CN107626261A - A kind of preparation method that diamond grade is improved using catalyst - Google Patents
A kind of preparation method that diamond grade is improved using catalyst Download PDFInfo
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- CN107626261A CN107626261A CN201710883650.9A CN201710883650A CN107626261A CN 107626261 A CN107626261 A CN 107626261A CN 201710883650 A CN201710883650 A CN 201710883650A CN 107626261 A CN107626261 A CN 107626261A
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Abstract
A kind of preparation method that diamond grade is improved using catalyst, belong to the field of superhard material preparation.Matched according to following ingredient percent：Nickel 29%, cobalt 1%, molybdenum 0.5% 1.5%, carbon 0.7%, iron surplus, the under nitrogen protection melting in intermediate frequency furnace, smelting temperature are 1700 DEG C；High temperature fusibility is atomized using water under high pressure, drop-wise is formed and alloy powder is rapidly solidificated into atomizing cup；Then the alloy powder after atomization is screened with target detection sieve, then alloy powder is mixed with graphite powder and is pressed into graphite synthetic rod, the diamond synthesis block in the cavity of cubic hydraulic press.The diamond block of synthesis is crushed, obtains diamond dust and the powder containing nickel, iron, cobalt and molybdenum, isolated high-grade diamond.The TI and TTI of diamond obtain a certain amount of raising, show that the quality of diamond increases.
Description
Technical field
The invention belongs to field prepared by superhard material, more particularly to Novel catalyst improves synthesized diamond
The method of grade.
Technical background
Allotrope of the diamond as carbon, it is the multi-functional superhard material for integrating a variety of excellent properties,
There are excellent physics, chemistry, electric property, be widely used in the fields such as industry, science and technology, national defence, health care, thus
The application study of diamond receives much concern.Wherein catalyst material auxiliary material indispensable in being synthesized as diamond,
It is in diamond building-up process so that the phase transformation activation energy and synthesis temperature of diamond, pressure are significantly reduced so as to make one
Make the key point that diamond is able to mass production.The catalyst material of synthesis of artificial diamond, which directly decides, synthesizes people
Make the grade of diamond.Fe at present70Ni30(70,30 be metallic element Fe, Ni mass percent respectively) powder catalyst is with it
Cheap cost advantage starts occuping market.
The researcher in China is on the distinctive cubic hinge press in China in recent years, using water smoke alloy powder catalyst,
Very big breakthrough is realized on HTHP diamond synthesis, the yield of diamond is greatly enhanced.Due to catalyst material
The importance of material, the country have carried out substantial amounts of research to catalyst material, substantially around synthesis temperature and pressure is reduced, increase
The problems such as adding per unit area yield, improving quality, expand kind, reduce cost, deploys.By adding variety classes in catalyst alloy powder
Additive with improve the grade of diamond and recycle purification after Fe-Ni catalyst can reduce diamond synthesis into
Originally, the problem of therefore this technology is well suited for improving current diamond market.
The content of the invention
In order to solve the problems, such as the low grade of HTHP diamond synthesis, the present invention, which proposes one kind and can circulated, to be made
The catalyst preparation method of diamond synthesis.
The present invention is achieved in the following ways：Height is improved by adding the iron nickel recycled with addition molybdenum powder
The grade of the diamond of warm high-pressure synthesis.
A kind of preparation method that diamond grade is improved using catalyst, it is characterised in that comprise the following steps：
(1) active ingredient using nickel powder, pure iron, cobalt powder and molybdenum powder as catalytic powder, according to following composition quality percentage
Than being matched：Nickel 29%, cobalt 1%, molybdenum 0.5%-1.5%, carbon 0.7%, iron surplus, under nitrogen protection in Medium frequency induction
Melting in stove, smelting temperature are 1700 DEG C；High temperature fusibility is atomized using water under high pressure, forms drop-wise fast rapid hardening in atomizing cup
Gu into alloy powder；
(2) alloy powder after step (1) atomization and then with target detection sieve is screened, then by alloy powder and stone
Ink powder is with 3：7 mass ratio mixing is pressed into graphite synthetic rod, the diamond synthesis block in the cavity of cubic hydraulic press
Body.
(3) the diamond block by step (2) synthesis crushes, and obtains diamond dust and containing nickel, iron, cobalt and molybdenum
Powder, isolated high-grade diamond.
The method of step (2) diamond synthesis block in the cavity of cubic hydraulic press, pressed using static state high-temperature is high
Into the method for diamond, comprise the following steps that：Graphite synthetic rod is put into the cavity of cubic hydraulic press, slowly pressurization exists
76MPa is pressurized to after 70s and then keeps pressure 300s；Continue to be pressurized to 94MPa from 76MPa with 20s time, in this pressure
Lower holding 30s makes inside cavity partial pressure balanced；Then it is pressurized to 96MPa with 20s time again and keeps 30s, then gradually drops
Pressure.50s does not heat up before cavity, and power is transferred to 5000w and keeps 350s to hydraulic press heating and incited somebody to action by transmitting medium after 50s
Temperature passes to cavity；Then power is reduced to 4920w and kept, and is voluntarily cooled down after power is adjusted to 0 after 470s；Step (2) is preferably adopted
Sieved with the target detection more than or equal to 200 mesh.
Diamond block is finally used crusher in crushing by step (3)；Fragment is divided by volume screen cloth and magnetic separation
From, after the completion of series of steps i.e. can obtain artificial synthesized diamond.
The purity 99.99% of metal pure iron；Cobalt powder purity 99.99%；Molybdenum powder purity 99.99%；Graphite powder purity
99.99%；Nickel powder 99.99%.
Experiment is cubic hydraulic press (preferably using the cubic hydraulic press of φ 38mm cavitys), there is provided required pressure
Condition and hydraulic press synthetic cavity are passed through electric current and heat the static high pressure high-pressure synthesis for making inside cavity reach a high temperature environment
Method.Subject raw material is nickel powder, raw metal pure iron, cobalt powder and molybdenum powder；In the experiment of diamond synthesis, by adding
The different forms changed in powder catalyst of the ratio of the molybdenum powder entered, wherein the powder morphology of spherical shape and sheet phychology powder
Response area difference can cause the grade of synthesized diamond to bring certain difference；Same oxygen content number also to gold
The synthesis of hard rock has a certain impact.
The grade qualitative character of diamond provided by the present invention can there are as below methods is characterized：
1. the pattern of hydraulic atomized catalyst powder can obtain adding a certain amount of by scanning electron microscopic observation, by contrast
Molybdenum powder be advantageous to be powder particle spherical in shape, make that sheet before its surface area ratio is big, and simultaneous reactions area further expands.
2. the oxygen content of catalytic powder by inertia pulsed infrared instrument detect, after testing after, obtain the oxygen content in powder
Decrease, be advantageous to the yield of diamond synthesizing
3. synthesis after diamond impact flexibility and thermal toughness index detected by impact flexibility instrument, after testing after, obtain
TI and TTI to the diamond for adding a certain amount of molybdenum powder synthesis obtain a certain amount of raising, show the quality of diamond
Increase.
Brief description of the drawings
Fig. 1 is that the cavity of 500 cylinder diameter press 38 synthesizes 170/200 granularity process curve.
Alloy powder scanning electron microscope (SEM) photograph in Fig. 2 embodiments 1；
Alloy powder scanning electron microscope (SEM) photograph in Fig. 3 embodiments 2；
Alloy powder scanning electron microscope (SEM) photograph in Fig. 4 embodiments 3.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to grinding for this area
Study carefully personnel and further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the common of this area
For technical staff, under the premise for not departing from present inventive concept, it can also make certain adjustments and improvements.These all belong to
In protection scope of the present invention.
Technical pure iron staff is used in embodiment, nickel uses nickel powder, cobalt and molybdenum to use high purity graphite using technical pure powder, carbon.
Embodiment 1
Step 1, the first composition proportion using the nickel powder of recycling, pure iron and cobalt powder molybdenum powder as Novel catalyst powder：
In nickel (29%)-cobalt (1%)-molybdenum (0.5%)-carbon (the 0.7%) -100kg intermediate frequency furnaces of iron (surplus) under nitrogen protection
Melting, smelting temperature are 1700 DEG C；High temperature fusibility is atomized using water under high pressure, drop-wise is formed and is rapidly solidificated into atomizing cup
Alloy powder (scanning electron microscope (SEM) photograph of alloy powder is shown in Fig. 2).
Step 2, then sieved with the target detections of 280 mesh to sieve the alloy powder after atomization, then by alloy powder with
Graphite powder is with 3:7 ratio mixing is pressed into graphite synthetic rod and synthesized in the domestic cubic hydraulic press of φ 38mm cavitys.
Graphite synthetic rod is put into the cavity of cubic hydraulic press, then slowly pressurization is pressurized to 76MPa after 70s
Keep pressure 300s；Continue to be pressurized to 94MPa from 76MPa with 20s time, keep 30s to make inside cavity point at this pressure
Pressure is balanced；Then it is pressurized to 96MPa with 20s time again and keeps 30s, then slowly decompression.50s does not heat up before cavity,
Power is transferred to 5000w and keeps 350s to be heated to hydraulic press and temperature is passed into cavity by transmitting medium after 50s；Then power
It is reduced to 4920w and keeps, is voluntarily cooled down after power is adjusted to 0 after 470s；
Implementation result：The oxygen content of powder is 3820ppm during the diamond that the present embodiment is prepared, its
In contained silicon, oxygen, phosphorus, sulphur impurity total content be 0.25%；Synthesize gold with the catalytic alloy powder of iron-nickel-cobalt-molybdenum-carbon
The quality of hard rock obtains a certain amount of raising, shows as：Thermal toughness index TTI (1000 DEG C)：62, magnetic susceptibility：45×10- 5SI, rod production：836.5 carats/kilogram, cold shock toughness (TI)： 90.
Embodiment 2
Step 1, the first composition proportion using the nickel powder of recycling, pure iron and cobalt powder molybdenum powder as Novel catalyst powder：
Melted in nickel (29%)-cobalt (1%)-molybdenum (1%)-carbon (the 0.7%) -100kg intermediate frequency furnaces of iron (surplus) under nitrogen protection
Refining, smelting temperature are 1700 DEG C；High temperature fusibility is atomized using water under high pressure, drop-wise is formed and conjunction is rapidly solidificated into atomizing cup
Bronze end (scanning electron microscope (SEM) photograph of alloy powder is shown in Fig. 3).
Step 2, then sieved with the target detections of 280 mesh to sieve the alloy powder after atomization, then by alloy powder with
Graphite powder is with 3:7 ratio mixing is pressed into graphite synthetic rod and synthesized in the domestic cubic hydraulic press of φ 38mm cavitys.
Graphite synthetic rod is put into the cavity of cubic hydraulic press, then slowly pressurization is pressurized to 76MPa after 70s
Keep pressure 300s；Continue to be pressurized to 94MPa from 76MPa with 20s time, keep 30s to make inside cavity point at this pressure
Pressure is balanced；Then it is pressurized to 96MPa with 20s time again and keeps 30s, then slowly decompression.50s does not heat up before cavity,
Power is transferred to 5000w and keeps 350s to be heated to hydraulic press and temperature is passed into cavity by transmitting medium after 50s；Then power
It is reduced to 4920w and keeps, is voluntarily cooled down after power is adjusted to 0 after 470s；
Implementation result：The oxygen content for the powder surveyed during the diamond that the present embodiment is prepared is
3810ppm, silicon contained therein, oxygen, phosphorus, sulphur impurity total content are 0.22%；With the catalytic alloy powder of iron-nickel-cobalt-molybdenum-carbon
What end synthesized the quality of diamond obtains a certain amount of raising, shows as：Thermal toughness index TTI (1000 DEG C)：68, magnetization
Rate：42×10-5SI, rod production：886.5 carats/kilogram, cold shock toughness (TI)：92
Embodiment 3
Step 1, the first composition proportion using the nickel powder of recycling, pure iron and cobalt powder molybdenum powder as Novel catalyst powder：
In nickel (29%)-cobalt (1%)-molybdenum (1.5%)-carbon (the 0.7%) -100kg intermediate frequency furnaces of iron (surplus) under nitrogen protection
Melting, smelting temperature are 1700 DEG C；High temperature fusibility is atomized using water under high pressure, drop-wise is formed and is rapidly solidificated into atomizing cup
Alloy powder (scanning electron microscope (SEM) photograph of alloy powder is shown in Fig. 4).
Step 2, then sieved with the target detections of 280 mesh to sieve the alloy powder after atomization, then by alloy powder with
Graphite powder is with 3:7 ratio mixing is pressed into graphite synthetic rod and synthesized in the domestic cubic hydraulic press of φ 38mm cavitys.
Graphite synthetic rod is put into the cavity of cubic hydraulic press, then slowly pressurization is pressurized to 76MPa after 70s
Keep pressure 300s；Continue to be pressurized to 94MPa from 76MPa with 20s time, keep 30s to make inside cavity point at this pressure
Pressure is balanced；Then it is pressurized to 96MPa with 20s time again and keeps 30s, then slowly decompression.50s does not heat up before cavity,
Power is transferred to 5000w and keeps 350s to be heated to hydraulic press and temperature is passed into cavity by transmitting medium after 50s；Then power
It is reduced to 4920w and keeps, is voluntarily cooled down after power is adjusted to 0 after 470s；Step (2) is preferably using the target more than or equal to 200 mesh
Detection sieve.
Implementation result：The oxygen content for the powder surveyed during the diamond that the present embodiment is prepared is
3810ppm, silicon contained therein, oxygen, phosphorus, sulphur impurity total content are 0.28%；With the catalytic alloy powder of iron-nickel-cobalt-molybdenum-carbon
What end synthesized the quality of diamond obtains a certain amount of raising, shows as：Thermal toughness index TTI (1000 DEG C)：65, magnetization
Rate：45×10-5SI, rod production：840 carats/kilogram, cold shock toughness (TI)： 91.
Claims (6)
1. a kind of preparation method that diamond grade is improved using catalyst, it is characterised in that comprise the following steps：
(1) active ingredient using nickel powder, pure iron, cobalt powder and molybdenum powder as catalytic powder, enters according to following ingredient percent
Row proportioning：Nickel 29%, cobalt 1%, molybdenum 0.5%-1.5%, carbon 0.7%, iron surplus, melted under nitrogen protection in intermediate frequency furnace
Refining, smelting temperature are 1700 DEG C；High temperature fusibility is atomized using water under high pressure, drop-wise is formed and alloy is rapidly solidificated into atomizing cup
Powder；
(2) alloy powder after step (1) atomization and then with target detection sieve is screened, then mixes alloy powder and graphite powder
Graphite synthetic rod is made in combined pressure, the diamond synthesis block in the cavity of cubic hydraulic press.
(3) the diamond block by step (2) synthesis crushes, and obtains diamond dust and the powder containing nickel, iron, cobalt and molybdenum,
Isolated high-grade diamond.
2. according to a kind of preparation method that diamond grade is improved using catalyst described in claim 1, it is characterised in that alloy
Powder is with graphite powder with 3:The mixing compacting of 7 mass ratios.
3. according to a kind of preparation method that diamond grade is improved using catalyst described in claim 1, it is characterised in that step
(2) in the cavity of cubic hydraulic press diamond synthesis block method, using the side of static state high-temperature high-pressure synthetic diamond
Method, comprise the following steps that：Graphite synthetic rod is put into the cavity of cubic hydraulic press, slowly pressurization is pressurized to after 70s
76MPa and then holding pressure 300s；Continue to be pressurized to 94MPa from 76MPa with 20s time；30s is kept to make chamber at this pressure
Internal body portion pressure is balanced；Then it is pressurized to 96MPa with 20s time again and keeps 30s, then gradually decompression；50s does not rise before cavity
Temperature, power is transferred to 5000w and keeps 350s to be heated to hydraulic press and temperature is passed into cavity by transmitting medium after 50s；Then
Power is reduced to 4920w and kept, and is voluntarily cooled down after power is adjusted to 0 after 470s.
4. according to a kind of preparation method that diamond grade is improved using catalyst described in claim 1, it is characterised in that step
(2) preferably sieved using the target detection more than or equal to 200 mesh.
5. according to a kind of preparation method that diamond grade is improved using catalyst described in claim 1, it is characterised in that step
(3) diamond block is finally used into crusher in crushing；Fragment is separated by volume screen cloth and magnetic separation, series of steps
After the completion of i.e. can obtain artificial synthesized diamond.
6. according to a kind of preparation method that diamond grade is improved using catalyst described in claim 1, it is characterised in that metal
The purity 99.99% of pure iron；Cobalt powder purity 99.99%；Molybdenum powder purity 99.99%；Graphite purity 99.99%；Nickel powder
99.99%.
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| CN112064120A (en) * | 2020-08-13 | 2020-12-11 | 中南钻石有限公司 | Seed crystal for large-size cultivation of diamond and preparation method thereof |
| CN112808169A (en) * | 2020-12-30 | 2021-05-18 | 福沃莱德(辽宁省)高新科技股份公司 | Diamond production process relating to cubic hydraulic press |
| CN115739100A (en) * | 2022-12-14 | 2023-03-07 | 郑州佳睿福新材料科技有限公司 | Spontaneous nucleation white diamond catalyst and production device thereof |
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Application publication date: 20180126 |