CN102409291B - Method and device for preparing diamond film doped with ultrafine nano-structural metal particles - Google Patents
Method and device for preparing diamond film doped with ultrafine nano-structural metal particles Download PDFInfo
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- CN102409291B CN102409291B CN201110367263.2A CN201110367263A CN102409291B CN 102409291 B CN102409291 B CN 102409291B CN 201110367263 A CN201110367263 A CN 201110367263A CN 102409291 B CN102409291 B CN 102409291B
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- 239000010432 diamond Substances 0.000 title claims abstract description 77
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 77
- 239000002923 metal particle Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 36
- 239000010439 graphite Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 claims abstract description 35
- 239000002184 metal Substances 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 14
- 239000012528 membrane Substances 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 11
- 230000008021 deposition Effects 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 230000006835 compression Effects 0.000 abstract description 6
- 238000007906 compression Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 239000013077 target material Substances 0.000 abstract description 6
- 230000007704 transition Effects 0.000 abstract description 3
- 210000002381 plasma Anatomy 0.000 abstract 2
- 238000005299 abrasion Methods 0.000 abstract 1
- 230000001939 inductive effect Effects 0.000 abstract 1
- 239000010408 film Substances 0.000 description 18
- 239000000956 alloy Substances 0.000 description 12
- 229910045601 alloy Inorganic materials 0.000 description 12
- 239000004606 Fillers/Extenders Substances 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 238000009434 installation Methods 0.000 description 6
- 238000005229 chemical vapour deposition Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- -1 heating unit Substances 0.000 description 1
- 244000239634 longleaf box Species 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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Abstract
The invention relates to a method and a device for preparing a diamond film doped with ultrafine nano-structural metal particles. The device for preparing the diamond film doped with the metal particles comprises a control system, a target material system, a workpiece control system and an auxiliary system. The method comprises the following steps of: focusing strong laser emitted by a high-power pulse laser device on the surface of a high-purity graphite target material under vacuum; inducing a large quantity of plasmas by using high-energy laser to bombard the surface of a base material which is uniformly heated in advance at a high speed; and performing rapid phase transition on the surface of the base material to form the diamond film. Laser emitted by a quasimolecule laser device is focused on a metal target material, a large quantity of plasmas consisting of a large quantity of metal particles are induced on the surface of the metal target material by using high-energy-density laser to bombard the surface of the prepared diamond film, and gaps on the surfaces of the particles of the diamond film are effectively and tightly filled by a large number of metal particles to form a uniform metal film. By the method and the device, the surface of the diamond film is modified, and the compression strength and the abrasion resistance of the diamond film are improved.
Description
Technical field
The present invention relates to manually manufacture diamond thin field, refer in particular to a kind of thin diamond membrane preparation method and device of the superfine nano structural metal particle that adulterates, be particularly useful for preparing large-area diamond thin.
Background technology
Diamond thin has many-sided premium properties, the wear resistance of becoming reconciled as high hardness, fabulous chemical stability and high thermal conductivity, and the performance such as high temperature resistant and radioprotective and enjoy people's concern, diamond thin has important effect in much industry and new technical field because of its numerous excellent properties.Now the existing several different methods of people is prepared diamond thin, and Preliminary Applications at aspects such as mechanical, electrical, light, sound.
Nineteen fifty-five, the people such as the Bundy of GE as carbon source, synthesize first artificial diamond with graphite under the high temperature of 1500K and the condition of high voltage of 8GPa as catalyzer with transition metal such as Fe, Ni, Co, and this method also claims high pressure menstruum method.1961, people were not in the situation that adopting catalyzer, by directly graphite being changed into diamond under the ultra-high voltage of 30GPa and the hot conditions of 1500K.Since 1974, the people such as Setaka, Matsumoto of Japan adopt the methods such as hot filament, microwave and direct-current discharge to excite the carbonaceous gass such as CH4, on the base material of diamond seed and non-diamond, carry out the research of diamond film, prepare after diamond thin, people have developed multiple low pressure gas phase deposition method, all successfully prepare diamond thin.Growth by lower pressure phase diamond technology can be divided into three types below: the firstth, and chemical vapor deposition (CVD); Equations of The Second Kind is physical vapor deposition (PVD); The 3rd class is chemical vapor transportation deposition (CVT).According to the difference of mode of excitation, CVD technology is mainly divided into the preparation methods such as hot-wire chemical gas-phase deposition, plasma activated chemical vapour deposition, combustion flame chemical vapour deposition.The equipment that utilizes in addition plasma to prepare film also becomes a kind of having great application prospect, as DC plasma jet makes progress preparing aspect diamond thin.
The above-mentioned various methods of preparing diamond thin, exist equipment huge, control complicated, the problem that the diamond thin thinner thickness of preparation and film and base material bonding strength are lower, because of these drawbacks limit prepare the industrialized popularization of diamond thin.Simultaneously along with the widespread use of diamond cutter in industries such as modern mechanical processing, building decorations, people, to having proposed more and more higher requirement in the ultimate compression strength of cutter, end-use performance and work-ing life, therefore seem very important to the surface modification of large-area diamond film.
Summary of the invention
The object of the invention is the deficiency for above technology, a kind of thin diamond membrane preparation method of the superfine nano structural metal particle that adulterates is provided.The light laser that the method adoption of innovation high power pulsed laser device sends focuses on graphite target induces a large amount of plasma bodys to bombard at a high speed the substrate surface of homogeneous heating in advance, at substrate surface, form diamond thin, simultaneously by excimer laser to diamond thin doping metals particle, realize the surface modification of diamond thin, strengthened ultimate compression strength and the wear resistance of diamond thin.The reaction yield that the method is prepared diamond thin is high, and thin film layer purity is high, can realize automatization, safe and reliable, especially can prepare large-area diamond thin and can also realize diamond film surface modification simultaneously.
The thin diamond film preparation concrete grammar of doping superfine nano structural metal particle is: the light laser that high power pulsed laser device sends sees through high pressure resistant glass window B through collimator and extender mirror and focuses on the high purity graphite target material surface under vacuum condition, graphite target is with certain speed rotation, high-octane induced with laser goes out a large amount of plasma bodys and bombards at a high speed the substrate surface of homogeneous heating in advance, at substrate surface, forms fast diamond thin.Traverser makes base material and target in different relative positions, thereby realizes the large-area diamond thin of preparation.The laser line focus lens A that excimer laser sends sees through high pressure resistant glass window A and focuses in the metal targets with certain speed autobiography, the plasma body that the metallics by a large amount of that the laser of high-energy-density goes out at metal targets spatial induction forms bombards at a high speed the diamond film surface of having prepared, a large amount of metallicss is closely filled up the gap of diamond thin particle surface effectively, formed the uniform metallic membrane of one deck, thereby realized the modification of diamond film surface, improved the performance such as ultimate compression strength, wear resistance of diamond thin.Carbon atom generation chemical reaction generation metallic carbide of a large amount of charged particle and diamond film surface in plasma body simultaneously, formed in conjunction with transition layer firmly, improve the bonding strength between metallic membrane and diamond thin, extended the work-ing life of metallic film.
The inventive system comprises Controlling System, target system, workpiece Controlling System and subsystem.
Described Controlling System comprises: computer, digitial controller and laser controller.Digitial controller upper end is connected with computer, and lower end is connected with laser controller, and laser controller is connected with excimer laser with high power pulsed laser device respectively.Computer control motor A and motor B control respectively laser controller and worktable by digitial controller simultaneously.Laser controller is controlled high power pulsed laser device and excimer laser.
Described target system comprises: rotating base stationary installation, rotating base A, motor A, metal targets support, metal targets, rotating base B, motor B, graphite target support and graphite target.Rotating base stationary installation is fixed on the top, top of airtight working chamber.Metal targets support is used for fixing metal target, and is connected with the rotation axis of motor A, and motor A rotates and drives metal targets rotation, and it is upper that motor A is fixed on rotating base A, and rotating base A is arranged on the lower left side of rotating base stationary installation.Graphite target support is used for fixedly graphite target, and is connected with the rotation axis of motor B, and motor B rotates and drives graphite target rotation, and it is upper that motor B is fixed on rotating base B, and rotating base B is arranged on the lower right side of rotating base stationary installation.Rotating base A becomes symmetrical distribution in rotating base stationary installation with rotating base B.By rotation rotating base A and rotating base B, regulate respectively the angle in metal targets and graphite target and substrate surface horizontal direction.
Described workpiece Controlling System comprises: computer, digitial controller, base material, heating unit, base material fixing device and worktable.Base material is clamped on heating unit and is fixed in base material fixing device together with heating unit.Computer controlled refrigerating/heating apparatus, digitial controller by control worktable regulate base material and and target between relative position.
Described subsystem comprises: collimator and extender mirror, vacuum pump, temperature sensor, temperature indicator, pressure transmitter and pressure display unit.Collimator and extender mirror is on the right of high pressure resistant glass window B, and described collimator and extender mirror comprises condenser lens B and concavees lens.Vacuum pump is positioned at the bottom righthand side of airtight working chamber.Temperature sensor is placed in base material left side and is connected with the temperature indicator outside airtight working chamber, and temperature sensor and temperature indicator are respectively used to measure and observe the working temperature of base material.Pressure transmitter is positioned at the right lower quadrant of airtight working chamber and is connected with the pressure display unit outside airtight working chamber, and pressure transmitter and pressure display unit are respectively used to measure and observe the pressure in airtight working chamber.
Feature of the present invention must realize under specific processing condition, and its processing condition are that base material upper surface is 2mm～3mm to metal targets and graphite target vertical range bottom; Described base material is silicon-base alloy, and described metal targets is titanium or the nickel of content 99.9%, and described graphite target is the graphite of content 99.99%; The rotating speed of motor A and motor B is respectively 6r/min and 10r/min; Angle in metal targets and graphite target and substrate surface horizontal direction is respectively 133 °～137 ° and 43 °～47 °; The working temperature of base material is 200 ℃～250 ℃; Pressure in airtight working chamber is 1 * 10
-3pa ~ 5 * 10
-3pa; The pulsewidth of high power pulsed laser device is 20ns, pulse-repetition frequency 50Hz, and power density is 10
9w/cm
2; The pulsewidth of excimer laser is 25ns, and pulse-repetition is 10Hz, and energy density is 3.0J/cm
2.
The innovation of the technology of the present invention, be to have overcome prior art equipment huge, control complicated, the shortcomings such as the diamond thin thinner thickness of preparation and thickness distribution are inhomogeneous, prepared the uniform diamond thin of large-area thickness distribution, realize the modification of diamond film surface simultaneously, obtained the diamond thin of doping superfine nano structural metal particle.The light laser that high power pulsed laser device sends focuses on high purity graphite target material surface and induces a large amount of plasma body high speed bombarding base material surfaces, in substrate surface fast deposition, forms diamond thin.By heating unit, base material is carried out to homogeneous heating, being uniformly distributed of substrate surface temperature created favourable condition to depositing large-area, high-quality diamond thin, makes diamond thin thickness distribution even, improved the conjugation of diamond thin and base material.The plasma body that the metallics by a large amount of that the laser that excimer laser sends goes out at metal targets spatial induction forms bombards at a high speed the diamond film surface of having prepared, not only effectively closely fill up the gap of diamond thin particle surface, and in plasma body, the carbon atom generation chemical reaction of a large amount of charged particle and diamond film surface generates metallic carbide, formed in conjunction with transition layer firmly, improved the bonding strength between metallic membrane and diamond thin, extended the work-ing life of diamond thin, ultimate compression strength and wear resistance have been improved, this has very important meaning to the application of diamond thin as diamond cutter etc.
The concrete implementation step of the inventive method:
A. use dehydrated alcohol and washed with de-ionized water substrate surface, to remove surperficial pollutent;
B. pretreated base material is clamped on heating unit, metal targets and graphite target are separately fixed on metal targets support and graphite target support;
C. rotate rotating base A and rotating base B and regulate respectively the angle in metal targets and graphite target and substrate surface horizontal direction;
D. in substrate side, stick temperature sensor, traverser regulates substrate surface to graphite target vertical range bottom.Vacuum pump is taken out the gas in airtight working chamber, and computer controlled refrigerating/heating apparatus is to carrying out base material homogeneous heating;
E. open motor B-source and high power pulsed laser device, the parameters such as laser energy, pulse width are set by laser controller.High power pulsed laser device sends on the graphite target that light laser focuses on rotation, and induces a large amount of plasma body high speed bombarding base material surfaces, at substrate surface formation of deposits diamond thin.
F. close motor B and high power pulsed laser device, adjusting operating platform is to suitable position.Open motor A and excimer laser, the parameter of excimer laser is set.Excimer laser sends laser focusing on metal targets, and the plasma body that the metallics by a large amount of that laser goes out at metal targets spatial induction forms bombards at a high speed the diamond film surface of having prepared, and has formed the uniform metallic membrane of one deck.After question response completes, close all power supplys, take off base material.
The bright advantage of this law is as follows:
1. the diamond film layer purity that prepared by the inventive method is high and thin diamond film thickness is thick, and film and base material bonding strength are high;
2. the inventive method can be prepared large-area diamond thin, and diamond thin thickness distribution is even;
3. compare with additive method, doped diamond thin films ultimate compression strength prepared by the inventive method is high, wear resistance good;
4. to prepare the reaction yield of diamond thin high, pollution-free for the inventive method;
5. the method can realize automatization, controls simple, safe and reliable.
Accompanying drawing explanation
Fig. 1: the schematic diagram of device of the thin diamond membrane preparation method of doping superfine nano structural metal particle.
Attached number in the figure: 1. pressure transmitter; 2. pressure display unit; 3. temperature indicator; 4. excimer laser; 5. condensing lens A; 6. high pressure resistant glass window A; 7. rotating base A; 8. motor A; 9. metal targets support; 10. metal targets; 11. base materials; 12. temperature sensors; 13. base material fixing device; 14. worktable; 15. rotating base stationary installations; 16. rotating base B; 17. motor B; 18. graphite target supports; 19. graphite targets; 20. plasma bodys; 21. airtight working chambers; 22. high pressure resistant glass window B; 23. laser beams; 24. diamond thins; 25. heating units; 26. computers; 27. collimator and extender mirrors; 28. condenser lens B; 29. concavees lens; 30. high power pulsed laser devices; 31. vacuum pumps; 32. digitial controllers; 33. laser controllers.
Embodiment
Below in conjunction with accompanying drawing use-case, describe the working condition of the method and apparatus that the present invention proposes in detail, but be not used for limiting the present invention.
Example 1
Surface with dehydrated alcohol and washed with de-ionized water silicon-base alloy, silicon-base alloy after cleaning is clamped on heating unit 25, then metal targets 10 and graphite target 19 are separately fixed on metal targets support 9 and graphite target support 18, regulating rotating base A 7 and rotating base B16 to make metal targets 10 and graphite target 19 is 135 ° and 45 ° with the angle in silicon-base alloy surface level direction, in the side of silicon-base alloy, stick after temperature sensor 12, the position of adjusting operating platform 14, making silicon-base alloy upper surface is 2.5mm to graphite target 19 vertical range bottom.With vacuum pump 31, take out the gas in airtight working chamber 21, observe pressure display unit 2, make interior pressure reach 3 * 10
-3pa, computer 26 is controlled 25 pairs of silicon-base alloy heating of heating unit, observe temperature indicator 3, making silicon-base alloy temperature is 200 ℃, after silicon-base alloy temperature-stable, open motor B17 power supply and high power pulsed laser device 30, regulate the parameter of high power pulsed laser device 30, pulsewidth is 20 ns, pulse-repetition frequency 50Hz, power density is 10
9w/cm
2.High power pulsed laser device 30 sends light laser and focuses on the graphite target 19 that rotational velocity is 10r/min through high pressure resistant glass window B22 through collimator and extender mirror 27, and induce a large amount of plasma body 20 to bombard at a high speed silicon-base alloy surface, at silicon-base alloy surface deposition, form diamond thin 24.Close motor B17 and high power pulsed laser device 30, adjusting operating platform 14 is to suitable position.Open motor A8 and excimer laser 4, by laser controller 33 parameters, pulsewidth is 25ns, and pulse-repetition is 10Hz, and energy density is 3.0J/cm
2.Excimer laser 4 sends laser line focus lens A5 and focuses in the metal targets 10 that rotational velocity is 6r/min, the plasma body that the metallics by a large amount of that laser goes out at metal targets 10 spatial inductions forms bombards at a high speed diamond thin 24 surfaces of having prepared, and has formed layer of metal film.After question response completes, close all power supplys, take off silicon-base alloy.
Claims (2)
1. the adulterate thin diamond membrane preparation method of superfine nano structural metal particle, is characterized in that, step is:
A. use dehydrated alcohol and washed with de-ionized water base material (11) surface;
B. pretreated base material (11) is clamped in to heating unit (25) upper, metal targets (10) and graphite target (19) are separately fixed on metal targets support (9) and graphite target support (18);
C. rotate rotating base A(7) and rotating base B(16) angle in metal targets (10) and graphite target (19) and base material (11) surface level direction regulated respectively; Angle in metal targets and graphite target and substrate surface horizontal direction is respectively 133 °～137 ° and 43 °～47 °;
D. in base material (11) side, stick temperature sensor, traverser (14) regulates base material (11) upper surface to graphite target (19) vertical range bottom, and base material upper surface is 2mm～3mm to graphite target vertical range bottom; Vacuum pump (31) is taken out the gas in airtight working chamber (21), and computer (26) is controlled heating unit (25) base material (11) is carried out to homogeneous heating; The working temperature of base material is 200 ℃～250 ℃; Pressure in airtight working chamber is 1 * 10
-3pa ~ 5 * 10
-3pa;
E. open motor B(17) power supply and high power pulsed laser device (30), by laser controller (33), laser energy, pulse width parameter are set, high power pulsed laser device (30) sends on the graphite target (19) that light laser (23) focuses on rotation, and induce a large amount of plasma body (20) high speed bombarding base material (11) surface, at base material (11) surface deposition, form diamond thin (24); The pulse width of implementing high power pulsed laser device is 20ns, pulse-repetition 50Hz, and power density is 10
9w/cm
2;
F. close motor B(17) and high power pulsed laser device (30), adjusting operating platform (14) is to suitable position; Open motor A(8) and excimer laser (4), the parameter of excimer laser (4) is set, the pulse width of excimer laser is 25ns, and pulse-repetition is 10Hz, and energy density is 3.0J/cm
2; Excimer laser (4) sends laser focusing on metal targets (10), the plasma body that the metallics by a large amount of that laser goes out at metal targets (10) spatial induction forms bombards at a high speed diamond thin (24) surface of having prepared, formed the uniform metallic membrane of one deck, after question response completes, close all power supplys, take off base material.
2. the thin diamond membrane preparation method of a kind of superfine nano structural metal particle that adulterates according to claim 1, is characterized in that, the rotating speed of motor A and motor B is respectively 6r/min and 10r/min.
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|---|---|---|---|
| CN201110367263.2A CN102409291B (en) | 2011-11-18 | 2011-11-18 | Method and device for preparing diamond film doped with ultrafine nano-structural metal particles |
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| CN102409291B true CN102409291B (en) | 2014-04-09 |
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| CN103408005B (en) * | 2013-07-29 | 2015-07-08 | 江苏大学 | Device and method for improving preparation efficiency of diamonds |
| CN104593732A (en) * | 2015-01-29 | 2015-05-06 | 张晓军 | System and method of multi-element pulsed laser deposition for synthesizing composite material in batches |
| CN110578131B (en) * | 2019-10-18 | 2021-05-18 | 永固集团股份有限公司 | Laser chemical vapor deposition ceramic layer production line and production process for spherical part of lightning protection device |
| CN113445007A (en) * | 2021-05-28 | 2021-09-28 | 松山湖材料实验室 | Pulsed laser deposition apparatus and method |
| CN114083139B (en) * | 2021-12-31 | 2023-05-05 | 华侨大学 | Processing device and processing method for laser-induced active ion etching diamond |
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| JP3760175B2 (en) * | 1998-03-04 | 2006-03-29 | 株式会社神戸製鋼所 | Diamond film formation method |
| JP2011099137A (en) * | 2009-11-05 | 2011-05-19 | Fuji Electric Holdings Co Ltd | Method for depositing diamond film |
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| Title |
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| "用激光沉积法在金刚石颗粒表面制备金属薄膜";罗飞;《中国优秀博硕士学位论文全文数据库》;20050715(第3期);第30-32页 * |
| JP特开2011-99137A 2011.05.19 |
| 罗飞."用激光沉积法在金刚石颗粒表面制备金属薄膜".《中国优秀博硕士学位论文全文数据库》.2005,(第3期),第30-32页. |
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Effective date of registration: 20200623 Address after: No. 159, Chengjiang Middle Road, Jiangyin City, Wuxi City, Jiangsu Province Patentee after: Jiangyin Intellectual Property Operation Co.,Ltd. Address before: No. 101, Nanxu Avenue, Zhenjiang City, Jiangsu Province Patentee before: JIANGSU HUIZHI INTELLECTUAL PROPERTY SERVICES Co.,Ltd. |
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Addressee: Xu Yingying Document name: Notice of amendment |
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Effective date of registration: 20230329 Address after: 035400 Yangfang Township Zhuangli Industrial Park, Dingxiang County, Xinzhou City, Shanxi Province Patentee after: Shanxi yademas Material Technology Co.,Ltd. Address before: No. 159, Chengjiang Middle Road, Jiangyin City, Wuxi City, Jiangsu Province Patentee before: Jiangyin Intellectual Property Operation Co.,Ltd. |
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