CN105833880B - A kind of multicomponent alloy catalyst and the preparation method and application thereof for diamond synthesis - Google Patents
A kind of multicomponent alloy catalyst and the preparation method and application thereof for diamond synthesis Download PDFInfo
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- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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- 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
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Abstract
The present invention relates to a kind of multicomponent alloy catalyst for diamond synthesis, alloying component is：Nickel 25~30%, tungsten 0.5~2%, titanium 0.5~1.5%, carbon 0.5~2 ‰, surplus are iron.The invention further relates to the preparation method of the multicomponent alloy catalyst and its applications in diamond synthesis.Multicomponent alloy catalyst provided by the invention is formed using iron, nickel, tungsten, titanium and carbon as raw material using special ratios, it can be ensured that the excellent properties such as multicomponent alloy catalyst alloy ingredient is uniform, and the impurity contents such as oxygen, silicon, sulphur, phosphorus are low.Present invention preferably employs water atomization process to be prepared, and has the performances such as low manufacture cost, product qualification rate height.The high quality synthetic diamond that stick production is high, cold heat impact flexibility is strong and magnetic susceptibility is low can be prepared using multicomponent alloy catalyst provided by the invention.
Description
Technical field
The present invention relates to diamond synthesizing fields, and in particular to a kind of synthesis high grade diamond catalyst material.
Background technology
Diamond has high hardness and good calorifics, optics, electric property, in stone material, building, engineering
The fields such as ceramics, automobile, Aeronautics and Astronautics play great effect.Artificially synthesizing diamond passes through more than 50 years hair in China
Exhibition, has formd complete and huge infant industry's system.Catalyst is in diamond building-up process, by significantly dropping
Temperature and pressure needed for low diamond synthesis and the substance for realizing diamond mass production.Synthesis of artificial diamond
Catalyst material directly decides the grade for synthesizing diamond, is the core starting materials of synthesis of artificial diamond.
Early stage is with Ni70Mn25Co5(70,25,5 be the mass percent of metallic element Ni, Mn, Co respectively) is the piece of representative
Shape catalyst material plays an important role on stablizing diamond synthesis.Recent years, the technical staff in China is in China spy
On some cubic hinge press, Fe is used70Ni30(70,30 be the mass percent of metallic element Fe, Ni respectively) water mist alloy
Powder catalyst, obtains very ten-strike on artificially synthesizing diamond, and it is big to establish China's diamond yield first at one stroke
The status of state.
But use the self-produced Fe in China70Ni30The diamond that water mist alloy powder catalyst synthesizes, mostly in, low
Based on shelves diamond product.For high-grade diamond product, a large amount of imports are still needed to.To find out its cause, being primarily due to use water
The Fe of atomization method production70Ni30The impurity contents such as oxygen, silicon, sulphur, the phosphorus of alloy powder it is higher (oxygen content is generally up to 4000~
7000ppm, content of impurities are up to 0.5~1%).This grade that restrict diamond improves, and is mainly manifested in high-strength material ratio
Low, per unit area yield is low, and granularity concentration ratio is low, and impact flexibility is low, and magnetism is big etc..This becomes China and makes the country prosperous from diamond big country to diamond
The major obstacle strided forward.
Invention content
The purpose of the present invention is overcoming the deficiencies of existing technologies, a kind of polynary conjunction for synthesizing high grade diamond is provided
Golden catalyst.
Specifically, multicomponent alloy catalyst of the present invention, by percentage to the quality, alloying component is：Nickel 25~
30%, tungsten 0.5~2%, titanium 0.5~1.5%, carbon 0.5~2 ‰, surplus is iron.
Preferably, alloying component is：Nickel 26~27%, tungsten 1~1.5%, titanium 0.6~1%, carbon 0.7~0.8 ‰ are remaining
Amount is iron.
Percentage of the present invention is each element mass percent shared in the multicomponent alloy catalyst.
Catalytic alloy provided by the invention forms Fe-Ni-W-Ti alloys with special ratios by iron, nickel, tungsten, titanium and carbon and touches
Matchmaker, by the way that tungsten and titanium are added at a specific ratio, when ensuring that gained catalyst is used for diamond synthesis, the stick of gained diamond
The qualities such as production, intensity, magnetism are better than the catalyst of the composition of alloy such as traditional Fe-Ni-Co-Mn.
On the basis of the present invention selects composition of alloy, further the dosage of each ingredient in alloy is carried out preferably,
It may insure that the impurity content of alloy powder is effectively controlled and the quality of later stage diamond synthesis is correspondingly improved.
In multicomponent alloy catalyst provided by the invention, the particle weight of the mesh of 200 mesh of grain size~500 accounts for the multicomponent alloy and touches
80% or more of matchmaker's gross mass, the grain size of whole particles is in the range of the mesh of 200 mesh~500 in the preferably described multicomponent alloy catalyst
Interior, above-mentioned particle diameter distribution may insure the uniformity that catalyst is mixed with the particle size matching of graphite and with graphite, after also ensuring that
The particle size uniformity and product stability of phase diamond synthesis.
Invention also provides the preparation methods of the multicomponent alloy catalyst.Specifically, the method includes following
Step：(1) raw material for taking each alloying component carries out melting under the conditions of inert gas shielding, obtains aluminium alloy；(2) high pressure is used
The aluminium alloy is atomized into powdery granule by water atomization process.
The present invention carries out preferably the addition sequence of each alloy raw material in step (1), to ensure gained each ingredient of aluminium alloy
Between be uniformly mixed, realize best application effect.Specifically, the step (1) is specially：After nickel plate is melted, it is added
Titanium plate and graphite form Ni-Ti-carbon alloy, sequentially add tungsten powder, iron staff, melting is carried out under the conditions of inert gas shielding,
Obtain aluminium alloy.
The present invention further in step (1) smelting temperature and condition carry out it is preferred, with each in enhancing gained aluminium alloy
Synergy between ingredient.Specifically, the step (1) is preferably：In 150~170KW, 3500~4500Hz, entrance
Be continually fed into inert gas smelting furnace it is molten in, after nickel plate is melted, titanium plate and graphite is added, forms Ni-Ti-carbon alloy, then
Tungsten powder, iron staff are sequentially added, melting to temperature reaches 1550~1600 DEG C, keeps the temperature 3~10 minutes, obtains aluminium alloy.Wherein, described
1550~1600 DEG C of temperature refers to the temperature of gained mixed liquor after each alloy fully melts in smelting furnace.Wherein, 3~10 are kept the temperature
The purpose of minute is to ensure that aluminium alloy can be sufficiently mixed under best temperature condition, preferably keeps the temperature 5min.
A straight-through inert gas in preparation process in step (1) described fusion process, preferably logical nitrogen.
In order to ensure gained catalytic alloy has excellent comprehensive performance, the mist of step (2) the hydraulic atomized method
It is preferably 35 ± 2MPa to change pressure.
The method of the invention can further comprise that water atomization products obtained therefrom is dried and sieved, to obtain drying simultaneously
Product with preferable particle size.The drying preferably carries out under vacuum.The screening is it is ensured that 200 mesh in products obtained therefrom
~500 mesh powder proportions can reach 80% or more.
This field convenient source can be selected in each ingredient in alloy of the present invention.Specifically, the optional recruitment of iron staff
Industry pure iron stick；Sheet nickel can be selected in the nickel plate；Industrial pure tungsten powder can be selected in the tungsten powder；Commercial titanium can be selected in the titanium plate
Plate；High purity graphite can be selected in the graphite.
The present invention passes through to raw material addition sequence, smelting temperature, the atomizing pressure etc. in multicomponent alloy catalyst preparation process
Parameter carries out comprehensively preferred, it can be ensured that in the multicomponent alloy catalyst that the method is prepared, the impurity such as oxygen, silicon, sulphur, phosphorus
Total content can be controlled in 0.5% or less；Wherein, oxygen content is 2000ppm~4000ppm.Although existing gas-atomised powders touch
The oxygen content of matchmaker up to 3000ppm hereinafter, but to use a large amount of inert gases in producing, cost is very high, complex process, and batch is raw
Production has been rarely employed；Scheme provided by the invention has low manufacture cost, easy to operate etc. apparent compared with gas-atomised powders catalyst
Advantage, and impurity content is low, and the Diamond Quality of gained multicomponent alloy catalyst synthesis is excellent, there is good application prospect.
The present invention further protects application of the multicomponent alloy catalyst in diamond synthesis.
Specifically, the application process is specially：By the multicomponent alloy catalyst and graphite raw material with weight ratio 3~5：
5~7 mix, preferably with weight ratio 4：6 mixing, diamond synthesis under the conditions of 5.0~5.5GPa, 1200~1500 DEG C.
The synthesis of the diamond carries out on domestic cubic hinge press.
The generated time of the diamond is 5~30min.According to generated time in 5~30min differences, granularity peak can be synthesized
It is worth the diamond of a certain granularity between the mesh of 400 mesh~30.
The present invention is by largely putting into practice discovery, and the diamond properties synthesized using the multicomponent alloy catalyst are excellent, product
It is high；Wherein, stick produces>800 carats/kilogram, cold shock toughness (TI)>85, thermal toughness index (1000 DEG C of TTI)>60, magnetic susceptibility
<50×10-5SI。
The stick of the diamond produces：Contained diamond in the diamond synthesizing stick that per kilogram synthesizes through high temperature and pressure
Quality (carat).
The cold shock toughness (TI) of the diamond refers to：At room temperature, to a certain amount of diamond in defined impact
Stipulated number is impacted under frequency, unbroken diamond accounts for the percentage of total diamond, is multiplied by the numerical value corresponding to 100.Usually
It is detected using analysis of diamond impact toughness index analyzer, reference standard：JB/T7989-1997.
The thermal toughness index (TTI) of the diamond refers to：(usual 900~1100 DEG C) at a certain temperature, filled with
In the heating furnace of argon gas protection, stipulated number, unbroken gold are impacted under defined frequency of impact to a certain amount of diamond
Hard rock accounts for the percentage of total diamond, is multiplied by the numerical value corresponding to 100.It is carried out usually using diamond thermal toughness index analyzer
Detection.
The magnetic susceptibility of the diamond refers to：The size for characterizing diamond magnetism, usually using diamond susceptibility analysis
Instrument or magnetic separation machine testing.
Compared with prior art, multicomponent alloy catalyst provided by the invention is using iron, nickel, tungsten, titanium and carbon as raw material, using spy
Certainty ratio forms, it can be ensured that the superiority such as multicomponent alloy catalyst alloy ingredient is uniform, and the impurity contents such as oxygen, silicon, sulphur, phosphorus are low
Matter.Present invention preferably employs water atomization process to be prepared, and has the performances such as low manufacture cost, product qualification rate height.Using this
It is artificial that the multicomponent alloy catalyst that invention provides can prepare the high grade that stick production is high, cold heat impact flexibility is strong and magnetic susceptibility is low
Diamond.
Specific implementation mode
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 26%, tungsten
1%, titanium 0.6%, carbon 0.7 ‰, surplus is iron.
The present embodiment additionally provides the preparation method of the multicomponent alloy catalyst, specially：Using 160KW, in 4000Hz
Frequency smelting furnace melting, in the continuous inflated with nitrogen of fire door in fusion process；After nickel plate is melted first, titanium plate and graphite is added, is formed
Ni-Ti-carbon alloy；Tungsten powder, iron staff are sequentially added, aluminium alloy temperature is maintained at 1570 DEG C when being all molten into alloy, heat preservation 5
Minute keeps alloying component uniform；Aluminium alloy is atomized by powder particle using hydraulic atomized method, atomizing pressure passes through for 35MPa
Vacuum drying, after dry, cross 200 mesh sieve to get.
Oxygen content is 3420ppm in multicomponent alloy catalyst provided in this embodiment, and oxygen, silicon, sulphur, phosphorus impurities total content are
0.25%.
Embodiment 2
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 27%, tungsten
1.2%, titanium 0.7%, carbon 0.8 ‰, surplus is iron.
The present embodiment additionally provides the preparation method of the multicomponent alloy catalyst, specially：Using 160KW, in 4000Hz
Frequency smelting furnace melting, in the continuous inflated with nitrogen of fire door in fusion process；After nickel plate is melted first, titanium plate and graphite is added, is formed
Ni-Ti-carbon alloy；Tungsten powder, iron staff are sequentially added, aluminium alloy temperature is maintained at 1580 DEG C when being all molten into alloy, heat preservation 5
Minute keeps alloying component uniform；Aluminium alloy is atomized by powder particle using hydraulic atomized method, atomizing pressure passes through for 36MPa
Vacuum drying, after dry, cross 200 mesh sieve to get.
Oxygen content is 3550ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.28%.
Embodiment 3
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 26%, tungsten
1.5%, titanium 1%, carbon 0.8 ‰, surplus is iron.
The present embodiment additionally provides the preparation method of the multicomponent alloy catalyst, specially：Using 160KW, in 4000Hz
Frequency smelting furnace melting, in the continuous inflated with nitrogen of fire door in fusion process；After nickel plate is melted first, titanium plate and graphite is added, is formed
Ni-Ti-carbon alloy；Tungsten powder, iron staff are sequentially added, aluminium alloy temperature is maintained at 1600 DEG C when being all molten into alloy, heat preservation 5
Minute keeps alloying component uniform；Aluminium alloy is atomized by powder particle using hydraulic atomized method, atomizing pressure passes through for 34MPa
Vacuum drying, after dry, cross 200 mesh sieve to get.
Oxygen content is 3400ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.22%.
Embodiment 4
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 25%, tungsten
0.5%, titanium 0.5%, carbon 0.5 ‰, surplus is iron.
Preparation method is the same as embodiment 1.
Oxygen content is 3450ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.28%.
Embodiment 5
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 30%, tungsten
2%, titanium 1.5%, carbon 2 ‰, surplus is iron.
Preparation method is the same as embodiment 1.
Oxygen content is 3480ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.32%.
Comparative example 1
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 28%, tungsten
0.2%, titanium 0.3%, carbon 3 ‰, surplus is iron.
Preparation method is the same as embodiment 1.
Oxygen content is 4280ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.55%.
Comparative example 2
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 26%, zinc
1%, titanium 0.6%, carbon 0.7 ‰, surplus is iron.
Preparation method is the same as embodiment 1.
Oxygen content is 4080ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.58%.
Comparative example 3
A kind of iron-nickel-tungsten-titanium-carbon complex alloy catalyst is present embodiments provided, alloying component is：Nickel 26%, tungsten
1%, aluminium 0.6%, carbon 0.7 ‰, surplus is iron.
Preparation method is the same as embodiment 1.
Oxygen content is 4210ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.50%.
Comparative example 4
Compared with Example 1, it differs only in, multicomponent alloy catalyst provided in this embodiment is prepared using aerosolization method
It forms.
Oxygen content is 3010ppm, oxygen, silicon, sulphur, phosphorus impurities total content in multicomponent alloy catalyst provided in this embodiment
0.24%.
Embodiment 6
A kind of method of artificially synthesizing diamond is present embodiments provided, specially：1 gained multicomponent alloy of embodiment is touched
Matchmaker is with graphite raw material with weight ratio 4：6 mixing, diamond synthesis under the conditions of 1350 DEG C, 5.2GPa.
The multicomponent alloy catalyst that the present embodiment is provided using Examples 1 to 5 and comparative example 1~4 respectively is raw material, in use
Diamond is prepared in the method for stating artificially synthesizing diamond.The performance test results of gained diamond are as shown in table 1.
Table 1：Diamond properties detect
| Multicomponent alloy catalyst source | Stick production (carat/kilogram) | Cold shock toughness | Thermal toughness index | Magnetic susceptibility |
| Embodiment 1 | 885 | 92 | 66 | 45×10-5SI |
| Embodiment 2 | 895 | 91 | 65 | 42×10-5SI |
| Embodiment 3 | 900 | 90 | 65 | 42×10-5SI |
| Embodiment 4 | 805 | 86 | 61 | 46×10-5SI |
| Embodiment 5 | 811 | 86 | 62 | 47×10-5SI |
| Comparative example 1 | 788 | 78 | 57 | 51×10-5SI |
| Comparative example 2 | 782 | 77 | 57 | 52×10-5SI |
| Comparative example 3 | 785 | 76 | 58 | 54×10-5SI |
| Comparative example 4 | 882 | 92 | 66 | 44×10-5SI |
As shown in Table 1, the diamond stick production height of the multicomponent alloy catalyst synthesis provided using invention, cold heat impact flexibility
Strong and magnetic susceptibility is low, has excellent performance；Although suitable with the Diamond Quality that powder catalyst made of aerosolization synthesizes, this hair
The multicomponent alloy catalyst of bright offer is prepared using water atomization process, what cost was prepared significantly lower than aerosolization method
Powder catalyst.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (8)
1. a kind of multicomponent alloy catalyst for diamond synthesis, which is characterized in that by percentage to the quality, alloying component
For：Nickel 25~30%, tungsten 0.5~2%, titanium 0.5~1.5%, carbon 0.5~2 ‰, surplus are iron；In the multicomponent alloy catalyst,
The particle weight of the mesh of 200 mesh of grain size~500 accounts for 80% or more of the multicomponent alloy catalyst gross mass；
The multicomponent alloy catalyst is prepared using the method included the following steps：
(1) it is continually fed into the smelting furnace of inert gas in 150~170KW, 3500~4500Hz, entrance, after nickel plate is melted,
Titanium plate and graphite is added, forms Ni-Ti-carbon alloy, sequentially adds tungsten powder, iron staff, melting to temperature reaches 1550~1600
DEG C, 3~10 minutes are kept the temperature, aluminium alloy is obtained；
(2) aluminium alloy is atomized into powdered under conditions of 35 ± 2MPa of atomizing pressure using hydraulic atomized method
Grain.
2. multicomponent alloy catalyst according to claim 1, which is characterized in that its alloying component is：Nickel 26~27%, tungsten 1
~1.5%, titanium 0.6~1%, carbon 0.7~0.8 ‰, surplus is iron.
3. the preparation method of multicomponent alloy catalyst described in claim 1~2 any one, which is characterized in that include the following steps：
(1) it is continually fed into the smelting furnace of inert gas in 150~170KW, 3500~4500Hz, entrance, after nickel plate is melted,
Titanium plate and graphite is added, forms Ni-Ti-carbon alloy, sequentially adds tungsten powder, iron staff, melting to temperature reaches 1550~1600
DEG C, 3~10 minutes are kept the temperature, aluminium alloy is obtained；
(2) aluminium alloy is atomized into powdered under conditions of 35 ± 2MPa of atomizing pressure using hydraulic atomized method
Grain.
4. the polynary conjunction that multicomponent alloy catalyst or claim 3 the method are prepared described in claim 1~2 any one
Application of the golden catalyst in diamond synthesis.
5. application according to claim 4, which is characterized in that by the multicomponent alloy catalyst and graphite raw material with weight ratio
3~5：5~7 mixing, diamond synthesis under the conditions of 5.0~5.5GPa, 1200~1500 DEG C.
6. application according to claim 5, which is characterized in that by the multicomponent alloy catalyst and graphite raw material with weight ratio
4：6 mixing.
7. application according to claim 5 or 6, which is characterized in that the synthesis of the diamond is in domestic cubic hinge press
Upper progress.
8. application according to claim 5 or 6, which is characterized in that the generated time of the diamond is 5~30min.
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| CN102962069A (en) * | 2012-11-30 | 2013-03-13 | 北京安泰钢研超硬材料制品有限责任公司 | Catalyst for synthesizing boron-containing diamond and preparation method thereof |
| CN105126853A (en) * | 2015-07-31 | 2015-12-09 | 河南省亚龙金刚石制品有限公司 | Catalyst for synthesizing high-quality gem grade diamond large single crystal and preparation method thereof |
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| US9765572B2 (en) * | 2013-11-21 | 2017-09-19 | Us Synthetic Corporation | Polycrystalline diamond compact, and related methods and applications |
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| CN102962069A (en) * | 2012-11-30 | 2013-03-13 | 北京安泰钢研超硬材料制品有限责任公司 | Catalyst for synthesizing boron-containing diamond and preparation method thereof |
| CN105126853A (en) * | 2015-07-31 | 2015-12-09 | 河南省亚龙金刚石制品有限公司 | Catalyst for synthesizing high-quality gem grade diamond large single crystal and preparation method thereof |
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Effective date of registration: 20201013 Address after: 100018 Beijing Chaoyang District pine Park No. 1 Patentee after: Sinoma intraocular lens Research Institute Co., Ltd Patentee after: BEIJING SINOMA SYNTHETIC CRYSTALS Co.,Ltd. Address before: 100018 Beijing city Chaoyang District dam pine Park No. 1 hospital Patentee before: BEIJING SINOMA SYNTHETIC CRYSTALS Co.,Ltd. |
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