CN1310834C - Method for refining superfine artificial diamond - Google Patents
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- CN1310834C CN1310834C CNB2005100185776A CN200510018577A CN1310834C CN 1310834 C CN1310834 C CN 1310834C CN B2005100185776 A CNB2005100185776 A CN B2005100185776A CN 200510018577 A CN200510018577 A CN 200510018577A CN 1310834 C CN1310834 C CN 1310834C
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Abstract
The present invention relates to a method for purifying artificial ultra-fine diamond, which relates to a method for refining artificial ultra-fine diamond. Pretreated ultra-fine diamond is added to mixed acid to be dispersed by ultrasonic waves; reactions are carried out for certain time under the conditions of middle temperature and high pressure, and reactants are taken out; ultra-fine diamond powder is obtained by solid-liquid separation, wash and desiccation, wherein the content of incombustible residues is less than 0.1 wt%, and the content of silicon dioxide is less than 0.01 wt%. The method has the advantages of simple technology and short production period, greatly reduces the consumption of acid, avoids bad working conditions and serious environment pollution brought by acid boiling technology, and greatly reduces production cost simultaneously.
Description
Technical field
The present invention relates to a kind of method of the superfine artificial diamond of purifying.
Background technology
Adamantine synthetic have static pressure method, blast lash method and detonation method etc., the diamond of the different-grain diameter grade that these synthetic methods obtain must just can be applied to different purposes with classification through purifying.The man-made diamond that wherein has macro-scale has obtained to use widely, and the adamantine applied research of nanometer (ultra-fine) yardstick, through ten years development, aspects such as modification, polymer composites, computer chip and printed wiring at super finishing polish, scuff-resistant coating, lubricating oil, obtain noticeable achievement, and shown very fine prospect.Yet, more and more high along with going deep into of ultra-fine diamond applied research to the requirement of its purity, in specific end use, very tight to the content requirement of its impurity (mainly referring to graphite, agraphitic carbon, silicon-dioxide and some metallic element).Seek out the high pure and ultra-fine diamond that meets this requirement, adopt conventional method of purification to be difficult to accomplish.
As everyone knows, in the synthetic and production process of man-made diamond, heavy task is that it is purified, and cost for purification accounts for the major part of producing the diamond cost.For the adamantine purification processes of macro-scale, adopt conventional method of purification, foreign matter content generally can both be controlled less than 0.5wt%.Purification process mainly comprises three parts:
4. remove metal solvent.Acid treatment, electrolysis process are arranged or two kinds of technologies are combined.
5. remove graphite and agraphitic carbon.With nitric acid, sulfuric acid and perchloric acid etc., use separately or the use of composition mixing acid, need to add inorganic oxidizer (as potassium permanganate and potassium bichromate) sometimes.Also can under hot conditions, add inorganic oxidizer and handle.Disclose under the temperature of 250～500 ℃ of scopes as United States Patent (USP) 3348918, mixed with lead oxide catalyst, selective oxidation is removed non-diamond carbon; Deutsches Wirtschafts Patent DD224575A discloses and a kind of copper salt solution has been mixed with diamond, remove non-diamond carbon, method be copper salt solution when being higher than 450 ℃ of temperature, be decomposed into cupric oxide or Red copper oxide, and under 540 ℃ of high temperature, join in the oxygen-containing gas and react; The open CN1211535A of patent application makes catalyzer with silver suboxide or silver suboxide is removed non-diamond carbon as the doping agent of cupric oxide under 300～500 ℃ of temperature.
6. remove agalmatolite.With hydrofluoric acid or soda boiling.Hydrofluoric acid treatment is under normal pressure, carries out in the water-bath, and soda boiling is divided into high temperature and cold condition again, decides on different diamond synthetic methods.
High temperature in the aforesaid method removes the method for non-diamond carbon can not complete oxidation graphite, and under hot conditions, ultra-fine diamond there is certain oxygenizement, (the different synthetic method of the aerial oxidizing temperature of ultra-fine diamond is slightly different not to be suitable for the purification of ultra-fine diamond, its oxidizing temperature is minimum to be about 430 ℃).
Also will be in the purification process of routine in conjunction with physical purification method, as shaking table, magnetic separation and heavy-fluid etc., method of purification is similar.
Chemical method is mainly still adopted in purification for ultra-fine diamond at present, as:
People such as Shi Wensheng (functional materials 1997,28 (5) 522-525 pages or leaves) handle and hydrofluoric acid water bath processing detonation method synthesizing superfine diamond with concentrated nitric acid and the boiling of vitriol oil mixed solution, removed most of impurity, but the chemical ingredients detected result is not provided, and X-ray powder crystal diffraction analysis 2 θ angles are at 20 °～40 ° amorphous bags that still have certain intensity.
People such as Wang Dazhi (Journal of Inorganic Materials Vol.10, No.3Sept., 1995, the 281-287 page or leaf) with handling detonation method synthetic ultra-fine diamond down with the hydrofluoric acid normal pressure again after perchloric acid and the immersion of nitric acid mixing acid, has only X-ray powder crystal diffraction analysis collection of illustrative plates, the bad judgement of removal of impurities result.
The method of purification of open CN 1385366 ultra-fine diamonds of patent application then adopts the vitriol oil and potassium permanganate mixed solution oxidizing reaction, handles detonation method synthetic ultra-fine diamond, and X-ray powder crystal diffraction analysis collection of illustrative plates only is provided.People such as Chen Pengwan (Chinese Journal Of High Pressure Physics Vol.13, No.1Mar., 1999,59-63 page or leaf) adopt the vitriol oil and potassium permanganate mixed solution purification detonation method synthetic ultra-fine diamond, analyze collection of illustrative plates but provided laser Raman spectroscopy, at 1600cm
-1Near shown the Raman peak of graphite broadening.
The method of the open CN 1480252A cerium salt purifying ultra-fine diamond particle of patent application is at detonation method synthetic ultra-fine diamond, with ceric ammonium nitrate or ammonium cerous sulfate oxidation non-diamond carbon, with X-ray powder crystal diffraction analysis, only explained adamantine strong peak, and not mentioned non-diamond carbon is residual.
Russ P 2,081,821 openly use the vitriol oil and concentrated nitric acid oxidation non-diamond carbon, adopt to add nitric acid in batches.The open CN1400162A of patent application contains the half-finished purification process of diamond synthesis of non-diamond carbon, be with the vitriol oil and concentrated nitric acid equally, different is earlier with vitriol oil submergence diamond work in-process, after being heated to boiling under the normal pressure, add concentrated nitric acid to reactant lentamente, X-ray powder crystal diffraction spectra shows that the residual quantity of graphite is less than 5% in the product.
Day disclosure is speciallyyed permit flat 63-303806 blast lash method synthetic diamond and is handled with chloroazotic acid, nitrosonitric acid or concentrated nitric acid earlier, perhaps add potassium permanganate, sodium chlorate, hydrogen peroxide as required and carry out oxide treatment, can not remove graphite fully, handle also residual graphite three times with the nitration mixture of the vitriol oil, strong phosphoric acid and concentrated nitric acid again.
In sum, in numerous diamond methods of purification, do not relate to concrete chemical ingredients and detect index.China is man-made diamond big producing country, a large amount of low-quality diadusts is arranged, generally (not flammable residue mainly is silicon-dioxide and some metallic elements to its not flammable residue between 0.5～10wt%, wherein dioxide-containing silica is greater than 0.2wt%, often between 1～3wt%), and contain a spot of non-diamond carbon, need be further purified.This diadust is to stay by having isolated behind the macro-size diamond institute, and impurity concentration has the enrichment tendency, make not only to have sneaked into a large amount of impurity in the diadust, and the micro mist particle still forms with agglomerate, and the particle diameter of agglomerate is 50～200nm.Bonding force is very strong between interior each particle of agglomerate, and mechanicals efforts and physical force are done by no means, but the effect of Chemical bond power.Between the agglomerate particle, there is binding medium, promptly has impurity.Remove these impurity, must open agglomerate by means of brute force.For this quasi-diamond micro mist, the purification techniques of China is not high.
Summary of the invention
At above-mentioned deficiency, the objective of the invention is to propose a kind of time short, with acid less, cost is low, the ultra-fine adamantine stone flour can be purified to the method for not flammable residue less than the high-purity diamond micropowder of 0.1wt%.
To achieve these goals, technical scheme of the present invention is: the process for purification of superfine artificial diamond, its process is with the pretreated ultra-fine adamantine stone flour of process, add mixing acid (as hydrofluoric acid, nitric acid etc.) and use ultrasonic dispersing, under middle temperature condition of high voltage, react again, after solid-liquid separation, washing and drying, obtain not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide.
The inventive method comprises the steps:
1). will carry out further fragmentation with micronizer mill or ball mill through pretreated diadust, and make its particle diameter less than 1 μ m;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: (0.5～10ml); Carry out ultrasonication, ultrasonic time 0.5～6 hour, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is that any one or any two kinds in nitric acid, sulfuric acid and the perchloric acid mix with hydrofluoric acid, and any one in nitric acid, sulfuric acid and the perchloric acid or any two kinds are (0.1～8) with hydrofluoric acid blended volume ratio: 1;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 20%～60%, and temperature of reaction is 150～220 ℃, and the reaction times is 2～25 hours;
4). from autoclave, take out solid-liquid mixtures, adopt whizzer or membrane filter plant to separate, with deionized water wash to pH=3～4;
5). take out the diamond after washing, adopt oven dry, spraying drying, lyophilize or vacuum-drying, obtain not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide.
In described nitric acid, sulfuric acid and the perchloric acid any two kinds when mixing with hydrofluoric acid, any two kinds is (0.05～4) with hydrofluoric acid blended volume ratio in nitric acid, sulfuric acid and the perchloric acid: (0.05～4): 1.
The diamond powder of the pretreated diadust of described process for passing through pulverizing, size classification or having adopted the conventional adamantine method of purifying to handle, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder.
The present invention compares with other method of purification, has following characteristics:
1. by hyperacoustic mechanical effect, cavatition and heat effect, brute force is opened agglomerate, disperses the reaction system.
2. warm hot high pressure is handled in, has strengthened the infiltration and the diffusibility of solvent, has accelerated speed of response.
3. hydrofluoric acid mixes use with oxidizing acid, and except effect separately (hydrofluoric acid silica removal, oxidizing acid removes agraphitic carbon, graphite and metallic impurity), synergistic effect is obvious.
4. shorten the working hour, reduced sour consumption, and abominable working conditions and the serious environmental pollution of having avoided acid treatment to bring, simultaneously production cost is greatly reduced.
6. obtain the noncombustibles residue less than 0.1wt%; The high pure and ultra-fine diadust of the content＜0.01wt% of silicon-dioxide.
The present invention is applicable to the purification of low-quality synthetic diamond micropowder.Ultra-fine diamond micro mist through method purification of the present invention, can be applicable to the aspects such as modification, polymer composites, computer chip and printed wiring of super finishing polish, coating, lubricating oil, have important application prospects in fields such as electronics, optical communication, machinery, chemical industry, national defence.
Description of drawings
Fig. 1 is the diadust X-ray powder crystal diffractogram of purifying without the inventive method among the embodiment 1
Fig. 2 is the X-ray powder crystal diffractogram of the embodiment of the invention 1
Fig. 3 is the diadust laser Raman spectroscopy collection of illustrative plates of purifying without present method among the embodiment 2
Fig. 4 is the laser Raman spectroscopy collection of illustrative plates of the embodiment of the invention 2
Embodiment
Only for explaining, the method that the present invention is described does not play any restriction to following Example.
Embodiment 1:
The former powder of diamond is pulverized through airflow milling.
(this micro mist is through 1000 ℃ of calcinations through broken diadust to take by weighing 10g, burning decrement equals 97.10wt%, dioxide-containing silica equals 2.50wt%, X-ray powder crystal diffraction detects has tangible impurity peaks for 20～40 ° at 2 θ angles, see Fig. 1), in the tetrafluoroethylene cup, add 5ml hydrofluoric acid, 20ml nitric acid, ultrasonication 0.5 hour, move into the autoclave of 70ml band inner liner polytetrafluoroethylene, put into baking oven, in 170 ℃ of heating 5 hours, after the cooling, from baking oven, take out, open autoclave and pour out supernatant liquid, flush out diamond, centrifuge washing is to pH=4, add 500ml deionized water ultrasonic dispersing, the direct spraying drying of suspension obtains diamond powder.After testing: 1000 ℃ of burning decrements equal 99.96wt%; Dioxide-containing silica equals 0.0025wt%; X-ray powder crystal diffraction detects does not see non-diamond thing phase, sees Fig. 2.
Embodiment 2:
Take by weighing 20g through broken diadust (this micro mist under normal pressure with hydrofluoric acid, nitric acid, perchloric acid and sulfuric acid repeated treatments 4 times, after testing: 1000 ℃ of calcinations, burning decrement equals 99.70wt%, dioxide-containing silica equals 0.25wt%, laser Raman spectroscopy figure occurs seeing Fig. 3 than higher graphite peaks).In the tetrafluoroethylene cup, add 5ml hydrofluoric acid, 20ml nitric acid, ultrasonication 1 hour moves into the autoclave that 70ml is with inner liner polytetrafluoroethylene, puts into baking oven, in 190 ℃ of heating 4 hours, after the cooling, from baking oven, take out, open autoclave and pour out acid solution, take out diamond, centrifuge washing is to pH=4, again centrifugal classification, diamond vacuum-drying with after the classification obtains diamond powder.After testing: 1000 ℃ of burning decrements equal 99.95wt%; Dioxide-containing silica equals 0.0032wt%; Laser Raman spectroscopy detects does not see graphite peaks, sees Fig. 4.
Embodiment 3:
The process for purification of superfine artificial diamond, step is as follows:
1). will carry out further fragmentation with micronizer mill through pretreated diadust, and make its particle diameter less than 1 μ m; The diamond powder that it is meant process pulverizing, size classification or has adopted the conventional adamantine method of purifying to handle through pretreated diadust, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: 0.5ml; Carry out ultrasonication, ultrasonic time 6 hours, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is hydrofluoric acid and perchloric acid, and the volume ratio of hydrofluoric acid and perchloric acid is 1: 0.1;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 20%, and temperature of reaction is 150 ℃, and the reaction times is 25 hours;
4). from autoclave, take out solid-liquid mixtures, adopt whizzer to separate, with deionized water wash to pH=3;
5). take out the diamond after washing, adopt oven dry, obtain not flammable residue＜0.1wt%; The high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide.
Embodiment 4:
The process for purification of superfine artificial diamond, step is as follows:
1). will carry out further fragmentation with ball mill through pretreated diadust, and make its particle diameter less than 1 μ m; The diamond powder that it is meant process pulverizing, size classification or has adopted the conventional adamantine method of purifying to handle through pretreated diadust, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: 10ml; Carry out ultrasonication, ultrasonic time 0.5 hour, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is hydrofluoric acid and sulfuric acid, and hydrofluoric acid and vitriolic volume ratio are 1: 8;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 60%, and temperature of reaction is 220 ℃, and the reaction times is 20 hours;
4). from autoclave, take out solid-liquid mixtures, adopt membrane filter plant to separate, with deionized water wash to pH=4;
5). take out the diamond after washing, adopt spraying drying, obtain not flammable residue＜0.1wt%; The high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide.
Embodiment 5:
The process for purification of superfine artificial diamond, step is as follows:
1). will carry out further fragmentation with micronizer mill through pretreated diadust, and make its particle diameter less than 1 μ m; The diamond powder that it is meant process pulverizing, size classification or has adopted the conventional adamantine method of purifying to handle through pretreated diadust, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: 1ml; Carry out ultrasonication, ultrasonic time 2 hours, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is two kinds in nitric acid and sulfuric acid and the mixing of hydrofluoric acid, and two kinds of blended volume ratios with hydrofluoric acid of nitric acid and sulfuric acid are 2: 1, and wherein nitric acid, vitriolic volume ratio are 1: 1;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 30%, and temperature of reaction is 180 ℃, and the reaction times is 5 hours;
4). from autoclave, take out solid-liquid mixtures, adopt whizzer to separate, with deionized water wash to pH=3.5;
5). take out the diamond after washing, adopt vacuum-drying, obtain not flammable residue＜0.1wt%; The high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide, after 6 hours, burning decrement is greater than 99.90wt% through 1000 ℃ of calcinations for the ultra-fine adamantine stone powder.
Embodiment 6:
The process for purification of superfine artificial diamond, step is as follows:
1). will carry out further fragmentation with micronizer mill through pretreated diadust, and make its particle diameter less than 1 μ m; The diamond powder that it is meant process pulverizing, size classification or has adopted the conventional adamantine method of purifying to handle through pretreated diadust, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: 3ml; Carry out ultrasonication, ultrasonic time 4 hours, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is two kinds in sulfuric acid and perchloric acid and the mixing of hydrofluoric acid, and sulfuric acid and perchloric acid are 4: 1 with hydrofluoric acid blended volume ratio for two kinds, and wherein the volume ratio of sulfuric acid, perchloric acid is 1: 1;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 50%, and temperature of reaction is 200 ℃, and the reaction times is 20 hours;
4). from autoclave, take out solid-liquid mixtures, adopt membrane filter plant to separate, with deionized water wash to pH=3.5;
5). take out the diamond after washing, adopt lyophilize, obtain not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide, after 6 hours, burning decrement is greater than 99.90wt% through 1000 ℃ of calcinations for the ultra-fine adamantine stone powder.
Embodiment 7:
The process for purification of superfine artificial diamond, step is as follows:
1). will carry out further fragmentation with micronizer mill through pretreated diadust, and make its particle diameter less than 1 μ m; The diamond powder that it is meant process pulverizing, size classification or has adopted the conventional adamantine method of purifying to handle through pretreated diadust, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: 5ml; Carry out ultrasonication, ultrasonic time 4 hours, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is that two kinds in nitric acid and perchloric acid mix with hydrofluoric acid, and nitric acid and perchloric acid are 5: 1 with hydrofluoric acid blended volume ratio for two kinds, and wherein the volume ratio of nitric acid, perchloric acid is 1: 1;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 40%, and temperature of reaction is 220 ℃, and the reaction times is 2 hours;
4). from autoclave, take out solid-liquid mixtures, adopt membrane filter plant to separate, with deionized water wash to pH=3.5;
5). take out the diamond after washing, adopt lyophilize, obtain not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide, after 6 hours, burning decrement is greater than 99.90wt% through 1000 ℃ of calcinations for the ultra-fine adamantine stone powder.
Claims (3)
1. the process for purification of superfine artificial diamond is characterized in that comprising the steps:
1). will carry out further fragmentation with micronizer mill or ball mill through pretreated diadust, and make its particle diameter less than 1 μ m;
2). add mixing acid and carry out ultrasonication, the solid-liquid ratio of ultra-fine diamond and mixing acid is 1g: (0.5～10ml); Carry out ultrasonication, ultrasonic time 0.5～6 hour, ultrasonic heating and temperature control is at 30～80 ℃; Wherein mixing acid is that any one or any two kinds in nitric acid, sulfuric acid and the perchloric acid mix with hydrofluoric acid, and any one in nitric acid, sulfuric acid and the perchloric acid or any two kinds are (0.1～8) with hydrofluoric acid blended volume ratio: 1;
3). will move in the autoclave through the solid-liquid mixtures of ultrasonication, the compactedness of autoclave is 20%～60%, and temperature of reaction is 150～220 ℃, and the reaction times is 2～25 hours;
4). from autoclave, take out solid-liquid mixtures, adopt whizzer or membrane filter plant to separate, with deionized water wash to pH=3～4;
5). take out the diamond after washing, adopt oven dry, spraying drying, lyophilize or vacuum-drying, obtain not flammable residue＜0.1wt%, the high pure and ultra-fine diamond powder of the content＜0.01wt% of silicon-dioxide.
2. the process for purification of superfine artificial diamond according to claim 1, it is characterized in that: in described nitric acid, sulfuric acid and the perchloric acid any two kinds when mixing with hydrofluoric acid, any two kinds is (0.05～4) with hydrofluoric acid blended volume ratio in nitric acid, sulfuric acid and the perchloric acid: (0.05～4): 1.
3. the process for purification of superfine artificial diamond according to claim 1, it is characterized in that: the diamond powder of the pretreated diadust of described process for passing through pulverizing, size classification or having adopted the conventional adamantine method of purifying to handle, after 6 hours, burning decrement is less than 99.90wt% through 1000 ℃ of calcinations for its diamond powder.
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