CN114100612A - Synthetic column with gradient component structure for synthesizing gem grade diamond and preparation method - Google Patents
Synthetic column with gradient component structure for synthesizing gem grade diamond and preparation method Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 62
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 14
- 239000010437 gem Substances 0.000 title claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 25
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 25
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000010439 graphite Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000003825 pressing Methods 0.000 claims abstract description 17
- 238000007731 hot pressing Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000007872 degassing Methods 0.000 claims abstract description 8
- 238000011068 loading method Methods 0.000 claims abstract description 7
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 229910052802 copper Inorganic materials 0.000 claims description 32
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 14
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000011049 filling Methods 0.000 abstract description 6
- 229910001751 gemstone Inorganic materials 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
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- 229910002546 FeCo Inorganic materials 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
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- 239000004215 Carbon black (E152) Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
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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
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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Abstract
The invention provides a gradient component structure synthetic column for synthesizing gem-grade diamond and a preparation method thereof, and the method specifically comprises the following steps: mixing, degassing, multilayer loading, cold pressing and hot pressing treatment to obtain the synthetic column material with gradient structural components. The invention takes Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials; drying and degassing in argon atmosphere; preparing premixed powder with different components by mixing; sequentially filling premixed powder with different components into a graphite mold in a multilayer filling mode; and then preparing the synthetic column with the gradient component structure by adopting a hot-pressing sintering mode. The novel synthesis column with the gradient component structure is designed at the seed crystal end and the graphite end of the diamond, so that the novel catalyst material which can greatly reduce rare and noble elements used for synthesizing the diamond with the precious stone grade and can achieve the purposes of stability and cost saving is obtained.
Description
Technical Field
The invention relates to the technical field of superhard materials, in particular to a synthetic column material with a gradient component structure for synthesizing gem-grade diamond and a preparation method thereof.
Background
Diamond is a cubic-centered isometric crystal composed of carbon elements, and is a very versatile ultra-hard material with extreme functionalities, such as thermal, optical, mechanical, electronic, and chemical. Generally, the cut gem grade large-grain diamond is generally called diamond, and especially type IIa diamond is considered to be a very potential defect-free substrate, and has important application in the advanced fields of quantum field, high-precision sensor, high-resolution imaging technology and the like.
Methods for preparing large single crystals of high purity diamond include Chemical Vapor Deposition (CVD) and high temperature High Pressure (HPHT) methods. However, there are still many technical problems with both high purity diamond synthesis methods. CVD diamond, for example, is a process in which hydrogen and hydrocarbon gases are decomposed into hydrocarbon reactive groups by high temperature, and then diamond is deposited on a substrate material, and has problems of hydrogen, stress and defects in large single crystals. Meanwhile, alloy elements such as Fe, Ni and Co are often used as catalysts for high-temperature and high-pressure diamond, so that the problem of metal impurities in the generated large single crystal is caused. Therefore, the key point of synthesizing diamond at high temperature and high pressure is how to design catalyst materials and structures thereof, thereby obtaining colorless gem grade diamond crystals and meeting the requirements of national defense, science and technology and jewelry.
At present, the diamond catalyst mainly comprises alloy elements such as Fe, Ni, Co and the like, particularly, precious diamond such as Russian NDT, Canadian AOTC and the like, and more mainly comprises FeCo alloy, and the main preparation method comprises metal smelting alloying and hot-pressing sintering. Generally, the cobalt content of the FeCo catalyst is between 40wt.% and 60wt.% to synthesize high quality diamond, but the temperature range for effectively synthesizing high quality diamond is < 10 ℃. However, the average content of Co element in the earth's crust is 0.001 mass%, and is an important raw material for lithium batteries, heat-resistant alloys, cemented carbides, corrosion-resistant alloys, magnetic alloys, and various cobalt salts. Therefore, the reduction of the Co element consumption in the catalyst material through material and structure design plays an important role in reducing the production cost and ensuring the production safety.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a synthetic column material with a gradient component structure for synthesizing gem-grade diamond and a preparation method thereof, and the preparation method greatly reduces the content of Co element and improves the quality of the synthetic diamond.
The technical scheme adopted by the invention is as follows: a gradient component structure synthesis column for synthesizing gem grade diamond comprises 60-0 wt.% of Co, 0-10 wt.% of Ti, 0-5 w.% of Al, 0-5 wt.% of Cu and the balance of Fe.
Further, the high Co content end of the gradient component structure synthesis column is in contact with the diamond seed crystal, and the high Ti, Al and Cu content end is in contact with the graphite.
Further, the preparation of the gradient component structure synthetic column takes Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials of the synthetic column, and the particle size of the powder is 30-50 mu m.
A method for preparing a synthetic column with a gradient component structure for synthesizing gem grade diamond comprises the following steps:
step 1: mixing, namely mixing 60-0 wt.% of Co powder, 0-10 wt.% of Ti powder, 0-5 wt.% of Al powder, 0-5 wt.% of Cu powder and the balance of Fe powder according to different proportions, and uniformly mixing by using a ball mill to prepare premixes with different alloy components;
step 2: degassing, namely degassing and drying the premix in an argon atmosphere;
and step 3: loading in multiple layers, namely loading degassed premix with different components into a graphite mold;
and 4, step 4: cold pressing, namely performing cold pressing pretreatment on the graphite mold subjected to multilayer loading;
and 5: and (3) hot-pressing sintering, namely preparing the synthetic column with the gradient component structure by using the graphite die subjected to cold pressing in a hot-pressing sintering mode.
Further, the degassing process in the step 2 is carried out under the condition of 2-10 ℃ for min-1Heating to 50-200 ℃ at the speed of (1-5) hours.
Furthermore, the number of the synthetic columns for the gradient components of the layered charging in the step 3 is 5-20 layers, and the thickness of each layer is 0.1-2 mm.
Further, the cold pressing pressure of the synthetic column in the step 4 is 0-35 MPa, and the pressure maintaining time is 1-10 min.
Further, in the step 5, the hot-pressing sintering pressure is 0-35 MPa, the temperature is 1000-1700 ℃, the sintering time is 10-300 min, and the vacuum degree is less than 10-3Pa。
The invention has the following beneficial effects:
1. the invention effectively reduces the content of Co element and improves the content of Ti, Al and Cu element by designing and preparing the synthetic column with the gradient component structure, thereby having obvious economic benefit.
2. According to the invention, by designing and preparing the synthesis column with the gradient component structure, the preset diamond seed crystals can be in the catalyst with sufficient and uniformly dispersed alloy elements in the synthesis process of the diamond, so that the smooth transformation of the graphite phase to the diamond phase is ensured; meanwhile, the influence of nitrogen elements in the growth process can be effectively reduced, and the yield of high-grade diamond can be effectively improved.
3. The grade and proportion of the high-grade diamond obtained by the gem-grade diamond synthesized by the method are obviously higher than those of the high-grade diamond synthesized by the common method, and considerable economic benefit is brought.
Drawings
FIG. 1 is a schematic structural diagram of a gradient composition structure synthesis column according to the present invention;
FIG. 2 is a temperature and pressure process diagram of the preparation of a gradient component structure synthetic column by hot-pressing sintering in the example.
Detailed Description
The invention will be further described with reference to the accompanying drawings.
The invention relates to a gradient component structure synthesis column for synthesizing gem-grade diamond, which is synthesized by adopting commercial Fe powder, Co powder, Ti powder, Al powder and Cu powder with the purity of not less than 99.99wt.% and the granularity of 30-50 mu m. The synthesized gradient component structure synthetic column is shown in FIG. 1, which is a synthetic column prepared from 8 layers of premix.
Example 1
In the synthesis column with the gradient component structure in the embodiment, the cobalt content of the synthesis column with the gradient component structure is 60-0 wt.%, the content of Ti, Al and Cu is 0-10 wt.%, 0-5 wt.% and 0-5 wt.%, respectively, and the balance is Fe.
The high Co content end of the gradient component structure synthesis column is in contact with the diamond seed crystal, and the high Ti, Al and Cu content end is in contact with the graphite.
The method for preparing the synthetic column with the gradient component structure comprises the step of taking Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials of the synthetic column, wherein the particle size of the powder is 30-50 mu m.
The preparation method of the synthesis column with the gradient component structure comprises the following steps:
step 1: mixing the raw materials according to different proportions, and uniformly mixing by using a ball mill to prepare 13 premixes with different components
1、Fe-60wt.%Co、
2、Fe-55wt.%Co、
3、Fe-50wt.%Co、
4、Fe-45wt.%Co、
5、Fe-40wt.%Co、
6、Fe-35wt.%Co-0.2wt.%Ti-35wt.%-0.1wt.%Al-0.1wt.%Cu、
7、Fe-30wt.%Co-0.4wt.%Ti-0.2wt.%Al-0.2wt.%Cu、
8、Fe-25wt.%Co-0.8wt.%Ti-0.3wt.%Al-0.3wt.%Cu、
9、Fe-20wt.%Co-1.6wt.%Ti-0.4wt.%Al-0.4wt.%Cu、
10、Fe-15wt.%Co-3.2wt.%Ti-0.5wt.%Al-0.5wt.%Cu、
11、Fe-10wt.%Co-5wt.%Ti-0.6wt.%Al-0.6wt.%Cu、
12、Fe-5wt.%Co-5wt.%Ti-0.7wt.%Al-0.7wt.%Cu、
13、Fe-5wt.%Ti-0.7wt.%Al-0.7wt.%Cu。
Step 2: mixing the premix with 5% hydrogen and argon at 5 deg.C for 5min-1After heating to 150 ℃ for 2 h.
And step 3: sequentially filling No. 1-13 premix with different components into a graphite mold; wherein, the number of the layers is 13, and the thickness of each layer is 0.62 mm.
And 4, step 4: carrying out cold pressing pretreatment on the layered charging graphite mold; wherein the cold pressing pressure is 30MPa, and the pressure maintaining time is 5 min.
And 5: preparing a synthetic column with a gradient component structure by using a hot-pressing sintering mode; wherein the pressure is 30MPa, the temperature is 1300 ℃, the sintering time is 60min, the vacuum degree is less than 10-3Pa; the temperature and pressure curves are shown in fig. 2.
By using the synthetic columns prepared in this example, the amount of Co element used was reduced by about 50% compared to the Fe-60wt.% Co comparative example. Then, the gem-grade diamond grown by the synthetic column is subjected to model selection, microscopic examination and other detection, and the synthetic diamond is screened to have the high-quality content of more than or equal to 60 wt%.
Example 2
In the synthesis column with the gradient component structure of the embodiment, the content of Co in the synthesis column with the gradient component structure is 60-0 wt.%, and the contents of Ti, Al and Cu are 0-10 wt.%, 0-5 wt.% and 0-5 wt.%, respectively, with the balance being Fe.
The high Co content end of the gradient component structure synthesis column is in contact with the diamond seed crystal, and the high Ti, Al and Cu element end is in contact with the graphite.
The preparation method of the gradient component structure synthetic column takes Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials of the synthetic column, and the particle size of the powder is 30-50 mu m.
The preparation method of the synthesis column with the gradient component structure comprises the following steps:
step 1: mixing: mixing the raw materials according to different proportions, and uniformly mixing the raw materials by using a ball mill to prepare 9 premixes with different components, wherein the components are as follows:
1、Fe-40wt.%Co、
2、Fe-35wt.%Co、
3、Fe-30wt.%Co、
4、Fe-25wt.%Co、
5、Fe-20wt.%Co-0.2wt.%Ti-35wt.%-0.1wt.%Al-0.1wt.%Cu、
6、Fe-15wt.%Co-0.4wt.%Ti-0.2wt.%Al-0.2wt.%Cu、
7、Fe-10wt.%Co-0.8wt.%Ti-0.3wt.%Al-0.3wt.%Cu、
8、Fe-5wt.%Co-1.6wt.%Ti-0.4wt.%Al-0.4wt.%Cu、
9、Fe-3.2wt.%Ti-0.5wt.%Al-0.5wt.%Cu。
step 2: will be provided withThe premix is added in 5% hydrogen and argon atmosphere at 5 deg.C for 5min-1After heating to 150 ℃ for 2 h.
And step 3: sequentially filling No. 1-9 premix with different components into a graphite mold; wherein, the number of the layers is 9, and the thickness of each layer is 0.90 mm.
And 4, step 4: carrying out cold pressing pretreatment on the layered charging graphite mold; wherein the cold pressing pressure is 30MPa, and the pressure maintaining time is 5 min.
And 5: preparing a synthetic column with a gradient component structure by using a hot-pressing sintering mode; wherein the pressure is 30MPa, the temperature is 1200 ℃, the sintering time is 90min, and the vacuum degree is less than 10-3Pa。
By using the synthetic columns prepared in this example, the amount of Co element used was reduced by about 35% compared to the Fe-40wt.% Co comparative example. Subsequently, the gem-grade diamond grown by the synthetic column is subjected to model selection, microscopic examination and other detection, and the synthetic diamond is screened to have the high-quality content of more than or equal to 65wt%, but the crystal face is more complete than that of the synthetic diamond in the embodiment 1, the crystal form is complete and full, the impurities at the bottom are less, the melting pit is less, but the growth speed is slower.
Example 3
In the synthesis column with the gradient component structure of the embodiment, the content of Co in the synthesis column with the gradient component structure is 60-0 wt.%, and the contents of Ti, Al and Cu are 0-10 wt.%, 0-5 wt.% and 0-5 wt.%, respectively, with the balance being Fe.
The high Co element content end of the gradient component structure synthesis column is in contact with the diamond seed crystal, and the high Ti, Al and Cu element contents are in contact with the graphite.
The preparation method of the gradient component structure synthetic column takes Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials of the synthetic column, and the particle size of the powder is 30-50 mu m.
The preparation method of the synthesis column with the gradient component structure comprises the following steps:
step 1: mixing: mixing the raw materials according to different proportions, and uniformly mixing by using a ball mill to prepare 11 premixes with different components
1、Fe-50wt.%Co、
2、Fe-45wt.%Co、
3、Fe-40wt.%Co、
4、Fe-35wt.%Co、
5、Fe-30wt.%Co、
6、Fe-25wt.%Co-0.2wt.%Ti-35wt.%-0.1wt.%Al-0.1wt.%Cu、
7、Fe-20wt.%Co-0.4wt.%Ti-0.2wt.%Al-0.2wt.%Cu、
8、Fe-15wt.%Co-0.8wt.%Ti-0.3wt.%Al-0.3wt.%Cu、
9、Fe-10wt.%Co-1.6wt.%Ti-0.4wt.%Al-0.4wt.%Cu、
10、Fe-5wt.%Co-3.2wt.%Ti-0.5wt.%Al-0.5wt.%Cu、
11、Fe-5wt.%Ti-0.6wt.%Al-0.6wt.%Cu。
Step 2: mixing the premix with 5% hydrogen and argon at 5 deg.C for 5min-1After heating to 150 ℃ for 2 h.
And step 3: sequentially filling No. 1-11 premix with different components into a graphite mold; wherein, the number of the layers is 11, and the thickness of each layer is 0.75 mm.
And 4, step 4: carrying out cold pressing pretreatment on the layered charging graphite mold; wherein the cold pressing pressure is 30MPa, and the pressure maintaining time is 5 min.
And 5: preparing a synthetic column with a gradient component structure by using a hot-pressing sintering mode; wherein the pressure is 30MPa, the temperature is 1250 ℃, the sintering time is 60min, the vacuum degree is less than 10-3Pa。
By using the synthetic columns prepared in this example, the amount of Co element used was reduced by about 45% compared to the Fe-50wt.% Co comparative example. Subsequently, the gem-grade diamond grown by the synthetic column is subjected to model selection, microscopic examination and other detection, and the screened synthetic diamond has high quality content of more than or equal to 62wt%, but the crystal face is irregular compared with the example 1, the 311 crystal face appears more, the crystal face growth lines are obvious, and the impurity content is low.
Comparative example
In the synthesis column with the gradient component structure of the embodiment, the content of Co in the synthesis column with the gradient component structure is 60-0 wt.%, and the contents of Ti, Al and Cu are 0-10 wt.%, 0-5 wt.% and 0-5 wt.%, respectively, with the balance being Fe.
The high Co content end of the gradient component structure synthesis column is in contact with the diamond seed crystal, and Ti, Al and Cu are in contact with graphite.
The preparation method of the gradient component structure synthetic column takes Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials of the synthetic column, and the particle size of the powder is 30-50 mu m.
The preparation method of the synthesis column with the gradient component structure comprises the following steps:
step 1: mixing the raw materials according to the proportion of Fe-60wt.% Co-5wt.% Ti-0.5wt.% Al-0.5wt.% Cu, and uniformly mixing by using a ball mill to prepare the premix.
Step 2: mixing the premix with 5% hydrogen and argon at 5 deg.C for 5min-1After heating to 150 ℃ for 2 h.
And step 3: and (3) filling a graphite mold with a premix of fixed components.
And 4, step 4: carrying out cold pressing pretreatment on the layered charging graphite mold; wherein the cold pressing pressure is 30MPa, and the pressure maintaining time is 5 min.
And 5: preparing a synthetic column with a gradient component structure by using a hot-pressing sintering mode; wherein the pressure is 30MPa, the temperature is 1400 ℃, the sintering time is 60min, and the vacuum degree is less than 10-3Pa; the temperature and pressure curves are shown in fig. 2.
The consumption of Co element of the gem-grade diamond grown by the synthetic column is obviously increased, and the material cost is obviously improved.
The method utilizes the gem-grade diamond grown by the synthesis column to screen out that the content of high-quality (first-class A material) in the synthesized diamond is more than or equal to 80wt.%, and the high-quality (first-class A material) of the normally used catalyst material synthesized diamond accounts for 20-30 wt.%; and the color can reach DE color (conventional catalyst color EFG).
The invention overcomes the problems that the content of Co element in the integral synthetic column is high, and the content of nitrogen removing elements such as Ti, Al and the like is low in the prior art. The diffusion of carbon element can be more effectively controlled by applying a gradient component structure synthetic column with high Co content at the diamond seed crystal end; the nitrogen removal effect is effectively exerted by applying a gradient component structure synthetic column with high Ti, Al and Cu contents at the graphite end. By designing and preparing the synthetic column with the gradient component structure, alloy elements in the catalyst at the periphery of the diamond seed crystal in the synthetic process are fully and uniformly dispersed, and the growth efficiency of diamond is effectively improved. Meanwhile, the diffusion of nitrogen element is effectively prevented while the diffusion of carbon is ensured, and finally the high-quality gem-grade diamond is synthesized.
Claims (8)
1. A synthetic gem grade diamond of gradient composition structure synthesizes post which characterized in that: the alloy comprises 60-0 wt.% of Co, 0-10 wt.% of Ti, 0-5 w.% of Al, 0-5 wt.% of Cu and the balance of Fe.
2. A graded composition synthetic cylinder for synthesizing gemstone-grade diamond according to claim 1, wherein: the high Co content end of the gradient component structure synthesis column is in contact with the diamond seed crystal, and the high Ti, Al and Cu content end is in contact with the graphite.
3. A graded composition synthetic cylinder for synthesizing gemstone-grade diamond according to claim 1, wherein: the preparation method of the gradient component structure synthetic column takes Fe powder, Co powder, Ti powder, Al powder and Cu powder as raw materials of the synthetic column, and the particle size of the powder is 30-50 mu m.
4. A method for preparing a synthetic column with a gradient component structure for synthesizing gem grade diamond is characterized by comprising the following steps:
step 1: mixing, namely mixing 60-0 wt.% of Co powder, 0-10 wt.% of Ti powder, 0-5 wt.% of Al powder, 0-5 wt.% of Cu powder and the balance of Fe powder according to different proportions, and uniformly mixing by using a ball mill to prepare premixes with different alloy components;
step 2: degassing, namely degassing and drying the premix in an argon atmosphere;
and step 3: loading in multiple layers, namely loading degassed premix with different components into a graphite mold;
and 4, step 4: cold pressing, namely performing cold pressing pretreatment on the graphite mold subjected to multilayer loading;
and 5: and (3) hot-pressing sintering, namely preparing the synthetic column with the gradient component structure by using the graphite die subjected to cold pressing in a hot-pressing sintering mode.
5. The method of claim 4, wherein the step of forming a graded-composition diamond post comprises: the degassing process in the step 2 is carried out under the condition of 2-10 ℃ min-1Heating to 50-200 ℃ at the speed of (1-5) hours.
6. The method of claim 4, wherein the step of forming a graded-composition diamond post comprises: the number of the synthetic columns for the layered charging gradient components in the step 3 is 5-20, and the thickness of each layer is 0.1-2 mm.
7. The method of claim 4, wherein the step of forming a graded-composition diamond post comprises: the cold pressing pressure of the synthetic column in the step 4 is 0-35 MPa, and the pressure maintaining time is 1-10 min.
8. The method of claim 4, wherein the step of forming a graded-composition diamond post comprises: in the step 5, the hot-pressing sintering pressure is 0-35 MPa, the temperature is 1000-1700 ℃, the sintering time is 10-300 min, and the vacuum degree is less than 10-3Pa。
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| CN112915922A (en) * | 2021-01-27 | 2021-06-08 | 山东昌润钻石股份有限公司 | Primary synthesis method of superfine diamond |
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| CN112915922A (en) * | 2021-01-27 | 2021-06-08 | 山东昌润钻石股份有限公司 | Primary synthesis method of superfine diamond |
Non-Patent Citations (3)
| Title |
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| 于昆鹏;李尚升;明黄亮;王健康;韩飞;高广进;郭明明;王君卓;宿太超;胡美华;胡强;吴玉敏;: "金刚石合成用触媒的应用及展望", 人工晶体学报, vol. 47, no. 08, pages 1714 - 1721 * |
| 尤悦等: "高温高压下金刚石大单晶研究进展", 《物理学报》, vol. 69, no. 23, pages 238101 - 1 * |
| 臧传义, 付星球, 望贤成, 马红安, 贾晓鹏: "在Fe-Al-C系统中合成优质IIa型宝石级金刚石单晶", 金刚石与磨料磨具工程, no. 05, pages 10 - 12 * |
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