CN100364664C - Powder catalyst for synthesizing high strength and excellent quality diamond with low prodn. cost - Google Patents
Powder catalyst for synthesizing high strength and excellent quality diamond with low prodn. cost Download PDFInfo
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- CN100364664C CN100364664C CNB2005100851851A CN200510085185A CN100364664C CN 100364664 C CN100364664 C CN 100364664C CN B2005100851851 A CNB2005100851851 A CN B2005100851851A CN 200510085185 A CN200510085185 A CN 200510085185A CN 100364664 C CN100364664 C CN 100364664C
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- 239000010432 diamond Substances 0.000 title claims abstract description 65
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 65
- 239000003054 catalyst Substances 0.000 title claims abstract description 61
- 230000002194 synthesizing effect Effects 0.000 title abstract description 7
- 239000000843 powder Substances 0.000 title description 32
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 12
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 24
- 238000003786 synthesis reaction Methods 0.000 claims description 24
- 238000005275 alloying Methods 0.000 claims description 10
- 239000011573 trace mineral Substances 0.000 claims description 9
- 235000013619 trace mineral Nutrition 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 32
- 239000011572 manganese Substances 0.000 description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 20
- 229910045601 alloy Inorganic materials 0.000 description 16
- 239000000956 alloy Substances 0.000 description 16
- 239000000203 mixture Substances 0.000 description 15
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 14
- 229910001573 adamantine Inorganic materials 0.000 description 14
- 238000000034 method Methods 0.000 description 13
- 239000011362 coarse particle Substances 0.000 description 7
- 235000012041 food component Nutrition 0.000 description 7
- 239000005417 food ingredient Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 239000010437 gem Substances 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000009689 gas atomisation Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910005800 NiMnCo Inorganic materials 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 238000000462 isostatic pressing Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910003271 Ni-Fe Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- -1 and wherein Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
A powdered catalyst for synthesizing high-strength and high-quality diamond with low cost contains proportionally Ni, Mn, C, N, O, one or more of Cr, Ce and Si, and Fe. The resultant diamond has high output rate, integrity, transparency and thermal stability.
Description
Technical field
The present invention relates to the diamond synthesis fine catalyst, a kind of low-cost high-strength gem grade diamond fine catalyst of more specifically saying so.
Background technology
At present, produce diamond catalyst material commonly used and mainly contain Ni-based, iron-based and cobalt-base alloys, cobalt-base catalyst urges fusibleness good, but costs an arm and a leg, and domesticly seldom uses.Nickel-base catalyst diamond synthesis output is low slightly, but gained diamond good crystalline, and crystals impurity is few, a little less than the magnetic, have high compression strength; Ferrum-based catalyst is active big, synthetic per unit area yield height, and molten carbon ability is strong, and synthetic parameters is also better.At present, domestic diamond industry is generally used sheet NiMnCo catalyst, and coarse granule, high-strength diamond output capacity are extremely low, and can't the above diamond of Synthetic 2 0kg.Catalyst form has very big influence to synthetic adamantine performance and output, fine catalyst has overcome the drawback of sheet catalyst lumber recovery, fine catalyst can fully mix with the graphite powder, contact area is big, can increase substantially synthetic per unit area yield, help synthesising coarse particle, high-strength diamond, and adopt the alternative Ni of Fe to prepare the catalyst based cost that helps reducing significantly catalyst of Fe.
" a kind of catalytic alloy powder and production method thereof " by name, the patent No. are 95110188.9 patent of invention, are to adopt mechanical alloying production to be used for the catalyst alloy powder of diamond.Alloying component is for by weight percentage: Fe:60-75%, and Mn:20-30%, Cr:4-10%, M:0.05-0.5%, M represent one or more among micro-B, Mg, Zr, Ce, the La.Publication number is the sheet production technology for CN1406665A provides a kind of no cobalt not have the catalyst based alloy preparation method of manganese Ni-Fe, alloying component is Fe:60-80%, surplus is Ni and trace element,, good crystalline dark with its synthetic diamond color, internal flaw are few, intensity height, Heat stability is good when using its diamond synthesis, have that synthesis pressure is low, the synthesis temperature wide ranges, the per unit area yield height, advantage such as building-up process is easy to control.
Summary of the invention
The object of the present invention is to provide a kind of need not be as metal Co or less with low-cost synthesising coarse particle, the high-strength diamond fine catalyst of precious metal such as metal Ni.
For achieving the above object, the present invention takes following technical scheme:
A kind of low-cost synthesising coarse particle of the present invention, high-strength diamond fine catalyst, percentage meter by weight, its alloying component is Ni:20～45%, Mn:0～5%, C:0.1～0.5%, N:50～180PPm, O:80～300PPm, surplus is Fe.
Low-cost synthesizing high-strength gem grade diamond of the present invention can contain trace element with fine catalyst, this low cost synthesizing high-strength gem grade diamond fine catalyst, percentage meter by weight, its alloying component is Ni:20～45%, Mn:0～5%, C:0.1～0.5%, trace element: 0.015～0.1%, N:50～180PPm, O:80～300PPm, surplus is Fe, and wherein, trace element is one or more among Cr, Ce and the Si.
Use in the fine catalyst at the low-cost synthesizing high-strength gem grade diamond that contains trace element, optimal technical scheme is: percentage meter by weight, its alloying component is Ni:28～30%, C:0.1～0.2%, trace element: 0.015～0.06%, Mn:0.15～0.4%, N:80～150PPm, O:100～120PPm, surplus is Fe.
With in the fine catalyst, described fine catalyst particle is spherical in shape or class is spherical at diamond of the present invention.
Blending theory according to diamond, in the system constituent element, add among an amount of Mn, C, Cr, V, Nb, the Ce one or more, add a spot of C, can reduce the oxygen content in the alloy, adding Mn, V, Nb are the alternate active elements of diamond and graphite, add Mn and can make catalyst soak into graphite more consumingly in the catalyst matrix alloy, thereby help adamantine synthetic; Adding Cr can promote the dissolving of carbon, reduce the temperature when synthesizing, solid solution is in catalyst fully, there is not segregation, also seldom entering becomes inclusion enclave in the diamond crystal, improve adamantine intensity, helps the synthetic of coarse granule, high-strength diamond, adding Si can improve the speed of growth of diamond crystal, increases adamantine heat endurance and compression strength.The suitable nitrogen content of fine catalyst helps the diamond color and is yellow; Control suitable oxygen content, help providing the catalytic activity of catalyst, reduce inclusion enclave in the diamond, improve adamantine heat endurance.
A kind of low-cost synthesising coarse particle of the present invention, high-strength diamond fine catalyst adopt fast cold atomization process preparation, the spherical in shape or spherical Fig. 1 of opinion of class of the fine catalyst particle of making.
Advantage of the present invention just is:
1. catalyst alloy powder disclosed in this invention is a kind of Fe based powders catalyst, the 3d electron hole of Fe is many, active big, stronger with the affinity of carbon atom, thereby making catalyst and graphite interact strengthens, molten carbon ability strengthens, and required synthesis pressure is low, with the NiMnCo alloy phase ratio of present extensive use, its cost of raw material reduces widely, makes to have the stronger market competitiveness;
2. diamond synthesis fine catalyst good sphericity of the present invention, specific area is big, can fully mix with the graphite powder, contact area is big, electric current reduces during diamond synthesis, and top hammer consumption is little, the utilization rate height of catalyst and graphite, diamond synthesizes the per unit area yield height, therefore can effectively reduce the production cost of diamond.
3. the present invention adopts fast cold atomization process to make the alloy powder composition even, and even tissue helps adamantine homogeneous nucleation and grows up, and improves the crystal perfection of diamond synthesis, thereby makes diamond have high compression strength.
4. fine catalyst of the present invention adds Mn, C, Cr, N etc. on matrix element Fe, Ni basis, Mn increases the wellability of catalyst and graphite, and C reduces oxygen content, and N helps the diamond color and is yellow, and Cr promotes the dissolving of carbon to improve diamond intensity;
5. fine catalyst of the present invention mixes the back diamond synthesis with graphite powder, pure in the crystal body after synthetic, the inclusion enclave total amount is few, and do not comprise low melting point element such as Mn, comparatively tiny dispersion distributes, showing as random arrangement, thereby make diamond have good thermal shock intensity, is to make the desirable feedstock of diamond tool goods shown in Fig. 2, table 1.
Product oxygen content≤200PPm of the present invention, good sphericity, alloying component is even, adopt the synthetic diamond φ 32mm cavity per unit area yield of this catalyst up to more than the 32Ct, isostatic pressing strength is higher than the diamond recovery rate of 20Kg greater than 10%, and 60 orders account for more than 70% with thick ratio in the diamond, diamond crystal percentage of head rice height, transparency is good, has good heat endurance, is the desirable feedstock of making instrument goods such as diamond saw blade.
Description of drawings
Fig. 1 is the ESEM pattern photo of Fe based powders catalyst of the present invention
Fig. 2 is the ESEM pattern photo of synthetic coarse granule high-strength diamond of the present invention
Fig. 3 is that the synthetic diamond inclusion enclave of Fe based powders catalyst of the present invention distributes
The specific embodiment
Below the invention will be further elaborated with embodiment, will help product of the present invention and advantage thereof are further described, and the present invention is not subjected to the restriction of these embodiment, and protection scope of the present invention is limited by claims.
Embodiment 1
A kind of synthesising coarse particle in the present embodiment, high-strength diamond fine catalyst, percentage meter by weight, its alloying ingredient composition are that Ni:30%, Mn:0.2%, C:0.2%, surplus are Fe.
Take by weighing purity and be 99.9% Ni, Fe, Mn batching, under inert gas shielding, in intermediate frequency furnace, will prepare burden melt after, prepare the diamond synthesis fine catalyst by the vacuum/inert gas atomization technique.The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:29.8%, Mn:0.16%, C:0.18%, and N:150PPm, O:120PPm surplus are Fe.
With the alloy screening, get particle size range and evenly mix by a certain percentage with the graphite powder for-200 purpose alloyed powders, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 40/45 order is as shown in table 1.
Embodiment 2
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:30%, Mn:0.3%, C:0.2%, Cr:0.02%, surplus is Fe.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:29.92%, Mn:0.28%, C:0.18%, Cr:0.018%, N:160PPm, O:150PPm, and surplus is Fe.
Get and be of a size of-200 purpose alloyed powders and the graphite powder mixes by a certain percentage, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 40/45 order sees Table 1.
Embodiment 3
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:25%, Mn:0.2%, C:0.4%, surplus is Fe.
To prepare burden pours into the prealloy ingot after the fusing immediately, with after the prealloy ingot fusing, produces novel synthesising coarse particle, high strenght diamond fine catalyst by the vacuum/inert gas atomization technique again.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:24.75%, Mn:0.16%, C:0.38%, N:120PPm, O:120PPm, and surplus is Fe.
Get particle size range and mix by a certain percentage for-150 purpose alloyed powders and graphite powder, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 50/60 order sees Table 1.
Embodiment 4
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:30%, Mn:0.3%, C:0.2%, Cr:0.02%, Si:0.02%, surplus are Fe.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:29.92%, Mn:0.26%, C:0.18%, Cr:0.018%, and Si:0.017%, N:140PPm, O:130PPm, surplus is Fe.
Get and be of a size of-200 purpose alloyed powders and the graphite powder mixes by a certain percentage, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 45/50 order sees Table 1.
Embodiment 5
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:25%, Mn:5%, C:0.2%, surplus is Fe.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:24.8%, Mn:4.8%, C:0.18%, N:160PPm, and O:180PPm, surplus is Fe.
Get and be of a size of-200 purpose alloyed powders and the graphite powder mixes by a certain percentage, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 45/50 order sees Table 1.
Embodiment 6
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:30%, C:0.5%, surplus is Fe.
To prepare burden pours into the prealloy ingot after the fusing immediately, with after the prealloy ingot fusing, produces novel synthesising coarse particle, high-strength diamond fine catalyst by the vacuum/inert gas atomization technique again.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:29.52%, C:0.48%, N:120PPm, O:120PPm, and surplus is Fe.
Get particle size range and mix by a certain percentage for-150 purpose alloyed powders and graphite powder, diamond synthesis under certain pressure and temperature, wherein the adamantine performance of 45/50 order sees Table 1.
Embodiment 7
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:45%, Mn:0.3%, C:0.2%, Cr:0.02%, Si:0.02%, Ce:0.06%, surplus is Fe.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:44.8%, Mn:0.28%, C:0.18%, Cr:0.017%, and Si:0.017%, Ce:0.03%, N:140PPm, O:130PPm, surplus is Fe.
Get and be of a size of-200 purpose alloyed powders and the graphite powder mixes by a certain percentage, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 45/50 order sees Table 1.
Embodiment 8
Its equipment and method of operating be substantially with embodiment 1, uniquely be not both, and percentage meter by weight, the food ingredient of its alloy is: Ni:30%, Mn:0.3%, C:0.2%, Ce:0.06%, surplus is Fe.
The novel powder catalyst that makes is analyzed, and its alloyed powder composition is Ni:29.7%, Mn:0.27%, C:0.18%, Ce:0.035%, N:120PPm, O:150PPm, and surplus is Fe.
Get and be of a size of-200 purpose alloyed powders and the graphite powder mixes by a certain percentage, diamond synthesis under certain pressure and temperature, granularity 〉=60 purpose ratios account for more than 70%, and wherein the adamantine performance of 40/45 order sees Table 1.
The performance of table 1 Fe-Ni fine catalyst diamond synthesis
| Embodiment | Isostatic pressing strength Kg | TI (％) | TTI(％) 1100℃ |
| 1 | 25 | 87 | 75 |
| 2 | 28 | 91 | 82 |
| 3 | 29 | 90 | 81 |
| 4 | 25 | 85 | 77 |
| 5 | 23 | 80 | 70 |
| 6 | 26 | 87.7 | 78.2 |
| 7 | 24 | 81 | 69.5 |
| 8 | 26 | 85.5 | 74.2 |
Claims (4)
1. diamond synthesis fine catalyst is characterized in that: percentage meter by weight, and its alloying component is Ni:20～45%, Mn:0～5%, C:0.1～0.5%, N:50～180PPm, O:80～300PPm, surplus is Fe.
2. diamond synthesis fine catalyst, it is characterized in that: percentage meter by weight, its alloying component is Ni:20～45%, Mn:0～5%, C:0.1～0.5%, trace element: 0.015～0.1%, N:50～180PPm, O:80～300PPm, surplus is Fe, wherein, trace element is one or more among Cr, Ce and the Si.
3. a kind of diamond synthesis fine catalyst according to claim 2, it is characterized in that: percentage meter by weight, its alloying component is Ni:28～30%, C:0.1～0.2%, trace element: 0.015～0.06%, Mn:0.15～0.4%, N:80～150PPm, O:100～120PPm, surplus is Fe.
4. according to any described diamond synthesis fine catalyst of claim 1-3, it is characterized in that: described fine catalyst particle is spherical in shape or class is spherical.
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| CNB2005100851851A CN100364664C (en) | 2005-07-25 | 2005-07-25 | Powder catalyst for synthesizing high strength and excellent quality diamond with low prodn. cost |
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| CN105903470A (en) * | 2016-06-13 | 2016-08-31 | 安庆市凯立金刚石科技有限公司 | Catalytic agent for carbon fiber diamond synthesis |
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2005
- 2005-07-25 CN CNB2005100851851A patent/CN100364664C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5696712A (en) * | 1979-12-28 | 1981-08-05 | Yoshiharu Ozaki | Synthesis of diamond |
| SU930800A1 (en) * | 1980-07-18 | 1982-10-23 | Московский Ордена Ленина,Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Государственный Университет Им.М.В.Ломоносова | Catalyst for synthesis of diamonds |
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| CN1465432A (en) * | 2003-01-14 | 2004-01-07 | 湖南三一新材料有限公司 | Ferrous-nickel base catalyst alloy for synthesizing artificial diamond |
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