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Preparation method of catalyst for gemstone-grade artificial diamond single crystal, and catalyst

A technology of artificial diamond and catalyst, applied in the field of materials, can solve the problems of diamond single crystal yellowish color, difficult removal of impurity nitrogen atoms, and uneven microscopic distribution, and achieve the effect of improving nitrogen removal efficiency and reducing formation probability

Active Publication Date: 2018-05-18
王国伟
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The first problem is: after the catalyst is melted and the diamond single crystal begins to grow, due to the uneven microscopic distribution of the elements in the Fe-Ni-Cu-Ti(Al) alloy in the catalyst, in the low-content Ti(Al) micro-area , the impurity nitrogen atoms are not easy to remove, causing the diamond single crystal to turn yellow; in the Ti(Al)-enriched micro-region, it is easy to form trace Ti(Al) carbides, and enter the diamond single crystal to form inclusion impurities
[0011] The second problem is: the permalloy rods and Ti(Al) foils used in the catalyst must be machined, shaped and cut before use.

Method used

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  • Preparation method of catalyst for gemstone-grade artificial diamond single crystal, and catalyst
  • Preparation method of catalyst for gemstone-grade artificial diamond single crystal, and catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Prepare a catalyst alloy with a total mass of 1 kg and a mass percentage (nominal composition) of 75% Fe, 19% Ni, 4% Ti, and 2% Cu.

[0033] First weigh FeNi20 alloy powders with different particle sizes according to Table 1

[0034] Table 1 The weight of FeNi20 alloy powder with different particle sizes

[0035] Particle size (micron)

100-80

80-60

60-40

40-20

total

Mass percentage (%)

10％

20％

60％

10％

100％

Weighing mass (g)

93.85

187.7

563.1

93.85

938.5

[0036]Subsequently, according to Table 2, 35%Cu-65%Ti alloy powders with different particle sizes were weighed.

[0037] Table 2 The weight of 35% Cu-65% Ti alloy powder with different particle sizes

[0038] Particle size (micron)

100-80

80-60

60-40

40-20

total

Mass percentage (%)

5％

40％

30％

25％

100％

Weighing mass (g)

3.075

24.6

18.45

15.375

61.5

[0039] Aft...

Embodiment 2

[0042] Example 2: Prepare a catalyst alloy with a total mass of 1 kg and a mass percentage of 65.8% Fe, 28.2% Ni, 3% Al, and 3% Cu.

[0043] First weigh FeNi30 alloy powders with different particle sizes according to Table 3

[0044] Table 3 Weighing quality of FeNi30 alloy powders with different particle sizes

[0045] Particle size (micron)

100-80

80-60

60-40

40-20

total

Mass percentage (%)

5％

35％

40％

20％

100％

Weighing mass (g)

47

329

376

188

940

[0046] Subsequently, according to Table 4, 50% Cu-50% Ti alloy powders with different particle sizes were weighed.

[0047] Table 4 Weighing mass of 50%Al-50%Ti alloy powder with different particle sizes

[0048] Particle size (micron)

100-80

80-60

60-40

40-20

total

Mass percentage (%)

10％

40％

35％

15％

100％

Weighing mass (g)

3.075

24.6

18.45

15.375

60

[0049] After uniformly mixing ...

Embodiment 3

[0052] Example 3: Prepare a catalyst alloy with a total mass of 1 kg and a mass percentage (nominal composition) of 78% Fe, 18% Ni, 2.5% Ti, and 1.5% Cu. FeNi20 pre-alloyed powder and 35% Cu-65% Ti alloy powder are used. Grading mode is identical with embodiment 1.

[0053] After uniformly mixing 8 kinds of alloy powders with a total mass of 1 kg with different particle sizes with a 3-dimensional mixer, 2.5 grams of alloy powders were weighed each time and filled into a warm-pressing mold. Press at 150°C and 300MPa to form a cylinder with a relative density of 70%.

[0054] Put the prepared alloy cylinder into a hydrogen reduction furnace, incubate in a 10% hydrogen-90% argon atmosphere at 1000°C for 0.5 hours, and then in a pure argon atmosphere at 900°C for 1 hour. After cooling with the furnace, a catalyst alloy cylinder with a diameter of 10 mm, a height of 4 mm and a relative density greater than 99% was obtained. storage, backup.

[0055] Using the above catalyst, on...

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Abstract

The invention relates to a preparation method of a catalyst for a gemstone-grade artificial diamond single crystal, and a catalyst, wherein the metal catalyst is Fe-Ni-Ti-Cu-based catalyst alloy or aFe-Ni-Al-Cu-based catalyst alloy. The preparation method comprises: selecting raw materials and the ratio thereof, screening to achieve different particle size grades, preparing the material accordingto different particle size grades, uniformly mixing, carrying out warm pressing molding, controlling the warm pressing process to achieve the relative density of a molding billet of 70-80%, carryingout high-temperature hydrogen reduction sintering on the molding billet to achieve the relative density of the sintered cylindrical catalyst of more than 99%, cooling, and storing. According to the present invention, with the cylindrical catalyst, the nitrogen removal efficiency can be increased, the formation of inclusions can be reduced, and the growth speed and the clarity index of the gemstone-grade artificial diamond single crystal can be improved.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a method for preparing a catalyst for a gem-grade artificial diamond single crystal and the catalyst. Background technique [0002] When using ultra-high pressure equipment such as six-sided top and BARS (pressless ball-type ultra-high pressure synthesis device) to grow gem-grade synthetic diamond single crystals, generally use figure 1 A cube (referred to as a synthetic block) composed of the structural consumables shown. It includes tungsten carbide anvil 1, pyrophyllite pressure transmission medium 2, graphite heating tube 3, MgO cover 4, carbon source 5, MgO tube 6, metal catalyst 7, seed crystal 8, MgO crystal bed 9 and conductive steel cap 10 . When working, the tungsten carbide anvil 1 of the ultra-high pressure equipment is pushed by the pressure source, and evenly squeezes the composite block from six directions: up and down, front and rear, left and righ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755C30B29/04
CPCB01J23/755C30B29/04
Inventor 曹大呼龙政鑫李培培
Owner 王国伟