CN111659318A - Assembly block for high-temperature and high-pressure modification of diamond cultivated by CVD and modification method - Google Patents
Assembly block for high-temperature and high-pressure modification of diamond cultivated by CVD and modification method Download PDFInfo
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- CN111659318A CN111659318A CN202010541379.2A CN202010541379A CN111659318A CN 111659318 A CN111659318 A CN 111659318A CN 202010541379 A CN202010541379 A CN 202010541379A CN 111659318 A CN111659318 A CN 111659318A
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- heating
- cvd
- diamond
- heat preservation
- temperature
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- 239000010432 diamond Substances 0.000 title claims abstract description 51
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 46
- 238000012986 modification Methods 0.000 title claims abstract description 24
- 230000004048 modification Effects 0.000 title claims abstract description 24
- 238000002715 modification method Methods 0.000 title claims abstract description 8
- 238000005229 chemical vapour deposition Methods 0.000 title description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 76
- 238000004321 preservation Methods 0.000 claims abstract description 48
- 229910052903 pyrophyllite Inorganic materials 0.000 claims abstract description 18
- 238000009434 installation Methods 0.000 claims abstract description 15
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims description 25
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 18
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 18
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 239000010459 dolomite Substances 0.000 claims description 9
- 229910000514 dolomite Inorganic materials 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011733 molybdenum Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910001209 Low-carbon steel Inorganic materials 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims 3
- 238000009413 insulation Methods 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 208000037998 chronic venous disease Diseases 0.000 description 14
- 239000013078 crystal Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000004575 stone Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 108700028490 CAP protocol 2 Proteins 0.000 description 1
- 238000005267 amalgamation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/06—Processes using ultra-high pressure, e.g. for the formation of diamonds; Apparatus therefor, e.g. moulds or dies
- B01J3/065—Presses for the formation of diamonds or boronitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses an assembly block for high-temperature and high-pressure modification of diamond cultivated by CVD and a modification method, and mainly relates to the technical field of synthesis of superhard materials. Including being located outer pyrophyllite piece, be equipped with the installation cavity that runs through it in the pyrophyllite piece, the both ends of installation cavity all set up the electrically conductive cap that corresponds rather than the cross-section, be equipped with the heating plate rather than contacting on the medial surface of electrically conductive cap, two be equipped with the heating pipe between the heating plate, the axial vertical heating plate of heating pipe, just the both ends ring terminal surface of heating pipe contacts with the heating plate of homonymy respectively, first heat preservation pipe has been cup jointed to the outside of heating pipe, be equipped with two heat preservation posts in the heating pipe, two be used for placing the diamond between the heat preservation post. The invention has the beneficial effects that: can conduct ultrahigh pressure and generate heat to modify the CVD cultivated diamond, improve the crystallization quality of the diamond and improve the color and the purity grade of the diamond.
Description
Technical Field
The invention relates to the technical field of superhard material synthesis, in particular to an assembly block for high-temperature and high-pressure modification of diamond cultivated by CVD and a modification method.
Background
The laboratory cultured diamond is a diamond which is generated and manufactured by simulating the crystallization characteristics of natural diamond by an artificial method, and is a diamond which is real in every aspect: chemical, physical, atomic and light, all properties being the same as natural diamond. CVD method is the main method for producing large-grain cultivated diamond, in the metastable zone of diamond, adopting the condition of low temperature and high pressure, about 900 ℃, in the vacuum reaction chamber, using microwave to heat the gas-methane (CH4) containing C and hydrogen, generating plasma, decomposing C from the state of gas compound into single free atomic state, through diffusion and convection, finally the diamond structure is deposited on the substrate or seed crystal and continuously grows up. Although the method is easy to grow the carat-grade gem-grade diamond, the grown diamond has poor color and transparency.
CVD diamond is easy to have more crystal defects such as vacancies, non-diamond crystal structure defects and the like due to the limitation of the growth method, and the grown diamond is difficult to reach D, E, F-grade color and VVS and above cleanliness standard, so that the problems need to be improved through subsequent modification treatment.
Disclosure of Invention
The invention aims to provide an assembly block for high-temperature and high-pressure modification of CVD cultured diamonds and a modification method, which can conduct ultrahigh pressure and generate heat to modify the CVD cultured diamonds, improve the crystallization quality of the diamonds and improve the color and the purity grade of the diamonds.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the utility model provides a CVD cultivates modified equipment piece of using of diamond high temperature high pressure, is including being located outer pyrophyllite piece, be equipped with the installation cavity that runs through it in the pyrophyllite piece, the both ends of installation cavity all set up the electrically conductive cap that corresponds rather than the cross-section, be equipped with the heating plate rather than contacting on the medial surface of electrically conductive cap, two be equipped with the heating pipe between the heating plate, the axial vertical heating plate of heating pipe, just the both ends ring terminal surface of heating pipe contacts with the heating plate of homonymy respectively, first heat preservation pipe has been cup jointed to the outside of heating pipe, be equipped with two heat preservation posts, two in the heating pipe be used for placing the diamond between the heat preservation post.
The installation cavity is internally embedded with a second heat preservation pipe, and the heating plate is arranged in the second heat preservation pipe.
The installation cavity is circular, electrically conductive cap, heating plate, first heat preservation pipe, heating pipe and heating post are the circular member, just the external diameter of electrically conductive cap, heating plate and first heat preservation pipe suits with the internal diameter of installation cavity.
The first heat preservation pipe and the heating pipe are the same in length, and the height of the heat preservation column is half of the height of the heating pipe.
The conductive cap comprises a metal bowl and a filling core, wherein the metal bowl is made of high-temperature-resistant metal materials, the filling core is made of high-temperature-resistant ceramic materials, and the filling core is arranged on the inner side end face of the conductive cap.
The metal bowl is made of any one of low-carbon steel, molybdenum and titanium;
and/or
The filling core is made of any one of dolomite, zirconia ceramics, magnesia ceramics and alumina ceramics.
The heating sheet and/or the heating pipe are/is made of any one of artificial carbon, graphite plates and molybdenum.
The first heat-preservation pipe is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics;
and/or
The second heat preservation pipe is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics;
and/or
The heat preservation column is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics.
The pyrophyllite piece includes the stone monomer of two symmetries that set up from top to bottom, and two stone monomers amalgamation constitute the pyrophyllite piece from top to bottom, electrically conductive cap combination is in the free outer end opening of stone.
In another aspect of the invention, a high-temperature high-pressure modification method for CVD cultured diamond uses the assembly block, the CVD cultured diamond is placed between two heat preservation columns, six faces of the assembly block are pressed by a top hammer of a high-temperature high-pressure synthesis press during modification, pressure required by modification is generated, and temperature required by modification is generated by electrifying a heating piece and a heating pipe.
Compared with the prior art, the invention has the beneficial effects that:
the invention can modify CVD diamond, and the assembled block can be put into a high-temperature high-pressure synthesis press, and can realize ultrahigh pressure of 8GPa and high temperature of more than 2000 ℃, thereby realizing modification treatment of CVD diamond and obviously improving the color and transparency of the diamond. Repairing vacancy, non-diamond crystal and other structural defects to reach D, E, F level color and VVS and above purity standard.
Drawings
FIG. 1 is a schematic exploded view of the assembly of the present invention.
FIG. 2 is a schematic diagram of the present invention in combination.
Fig. 3 is a schematic view of the internal structure of the present invention.
FIG. 4 is a pictorial representation of the present invention.
Figure 5 is a drawing of an assembly of the invention.
FIG. 6 shows CVD grown diamonds prior to modification using the present invention.
FIG. 7 is a CVD grown diamond of the present invention modified using the techniques of the present invention.
Reference numerals shown in the drawings:
1. pyrophyllite blocks; 2. a conductive cap; 3. a heating plate; 4. heating a tube; 5. a first heat-insulating tube; 6. a second insulating tube; 7. a heat-insulating column; 8. a mounting cavity; 9. filling a core; 10. a metal bowl.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.
The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.
Example 1: CVD cultivates modified equipment piece of using of diamond high temperature high pressure
Comprises a pyrophyllite block 1, a conductive cap 2, a heating sheet 3, a heating pipe 4, a first heat preservation pipe 5, a second heat preservation pipe 6 and a heat preservation column 7.
The pyrophyllite block 1 is located on the outermost periphery, can transmit pressure on a top hammer of a high-temperature and high-pressure synthetic press to the inside of an assembly block for transmitting pressure and sealing media, has a certain sealing effect, can seal the pressure inside the assembly block, and ensures the safety of high-temperature and high-pressure modification. The pyrophyllite block 1 is centered and is provided with a cylindrical mounting cavity 8 which is communicated up and down. The other components comprise a conductive cap 2 multiplied by 2, a heating sheet 3 multiplied by 2, a heating pipe 4 multiplied by 1, a first heat preservation pipe 5 multiplied by 1, a second heat preservation pipe 6 multiplied by 1 and a heat preservation column 7 multiplied by 2; wherein the second heat preservation pipe 6 is fixedly embedded on the inner wall of the installation cavity 8.
The conductive cap 2 is composed of a metal bowl 10 and a filling core 9 in the bowl, the metal bowl 10 is made of low-carbon steel and plays a role in conducting electricity and transmitting pressure, and the filling core 9 in the bowl is made of dolomite and plays a role in heat preservation and transmitting pressure. The metal bowl 10 is cylindrical, the outer diameter of the metal bowl corresponds to the inner diameter of the installation cavity 8, the metal bowl can be inserted into the installation cavity 8, and when the metal bowl is specifically assembled, the metal bowl is located at two ends of the installation cavity 8, and the filling core 9 is assembled relatively. The end face of the inner side of the conductive cap 2 is positioned in the second heat preservation pipe 6.
The heating sheets 3 are round metal sheets and are made of molybdenum through processing, the outer diameter of each heating sheet corresponds to the outer diameter of the conductive cap 2, and the two heating sheets 3 are symmetrically assembled in the installation cavity 8, are located on the inner side of the conductive cap 2 and are in contact with the conductive cap 2. The conductive cap 2 plays a role of heating by energization.
The first heat preservation pipe 5 is arranged between the two heating sheets 3, and the annular end surfaces of the two sides of the first heat preservation pipe are respectively contacted with the opposite side surfaces of the two heating sheets 3. The outer diameter of the first heat preservation pipe 5 is matched with the inner diameter of the installation cavity 8, a heating pipe 4 is sleeved in the first heat preservation pipe 5, the heating pipe 4 is also made of molybdenum through processing, the outer diameter corresponds to the inner diameter of the first heat preservation pipe 5, and the heating effect is achieved through electrifying.
Two heat preservation posts 7 are assembled in the heating pipe 4, and the heat preservation posts 7 are cylindrical parts and are half as high as the heating pipe 4.
The first heat-preservation pipe 5, the second heat-preservation pipe 6 and the heat-preservation column 7 are made of zirconia ceramics and play roles in heat preservation and pressure transmission.
The modification method using the combined block is as follows:
1) assembling: preparing a pyrophyllite block, assembling a conductive cap 2 and heating sheets 3 symmetrically according to two ends, assembling a first heat preservation pipe 5 and a heating pipe 4 between the two heating sheets 3 from outside to inside, assembling two heat preservation columns 7 in the heating pipe 4, and placing diamond to be modified between the heat preservation columns 7.
2) The assembly block with the diamond arranged therein is arranged on a high-temperature high-pressure synthesis press, six faces of the assembly block are extruded by a nail hammer to generate pressure of 8-9 GPa required for modification, and the heating plate 3 and the heating pipe 4 are electrified to generate temperature of 1800-2200 ℃ required for modification.
Example 2: CVD cultivates modified equipment piece of using of diamond high temperature high pressure
Most of the structure of the assembled block is the same as that of embodiment 1, and the two examples differ in the specific structure of the pyrophyllite block 1, and the materials used for the various components.
1) Structure of pyrophyllite block 1: in this example, the pyrophyllite block adopts a structure divided into an upper block and a lower block, which is convenient to assemble.
2) The conductive cap 2, the heating plate 3, the heating pipe 4, the first insulating pipe 5, the second insulating pipe 6 and the insulating column 7 are made of the following materials:
the metal bowl 10 of the conductive cap 2 is made of titanium; the filling core 9 of the conductive cap 2 is made of alumina ceramic material;
artificial carbon is used for the heating sheet 3 and the heating pipe 4;
the first heat-insulating pipe 5, the second heat-insulating pipe 6 and the heat-insulating column 7 are made of magnesia ceramics.
The above-described components are different from those of embodiment 1 in structure except for the materials used.
Claims (10)
1. The utility model provides a CVD cultivates diamond high temperature high pressure and is modified with equipment piece, a serial communication port, including being located outer pyrophyllite piece, be equipped with the installation cavity that runs through it in the pyrophyllite piece, the both ends of installation cavity all set up the electrically conductive cap that corresponds rather than the cross-section, be equipped with the heating plate rather than contacting on the medial surface of electrically conductive cap, two be equipped with the heating pipe between the heating plate, the axial vertical heating piece of heating pipe, just the both ends ring terminal surface of heating pipe contacts with the heating plate of homonymy respectively, a heat preservation pipe has been cup jointed to the outside of heating pipe, be equipped with two heat preservation posts in the heating pipe, two be used for placing the diamond between the heat preservation post.
2. The assembly block for high-temperature and high-pressure modification of CVD cultured diamond according to claim 1, wherein a second thermal insulation tube is embedded on the inner wall of the mounting cavity, and the heating plate is arranged inside the second thermal insulation tube.
3. The assembly block for high-temperature and high-pressure modification of CVD cultured diamond according to claim 1, wherein the mounting cavity is circular, the conductive cap, the heating plate, the first heat preservation pipe, the heating pipe and the heating column are all circular, and the outer diameters of the conductive cap, the heating plate and the first heat preservation pipe are adapted to the inner diameter of the mounting cavity.
4. The assembled block for high-temperature and high-pressure modification of CVD diamond according to claim 1, wherein the first heat-insulating tube and the heating tube have the same length, and the height of the heat-insulating column is half of the height of the heating tube.
5. The assembly block for high temperature and high pressure modification of CVD diamond according to claim 1, wherein the conductive cap comprises a metal bowl and a filler, the metal bowl is made of a high temperature resistant metal material, the filler is made of a high temperature resistant ceramic material, and the filler is arranged on the inner end face of the conductive cap.
6. The assembly block for high-temperature and high-pressure modification of CVD cultured diamond according to claim 5, wherein the metal bowl is made of any one of low-carbon steel, molybdenum and titanium;
and/or
The filling core is made of any one of dolomite, zirconia ceramics, magnesia ceramics and alumina ceramics.
7. The assembly block for high-temperature and high-pressure modification of CVD cultured diamond according to claim 1, wherein the heating plate and/or the heating tube is made of any one of artificial carbon, graphite plate and molybdenum.
8. The assembly block for high-temperature and high-pressure modification of CVD cultured diamond according to claim 2, wherein the first heat preservation pipe is made of any one of dolomite or zirconia ceramic, magnesia ceramic and alumina ceramic;
and/or
The second heat preservation pipe is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics;
and/or
The heat preservation column is made of any one of dolomite or zirconia ceramics, magnesia ceramics and alumina ceramics.
9. The assembled block for high temperature and high pressure modification of CVD cultured diamond according to claim 1, wherein the pyrophyllite block comprises two symmetrical monolithic blocks, the monolithic blocks are spliced up and down to form the pyrophyllite block, and the conductive cap is combined with the outer end opening of the monolithic block.
10. A high-temperature high-pressure modification method for CVD cultured diamond, which is characterized in that the assembly block according to any one of claims 1 to 9 is used, the CVD cultured diamond is placed between two heat preservation columns, six faces of the assembly block are pressed by a high-temperature high-pressure synthesis press top hammer during modification, pressure of 8-9 GPa is generated, and the temperature of 1800-2200 ℃ is generated by electrifying a heating plate and a heating pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010541379.2A CN111659318B (en) | 2020-06-15 | 2020-06-15 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010541379.2A CN111659318B (en) | 2020-06-15 | 2020-06-15 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111659318A true CN111659318A (en) | 2020-09-15 |
| CN111659318B CN111659318B (en) | 2023-10-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010541379.2A Active CN111659318B (en) | 2020-06-15 | 2020-06-15 | Assembled block for high-temperature high-pressure modification of CVD cultivated diamond and modification method |
Country Status (1)
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|---|---|
| CN (1) | CN111659318B (en) |
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2020
- 2020-06-15 CN CN202010541379.2A patent/CN111659318B/en active Active
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| 买潇: "褐色金刚石的改色机理和温压行为" * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111659318B (en) | 2023-10-27 |
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Denomination of invention: An assembly block and modification method for CVD cultivation of diamond high-temperature and high-pressure modification Granted publication date: 20231027 Pledgee: China Construction Bank Liaocheng Shizhong Sub branch Pledgor: SHANDONG LIAOCHENG JUNRUI SUPERHARD MATERIAL Co.,Ltd. Registration number: Y2024980005671 |