CN109136794B - Integral PCBN blade and preparation method thereof - Google Patents
Integral PCBN blade and preparation method thereof Download PDFInfo
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- CN109136794B CN109136794B CN201811016010.9A CN201811016010A CN109136794B CN 109136794 B CN109136794 B CN 109136794B CN 201811016010 A CN201811016010 A CN 201811016010A CN 109136794 B CN109136794 B CN 109136794B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- GJNGXPDXRVXSEH-UHFFFAOYSA-N 4-chlorobenzonitrile Chemical compound ClC1=CC=C(C#N)C=C1 GJNGXPDXRVXSEH-UHFFFAOYSA-N 0.000 title claims abstract 7
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000001681 protective effect Effects 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims abstract description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 10
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract 1
- 238000005520 cutting process Methods 0.000 description 9
- 238000003754 machining Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses an integral PCBN blade and a preparation method thereof, wherein the preparation method comprises the following steps: 1) carrying out heat treatment on cobalt powder, nickel powder, silicon powder and palladium powder in the presence of protective gas, and then cooling and carrying out primary ball milling to obtain a ball-milled material; 2) performing secondary ball milling on the ball milled material, alumina, titanium nitride and silicon carbide to obtain a mixture; 3) mixing the mixture, potassium titanate whiskers and graphene to obtain a binder; 4) and mixing the CBN single crystal powder and the binder, and then pressing in the presence of protective gas to obtain the integral PCBN blade. The integral PCBN blade has excellent fracture toughness, and the preparation method has the advantages of simple process and easily obtained raw materials.
Description
Technical Field
The invention relates to a PCBN blade, in particular to an integral PCBN blade and a preparation method thereof.
Background
With the rapid development of manufacturing technology, cutting machining is used as a basic process of manufacturing technology, and enters a new development stage characterized by the development of efficient cutting, the development of new cutting processes and machining methods, and the provision of complete technologies. Meanwhile, the development of manufacturing techniques and difficult-to-machine materials has pushed the development of cutting tools, which are also developed in the direction of high-speed cutting, high-precision and dry machining. The application of the superhard cutter capable of realizing high-efficiency, high-stability and long-service-life machining is gradually popularized, and the superhard cutter plays an important role in the fields of automobiles, aerospace, energy sources, military, molds and the like.
In machining, the material of the tool is one of the key factors determining the machining efficiency, the machining quality and the machining cost, and the correct selection and application of the tool material are very important. Modern tool materials are mainly high-speed steel, cemented carbide and ceramics, their main hard phase components are carbides, nitrides and oxides, and after the addition of a binding material, the hardness of the tool is below HV 2000. For some modern difficult-to-machine materials, the hardness cannot meet the requirement, and then the superhard cutter material is produced. PCBN (polycrystalline cubic boron nitride) cutters, ceramic cutters, coating cutters and the like have high hardness, wear resistance and chemical stability, and can meet the requirements of green manufacturing such as high-speed cutting, dry cutting, hard cutting and the like. As the PCBN cutter has incomparable superiority in various aspects such as machining precision, cutting efficiency, cutter life and the like, the popularization and the application of the PCBN cutter can create huge economic benefits.
Although PCBN inserts have excellent hardness, wear resistance, thermal stability, thermal conductivity, young's modulus, thermal expansion, PCBN inserts have poor fracture toughness, less than half that of ceramic cutters, which has limited the development of PCBN inserts.
Disclosure of Invention
The invention aims to provide an integral PCBN blade and a preparation method thereof.
In order to achieve the above object, the present invention provides a method for manufacturing a monolithic PCBN blade, comprising:
1) carrying out heat treatment on cobalt powder, nickel powder, silicon powder and palladium powder in the presence of protective gas, and then cooling and carrying out primary ball milling to obtain a ball-milled material;
2) performing secondary ball milling on the ball milled material, alumina, titanium nitride and silicon carbide to obtain a mixture;
3) mixing the mixture, potassium titanate whiskers and graphene to obtain a binder;
4) and mixing the CBN single crystal powder and the binder, and then pressing in the presence of protective gas to obtain the integral PCBN blade.
The invention also provides the integral PCBN blade which is prepared by the preparation method.
In the technical scheme, firstly, cobalt powder, nickel powder, silicon powder and palladium powder are subjected to heat treatment and ball milling to obtain a ball-milled material; and then adding alumina, titanium nitride and silicon carbide, performing secondary ball milling to obtain a mixture, and finally adding potassium titanate whisker and graphene, and mixing to obtain the integral PCBN blade. The prepared integral PCBN blade has excellent toughness under the combined action of all components, and the popularization of the integral PCBN blade is facilitated.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The invention provides a preparation method of an integral PCBN blade, which comprises the following steps:
1) carrying out heat treatment on cobalt powder, nickel powder, silicon powder and palladium powder in the presence of protective gas, and then cooling and carrying out primary ball milling to obtain a ball-milled material;
2) performing secondary ball milling on the ball milled material, alumina, titanium nitride and silicon carbide to obtain a mixture;
3) mixing the mixture, potassium titanate whiskers and graphene to obtain a binder;
4) and mixing the CBN single crystal powder and the binder, and then pressing in the presence of protective gas to obtain the integral PCBN blade.
In step 1) of the present invention, the conditions of the heat treatment may be selected within a wide range, but in order to further improve the fracture toughness of the produced monolithic PCBN insert, it is preferable that in step 1), the heat treatment satisfies the following conditions: the treatment temperature is 850 ℃ and 950 ℃, and the treatment time is 2-4 h.
In step 1) of the present invention, the amount of each material may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN blade, it is preferable that the weight ratio of the cobalt powder, nickel powder, silicon powder, and palladium powder in step 1) is 5: 2-2.8: 0.2-0.6: 0.05-0.15.
In step 1) of the present invention, the conditions for the primary ball milling may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, it is preferable that in step 1), the primary ball milling satisfies the following conditions: the mass ratio of the big balls to the small balls is 2: 0.8-1.2, the mass ratio of the grinding balls to the materials is 10: 0.8-1.2, the rotating speed is 1200-1400rpm, and the ball milling time is 40-60 min.
In step 2) of the present invention, the amount of each material may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, it is preferable that the weight ratio of ball mill, alumina, titanium nitride, silicon carbide in step 2) is 10: 4-6: 0.5-1: 0.4-0.8.
In step 2) of the present invention, the conditions for the secondary ball milling may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, it is preferable that in step 2), the secondary ball milling satisfies the following conditions: the mass ratio of the big balls to the small balls is 2: 0.8-1.2, the mass ratio of the grinding balls to the materials is 10: 2-3, the rotating speed is 1700-1900rpm, and the ball milling time is 1.5-2 h.
In step 3) of the present invention, the amount of each material may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, it is preferable that in step 3), the weight ratio of the mixture, potassium titanate whiskers, graphene is 10: 0.8-1.2: 0.1-0.3.
In step 3) of the present invention, the specification of the potassium titanate whiskers may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, preferably, in step 3), the potassium titanate whiskers satisfy: the average diameter is 1-8um, and the average length is 30-200 um.
In step 4) of the present invention, the amount of each material may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, the weight ratio of the CBN single crystal powder to the binder in step 4) is 7: 2-2.5;
in step 4) of the present invention, the conditions for pressing may be selected within a wide range, but in order to further improve the fracture toughness of the resulting monolithic PCBN insert, it is preferred that in step 4) the conditions for pressing are: the temperature is 1800-1850 ℃, the pressure is 5.5-5.7GPa, and the pressing time is 3-5 min.
The invention also provides the integral PCBN blade which is prepared by the preparation method.
The present invention will be described in detail below by way of examples.
Example 1
1) Mixing cobalt powder, nickel powder, silicon powder and palladium powder according to the proportion of 5: 2.4: 0.4: performing heat treatment in the presence of protective gas (helium) at a weight ratio of 0.1 (the treatment temperature is 900 ℃, the treatment time is 3 h), cooling, and performing primary ball milling (the mass ratio of big balls to small balls is 2: 1, the mass ratio of grinding balls to materials is 10: 1, the rotating speed is 1300rpm, and the ball milling time is 50 min) to obtain a ball-milled material;
2) mixing the ball-milled material, aluminum oxide, titanium nitride and silicon carbide according to the weight ratio of 10: 5: 0.8: performing secondary ball milling at a weight ratio of 0.6 (the mass ratio of the big balls to the small balls is 2: 1, the mass ratio of the grinding balls to the materials is 10: 2.5, the rotating speed is 1800rpm, and the ball milling time is 1.8 h) to obtain a mixture;
3) mixing the mixture, potassium titanate whiskers (average diameter is 5um, average length is 100 um), and graphene is mixed according to the ratio of 10: 1: 0.2 by weight ratio to obtain the binder a 1.
Example 2
1) Mixing cobalt powder, nickel powder, silicon powder and palladium powder according to the proportion of 5: 2: 0.2: performing heat treatment in the presence of protective gas (helium) at a weight ratio of 0.05 (the treatment temperature is 850 ℃ and the treatment time is 4 hours), cooling, and performing primary ball milling (the mass ratio of large balls to small balls is 2: 0.8, the mass ratio of grinding balls to materials is 10: 0.8, the rotating speed is 1200rpm, and the ball milling time is 60 minutes) to obtain a ball-milled material;
2) mixing the ball-milled material, aluminum oxide, titanium nitride and silicon carbide according to the weight ratio of 10: 4: 0.5: performing secondary ball milling at a weight ratio of 0.4 (the mass ratio of the big balls to the small balls is 2: 0.8, the mass ratio of the grinding balls to the materials is 10: 2, the rotating speed is 1700rpm, and the ball milling time is 2 hours) to obtain a mixture;
3) mixing the mixture, potassium titanate whiskers (average diameter is 1um, average length is 200 um), and graphene is mixed according to the ratio of 10: 0.8: the binder A2 was obtained by mixing at a weight ratio of 0.1.
Example 3
1) Mixing cobalt powder, nickel powder, silicon powder and palladium powder according to the proportion of 5: 2.8: 0.6: performing heat treatment in the presence of protective gas (helium) at a weight ratio of 0.15 (the treatment temperature is 950 ℃, the treatment time is 2 hours), cooling, and performing primary ball milling (the mass ratio of large balls to small balls is 2: 1.2, the mass ratio of grinding balls to materials is 10: 1.2, the rotating speed is 1400rpm, and the ball milling time is 40 minutes) to obtain a ball-milled material;
2) mixing the ball-milled material, aluminum oxide, titanium nitride and silicon carbide according to the weight ratio of 10: 6: 1: performing secondary ball milling at a weight ratio of 0.8 (the mass ratio of the big balls to the small balls is 2: 1.2, the mass ratio of the grinding balls to the materials is 10: 3, the rotating speed is 1900rpm, and the ball milling time is 1.5 h) to obtain a mixture;
3) mixing the mixture, potassium titanate whiskers (with an average diameter of 8um and an average length of 30 um), graphene according to a ratio of 10: 1.2: 0.3 by weight ratio to obtain the binder a 3.
Comparative example 1
Binder B1 was prepared by the method of example 1, except that potassium titanate whiskers were not used.
Comparative example 2
Binder B2 was prepared according to the method of example 1, except that no graphene was used.
Application example 1
And (3) mixing CBN single crystal powder and a binder according to the weight ratio of 7: 2.3, followed by pressing in the presence of a shielding gas at 1800 c for 3min to obtain a monolithic PCBN insert, and then the fracture toughness of the monolithic PCBN insert was measured by the SENB method, and the results are shown in table 1.
TABLE 1
| Binder | A1 | A2 | A3 | B1 | B2 |
| Fracture toughness/Pa.m0.5 | 5.8 | 5.9 | 6.0 | 4.6 | 4.1 |
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (5)
1. A method of making a monolithic PCBN blade, comprising:
1) carrying out heat treatment on cobalt powder, nickel powder, silicon powder and palladium powder in the presence of protective gas, and then cooling and carrying out primary ball milling to obtain a ball-milled material;
2) performing secondary ball milling on the ball milled material, the alumina, the titanium nitride and the silicon carbide to obtain a mixture;
3) mixing the mixture, potassium titanate whiskers and graphene to obtain a binder;
4) mixing CBN single crystal powder and a binder, and then pressing in the presence of protective gas to obtain an integral PCBN blade;
wherein, in step 1), the heat treatment satisfies the following conditions: the treatment temperature is 850 ℃ and 950 ℃, and the treatment time is 2-4 h; in the step 1), the weight ratio of the cobalt powder, the nickel powder, the silicon powder and the palladium powder is 5: 2-2.8: 0.2-0.6: 0.05-0.15; in the step 2), the weight ratio of the ball mill matter, the alumina, the titanium nitride and the silicon carbide is 10: 4-6: 0.5-1: 0.4-0.8; in the step 3), the weight ratio of the mixture to the potassium titanate whisker to the graphene is 10: 0.8-1.2: 0.1-0.3; in the step 4), the weight ratio of the CBN single crystal powder to the binder is 7: 2-2.5; in step 4), the pressing conditions are as follows: the temperature is 1800-1850 ℃, the pressure is 5.5-5.7GPa, and the pressing time is 3-5 min.
2. The preparation method according to claim 1, wherein, in step 1), the primary ball milling satisfies the following condition: the mass ratio of the big balls to the small balls is 2: 0.8-1.2, the mass ratio of the grinding balls to the materials is 10: 0.8-1.2, the rotating speed is 1200-1400rpm, and the ball milling time is 40-60 min.
3. The preparation method according to claim 1, wherein, in the step 2), the secondary ball milling satisfies the following condition: the mass ratio of the big balls to the small balls is 2: 0.8-1.2, the mass ratio of the grinding balls to the materials is 10: 2-3, the rotating speed is 1700-1900rpm, and the ball milling time is 1.5-2 h.
4. The production method according to claim 1, wherein, in step 3), the potassium titanate whiskers satisfy: the average diameter is 1-8um, and the average length is 30-200 um.
5. A monolithic PCBN blade, produced by the production method of any one of claims 1 to 4.
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| CN201811016010.9A CN109136794B (en) | 2018-09-01 | 2018-09-01 | Integral PCBN blade and preparation method thereof |
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| CN201811016010.9A CN109136794B (en) | 2018-09-01 | 2018-09-01 | Integral PCBN blade and preparation method thereof |
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| CN102049538B (en) * | 2009-10-28 | 2012-08-08 | 河南富耐克超硬材料股份有限公司 | Cubic boron nitride blade and preparation method thereof |
| GB201002372D0 (en) * | 2010-02-12 | 2010-03-31 | Element Six Production Pty Ltd | A superhard multiphase material and method of using same |
| EP2890511A1 (en) * | 2012-08-31 | 2015-07-08 | Diamond Innovations, Inc. | Titanium diboride composition in pcbn |
| CN103274702A (en) * | 2013-06-14 | 2013-09-04 | 林金风 | Preparation method of cubic boron nitride (CBN) binding agent |
| CN105908041A (en) * | 2016-04-27 | 2016-08-31 | 富耐克超硬材料股份有限公司 | High-tenacity polycrystalline composite material, high-tenacity polycrystalline blade and preparation method of high-tenacity polycrystalline blade |
| CN106007730A (en) * | 2016-05-19 | 2016-10-12 | 富耐克超硬材料股份有限公司 | Method using coating cubic boron nitride to prepare polycrystalline cubic boron nitride |
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Effective date of registration: 20221230 Address after: 471000 No. 99, the north of Quanzhuang Village and the west of Jinqing Line, Geely District, Luoyang City, Henan Province Patentee after: Henan Lerui cutting tools Co.,Ltd. Address before: 241000 Business Incubation Park No. 415, Weiqi Road, Yijiang District, Wuhu City, Anhui Province Patentee before: WUHU QIANKAI MATERIAL TECHNOLOGY Co.,Ltd. |
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| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: 471000 No. 99, the north of Quanzhuang Village and the west of Jinqing Line, Geely District, Luoyang City, Henan Province Patentee after: Henan Lerui Chuangzhi Cutting Tools Co.,Ltd. Country or region after: China Address before: 471000 No. 99, the north of Quanzhuang Village and the west of Jinqing Line, Geely District, Luoyang City, Henan Province Patentee before: Henan Lerui cutting tools Co.,Ltd. Country or region before: China |