from the chemical compositions known as grain-oriented electrical steel sheets. Hereinafter, an example of a preferable chemical composition of the mother steel sheet will be described, but the chemical composition of the mother steel sheet is not limited to this.
[0018]
 For example, the mother steel sheet has a chemical composition of Si: 0.8% to 7%, C: more than 0% and 0.085% or less, acid-soluble Al: 0% to 0.065%, N: 0 in terms of chemical composition. % To 0.012%, Mn: 0% to 1%, Cr: 0% to 0.3%, Cu: 0% to 0.4%, P: 0% to 0.5%, Sn: 0% to It contains 0.3%, Sb: 0% to 0.3%, Ni: 0% to 1%, S: 0% to 0.015%, Se: 0% to 0.015%, and the balance is Fe and It preferably consists of impurities. The chemical composition of the mother steel sheet is a preferable chemical component for controlling the crystal orientation to the Goss texture integrated in the {110} <001> orientation. Among the elements in the base steel sheet, Si and C are basic elements, and acid-soluble Al, N, Mn, Cr, Cu, P, Sn, Sb, Ni, S, and Se are selective elements. Since these selective elements may be contained according to the purpose, it is not necessary to limit the lower limit value, and it is not necessary to substantially contain them. Further, even if these selective elements are contained as impurities, the effect of the present invention is not impaired. In the base steel sheet, the balance of the basic element and the selective element is composed of Fe and impurities.
 In the present embodiment, the “impurity” means an ore as a raw material, scrap, or an element that is inevitably mixed from the manufacturing environment or the like when the base steel sheet is industrially manufactured.
 In addition, grain-oriented electrical steel sheets generally undergo purification annealing during secondary recrystallization. In the purification annealing, the inhibitor-forming element is discharged to the outside of the system. In particular, the concentrations of N and S are significantly reduced to 50 ppm or less. Under normal purified annealing conditions, it reaches 9 ppm or less, further 6 ppm or less, and if purified annealing is sufficiently performed, it reaches a level that cannot be detected by general analysis (1 ppm or less).
 The chemical composition of the base steel sheet may be measured by a general method for analyzing steel. For example, the chemical composition of the mother steel sheet may be measured using ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectroscopy). Specifically, for example, a 35 mm square test piece is obtained from the center position of the mother steel plate after the coating is removed, and under the conditions based on the calibration curve prepared in advance by Shimadzu ICPS-8100 or the like (measuring device). It can be identified by measuring. In addition, C and S may be measured by using the combustion-infrared absorption method, and N may be measured by using the inert gas melting-thermal conductivity method. The chemical component of the grain steel sheet is a component obtained by analyzing the component of the grain steel sheet from which the glass film and the phosphorus-containing film described later are removed from the grain-oriented electromagnetic steel sheet by the method described later as the grain steel sheet.
[0019]
 The method for producing the grain steel sheet is not particularly limited, and a conventionally known method for producing a grain-oriented electrical steel sheet can be appropriately selected. As a preferable specific example of the production method, for example, C is 0.04 to 0.1% by mass, and the other slabs having the chemical composition of the mother steel sheet are heated to 1000 ° C. or higher for hot rolling. If necessary, hot-rolled sheet is annealed, and then cold-rolled once or twice or more with intermediate annealing in between to obtain a cold-rolled steel sheet, and the cold-rolled steel sheet is used, for example, in a wet hydrogen-inert gas atmosphere for 700. Examples thereof include a method of decarburizing and annealing by heating to about 900 ° C., further annealing and annealing if necessary, and finish annealing at about 1000 ° C.
 The thickness of the base steel plate is not particularly limited, but may be 0.10 mm or more and 0.50 mm or less, or 0.15 mm or more and 0.35 mm or less.
[0020]
 Examples of the glass coating include a coating having one or more oxides selected from forsterite (Mg2SiO4), spinel (MgAl2O4), and cordierite (Mg2Al4Si5O16).
[0021]
 The method for forming the glass film is not particularly limited, and a known method can be appropriately selected. For example, in a specific example of the method for producing a mother steel sheet, there is a method in which the finish annealing is performed after applying an annealing separator mainly composed of magnesia (MgO) to a cold-rolled steel sheet. The annealing separator also has an effect of suppressing sticking between steel sheets during finish annealing. For example, when the annealing separating agent containing magnesia is applied and finish annealing is performed, a glass film containing forsterite (Mg2SiO4) is formed on the surface of the mother steel sheet by reacting with silica contained in the mother steel sheet.
 The film thickness of the glass coating is not particularly limited, but may be 0.5 μm or more and 3 μm or less.
[0022]
 (2) Groove formation pattern and morphology of surface protrusions
 FIG. 1 is a plan view schematically showing an example of a groove pattern provided on the surface of a steel plate of the electrical steel sheet.
 FIG. 2 is a schematic view of a groove (for example, a groove 11) and surface protrusions existing around the groove in a cross section orthogonal to the longitudinal direction of the groove.
 FIG. 3 is a schematic view of a surface protrusion existing in a peripheral portion of a groove (for example, a groove 11) in a cross section including a groove longitudinal direction and a steel plate surface normal direction.
 In FIGS. 1 to 3, the rolling direction of the electromagnetic steel plate 1 is the X-axis direction, the plate width direction of the electromagnetic steel plate 1 (the direction orthogonal to the rolling direction in the same plane) is the Y-axis direction, and the electromagnetic steel plate 1 The plate thickness direction (direction orthogonal to the XY plane, that is, the normal direction of the steel plate surface) is defined as the Z-axis direction.
 As shown in FIG. 1, a linear groove 10 and an intermittent linear groove 11 are provided on the surface of a steel plate (surface of a mother steel plate) so as to extend along the plate width direction Y. In other words, in the present embodiment, the groove longitudinal direction of the groove 10 and the groove 11 coincides with the plate width direction Y. Surface protrusions are present in the groove 10 and the peripheral portion 12 of the groove 11.
 The grooves 10 and 11 may be provided so as to intersect the rolling direction X, and the groove longitudinal direction and the rolling direction X do not necessarily have to be orthogonal to each other. That is, it is not necessary that the groove longitudinal direction and the plate width direction Y coincide with each other.
[0023]
 As shown in FIG. 2, a surface protrusion 12 protruding from the steel plate surface (reference surface BL) extends along the groove longitudinal direction in the peripheral portion 100 of the groove 11, and the steel plate surface (in the peripheral portion 110 of the groove 11). A surface protrusion 13 protruding from the reference surface BL) extends along the longitudinal direction of the groove. In the present embodiment, the groove width direction of the groove 11 and the rolling direction X coincide with each other.
 Here, the region extending from one end a in the groove width direction of the groove 11 toward the outside in the groove width direction (the region between a and b in FIG. 2) is defined as the peripheral portion 100. Further, a region extending from the other end a'in the groove width direction of the groove 11 toward the outside in the groove width direction (the region between a'-b' in FIG. 2) is defined as the peripheral portion 110. As shown in FIG. 2, one end a in the groove width direction of the groove 11 and the other end a'in the groove width direction of the groove 11 are at the intersections of the contour line (cross-sectional curve) of the groove 11 and the reference surface BL, respectively. is there. The point b is an intersection of the contour line (cross-sectional curve) of the surface protrusion 12 and the reference surface BL, and is a point separated from one end a in the groove width direction to the outside in the groove width direction. The point b'is an intersection of the contour line (cross-sectional curve) of the surface protrusion 13 and the reference surface BL, and is separated from the other end a'in the groove width direction outward in the groove width direction.
 Further, in FIG. 2, the non-grooving region (non-grooving processed surface) of the grain-oriented electrical steel sheet 1 is set to the reference surface BL (reference height, including the surface of the steel sheet before groove formation) in the plate thickness direction. ing.
 As shown in FIG. 2, in the groove 11, in the section from one end a in the groove width direction to the other end a'in the groove width direction, a part of the base steel sheet of the main electromagnetic steel sheet 1 is formed by the groove forming process from the reference surface BL. It is a region formed by being removed.
 The groove width W of the groove 11 is a linear distance between one end a in the groove width direction and the other end a'in the groove width direction. The groove depth D of the groove 11 is the depth from the reference surface BL to the groove bottom (distance in the plate thickness direction Z). The point on the contour line of the groove 11 and existing at the deepest position in the plate thickness direction Z is defined as the groove bottom.
 The protrusion height T12 of the surface protrusion 12 is the height (distance in the plate thickness direction Z) from the reference surface BL to the tip of the surface protrusion 12. The protrusion height T13 of the surface protrusion 13 is the height (distance in the plate thickness direction Z) from the reference surface BL to the tip of the surface protrusion 13.
 The protrusion width of the surface protrusion 12 is a linear distance between one end a and a point b in the groove width direction. The protrusion width of the surface protrusion 13 is a linear distance between the other end a'in the groove width direction and the point b'.
 For various dimensions, a statistically sufficient number of measurements (for example, 50 measurements) is performed.
[0024]
 In the present embodiment, grooves of a predetermined length extending in a direction intersecting the rolling direction X are formed at predetermined intervals on the surface of the steel sheet of the electrical steel sheet 1 by a heat source such as a laser.
 In the present embodiment, the direction intersecting the rolling direction X includes a direction orthogonal to the rolling direction X in the XY plane (that is, a plate width direction Y), and is between the plate width direction Y and the groove longitudinal direction. The angle of may be in the range of ± 45 °, or may be in the range of ± 30 °.
[0025]
 The shape of the groove may be a linear shape extending in the plate width direction Y when the electromagnetic steel sheet 1 is viewed in a plan view, or may be an intermittent linear shape. The linear shape may be rectangular, elliptical, or the like when observed in an enlarged manner.
 When the shape of the grooves is intermittent, the distance between adjacent grooves in the plate width direction Y may be 1 μm to 1000 μm.
 On the other hand, the distance between adjacent grooves in the rolling direction X may be 1 to 10 mm, 3 to 6 mm, or 4 to 5 mm.
 In the present embodiment, the groove spacing is the second closest distance from the end (peripheral portion) of the first groove in a predetermined direction (plate width direction Y, rolling direction X, etc.). The shortest distance to the end (peripheral part) of the groove.
[0026]
 The average groove depth of the electrical steel sheet 1 may be 8 to 30 μm or 15 to 25 μm.
 The average groove depth is an average value of the measured values ​​of the groove depths D of 50 grooves for the grooves formed on the surface of the steel sheet.
 The method for measuring the groove depth D is as follows. First, a sample is taken from the steel sheet to be measured so that the cross section orthogonal to the groove longitudinal direction is exposed. The cross section of the sample is polished to reveal a cross section including the groove and its peripheral portion as shown in FIG. 2, and then the cross section is observed with an optical microscope or a scanning microscope to obtain a groove depth D (groove depth D). For example, the linear distance from the reference plane BL in FIG. 2 to the groove bottom) is measured. Such groove depth D is measured at each of the 50 points of the steel sheet to be measured. The average groove depth is a value obtained by averaging the measurement results of these 50 groove depths D.
[0027]
 Further, in the main electromagnetic steel sheet 1, the average groove width of the groove width W may be 1 to 200 μm.
 The average groove width is an average value of the measured values ​​of the groove widths W of 50 grooves for the grooves formed on the surface of the steel plate.
 The method for measuring the groove width W is as follows. First, a sample is taken from the steel sheet to be measured so that the cross section orthogonal to the groove longitudinal direction is exposed. The cross section of the sample is polished to reveal a cross section including the groove and its peripheral portion as shown in FIG. 2, and then the cross section is observed with an optical microscope or a scanning microscope to obtain a groove width W (for example,). The linear distance between a and a'in FIG. 2) is measured. Such groove width W is measured at each of the 50 points of the steel sheet to be measured. The average groove width is a value obtained by averaging the measurement results of these 50 groove widths W.
[0028]
 In the electrical steel sheet 1, the average height of the surface protrusions is more than 5 μm and 10 μm or less. When the average protrusion height of the surface protrusions is 5 μm or less, the iron loss reducing effect of the iron core cannot be sufficiently obtained. From the viewpoint of reducing the iron loss of the iron core, the average protrusion height of the surface protrusions is preferably 5.8 μm or more, and more preferably 6.0 μm or more.
 If the average protrusion height of the surface protrusions exceeds 10 μm, the insulating property between the laminated steel plates tends to deteriorate, which is not preferable. Therefore, the upper limit of the average protrusion height of the surface protrusion is 10 μm. The average protrusion height of the surface protrusions is preferably 7.3 μm or less.
 The average protrusion height of the surface protrusions is an average value of the measured values ​​of the protrusion heights (for example, T12 and T13 in FIG. 2) of 50 protrusions on the surface protrusions formed on the surface of the steel plate.
 The method for measuring the height of the protrusion is as follows. First, a sample is taken from the steel sheet to be measured so that the cross section orthogonal to the groove longitudinal direction is exposed. By polishing the cross section of the sample, a cross section including the groove and its peripheral portion as shown in FIG. 2 is revealed, and then the cross section is observed with an optical microscope or a scanning microscope to form a peripheral portion of the groove. The height of the existing surface protrusions (for example, T12 and T13 in FIG. 2) is measured. The height of such protrusions is measured at each of the 50 points of the steel sheet to be measured. The average protrusion height is a value obtained by averaging the measurement results of these 50 protrusion heights.
The shape of the surface protrusions is not particularly limited, and when a cross section obtained by cutting a grain-oriented electrical steel sheet perpendicular to the steel plate surface in a predetermined direction (plate width direction, rolling direction, etc.) is viewed from the front, a protrusion with a sharp tip is formed. It may be a bank shape with a flat tip.
[0029]
The average protrusion width of the surface protrusions is not particularly limited, but may be 1 to 10 μm. The average protrusion width is an average value of the measured values ​​of the protrusion widths at 50 places for the protrusions formed on the surface of the steel plate. The method for measuring the protrusion width is as follows. First, a sample is taken from the steel sheet to be measured so that the cross section orthogonal to the groove longitudinal direction is exposed. The cross section of the sample is polished to reveal a cross section including the groove and its peripheral portion as shown in FIG. 2, and then the cross section is observed with an optical microscope or a scanning microscope to form a peripheral portion of the groove. The protrusion width of the existing surface protrusion (for example, the linear distance between ab in FIG. 2 and the linear distance between a'-b') is measured. Such protrusion widths are measured at each of the 50 points of the steel sheet to be measured. The average protrusion width is a value obtained by averaging the measurement results of these 50 protrusion widths.
[0030]
In addition, the measurement result obtained by the surface roughness meter uses a method of polishing a cross section of a directional electromagnetic steel sheet perpendicular to the steel sheet surface along the rolling direction and observing it with an optical microscope or a scanning microscope. If it is the same as the measurement result obtained by the above, even if the groove depth (groove depth dimension) is determined from the groove length dimension (distance from the above reference plane to the groove tip) in the plate thickness direction. Good. Similarly, the protrusion height may be determined from the height dimension (distance in the plate thickness direction) from the reference surface to the tip of the surface protrusion.
[0031]
As shown in FIG. 3, in the electromagnetic steel plate 1, when the surface protrusion 12 (or 13 may be) is seen in the cross section including the groove longitudinal direction (plate width direction Y) and the plate thickness direction Z, the contour of the surface protrusion 12 The total length Lsum (= LP1 + LP2 + LP3 + LP5) in the groove longitudinal direction of the portion having a height of 50% or more of the height of the peak points (P1, P2, P3, P4, P5) appearing on the line is the groove length of the surface protrusion 12. It is 30% or more of the total length L in the direction. Focusing on the peak points P3 and P4 shown in FIG. 3, the mountain having the peak point P3 and the mountain having the peak point P4 are 50% or more higher than the height of the peak point P3 existing at a higher position. It is gently connected in the area of ​​Sa. In such a case, the mountain having the peak point P3 and the mountain having the peak point P4 are regarded as one mountain, and the height of the highest peak point P3 in this one mountain is 50% or more. Let LP3 be the length of the portion having the height in the groove longitudinal direction. Since the peak points P1, P2 and P5 do not apply to the above case, the length in the groove longitudinal direction may be obtained for each peak point. That is, in the mountain having the peak point P1, the length in the groove longitudinal direction of the portion having a height of 50% or more of the height of the peak point P1 is defined as LP1. Further, in the mountain having the peak point P2, the length in the groove longitudinal direction of the portion having a height of 50% or more of the height of the peak point P2 is defined as LP2. Further, in the mountain having the peak point P5, the length in the groove longitudinal direction of the portion having a height of 50% or more of the height of the peak point P5 is defined as LP5.
As described above, the ratio represented by (Lsum × 100) / L is defined as the protrusion continuity index. That is, in the electrical steel sheet 1, the morphology of the surface protrusions is controlled so that the protrusion continuity index is 30% or more.
[0032]
The condition that the average protrusion height of the surface protrusions is more than 5 μm and 10 μm or less is satisfied, and the protrusion continuity index is 30% or more (the condition that the length Lsum is 30% or more with respect to the length L) is satisfied. In that case, the iron loss reduction effect of the iron core is greatly increased. When the protrusion continuity index is less than 30%, the iron loss reducing effect of the iron core cannot be sufficiently obtained. From the viewpoint of reducing iron loss in the iron core, the protrusion continuity index is preferably 50% or more. Further, the upper limit of the protrusion continuity index is not particularly limited. The upper limit of the protrusion continuity index is mathematically 100%, but it is practically difficult to set the protrusion continuity index to 100%.
[0033]
The method for measuring the protrusion continuity index is as follows.
Using a device capable of measuring the three-dimensional shape of the surface of the steel plate to be measured, such as a laser microscope, the image of the surface of the steel plate including the groove is measured to identify the protrusion portion at a position higher than the reference surface BL in the peripheral portion of the groove. The protrusion continuity index is obtained from the length extending to the groove portion at the contour line position showing a value of 50% or more of the height value at the peak position of the continuous portion of the protrusion portion.
[0034]
As a method of forming a groove in the magnetic steel sheet 1, a laser irradiation method of forming a groove by irradiating the surface of the steel sheet with a laser (see JP-A-6-57335, International Publication No. 2016/171124) is used.
In the case of the laser irradiation method, the irradiation conditions are generally such that the laser output is 200 to 3000 W, the focused spot diameter in the rolling direction of the laser (diameter including 86% of the laser output) is 10 to 100 μm, and the laser is used. It is preferable to set the focusing spot diameter in the plate width direction to 10 to 1000 μm, the laser scanning speed to 5 to 100 m / s, and the laser scanning pitch (interval) to 2 to 10 mm. The desired groove shape can be obtained by appropriately adjusting these laser irradiation conditions within the above range.
[0035]
For groove formation, a continuously oscillating laser (laser capable of continuous oscillation) having a wavelength of 1.0 to 2.1 μm and having high light-collecting property may be used.
For example, examples of such a laser include a fiber laser, a thin disk type solid-state laser containing YAG, and the like. The laser light in the wavelength range of 1.0 to 2.1 μm is not easily absorbed by the plasma or metal vapor of metal ions generated at the processing point. Further, by using the continuous wave laser, there is no improvement and deterioration of iron loss due to the gap between the holes of the point train groove, which occurs in the pulse oscillation laser.
[0036]
As the fiber laser, a laser in which various laser media (excited atoms) are doped in the core of the fiber which is the oscillation medium may be used. For example, a fiber laser in which the core is doped with Yb (itribium) has an oscillation wavelength of 1.07 to 1.08 μm, and a fiber laser in which the core is doped with Er (erybium) has an oscillation wavelength of 1.55 μm and the core is Tm ( In the fiber laser doped with turium), the oscillation wavelength is 1.70 to 2.10 μm.
Further, the YAG laser, which is a high-power laser in the same wavelength range, has an oscillation wavelength of 1.06 μm. In the method using these fiber lasers and YAG lasers, the influence of laser absorption on plasma or metal vapor at the processing point is small.
[0037]
Further, in order to ensure high focusing property, the diameter of the focusing spot (focused beam diameter) may be 100 μm or less.
The fiber laser can collect light to the same extent as the core diameter, and in order to secure higher light collecting property, a fiber laser having a core diameter of 100 μm or less is suitable.
Further, in a solid-state laser such as a YAG laser, in a thin disk laser in which the oscillation medium is a thin disk type crystal, the surface area of ​​the crystal is large and cooling is easy. Deterioration is unlikely to occur, and minute light collection of 100 μm or less can be easily performed.
The diameter of the light-collecting spot and the groove width do not always match. For example, when the power density is high and the beam scanning speed V is small, the groove width becomes larger than the diameter of the focusing spot.
Further, when a laser with high accuracy as described above is used, even if the focal position of the laser beam is shifted (defocused) and the surface of the steel sheet is irradiated with the laser in order to form surface protrusions at a desired height. Good. The defocus may be set within a range of ± 1.2 mm from the focal position.
From the above, by controlling the focused beam diameter and the like to control the groove cross-sectional area, that is, the amount of melt removed, the amount of components that generate protrusions can be controlled, and the protrusion height can be controlled. Can be done.
[0038]
By the way, in a general laser irradiation method, at the same time as irradiating the laser beam, an assist gas such as air or an inert gas is sprayed onto a portion of the surface of the steel sheet to be irradiated with the laser beam. Such an assist gas plays a role of removing the components melted or evaporated from the steel sheet by laser irradiation. By spraying the assist gas, the laser beam reaches the surface of the steel sheet without being hindered by the molten or evaporated components, so that the grooves are stably formed.
By varying the flow rate of the assist gas between 0 and 100 (liters / minute) at time intervals of 0.02 to 0.2 msec, the present inventors have an average protrusion height of more than 5 μm and 10 μm. It has been found that the characteristic protrusion morphology of the electromagnetic steel plate 1 is as follows, and the protrusion continuity index is 30% or more. For example, as disclosed in the International Application Gazette (WO2016 / 171130), a method of spraying the assist gas at a constant flow rate set in the range of 10 to 1000 (liters / minute) is known. As described above, a method of increasing or decreasing the flow rate of the assist gas at a specific time interval is a completely unknown new method.
By forming surface protrusions satisfying specific conditions on the surface of the steel sheet, the present inventors introduce linear elastic strain similar to the strain-introduced laser magnetic domain control into the electromagnetic steel sheet when forming the laminated iron core. As a result, it was found that the iron core can be reduced in iron loss. Based on this finding, the present inventors have diligently researched a method capable of achieving both stable formation of grooves and low iron loss of the iron core, and as a result, have found a method of increasing or decreasing the flow rate of the assist gas at specific time intervals. It was.
The flow rate of the assist gas may be varied between the minimum value A1 and the maximum value A2 included in the range of 0 to 100 (liters / minute).
[0039]
(3) Groove Forming Method
FIG. 4 is a schematic view showing an example of a manufacturing apparatus including a laser light source and a laser beam irradiating apparatus used in the present embodiment. Note that FIG. 4 also shows the irradiation position of the laser beam irradiated to the grain-oriented electrical steel plate (steel plate) 1. An example of using a Yb-doped fiber laser as a laser medium as a laser light source will be described.
In FIG. 4, the steel plate 1 is a grain-oriented electrical steel plate having a plate width of 1000 mm after secondary recrystallization, and a glass coating is formed on the surface of the base steel. The steel plate 1 is passed through the steel plate 1 at a constant speed in the line direction (rolling direction, conveying direction) L at a line speed VL.
[0040]
The laser device 2 is a commercially available fiber laser having a maximum output of 2000 W, and the fiber core is doped with Yb as a laser medium, and its oscillation wavelength is 1.07 to 1.08 μm.
The diameter of the core is about 15 μm, and the laser oscillation mode of the output beam is a substantially basic Gauss mode.
The continuous wave (CW) laser light output from the laser device 2 is transmitted through the optical fiber 3 and reaches the laser irradiation device 4.
The laser irradiation device 4 includes a collimator 5, an icosahedron rotating polygon mirror 6, and an fθ lens 7 having a focal length of 200 mm.
The collimator 5 adjusts the diameter of the laser beam LB output from the transmission fiber 3.
Further, the rotating polygon mirror 6 deflects the laser beam LB and scans the steel plate 1 at high speed in the substantially plate width direction C, and the fθ lens 7 concentrates the laser beam LB.
[0041]
The rotation speed of the rotating polygon mirror 6 can be adjusted so that the beam scanning speed V on the steel plate 1 can be adjusted in the range of 2 to 50 m / s.
The scanning width of the focused beam on the steel plate 1 in the plate width direction is about 150 mm.
The focused beam diameter (diameter containing 86% of energy) d can be adjusted to 10 to 100 μm by changing the output beam diameter with the collimator 5.
A focus mechanism (not shown) is arranged between the rotating polygon mirror 6 and the fθ lens 7 having a focal length of 200 mm, and the distance between the fθ lens 7 and the steel plate can be adjusted by this focus mechanism. A laser beam is scanned onto the steel plate 1 by one surface of the rotating rotating polygon mirror 6, and a groove having a predetermined length (for example, the total length in the plate width direction) is formed on the steel plate 1 in the substantially width direction. To. The distance between the grooves adjacent to the L direction, that is, the irradiation pitch PL in the rolling direction (conveying direction) can be changed by adjusting the line speed VL and the polygon rotation speed.
[0042]
In this way, the laser irradiation device 4 is used to irradiate the steel plate 1 with the laser beam LB to form grooves in the rolling direction L at a constant scanning interval PL (= irradiation pitch, groove interval). That is, a laser beam is focused on the surface of the directional electromagnetic steel plate and irradiated while scanning to obtain a vector in a direction substantially perpendicular to the rolling direction of the directional electromagnetic steel plate (a direction intersecting the rolling direction and a vector perpendicular to the rolling direction). Grooves of a predetermined length extending in the including direction, for example, within ± 45 ° from this vertical direction) are formed at predetermined intervals in the transport direction.
Further, as described above, the flow rate of the assist gas during laser irradiation is controlled so as to fluctuate at a time interval of 0.02 to 0.2 msec with a flow rate of 0 to 100 (liters / minute).
The steel sheet 1 after the laser beam irradiation is coated with an insulating film that imparts electrical insulation and tension to the surface by a coating device (not shown).
[0043]
The present invention is not limited to the above embodiment. The above-described embodiment is an example, and any object having substantially the same configuration as the technical idea of ​​the present invention and exhibiting the same action and effect is included in the scope of the present invention.
Example
[0044]
(Examples 1 and 2, Comparative Examples 1 to 7) Compared to
a directional electromagnetic steel sheet (plate thickness 0.23 mm) having a high magnetic flux density in which the value of the magnetic flux density B8 at 800 A / m is 1.94 T, the steel sheet A linear groove with a width of about 50 μm and a depth of about 20 μm at intervals of 5 mm in the rolling direction at a scanning speed of 20 m / s using a 3 kW fiber laser with an elliptical beam shape of 40 μm in the rolling direction and 100 μm in the plate width direction. Was formed.
At that time, the laser beam is on the steel plate surface, in Example 1 a position close to 0.8 mm (−0.8 mm) from the focal position, in Example 2 a position 0.9 mm far from the focal position (+0.9 mm), Comparative Example 1. Is the focal position (± 0 mm), Comparative Example 2 is a position close to 0.4 mm (-0.4 mm) from the focal position, Comparative Example 3 is a position 0.5 mm far from the focal position (+0.5 mm), and Comparative Example 4 is the focal point. A position 1.1 mm far from the position (+1.1 mm), Comparative Example 5 is a position close to 1.2 mm (-1.2 mm) from the focal position, and Comparative Example 6 is a position 0.8 mm far from the focal position (+0.8 mm). In Comparative Example 7, irradiation was performed at a position (−1.1 mm) close to 1.1 mm from the focal position.
Further, under the conditions shown in Table 1 (minimum value A1 and maximum value A2 of assist gas flow rate, fluctuation time interval of assist gas flow rate), the flow rate of assist gas was increased or decreased at specific time intervals. In addition, Comparative Examples 1 to 5 show an example in which the minimum value A1 and the maximum value A2 of the assist gas flow rate are equal and the assist gas flow rate does not fluctuate with time, that is, an example in which the flow rate of the assist gas is controlled to be constant. There is.
Table 1 shows the measurement results of the average groove width, average groove depth, average protrusion height, protrusion continuity index, magnetic flux density, and iron loss of the obtained grain-oriented electrical steel sheet.
The iron loss of the grain-oriented electrical steel sheet was evaluated by a single plate measuring method after collecting a single plate (W100 mm × L500 mm) and subjecting it to strain relief annealing at 800 ° C. for 2 hours. Further, W17 / 50 is an iron loss value at 1.7 T / 50 Hz.
Further, the magnetic flux density B8 is defined by the magnetic flux density [T] generated when the magnetization force H is 800 A / m. In particular, in the case of a grain-oriented electrical steel sheet, B8 is the magnetic flux density when the steel sheet is magnetized in the rolling direction. The higher the B8, the higher the crystal orientation of the steel sheet (the larger the crystal orientation), and generally the lower the iron loss.
Regarding the protrusion continuity index, the steel plate surface image including the groove is measured using a device such as a laser microscope that can measure the three-dimensional shape of the steel plate surface to be measured, and the protrusion at a position higher than the reference surface BL in the groove peripheral portion. After identifying the portion, the protrusion continuity index was measured from the length extending to the groove portion at the contour line position showing a value of 50% or more of the height value at the peak position of the continuous portion of the protrusion portion.
[0045]
[table 1]

[0046]
Further, using the grain-oriented electrical steel sheets of Examples 1 and 2 and Comparative Examples 1 to 7, a 20 kVA single-phase wound steel core was prepared, and strain annealing was performed at 800 ° C. for 3 hours in an atmosphere of 100% nitrogen. did.
A primary winding (excited winding) and a secondary winding (search coil) were wound around these wound cores, and the core iron loss of each was measured with a wattmeter. The measurement results are shown in Table 2.
[0047]
[Table 2]

[0048]
 As shown in Table 1, in Examples 1 and 2, the flow rate of the assist gas is controlled to fluctuate between 0 and 100 (liters / minute) at a time interval of 0.02 to 0.2 msec. It was shown that the average protrusion height and the protrusion continuity index can be controlled within the range of the present invention. That is, in Examples 1 and 2, the average protrusion height could be controlled in the range of more than 5 μm to 10 μm or less, and the protrusion continuity index could be controlled to 30% or more. On the other hand, in Comparative Examples 1 to 7, as a result of not appropriately controlling the flow rate of the assist gas, one or both of the average protrusion height and the protrusion continuity index could not be controlled within the range of the present invention.
 However, as shown in Table 1, it can be seen that there is no significant difference in magnetic flux density and iron loss between the examples and the comparative examples when the electromagnetic steel sheet is viewed alone. That is, the average protrusion height and the protrusion continuity index do not significantly affect the magnetic flux density and iron loss of the electromagnetic steel sheet alone.
[0049]
 On the other hand, as shown in Table 2, in Examples 1 and 2, as a result of controlling the average protrusion height and the protrusion continuity index within the range of the present invention, the core iron loss is lower than that of Comparative Examples 1 to 7. It was shown to be. That is, if the wound steel core is manufactured using the grain-oriented electrical steel sheet of the present invention in which the average protrusion height of the surface protrusions is more than 5 μm and 10 μm or less and the protrusion continuity index is 30% or more, the iron loss is low. It was shown that a winding core can be obtained.
Code description
[0050]
1 Directional electromagnetic steel plate
2 Laser device
3 Optical fiber (transmission fiber)
4 Laser irradiation device
5 Collimator
6 Polygon mirror (rotating polygon mirror)
7 fθ lens
10 Groove (linear)
11 Groove (intermittent linear)
12 Surface protrusion
13 Surface Protrusion
100 Peripheral part
110 Peripheral part
The scope of the claims
[Claim 1]
In a directional electromagnetic steel plate having a grooved steel plate surface, in a
region extending from the groove width direction end portion of the groove toward the outside in the groove width direction, a surface protrusion protruding from the steel plate surface is a groove of the groove. When the surface protrusions are viewed in a cross section including the longitudinal direction of the groove and the normal direction of the surface of the steel plate , the
surface protrusions extend along the longitudinal direction and the average height of the surface protrusions is more than 5 μm and 10 μm or less.
The total length of the portion having a height of 50% or more of the height of the peak point appearing on the contour line of the surface protrusion in the groove longitudinal direction is 30% or more with respect to the total length of the surface protrusion in the groove longitudinal direction.
A directional electromagnetic steel sheet characterized by its length .

Documents

Orders

Section Controller Decision Date

Application Documents

# Name Date
1 202017032459-IntimationOfGrant14-12-2023.pdf 2023-12-14
1 202017032459-TRANSLATIOIN OF PRIOIRTY DOCUMENTS ETC. [29-07-2020(online)].pdf 2020-07-29
2 202017032459-PatentCertificate14-12-2023.pdf 2023-12-14
2 202017032459-STATEMENT OF UNDERTAKING (FORM 3) [29-07-2020(online)].pdf 2020-07-29
3 202017032459-Written submissions and relevant documents [14-11-2023(online)].pdf 2023-11-14
3 202017032459-REQUEST FOR EXAMINATION (FORM-18) [29-07-2020(online)].pdf 2020-07-29
4 202017032459-PROOF OF RIGHT [29-07-2020(online)].pdf 2020-07-29
4 202017032459-FORM 3 [31-10-2023(online)].pdf 2023-10-31
5 202017032459-PRIORITY DOCUMENTS [29-07-2020(online)].pdf 2020-07-29
5 202017032459-Correspondence to notify the Controller [26-10-2023(online)].pdf 2023-10-26
6 202017032459-US(14)-HearingNotice-(HearingDate-31-10-2023).pdf 2023-09-20
6 202017032459-FORM 18 [29-07-2020(online)].pdf 2020-07-29
7 202017032459-FORM 1 [29-07-2020(online)].pdf 2020-07-29
7 202017032459-Correspondence-090622-1.pdf 2022-06-13
8 202017032459-DRAWINGS [29-07-2020(online)].pdf 2020-07-29
8 202017032459-Correspondence-090622.pdf 2022-06-13
9 202017032459-DECLARATION OF INVENTORSHIP (FORM 5) [29-07-2020(online)].pdf 2020-07-29
9 202017032459-GPA-090622.pdf 2022-06-13
10 202017032459-COMPLETE SPECIFICATION [29-07-2020(online)].pdf 2020-07-29
10 202017032459-Others-090622.pdf 2022-06-13
11 202017032459-ABSTRACT [08-06-2022(online)].pdf 2022-06-08
11 202017032459-FORM-26 [31-08-2020(online)].pdf 2020-08-31
12 202017032459-CLAIMS [08-06-2022(online)].pdf 2022-06-08
12 202017032459-Verified English translation [12-10-2020(online)].pdf 2020-10-12
13 202017032459-DRAWING [08-06-2022(online)].pdf 2022-06-08
13 202017032459-FORM 3 [25-11-2020(online)].pdf 2020-11-25
14 202017032459-FER_SER_REPLY [08-06-2022(online)].pdf 2022-06-08
14 202017032459.pdf 2021-10-19
15 202017032459-FER.pdf 2021-12-09
15 202017032459-OTHERS [08-06-2022(online)].pdf 2022-06-08
16 202017032459-FER.pdf 2021-12-09
16 202017032459-OTHERS [08-06-2022(online)].pdf 2022-06-08
17 202017032459.pdf 2021-10-19
17 202017032459-FER_SER_REPLY [08-06-2022(online)].pdf 2022-06-08
18 202017032459-DRAWING [08-06-2022(online)].pdf 2022-06-08
18 202017032459-FORM 3 [25-11-2020(online)].pdf 2020-11-25
19 202017032459-CLAIMS [08-06-2022(online)].pdf 2022-06-08
19 202017032459-Verified English translation [12-10-2020(online)].pdf 2020-10-12
20 202017032459-ABSTRACT [08-06-2022(online)].pdf 2022-06-08
20 202017032459-FORM-26 [31-08-2020(online)].pdf 2020-08-31
21 202017032459-COMPLETE SPECIFICATION [29-07-2020(online)].pdf 2020-07-29
21 202017032459-Others-090622.pdf 2022-06-13
22 202017032459-DECLARATION OF INVENTORSHIP (FORM 5) [29-07-2020(online)].pdf 2020-07-29
22 202017032459-GPA-090622.pdf 2022-06-13
23 202017032459-Correspondence-090622.pdf 2022-06-13
23 202017032459-DRAWINGS [29-07-2020(online)].pdf 2020-07-29
24 202017032459-FORM 1 [29-07-2020(online)].pdf 2020-07-29
24 202017032459-Correspondence-090622-1.pdf 2022-06-13
25 202017032459-US(14)-HearingNotice-(HearingDate-31-10-2023).pdf 2023-09-20
25 202017032459-FORM 18 [29-07-2020(online)].pdf 2020-07-29
26 202017032459-PRIORITY DOCUMENTS [29-07-2020(online)].pdf 2020-07-29
26 202017032459-Correspondence to notify the Controller [26-10-2023(online)].pdf 2023-10-26
27 202017032459-PROOF OF RIGHT [29-07-2020(online)].pdf 2020-07-29
27 202017032459-FORM 3 [31-10-2023(online)].pdf 2023-10-31
28 202017032459-Written submissions and relevant documents [14-11-2023(online)].pdf 2023-11-14
28 202017032459-REQUEST FOR EXAMINATION (FORM-18) [29-07-2020(online)].pdf 2020-07-29
29 202017032459-STATEMENT OF UNDERTAKING (FORM 3) [29-07-2020(online)].pdf 2020-07-29
29 202017032459-PatentCertificate14-12-2023.pdf 2023-12-14
30 202017032459-TRANSLATIOIN OF PRIOIRTY DOCUMENTS ETC. [29-07-2020(online)].pdf 2020-07-29
30 202017032459-IntimationOfGrant14-12-2023.pdf 2023-12-14

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