CN100457251C - Method for preparing polycrystal diamond particle allocated with wide particle size - Google Patents
Method for preparing polycrystal diamond particle allocated with wide particle size Download PDFInfo
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- CN100457251C CN100457251C CNB2006100888935A CN200610088893A CN100457251C CN 100457251 C CN100457251 C CN 100457251C CN B2006100888935 A CNB2006100888935 A CN B2006100888935A CN 200610088893 A CN200610088893 A CN 200610088893A CN 100457251 C CN100457251 C CN 100457251C
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- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 65
- 239000010432 diamond Substances 0.000 title claims abstract description 65
- 239000002245 particle Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 238000009826 distribution Methods 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 230000001788 irregular Effects 0.000 claims abstract description 7
- 238000011068 loading method Methods 0.000 claims abstract description 4
- OBOXTJCIIVUZEN-UHFFFAOYSA-N [C].[O] Chemical group [C].[O] OBOXTJCIIVUZEN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000002360 explosive Substances 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 25
- 238000000465 moulding Methods 0.000 claims description 10
- 238000001228 spectrum Methods 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 6
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical compound [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 claims description 4
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- 241000978776 Senegalia senegal Species 0.000 claims 1
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- 239000000463 material Substances 0.000 abstract description 13
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- 238000010923 batch production Methods 0.000 abstract 1
- 238000005474 detonation Methods 0.000 description 17
- XTFIVUDBNACUBN-UHFFFAOYSA-N 1,3,5-trinitro-1,3,5-triazinane Chemical compound [O-][N+](=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)C1 XTFIVUDBNACUBN-UHFFFAOYSA-N 0.000 description 9
- 230000001133 acceleration Effects 0.000 description 7
- 238000004062 sedimentation Methods 0.000 description 7
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- 238000004880 explosion Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 3
- 229910001573 adamantine Inorganic materials 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
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- 229910001868 water Inorganic materials 0.000 description 3
- 244000215068 Acacia senegal Species 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 239000012153 distilled water Substances 0.000 description 2
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- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 240000001439 Opuntia Species 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 150000001721 carbon Chemical group 0.000 description 1
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- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
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- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000329 molecular dynamics simulation Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
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Abstract
A preparation method for the polycrystalline diamond particle with wide grain distribution is characterized in that the high-energy detonator is taken as the loading mean and the negative oxygen-carbon atom contained by the additionally added carbon source and the detonator is taken as the composite carbon source; the weight ratio between high-energy detonator and the additionally added carbon source is 1:7 through 1:9.5. The diamond obtained by the method of the invention has the granularity distribution ranging from 1 nm to 10000 nm, product has high purity which reaches between 50 percent and 70 percent calculated by the additionally added composite carbon source, and the purity of the products is higher than 95 percent. The irregular multi-blade externality formed by the gathering of fine grains with nano-dimension in the product grains has unique cutting function when in use for the polishing material. The invention method is synthesized in the enclosed container, the production process is easily controlled, the output is easy to be recovered, the invention has small effect to the environment, furthermore, the process and equipment are simple and convenient for implementing the batch production, and the disposable investment and production cost are low.
Description
Technical field
The present invention relates to the method for artificially synthesizing diamond, particularly relate to a kind of preparation method of polycrystalline diamond particulate (comprising nanoscale monocrystalline and micron order glomerocryst) of wide distribution of particle sizes.
Background technology
The method of artificially synthesizing diamond mainly contains static pressure method, dynamic high-pressure method, vapour deposition process and chemical reaction method.The most ripe and obtain than extensive use be static pressure method, promptly utilize the high temperature that quiet high pressure that the hydraulic pressure cubic hinge press produces and electric furnace produce and under catalyst action, graphite undergone phase transition to be converted into diamond.Its main feature is that equipment investment is bigger, the raw material complexity, Granularity Distribution from several micron in this scope of hundreds of micron, and particle is irregular monocrystalline, has sharp corners more.The dynamic high-pressure method claims explosion method again, comprise shock wave method, detonation wave method and sliding detonation method, be that the transient high temperature hot high pressure mechanical condition that utilizes explosive charge to produce makes in a certain way the graphite of assembling undergo phase transition to change into diamond, or the use oxygen negative explosive, the free carbon that produces under explosion condition generates diamond through coalescent, phase transformation and crystallization process.Through the primary product that obtain after the blast process are mixtures that diamond and a large amount of impurity form, and major impurity wherein is graphite, amorphous carbon, detonator lead fragment, packaging material fragment, also have protective medium residue etc. sometimes.Obtain purer diamond product at last through the chemical purification process again.What application was wider in the dynamic high-pressure method is shock wave method, promptly utilizes explosive-driven flying sheet to hit graphite, by impacting the HTHP that is produced, makes graphite change into diamond.Raw material moulding filling more complicated in this technology is not only wanted the packaged explosive powder column, also needs moulding graphite and metal to fly plate; This technology adopts the open explosion type production of outdoor sink usually, and is more serious to the vibrations and the noise pollution of environment, and product reclaims also difficulty; This technology products obtained therefrom particle mainly concentrates on a micron dimension, and product particle is the profile of comparison rule, and surface ratio is more smooth.Detonation synthesizing nano diamond technology, be to utilize the carbon in the oxygen negative explosive that diamond coalescent and phase transformation generation nano-scale takes place under the thermodynamic condition of explosive detonation, its products characteristics is that particle size concentrates on about 10 nanometers, d50=5-8, size distribution is between the 1-100 nanosection, the particle profile is spherical in shape, reunites easily.As China's patent: CN01114454.8 and CN02114842.2.
Summary of the invention
The present invention is directed to the product defects in the above-mentioned field, a kind of preparation method of polycrystalline diamond particulate of wide distribution of particle sizes is provided, its particle diameter distributes from the nanometer to the micron order, and product diversification more can adapt to the different market demands.
A kind of preparation method of polycrystalline diamond particulate of wide distribution of particle sizes is characterized in that: as the loading means, use the contained negative oxygen carbon atom of additional carbon and explosive itself as compounded carbons with high explosive.
Described high explosive and additional carbon weight ratio are: 1: 7-1: 9.5.
Described high explosive is made up of TNT, RDX and HMX.
The composition of described high explosive and weight ratio are: TNT: RDX: HMX=1: 8: 1-7: 2: 1.
Also contain PETN in the described high explosive.
Described additional carbon comprises one or more in charcoal, coke, graphite, the carbon black.
Described additional carbon granularity is at 100 orders-300 order.
Adopt when described high explosive is assembled with the additional carbon moulding and press-fit and annotate the mode of pretending and combining.
The structure of described high explosive and additional carbon moulding assembling is a Mach charge constitution.
Described Mach charge constitution is that TNT and additional carbon are dressed up the inner core powder column by notes, and RDX is wrapped up in powder column with HMX outward by press-fiting.
Also be added with the binding agent of 0.5%-10% when described TNT and additional carbon moulding assembling.
Described binding agent is one or more in paraffin, gum arabic or the cellulose.
Described wide size distribution is meant that particle diameter is distributed as 1nm-10000nm.
Described polycrystalline diamond particulate comprises nano cubic single-crystal diamond and micron polycrystalline diamond.
Nano cubic single-crystal diamond and micron polycrystalline diamond that the polycrystalline diamond of described wide size distribution obtains having spherical appearance by classification with a large amount of sharp corners and irregular contour, and polycrystalline diamond is to be assembled by numerous tiny nanoscale granule monocrystalline to form.
The habit analyzer of described nano cubic single-crystal diamond and micron polycrystalline diamond is German LE01530VP field emission scanning electron microscope.
The diffracting spectrum of described nano monocrystalline diamond is characterized as: characteristic peak is at 43 °, 75 °, 91 ° three place, and there is obvious broadening phenomenon the peak base; The diffracting spectrum of described micron polycrystalline diamond is characterized as: characteristic peak 41 °, 43 °, 75 °, 91 ° everywhere, 41 °, 43 ° to locate big of two peaks overlapping, 41 ° of peaks occur with the form of 43 ° acromion.
The present invention is to provide a kind of with the energy of high explosive as the means of loading, combine with additional carbon as generating adamantine carbon source with the carbon in the explosive, in airtight explosive container, ignite, collect explosion product and remove impurity, can obtain the polycrystalline diamond particulate through peroxidating.
Principle of the present invention is: oxygen negative explosive is when detonation, there is not oxidized excess carbon atom in the detonation process, can form free carbon in the explosive, as transforming adamantine a part of carbon source, add carbon black, graphite, precision processing charcoal or coke again as additional carbon simultaneously.The Molecular Dynamics Calculation of the nonequilibrium state effect of solid shows that the energy of wavefront can be 10 under the shock wave effect
-10Concentrate the energy of several electrons volt second on the inherent molecular link, be enough to the C-C key is opened.Additional carbon experiences the free carbon in explosive after pulverizing, key point, the free brief period in the detonation process like this, resets in diamond Thermodynamically stable district under certain protective medium effect, assembles, cooling, crystallization form polycrystalline diamond.High explosive and additional carbon weight ratio are: 1: 7-1: 9.5.Oxygen negative explosive used herein is TNT, and hexogen (RDX) and HMX (HMX), HMX play a part to strengthen the detonation condition, guarantee required quick-fried gentle detonation pressure.Can also add simultaneously a small amount of safe ammonia (PETN) replacement HMX and improve the stability of detonating.In addition,, make diamond such as quick-fried temperature detonation pressure generate required thermodynamic condition and be not being met, for this reason, can strengthen the detonation condition, promptly adopt a Mach powder charge by the design of charge constitution because the adding of additional carbon can cause the whole power of explosive to descend to some extent.TNT and additional carbon notes are dressed up the explosive inner core, RDX and HMX are press-fited the outer powder column of wrapping up in.If when the content of TNT hangs down, when notes are dressed up type, can add adhesive.
The present invention utilizes high explosive and the synthetic diadust of compounded carbons detonation to have the characteristics of wide size distribution, particle diameter is distributed between the 1nm-10000nm, utilize gravitational field and centrifugal force field principle of combining, control centrifugation time and centrifugal acceleration are carried out classification, under German LE01530VP field emission scanning electron microscope, scan, as can be seen, the present invention obtained having the nano cubic single-crystal diamond (as Fig. 3) of spherical appearance and have sharp corners and the micron polycrystalline diamond of irregular contour (as Fig. 4 a), and polycrystalline diamond be to assemble by numerous tiny nanoscale granules to form (as Fig. 4 b).The present invention compared with prior art, product comprises two kinds of crystal formations, except that nano monocrystalline diamond, mainly is the micron polycrystalline diamond that has obtained a kind of pattern uniqueness, because it has a large amount of sharp corners, have uniqueness when being used as polishing material and cut function efficiently.
Adopt Japanese XRD-6000 x ray diffractometer x of science (10 °～120 ° of its angles of diffraction) to measure, the diffracting spectrum of nano monocrystalline diamond is characterized as: characteristic peak is at 43 °, 75 °, 91 ° three place, and there is obvious broadening phenomenon the peak base; The diffracting spectrum of described micron polycrystalline diamond is characterized as: characteristic peak 41 °, 43 °, 75 °, 91 ° everywhere, 41 °, 43 ° to locate big of two peaks overlapping, 41 ° of peaks occur with the form of 43 ° acromion.(as Fig. 6).
The inventive method characteristics are: 1. the product particle distribution is wide, and particle diameter is distributed in the 1-10000nm scope; 2. can adjust the product particle degree by control proportion of raw material and charge constitution parameter and distribute, can obtain the different series of products of thickness; 3. product particle forms irregular multiple-cutting-edge mouth profile by the fine particle of nanoscale is coalescent, has unique cutting function when being used as polishing material; 4. product is difficult for reuniting, and is convenient to disperse to use; 5. diamond conversion ratio height reaches 50-70% by the compounded carbons total amount; 6. product purity is higher than 95%; 7. synthetic in closed container, production process is controlled easily, and product reclaims easily, has fewer environmental impacts; 8. technology, equipment are simple, are convenient to realize producing in batches, and one-time investment and production cost are all lower.
Description of drawings
Fig. 1: charging mould structure
Fig. 2: detonator powder column assembling schematic diagram
1-inner core powder column, 2-is wrapped up in powder column outward, 3-raw material powder column, 4-booster gains, 5-detonator.
Fig. 3: nano cubic single-crystal diamond transmission electron microscope picture
Fig. 4 a: micron polycrystalline diamond scanning outline drawing
Fig. 4 b enlarged drawing
Fig. 5: the diffracting spectrum of nano monocrystalline diamond
Fig. 6: the diffracting spectrum of micron polycrystalline diamond
Specific implementation method
The present invention is described in further detail below in conjunction with embodiment.
(1) batching
According to TNT: RDX: HMX=1: 8: 1-7: 2: 1, C: (RDX+TNT+HMX)=1: 7-1: 9.5 part by weight batching.Adopt to annotate dress and press-fit form and carry out powder charge.
Present embodiment batching consumption:
Employing utilizes Mach stem effect to improve synthesis pressure, be at TNT and additional carbon mixing powder column outer wrapping one deck detonating explosive RDX and HMX, make and in the inner core powder column, produce Mach reflection in the explosive detonation process, improve synthetic pressure with this, the also available PETN of section H MX replaces, and increases the stability of detonating.
With copper or aluminum temperature controlled water bath pot material, bath temperature is controlled at 85-98 ℃ when annotating dress, treat complete fusion after, pour the aluminium-making mould moulding into, notice that material feeding speed is slow, each powder column divides 3-4 injection, preventing forming shrinkage cavity in the middle of the powder column, and in time fill up rising head.As the content of TNT when low, bad adhesion during its fusion can add the binding agent of 0.5%-5.0%, and binding agent can be used paraffin, gum arabic, cellulose or the like.
Adopt twice moulding when press-fiting.
The charging mould structure as shown in Figure 1, it comprises an inner core powder column 1 and wraps up in powder column 2 (see figure 2)s outward.
The bulk drug column dimension: inner core powder column diameter of phi 5-60mm, wrap up in powder column diameter of phi 10-100mm outward, grain length 50-500mm.
(2) blast is synthetic
Assemble according to accompanying drawing 2.With No. 8 electrician's industry detonators 5, press-fit 8701 booster gains 4 and raw material powder column 3 and assemble earlier, put into protective medium.The protective medium here is meant one of argon gas, nitrogen, carbon dioxide, water or sodium chloride, sodium acid carbonate, ammonium hydrogencarbonate.Place steel contained explosion jar to ignite then.
(3) preliminary treatment detonation ash
The detonation ash that is mixed with impurity such as protective medium, assembled material is taken out from the blast jar,, under 100-200 ℃ of temperature, dry after the sedimentation, can obtain the detonation ash through washing, removing by filter mechanical admixture.
(4) purify
Batching
Material and specification: bombard ash-dry powder, water content≤1%; Perchloric acid---chemical pure;
Proportioning: detonation ash (g): perchloric acid (ml)=1: 5-1: 15
Reactant by the proportioning weighing, is dropped in the glass reactor, agitating heating, reaction is 2-5 hour under 200 ℃ of-250 ℃ of temperature, note controlling reaction temperature, and it is slow that programming rate is wanted.Treat that the material color becomes canescence by black and can stop heating.
(5) washing and drying
Use the distilled water cyclic washing to PH=6.0-8.0 the pulpous state product, put into baking oven and under 100 ℃ of-150 ℃ of temperature, dry, promptly obtain PCD dry powder.
(6) detect
Detecting instrument: Japanese XRD-6000 x ray diffractometer x of science, German LE01530VP field emission scanning electron microscope, HORABA-250 particle size analyzer.
Get dry powder 0.1 gram use emission scan electron microscopic observation appearance, Fig. 3 is the nano cubic single-crystal diamond with spherical appearance.Accompanying drawing 4a and Fig. 4 b are the electromicroscopic photograph of micron polycrystalline diamond, are sharp corner angle of multi-stylus and cutting edge irregular contour from visible its profile of Fig. 4 a, are to be assembled by numerous tiny nanometer nano sized particles to form from the visible polycrystalline diamond of Fig. 4 b.Fig. 4 b is the enlarged drawing of Fig. 4 a.
Get about 0.5 gram of power-product and detect scope 10-120 ° of the angle of diffraction (2 θ) with X-ray diffraction (XRD) instrument.The diffracting spectrum of nano monocrystalline diamond is characterized as: characteristic peak is at 43 °, 78 °, 91 ° three place, and there is obvious broadening phenomenon the peak base; The diffracting spectrum of described micron polycrystalline diamond is characterized as: characteristic peak 41 °, 43 °, 75 °, 91 ° everywhere, 72 °, 75 ° to locate big of two peaks overlapping, 41 ° of peaks (as Fig. 6) occur with the form of 43 ° acromion.
Get dry powder 0.1 gram and be scattered in 200 ml distilled waters or the deionized water, test its granularity with the normally used HORABA particle size analyzer of industry, its size distribution interval is in the 1nm-10 mu m range, and median particle diameter should be d
50=3.5 μ m-6.5 μ m.
See with X-ray diffraction (XRD) specimen to have or not assorted peak, with plasma emission spectrum (ICP) test impurity content.
By above test, promptly provable product is purer polycrystalline diamond, and the purity of product is on 95%.
(7) classification
Based on gravitational field classification principle and centrifugal field principle, we combine the classification that is used for PCD with the two.
The theoretical foundation of gravitational field classification principle is according to the Stokes' law under the laminar condition.In classification process, suppose that the flow field is to be undertaken by laminar condition, and hypothesis ultrafine solids particle is spherical in shape, is free settling in medium.Therefore can think in classification process, this superfine spherical particle is under the self gravitation field action, and during sedimentation, sinking speed increases gradually in medium (gas or liquid), meanwhile suffered resistance also increases, thereby the free settling acceleration also reduces gradually.When the resistance of medium equaled the gravity of particle, its sedimentation acceleration was zero.It is constant that sinking speed keeps.This speed is referred to as the terminal velocity V of particle
0, obtain by derivation
η in the formula---dielectric viscosity (Pas);
The diameter of d---particle (m);
Density (the kg/m of δ---particle
3);
ρ---density of medium (kg/m
3);
G---acceleration of gravity (m/s
2);
The sinking speed of V---particle (m/s)
Following formula shows that when certain by the material of classification, during the medium that is adopted certain (being that δ, ρ, η are certain), terminal velocity is only relevant with the diameter of particle.Therefore, according to the particle end speed difference of different-diameter, can carry out classification to the different particle of granule size.
Yet, for ultra-fine grain, the more important thing is that its particle is superfine, difference between the particle diameter is minimum, thereby it is minimum to the influence of the difference of gravity and end speed, therefore, be difficult to make ultra-fine grain to carry out fast accurately high-effective classifying by simple gravitational field effect, institute must be by other field of force to reach dispersion effect preferably.Adopt centrifugal field to reach grading effect preferably, also with these two kinds of field of force comprehensive utilizations to ultra-fine grain.
By the expression formula of above-mentioned terminal velocity degree as can be known, when when all identical, being improved the terminal velocity degree of particle by the material of classification, medium and particle grain size, key is to improve gravity acceleration g.Know by physics knowledge, adopt centrifugal force can make speed reach tens g, sometimes even can reach thousands of g to a hundreds of g.When the resistance of medium and centrifugal force reached balance, the sinking speed of particle in centrifugal force field reached maximum and is the fast vor of weighing apparatus, can obtain by deriving: vor=d
2A/18 η * (δ-ρ)
The centrifugal acceleration of a in the formula---particle in centrifugal force field can be represented by the formula: a=r ω
2
The angular velocity of rotation of ω---particle (rad/s);
The radius of turn of r---particle (m)
As can be seen from the above equation, when certain by the material of classification, medium is certain, and the viscosity of medium is certain, centrifugal acceleration or separating factor one timing, and the centrifugal sedimentation speed of particle is only relevant with the diameter of particle.Thereby can adopt the difference of centrifugal force field according to particle centrifugal sedimentation speed, the particles different to particle size carry out classification.Following formula also illustrates, when by the various characteristics one of the material of classification and medium regularly, the key that improves the centrifugal sedimentation speed of particle is to improve centrifugal acceleration a.Centrifugal by controlling (or sedimentation time) and centrifuge speed can be realized the classification to polycrystalline diamond.
Adopt low speed centrifuge (≤5000rpm) and supercentrifuge (≤10000rpm) the polycrystalline product is carried out classification, can obtain the product of the interior different grain size scope of 1nm-10000nm (10 μ m) scope according to demand,
Conclusion: 1. distribution of particle sizes wider range of product of the present invention, 1nm-10000nm, wherein d50≤100nm is mainly nano crystal, accounts for 11-25%; 100nm＜d50＜1 μ m accounts for the mixture that 23-44% is monocrystalline and glomerocryst; It is glomerocryst that d50 〉=1 μ m accounts for 26-60%, and wherein 1 μ m≤d50≤3 μ m account for 30% of total amount, is the perfect material of polishing usefulness.2. can adjust the product particle degree by control proportion of raw material and charge constitution parameter and distribute, 3. adamantine conversion ratio height reaches 50-70% by adding compounded carbons, and 4. product purity is higher than 95%.
Claims (14)
1. the preparation method of the polycrystalline diamond particulate of a wide distribution of particle sizes, it is characterized in that: with high explosive as the loading means, as compounded carbons, described additional carbon comprises one or more in charcoal, coke, graphite, the carbon black with the contained negative oxygen carbon atom of additional carbon and explosive itself.
2. preparation method according to claim 1, described high explosive and additional carbon weight ratio are: 1: 7-1: 9.5.
3. preparation method according to claim 2, described high explosive is made up of TNT, RDX and HMX, and its weight ratio is: TNT: RDX: HMX=1: 8: 1-7: 2: 1.
4. preparation method according to claim 3 also contains PETN in the described high explosive.
5. preparation method according to claim 1, described additional carbon granularity is at 100 orders-300 order.
6. preparation method according to claim 1 adopts when described high explosive is assembled with the additional carbon moulding to press-fit and annotate the mode of pretending and combining.
7. preparation method according to claim 1, the structure of described high explosive and additional carbon moulding assembling is a Mach charge constitution.
8. preparation method according to claim 7, described Mach charge constitution is that TNT and additional carbon are dressed up the inner core powder column by notes, RDX is wrapped up in powder column with HMX outward by press-fiting.
9. preparation method according to claim 8, described TNT and additional carbon moulding also are added with the binding agent of 0.5%-5% when assembling, and described binding agent is one or more in paraffin, gum arabic or the cellulose.
10, the polycrystalline diamond particulate of the wide distribution of particle sizes that obtains of the arbitrary preparation method of claim 1-9.
11. the polycrystalline diamond particulate of wide distribution of particle sizes according to claim 10, described wide size distribution is meant that particle diameter is distributed as 1nm-10000nm.
12. the polycrystalline diamond particulate of wide distribution of particle sizes according to claim 10, described polycrystalline diamond particulate comprise nano cubic single-crystal diamond and micron polycrystalline diamond.
13. the polycrystalline diamond particulate of wide distribution of particle sizes according to claim 12, the polycrystalline diamond of described wide size distribution obtains having the nano cubic single-crystal diamond of spherical appearance by classification, micron polycrystalline diamond with sharp corners and irregular contour, and polycrystalline diamond is to be assembled by numerous tiny nanoscale granules to form.
14. the polycrystalline diamond particulate of wide distribution of particle sizes according to claim 12, the diffracting spectrum of described nano monocrystalline diamond is characterized as: characteristic peak is at 43 °, 75 °, 91 ° three place, and there is obvious broadening phenomenon the peak base; The diffracting spectrum of described micron polycrystalline diamond is characterized as: characteristic peak 41 °, 43 °, 75 °, 91 ° everywhere, 41 °, 43 ° to locate big of two peaks overlapping, 41 ° of peaks occur with the form of 43 ° acromion.
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| CN102091569B (en) * | 2010-12-10 | 2013-06-05 | 解立峰 | Artificial diamond and preparation method thereof |
| CN102757044B (en) * | 2012-07-23 | 2013-06-05 | 河南省联合磨料磨具有限公司 | High-cutting-force diamond micro powder and preparation method thereof |
| CN103706299A (en) * | 2012-10-09 | 2014-04-09 | 长春师范学院 | Fine-grained diamond synthetic method |
| CN105566019A (en) * | 2014-10-13 | 2016-05-11 | 彭碳科技有限公司 | Formula and method for preparation of three-dimensional graphene-coated single-particle nano-diamond material |
| CN111389310B (en) * | 2020-03-25 | 2021-04-23 | 北京理工大学 | Method for synthesizing polycrystalline diamond by virtue of detonation of dry distillation plant straws |
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