CN110219044B - Laser marking growth method of single crystal diamond - Google Patents
Laser marking growth method of single crystal diamond Download PDFInfo
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- CN110219044B CN110219044B CN201910434088.0A CN201910434088A CN110219044B CN 110219044 B CN110219044 B CN 110219044B CN 201910434088 A CN201910434088 A CN 201910434088A CN 110219044 B CN110219044 B CN 110219044B
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- 239000013078 crystal Substances 0.000 title claims abstract description 94
- 239000010432 diamond Substances 0.000 title claims abstract description 76
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010330 laser marking Methods 0.000 title claims abstract description 22
- 230000007547 defect Effects 0.000 claims abstract description 22
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000002372 labelling Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 238000001020 plasma etching Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 229910001751 gemstone Inorganic materials 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/362—Laser etching
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/04—Diamond
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a laser marking growth method of single crystal diamond, which comprises the following steps: (S1) providing a single crystal diamond seed; (S2) providing a laser marking device, marking the surface of the single crystal diamond seed crystal with the laser marking device to form a defect; (S3) removing impurities generated during the labeling process; (S4) placing the marked single crystal diamond seed crystal into a chemical vapor deposition growth furnace, introducing hydrogen and methane in a ratio of 100:2 to 100:5, controlling the pressure in the furnace to be 10-15 KPa, controlling the temperature of the single crystal diamond seed crystal in the furnace to be 700-800 ℃, and enabling the growth time to be longer than 10 hours, so that the defect formed by the mark is covered but not filled, thereby realizing the formation of the mark in the single crystal diamond. The method is simple to operate and high in processing speed, marking inside the diamond is achieved through an economic and effective scheme, and the marks can be observed through magnifying equipment such as a magnifying glass or naked eyes.
Description
Technical Field
The present invention relates to the growth and surface processing of single crystal diamonds, and more particularly to a laser marking growth method for single crystal diamonds.
Background
Diamond has excellent physicochemical properties and is widely used in the field of handicraft processing. In order to meet the customization requirements of users, characters, trademarks and other marks are usually added inside the diamond in the machining process.
However, natural diamonds cannot be marked internally, but only on the surface of the diamond, and may be worn away. If the diamond surface is re-grown after inscription, polycrystallinity may develop around the mark, resulting in the mark being directly filled or wrapped and not visible.
In addition, the existing method for adding marks inside the diamond also has some defects:
1. the operation of marking by using gas as an etching source to etch the surface of the diamond to form defects is too complex and consumes a long time;
2. the cost of marking by processing diamond with focused ion beams is high, the method is complex and takes long time, and the size of the mark is limited and generally cannot be directly observed by naked eyes in a nanometer or micron scale.
Disclosure of Invention
The invention aims to provide a laser marking growth method of a single crystal diamond, which solves the problems to a certain extent, has simple operation and high processing speed, realizes marking in the diamond by an economic and effective scheme, and can observe the marked mark by a magnifying glass or naked eyes.
In order to achieve the above object, the present invention provides a laser marking growth method of single crystal diamond, comprising the steps of:
(S1) providing a single crystal diamond seed;
(S2) providing a laser marking device, with which defects are marked on the surface of the single crystal diamond seed crystal;
(S3) removing impurities generated during the labeling process;
(S4) placing the marked single crystal diamond seed crystal into a chemical vapor deposition growth furnace, introducing hydrogen and methane in a ratio of 100:2 to 100:5, controlling the pressure in the furnace to be 10-15 KPa, controlling the temperature of the single crystal diamond seed crystal in the furnace to be 700-800 ℃, and enabling the growth time to be longer than 10 hours, so that the defect formed by the mark is covered but not filled, thereby realizing the formation of the mark in the single crystal diamond.
The method adopts laser marking equipment to process and mark on the surface of the diamond to form the defect, then carries out secondary epitaxial growth on the surface of the defect, and covers but does not fill the defect in the growth process, thereby achieving the effect of forming the mark in the single crystal diamond. The laser marking equipment is simple to operate, high in processing speed and convenient to process in batches.
According to a preferred embodiment of the present invention, the single crystal diamond laser marking growth method of the present invention further comprises the step (S5):
after the marked single crystal diamond seed crystal grows, the ratio of hydrogen to methane in the furnace is adjusted to be 100: 8-100: 13, the pressure in the furnace is adjusted to be 25 KPa-30 KPa, and the temperature of the single crystal diamond seed crystal in the furnace is adjusted to be 1100-1300 ℃, so that the growth of the single crystal diamond is accelerated, and the economic benefit is improved.
According to a preferred embodiment of the present invention, the step (S3) specifically includes the steps of:
(S31) heating and immersing the marked single crystal diamond seed crystal with aqua regia to remove possible residual metal elements;
(S32) ultrasonically cleaning the single crystal diamond seed after marking with acetone to remove inorganic substances possibly existing;
(S33) ultrasonically cleaning the marked single crystal diamond seed crystal with deionized water to remove acetone possibly remaining;
(S34) ultrasonically cleaning the marked single crystal diamond seed crystal with alcohol to remove inorganic substances possibly existing;
(S35) performing plasma etching cleaning on the marked single crystal diamond seed crystal to remove graphite phase products generated during marking.
Preferably, the heating soaking time in the step (S31) is 2 to 4 hours, and the washing time in each of the steps (S32) to (S35) is 60 minutes.
According to a preferred embodiment of the present invention, the defect formed in the step (S2) is visible to the naked eye after being magnified by 0 to 50 times.
Preferably, in the step (S1), the thickness of the single crystal diamond seed crystal is greater than 0.2 mm.
The above and other objects, features, and advantages of the present invention will be further apparent from the following detailed description and the accompanying drawings.
Drawings
Fig. 1 is a schematic flow diagram of a single crystal diamond laser marking growth method in accordance with a preferred embodiment of the present invention.
Detailed Description
The invention is further described with reference to the drawings and the detailed description, and it should be noted that any combination of the embodiments or technical features described below can be used to form a new embodiment without conflict.
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art. The basic principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
It will be understood by those skilled in the art that in the present disclosure, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced devices or components must be in a particular orientation, constructed and operated in a particular orientation, and thus the above terms are not to be construed as limiting the present invention.
It is understood that the terms "a" and "an" should be interpreted as meaning that a number of one element or element is one in one embodiment, while a number of other elements is one in another embodiment, and the terms "a" and "an" should not be interpreted as limiting the number.
Referring to fig. 1 of the drawings, a laser marking growth method of single crystal diamond according to a preferred embodiment of the present invention will be illustrated in the following description, which includes the steps of:
(S1) providing a single crystal diamond seed;
(S2) providing a laser marking device, with which defects are marked on the surface of the single crystal diamond seed crystal;
(S3) removing impurities generated during the labeling process;
(S4) placing the marked single crystal diamond seed crystal into a chemical vapor deposition growth furnace, introducing hydrogen and methane in a ratio of 100:2 to 100:5, controlling the pressure in the furnace at 10KPa to 15KPa, controlling the temperature of the single crystal diamond seed crystal in the furnace at 700 ℃ to 800 ℃, and growing for more than 10 hours.
Experiments show that the single crystal diamond has good transverse epitaxial growth under the conditions that the temperature is 700-800 ℃ and the air pressure is 10-15 KPa, a single crystal grain is large, the growth rate is slow and is less than 10 mu m/h, the defect formed by the mark cannot be filled, the polycrystalline diamond cannot be generated, so that the defect formed by the mark is covered but not filled, and the mark is formed in the single crystal diamond.
It will be readily appreciated that the marked single crystal diamond may be used in, but is not limited to, gemstones, diamond cutters, diamond wire dies, and the like.
The method adopts laser marking equipment to process and mark on the surface of the diamond to form the defect, then carries out secondary epitaxial growth on the surface of the defect, and covers but does not fill the defect in the growth process, thereby achieving the effect of forming the mark in the single crystal diamond.
Preferably, in the step (S1), a single crystal diamond seed having a surface free from cracks, polycrystals, and defects, and a thickness of more than 0.2mm is preferably selected for the subsequent process marking, thereby ensuring the quality of the product.
In the step (S2), the laser marking device may be a general device in the prior art, and the specific structure and operation principle are not described herein. The laser marking equipment is simple to operate, high in machining speed and convenient to machine in batches. Preferably, a laser marking device with adjustable power is selected, so that marking defects with different requirements can be conveniently realized by adjusting the power. It is easily understood that the defect pattern formed by the mark may be, but is not limited to, a font, a trademark, etc., without being limited to a shape and a size.
Preferably, the defect formed in the step (S2) is visible to the naked eye after being magnified by 0 to 50 times by a simple magnifying tool such as a magnifying glass.
Specifically, the step (S3) specifically includes the steps of:
(S31) heating and immersing the marked single crystal diamond seed crystal with aqua regia to remove possible residual metal elements;
(S32) ultrasonically cleaning the single crystal diamond seed after marking with acetone to remove inorganic substances possibly existing;
(S33) ultrasonically cleaning the marked single crystal diamond seed crystal with deionized water to remove acetone possibly remaining;
(S34) ultrasonically cleaning the marked single crystal diamond seed crystal with alcohol to remove inorganic substances possibly existing;
(S35) performing plasma etching cleaning on the marked single crystal diamond seed crystal to remove graphite phase products generated during marking.
Preferably, the heating soaking time in the step (S31) is 2 to 4 hours, and the washing time in each of the steps (S32) to (S35) is 60 minutes.
Further, on the basis of the above steps, the laser marking growth method of single crystal diamond of the present invention further includes a step (S5), the step (S5) being provided after the step (S4):
after the marked single crystal diamond seed crystal grows, the ratio of hydrogen to methane in the furnace is adjusted to be 100:8 to 100:13, the pressure in the furnace is adjusted to be 25KPa to 30KPa, the temperature of the single crystal diamond seed crystal in the furnace is adjusted to be 1100 ℃ to 1300 ℃, so that the growth of the single crystal diamond is accelerated, the growth rate can reach 50 mu m/h at the fastest speed, and the economic benefit is improved.
It will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are given by way of example only and are not limiting of the invention. The objects of the invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the examples, and any variations or modifications of the embodiments of the present invention may be made without departing from the principles.
Claims (1)
1. A single crystal diamond laser marking growth method is characterized by comprising the following steps:
(S1) providing a single crystal diamond seed; the thickness of the single crystal diamond seed crystal is more than 0.2 mm;
(S2) providing a laser marking device, with which defects are marked on the surface of the single crystal diamond seed crystal; the formed defects are magnified by 0-50 times and then can be seen by naked eyes;
(S3) removing impurities generated during the labeling process; the method specifically comprises the following steps:
(S31) heating and immersing the marked single crystal diamond seed crystal with aqua regia to remove possible residual metal elements; the heating and soaking time is 2-4 hours;
(S32) ultrasonically cleaning the single crystal diamond seed after marking with acetone to remove inorganic substances possibly existing; the cleaning time is 60 minutes;
(S33) ultrasonically cleaning the marked single crystal diamond seed crystal with deionized water to remove acetone possibly remaining; the cleaning time is 60 minutes;
(S34) ultrasonically cleaning the marked single crystal diamond seed crystal with alcohol to remove inorganic substances possibly existing; the cleaning time is 60 minutes;
(S35) performing plasma etching cleaning on the marked single crystal diamond seed crystal to remove graphite phase products generated during marking; the cleaning time is 60 minutes;
(S4) placing the marked single crystal diamond seed crystal into a chemical vapor deposition growth furnace, introducing hydrogen and methane in a ratio of 100:2 to 100:5, controlling the pressure in the furnace at 10KPa to 15KPa, controlling the temperature of the single crystal diamond seed crystal in the furnace at 700 ℃ to 800 ℃, and controlling the growth time to be more than 10 hours;
(S5) after the marked single crystal diamond seed crystal grows, adjusting the ratio of hydrogen to methane in the furnace to be 100: 8-100: 13, adjusting the pressure in the furnace to be 25 KPa-30 KPa, and adjusting the temperature of the single crystal diamond seed crystal in the furnace to be 1100-1300 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910434088.0A CN110219044B (en) | 2019-05-23 | 2019-05-23 | Laser marking growth method of single crystal diamond |
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|---|---|---|---|
| CN201910434088.0A CN110219044B (en) | 2019-05-23 | 2019-05-23 | Laser marking growth method of single crystal diamond |
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| CN110219044A CN110219044A (en) | 2019-09-10 |
| CN110219044B true CN110219044B (en) | 2021-07-06 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108103571A (en) * | 2018-01-11 | 2018-06-01 | 宁波晶钻工业科技有限公司 | A kind of single-crystal diamond preparation facilities and method |
| CN108373345A (en) * | 2018-01-16 | 2018-08-07 | 华北水利水电大学 | Preprocess method before a kind of coating of laser marking blade |
| CN108582502A (en) * | 2018-05-07 | 2018-09-28 | 江苏锋泰工具有限公司 | Diamond saw blade and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170261855A1 (en) * | 2016-03-10 | 2017-09-14 | Uab Research Foundation | Methods for preparing encapsulated markings on diamonds |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108103571A (en) * | 2018-01-11 | 2018-06-01 | 宁波晶钻工业科技有限公司 | A kind of single-crystal diamond preparation facilities and method |
| CN108373345A (en) * | 2018-01-16 | 2018-08-07 | 华北水利水电大学 | Preprocess method before a kind of coating of laser marking blade |
| CN108582502A (en) * | 2018-05-07 | 2018-09-28 | 江苏锋泰工具有限公司 | Diamond saw blade and preparation method thereof |
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Address after: 315200 No. 777, Zhong Guan Xi Road, Zhuang City Street, Zhenhai District, Ningbo, Zhejiang. Patentee after: Ningbo Crystal Diamond Technology Co.,Ltd. Address before: 315200 No. 777, Zhong Guan Xi Road, Zhuang City Street, Zhenhai District, Ningbo, Zhejiang. Patentee before: Ningbo Jingduan Industrial Technology Co.,Ltd. |
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Address after: No. 998 Zhongguan Road, Jiaochuan Street, Zhenhai District, Ningbo City, Zhejiang Province, 315200 Patentee after: Ningbo Crystal Diamond Technology Co.,Ltd. Country or region after: China Address before: 315200 No. 777, Zhong Guan Xi Road, Zhuang City Street, Zhenhai District, Ningbo, Zhejiang. Patentee before: Ningbo Crystal Diamond Technology Co.,Ltd. Country or region before: China |