CN1439451A - Nano-diamond deagglomeration and grading method - Google Patents
Nano-diamond deagglomeration and grading method Download PDFInfo
- Publication number
- CN1439451A CN1439451A CN 02139764 CN02139764A CN1439451A CN 1439451 A CN1439451 A CN 1439451A CN 02139764 CN02139764 CN 02139764 CN 02139764 A CN02139764 A CN 02139764A CN 1439451 A CN1439451 A CN 1439451A
- Authority
- CN
- China
- Prior art keywords
- nano diamond
- acid
- diamond
- nano
- separating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a depolymerization and grading process method of a nano diamond aggregate, which mainly comprises the following process steps: 1) synchronously carrying out mechanical grinding and chemical modification on the nano-diamond, dispersing the nano-diamond into small aggregates with the average particle size of 7-200 nm, and 2) removing coarse nano-diamond and other components in the suspension; 3) adding a wetting agent, a surfactant, a dispersion stabilizer and a pH value regulator, and dispersing the diamond by adopting ultrasonic or (and) stirring; 4) grading the nano-diamond; the particle diameter of the composite material can be controllably adjusted between 7 and 200 nanometers, and the composite material can be widely applied to the fields of composite plating, (chemical mechanical) ultra-precise polishing, running-in (lubricating) oil, additives of wear-resistant materials and the like.
Description
Technical field: the invention belongs to the manufacture field of Nano diamond, its application relates to Ultraprecise polished, the compound plating of workpiece of artificial lens, the break-in oil of engine and the fields such as enhancing of material.
Background technology: the reason that the suspension of Nano diamond in water is difficult for stable existence mainly is because the surface of Nano diamond can be very high, in order to reduce the energy of system, often reach stable state between particle by drawing close mutually, also have, particle is thinner, distance between the particle is shorter, Van der Waals force between the particle impels them to reunite, in addition, effects such as the hydrogen bond on Nano diamond surface, the wet bridge of absorption also can cause the coalescent of particle, coalescent direct result is that the second particle particle diameter becomes big and sedimentation takes place, and causes the instability of system.
The reunion technology of separating of nano particle can be described as the prerequisite that nano-powder is effectively used.After the detonation synthesizing nano diamond is achieved success, carry out the research worker of application and development, with he (she) research emphasis be placed on it and separate aspect reunion technology and the stably dispersing in different systems thereof.Chigandva (G.A.Chigandva, V.A.Boonger, A.S.Chiganov.Colloid J.1993,55 (5): 774～775) use saturated AlCl
3Aqueous solution heat treated Nano diamond has obtained weight concentration and has been about 1% Nano diamond suspension, and its secondary granularity is in the hundreds of nanometers scope.Chen Pengwan (Chen Pengwan. the mechanism and the characteristic research [D] of the synthetic ultrafine diamond of blast. Beijing: Beijing Institute of Technology's doctorate paper, 1999) adopt water+Na respectively
3PO
4, ethanol, gelatin+Na
2CO
3Three kinds of medium dispersing nanometers of aqueous solution diamond, having obtained Nano diamond content is the colloidal sol of 0.75%wt, 0.35%wt, 0.9%wt, but leaves standstill after a period of time, Nano diamond takes place again to reunite and precipitation..Russia diamond center (the L V Agibalova of Co., Ltd, A PVoznyakovskii, V Yu Dolmatov.Sverkhtv.Mater., 1998 (4): 87～89.) scientist of (JSC DiamondCentre) uses ultrasonic power dispersing nanometer diamond in the aqueous solution, obtained stablizing the Nano diamond suspension more than 1 month, the average-size of aggregate is about 300nm.This center to Nano diamond the dispersion in non-aqueous system carried out studying (A P Voznyakovskii, V Yu Dolmatov, VV klyubin etc.Sverkhtv.Mater., 2000 (2): 64～71), adopt acetone, added the acetone of 5%wt water, and benzene, propyl alcohol etc. are as decentralized medium, and to defend diene modified Nano diamond surface effect best with poly-different, made and can stablize the Nano diamond suspension of depositing about 10 days.Up to the present, also nobody carries out the research of Nano diamond gradation aspect both at home and abroad.The application and the development of Nano diamond have seriously been restricted.
Summary of the invention: purpose of the present invention, be depolymerization and the classification problems that solves the Nano diamond aggregate, make that adamantine particle mean size is controlled between 7～200 nanometers in the Nano diamond suspension, and carry out fine graded, for its different purposes provide grade different Nano diamond products.
One, the depolymerization hard, soft aggregate of Nano diamond realizes through the following steps:
1) the employing air-flow is pulverized, high pressure liquid stream is pulverized or the mode of ball milling (vibratory milling and planetary mills), in nanometer
Add the surface chemical modification agent in the diamond, mechanical lapping and modification carried out synchronously, through pulverizing or
It is the aggregate of 7～200nm that mechanical lapping makes Nano diamond become particle mean size; Nano diamond with
The ratio of the gross weight of chemical modifier is 1: 0.001～0.5;
The XRD small angle scattering shows: the primary particle size as the Nano diamond of commodity selling exists
Between 1～60nm, be combined into average grain diameter at 2000nm with more weak active force between the primary particle
Aggregate, be to pulverize by above-mentioned three kinds of modes mentioning easily.Modifier is following
One or more combination: EDTA, citric acid, lauryl sodium sulfate, alkyl phenol polyoxy
Vinethene, tannic acid, sodium stearyl sulfate, calgon, sodium phosphate, titanate esters coupling
Agent, silane coupler, zircoaluminate coupling agent, oleic acid, enuatrol and glycerine.Like this, pulverize
After small agglomerates just more stable, be difficult to be gathered into once more the bigger aggregate of granularity, for following
Two steps provide advantage.
2) adopt centrifugation (in case of necessity, being aided with other machinery or chemical mode again), thick with after pulverizing
Particle Nano diamond and other Impurity removal reach the Nano diamond granularity to satisfy different application
The needs of purity, for the needs that transport or use from now on, also can it is true at a lower temperature
Empty dry, vacuum should be controlled at 10
2-10
4Pa, temperature should be strict controlled in 80～85 ℃ of scopes,
Must not surpass 85 ℃, otherwise can cause the change of Nano diamond surface characteristic;
3) add deionized water, wetting agent, surfactant, dispersion stabilizer and pH value conditioning agent, adopt
Ultrasonic or stirring disperses Nano diamond, makes and can stablize the Nano diamond suspension of depositing;
The interpolation of various additives is carried out in the following order, adds wetting agent earlier, makes the pH of solution
Value is controlled between 2～5, then, treated Nano diamond is put into, and adds an amount of again
Surfactant and dispersion stabilizer, last, add pH value conditioning agent, make the pH value of solution
Reach required value; The ratio of each component is as follows in the suspension:
Nano-diamond powder: 0.01～10.0%wt;
Wetting agent: its addition is controlled between 2～5 the pH value of dispersion;
Surfactant: 0.005～2%wt, and surfactant: Nano diamond=0.01: 1～1: 0.05;
Dispersion stabilizer: 0.01～2%wt, and dispersion stabilizer: Nano diamond=0.01: 1～1: 0.05;
PH value conditioning agent:, make the pH of Nano diamond suspension by regulating its kind and addition
Value is controlled between 3～11;
Deionized water: 85～99.6%wt.
Wetting agent is meant one or more the mixing in the following acid: hydrochloric acid, nitric acid, sulfuric acid, citric acid,
Tartaric acid, oxalic acid, acetic acid, salicylic acid, gallic acid and maleic acid;
Surfactant is used to improve the hydrophilicity and the surperficial charged situation of Nano diamond, and is said
Surfactant is triethanolamine, sodium phosphate, waterglass, dodecyl sodium sulfate, detergent alkylate sulphur
Acid sodium, lauryl sodium sulfate, calgon, sulfosalicylic acid, glycerine, 1, the 4-butanediol,
Phthalic acid, tannic acid, octadecenic acid, sodium oleate, 1-diglycol ethylene, EDTA and ten
One or more combinations in the SOS;
Dispersion stabilizer is meant polymeric dispersant and hyper-dispersant, and said polymeric dispersant is poly-second
Enol, carboxymethyl cellulose, sodium carboxymethylcellulose, polyethylene glycol, NPE, poly-
The combination of one or more in vinylpyrrolidone, the desugar condensation sodium lignin sulfonate; Hyper-dispersant is
Refer to the water miscible hyper-dispersant of a class, as gathering two sections copolymers of carboxyl siloxanes polyethylene glycol etc.
Said pH value conditioning agent is ammoniacal liquor, NaOH, potassium hydroxide, monoethanolamine, triethanolamine
In one or more.
The method that air-flow is pulverized is to use two strands of compressed air with equal pressure and flow to enter in line from both sides and pulverizes the district, material (Nano diamond and chemical modifier) then enters by mechanism and pulverizes the district, during two bursts of high velocity air head-on collisions, the Nano diamond granule impact in the mixed airflow is pulverized and modification.
It is earlier Nano diamond and surface modifier to be made into suspension that high pressure liquid stream is pulverized, then, by booster it is pressurizeed, when pressure reaches desirable value (more than the 200Mpa), spray to the diamond target plate at a high speed by injector, with its pulverizing and refinement, this process is capable of circulation carries out, until reaching required particle diameter.
Ball milling method refers to vibromill and planetary mills.Two, stage division:
Separate under the prerequisite of fully disperseing of reuniting at above-mentioned Nano diamond, adopt film pipe separate mode, by the classification of cross-flow separation equipment, after the classification, average particulate diameter is controllable adjustment between 7～200 nanometers.
Film pipe cross-flow hierarchy system is adopted in the classification of Nano diamond, block fenestra for preventing thick nano diamond particles, there is the pulse recoiling device in this system, can be in classification process towards the opposite direction of permeate flow, the fluid pressure pulse of implementation cycle property outside in recoil, thus guarantee the high efficiency of the not blocked and classification of fenestra.During the native system classification, applied pressure is about 2.5～3.0bar, and liquid flowing speed is adjustable between 4.0～8.0m/s.During classification, the concentration of Nano diamond should be controlled between 0.01～10%wt.
The Nano diamond suspension that adopts method of the present invention to make, even particle size distribution, dispersion stabilization is fabulous, can deposit 6 to 12 months, and tangible sedimentation does not take place.After cross-flow classification technique provided by the invention classification, particle size distribution obviously narrows down, and the technology stability of product increases substantially.Find when utilizing ZETASIZER3000HS to carry out granularity Detection that its average grain diameter is 7 to 200nm, the absolute value of the surperficial electrokinetic potential of Nano diamond can be controlled in more than the 35mv.
Description of drawings: Fig. 1: the size distribution of Nano diamond before the classification
Fig. 2: the size distribution after the cross-flow classification
Fig. 3: not classified Nano diamond suspension
Fig. 4: the size distribution after the cross-flow classification
The specific embodiment: utilize above-mentioned described method and step, the following example is set forth
Embodiment 1: adopt the air-flow disintegrating apparatus, with Nano diamond, the compound of enuatrol and glycerine (anharmonic ratio of Nano diamond and modifier total amount is 1: 0.05) adds simultaneously from charging aperture, the Nano diamond aggregate is smashed and in time stable by the mode of mechanical crushing and chemical modification synchronous effect, centrifugal removal particle diameter surpasses the coarse granule of 500nm, it is sneaked into to regulate the pH value with the oxalic acid wetting agent be in 3 the deionized water, add surfactant sodium phosphate and stable dispersant polyethylene glycol, wherein the addition of sodium phosphate is 0.1%wt, the weight ratio of itself and Nano diamond is 0.05: 1, the addition of polyethylene glycol is 0.05%wt, the anharmonic ratio of polyethylene glycol and Nano diamond is 0.025: 1, and be 9 with the pH value that ammoniacal liquor is regulated suspension, ultrasonic dispersion got final product in 10 minutes, can make weight concentration is 2%, average grain diameter is the diamond suspension (size distribution is seen accompanying drawing 1) of 166.5nm, after the film classification, can get narrower particle size distribution, particle mean size is in the diamond suspension (size distribution is seen accompanying drawing 2) of 98.5nm.
Embodiment 2: adopt liquid stream disintegrating apparatus, Nano diamond and sodium stearyl sulfate are prepared into suspension, the weight concentration of Nano diamond is 1%, the percentage by weight of sodium stearyl sulfate is 0.05%, the weight ratio of sodium stearyl sulfate and Nano diamond 0.05: 1, by booster it is pressurizeed, when pressure reaches 200Mpa, spray to the diamond target plate at a high speed by injector, the Nano diamond aggregate smashed and in time stable, then, centrifugation, remove the coarse granule that particle diameter surpasses 500nm, it is sneaked into citric acid, and to regulate the pH value be in 3.5 the deionized water, add surfactant oleic acid and stable dispersant polyvinyl alcohol, the addition of oleic acid is 0.1%wt, the addition of polyvinyl alcohol is 0.05%wt, oleic acid: Nano diamond is 0.1: 1, polyvinyl alcohol: Nano diamond is 0.05: 1, regulating the pH value with NaOH is 10, and ultrasonic dispersion 15 minutes makes the diamond suspension that particle mean size is 98.7nm (seeing accompanying drawing 3), after the cross-flow classification, can get narrower particle size distribution, particle mean size is in the diamond suspension (seeing accompanying drawing 4) of 82.1nm.
Claims (10)
1. adamantine separating reunited and stage division, it is characterized in that:
(1) separate the method for reunion:
1) the employing air-flow is pulverized, high pressure liquid stream is pulverized or the mode of ball milling, adds the surface in Nano diamond
Chemical modifier, through pulverize or mechanical lapping to make Nano diamond become particle mean size be 7～200nm's
Aggregate, the ratio of the gross weight of Nano diamond and chemical modifier are 1: 0.001～0.5;
2) thick nano diamond particles and other Impurity removal after the employing centrifugation will be pulverized;
3) add deionized water, wetting agent, surfactant, dispersion stabilizer and pH value conditioning agent, adopt
Ultrasonic or stirring disperses Nano diamond, makes and can stablize the Nano diamond suspension of depositing;
(2) stage division
Fully disperse the Nano diamond suspension of back concentration 0.01～10%wt with separating to reunite, adopt the film pipe
Separate mode, by the classification of cross-flow separation equipment, applied pressure is 2.5～3.0bar, liquid flowing speed is
4.0～8.0m/s, after the classification, average particulate diameter is controllable adjustment between 7～200 nanometers.
2. separating of a kind of Nano diamond according to claim 1 reunited and stage division, it is characterized in that: the interpolation of the various additives of step 3 is in proper order: add wetting agent earlier, the pH value of solution is controlled between 2～5, then, treated Nano diamond is put into, added surfactant and dispersion stabilizer again, last, add pH value conditioning agent, the pH value of solution is reached between 3～11.
3. separating of a kind of Nano diamond according to claim 1 reunited and stage division, and it is characterized in that: the diamond suspension that step 3 makes consists of:
Nano-diamond powder: 0.01～10.0%wt;
Surfactant: 0.005～2%wt, and surfactant: Nano diamond=0.011～1: 0.05;
Dispersion stabilizer: 0.01～2%wt, and dispersion stabilizer: Nano diamond=0.01: 1～1: 0.05;
Deionized water: 85～99.6%wt.
4. reunite and stage division according to separating of the described a kind of Nano diamond of claim 1, it is characterized in that: air-flow is pulverized and is: use two strands of compressed air with equal pressure and flow to enter in line from both sides and pulverize the district, material (Nano diamond and chemical modifier) then enters by mechanism and pulverizes the district, during two bursts of high velocity air head-on collisions, the Nano diamond granule impact in the mixed airflow is pulverized and modification.
High pressure liquid stream is pulverized: earlier Nano diamond and surface modifier are made into suspension, then, by booster it is pressurizeed, when pressure reaches desirable value (more than the 200Mpa), spray to the diamond target plate at a high speed by injector, with its pulverizing and refinement, this process is capable of circulation carries out, until reaching required particle diameter.
Ball milling method refers to vibromill and planetary mills.
5. separating of a kind of Nano diamond according to claim 1 reunited and stage division, it is characterized in that:: the chemical modifier that is adopted is following said one or more combination: EDTA, citric acid, lauryl sodium sulfate, APES, tannic acid, sodium stearyl sulfate, calgon, sodium phosphate, polyethylene glycol, titanate coupling agent, silane coupler, zircoaluminate coupling agent, oleic acid, enuatrol, glycerine.
6. separating of a kind of Nano diamond according to claim 1 reunited and stage division, it is characterized in that: wetting agent is meant one or more the mixing in the following acid: hydrochloric acid, nitric acid, sulfuric acid, citric acid, tartaric acid, oxalic acid, acetic acid, salicylic acid, gallic acid and maleic acid.
7. separating of a kind of Nano diamond according to claim 1 reunited and stage division, it is characterized in that: surfactant is triethanolamine, sodium phosphate, waterglass, dodecyl sodium sulfate, neopelex, lauryl sodium sulfate, calgon, sulfosalicylic acid, glycerine, 1, one or more combinations in 4-butanediol, phthalic acid, tannic acid, octadecenic acid, sodium oleate, 1-diglycol ethylene, EDTA and the sodium stearyl sulfate.
8. separating of a kind of Nano diamond according to claim 1 reunited and stage division, it is characterized in that: dispersion stabilizer is meant polymer dispersed and hyper-dispersant, and polymeric dispersant is one or more the combination in polyvinyl alcohol, carboxymethyl cellulose, sodium carboxymethylcellulose, polyethylene glycol, NPE, polyvinylpyrrolidone, the desugar condensation sodium lignin sulfonate; Hyper-dispersant is meant the water miscible hyper-dispersant of a class, as gathering two sections copolymers of carboxyl siloxanes polyethylene glycol etc.
9. separating of a kind of Nano diamond according to claim 1 reunited and stage division, and it is characterized in that: pH value conditioning agent is one or more in ammoniacal liquor, NaOH, potassium hydroxide, monoethanolamine, the triethanolamine.
10. separating of a kind of Nano diamond according to claim 1 reunited and stage division, it is characterized in that: film pipe cross-flow hierarchy system is adopted in classification, there is the pulse recoiling device in this system, can be in classification process towards the opposite direction of permeate flow, the recoil of the fluid pressure pulse of implementation cycle property outside in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02139764 CN1203915C (en) | 2002-11-18 | 2002-11-18 | Nano-diamond deagglomeration and grading method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02139764 CN1203915C (en) | 2002-11-18 | 2002-11-18 | Nano-diamond deagglomeration and grading method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1439451A true CN1439451A (en) | 2003-09-03 |
| CN1203915C CN1203915C (en) | 2005-06-01 |
Family
ID=27793424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02139764 Expired - Lifetime CN1203915C (en) | 2002-11-18 | 2002-11-18 | Nano-diamond deagglomeration and grading method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1203915C (en) |
Cited By (52)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331581C (en) * | 2004-05-14 | 2007-08-15 | 深圳市金刚源新材料发展有限公司 | Surface treatment method for Nano diamond fine particles added to lubricant |
| CN100388967C (en) * | 2004-12-02 | 2008-05-21 | 鸿富锦精密工业（深圳）有限公司 | Particle dispersing method and its device |
| US20090283718A1 (en) * | 2006-06-05 | 2009-11-19 | Central Glass Co., Ltd. | Method for preparing fluorinated nanodiamond liquid dispersion |
| CN101007252B (en) * | 2006-01-24 | 2010-11-10 | 河南省联合磨料磨具有限公司 | Apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond and its producing method |
| CN101898761A (en) * | 2010-07-13 | 2010-12-01 | 天津大学 | Method for Dispersing Detonation Nanodiamonds in Liquid Phase |
| CN101628728B (en) * | 2009-01-17 | 2011-04-06 | 汉寿金诚研磨材有限公司 | White alundum hyperfine abrasive micropowder preparation method |
| CN1957253B (en) * | 2004-05-20 | 2011-06-01 | 清美化学股份有限公司 | Method for evaluating quality of abrasive particles, method for polishing glass and abrasive composition for polishing glass |
| US20110232199A1 (en) * | 2007-10-15 | 2011-09-29 | Central Glass Company, Limited | Process for Production of Dispersion of Fluorinated Nano Diamond |
| CN102321396A (en) * | 2011-06-02 | 2012-01-18 | 杭州正博新型建筑材料有限公司 | Process for depolymerizing and purifying high-performance and environment-friendly phenylalanine ammonia lyase (PAL) flame-retardant material |
| CN102320565A (en) * | 2011-09-08 | 2012-01-18 | 苏州衡业新材料科技有限公司 | Single preparation technology who disperses the complex component nano material with universality |
| CN102344135A (en) * | 2010-08-03 | 2012-02-08 | 财团法人工业技术研究院 | Surface modified nanodiamond and method of forming the same |
| CN102391789A (en) * | 2011-08-19 | 2012-03-28 | 永州皓志稀土材料有限公司 | A kind of preparation method of nano-diamond polishing liquid |
| CN101489928B (en) * | 2006-06-05 | 2012-05-23 | 中央硝子株式会社 | Preparation method of fluorinated nano-diamond dispersion liquid |
| CN102489383A (en) * | 2011-12-02 | 2012-06-13 | 宝丰恒瑞新材料有限公司 | Dispersing agent used for silicon carbide micro powder water overflow grading and application method thereof |
| CN102601745A (en) * | 2012-03-22 | 2012-07-25 | 湖南大学 | Preparation method of resin binder diamond abrasive product used for accurate grinding |
| CN101433786B (en) * | 2007-11-15 | 2012-08-29 | 赢创德固赛有限责任公司 | Method of fractionating oxidic nanoparticles by crossflow membrane filtration |
| CN102753734A (en) * | 2010-01-22 | 2012-10-24 | 爱德有限公司 | Composite plating solution having diamond fine particles dispersed therein and method for producing same |
| CN102744399A (en) * | 2012-06-20 | 2012-10-24 | 兰州理工大学 | Dispersing method for nanometer copper powder aggregates |
| CN103254799A (en) * | 2013-05-29 | 2013-08-21 | 陈玉祥 | Hydrophilic diamond-suspended grinding and polishing solution and preparation method thereof |
| US8609188B2 (en) | 2010-07-01 | 2013-12-17 | Industrial Technology Research Institute | Surface modification of nano-diamonds and manufacturing method thereof |
| GB2503643A (en) * | 2012-04-27 | 2014-01-08 | Univ Newcastle | Method for separation of diamond particle clusters |
| US8658578B2 (en) | 2010-12-29 | 2014-02-25 | Industrial Technology Research Institute | Lubricating oil composition and method for manufacturing the same |
| CN104031724A (en) * | 2014-05-30 | 2014-09-10 | 成都天成鑫钻纳米科技股份有限公司 | Lithium-based lubricating grease containing nano-diamond and preparation method of lubricating grease |
| CN104031560A (en) * | 2013-03-07 | 2014-09-10 | 天津市乾宇超硬科技有限公司 | Water-based diamond polishing solution used for crystal processing |
| CN104059716A (en) * | 2014-07-02 | 2014-09-24 | 宝捷润滑油镇江有限公司 | Anti-oxidation automobile lubricating oil and preparation method thereof |
| CN104085888A (en) * | 2014-07-17 | 2014-10-08 | 长沙矿冶研究院有限责任公司 | Method for preparing detonation nanometer diamond dispersion |
| CN104128096A (en) * | 2014-07-15 | 2014-11-05 | 江苏凯孚碳素科技有限公司 | Ultrasound-assisted method and device for extracting nano-particles from nano-powder organic solvent suspension liquid |
| CN104388996A (en) * | 2014-10-30 | 2015-03-04 | 苏州禾川化学技术服务有限公司 | Black hole liquid and preparation method thereof |
| CN104532016A (en) * | 2014-12-23 | 2015-04-22 | 西安石油大学 | Cobalt leaching method of cobalt-leached composite acid based on synthetic polycrystalline diamond composite sheet |
| CN105153942A (en) * | 2015-07-28 | 2015-12-16 | 郑州磨料磨具磨削研究所有限公司 | Control method for grain size of abrasive material in nano diamond polishing solution |
| CN105271173A (en) * | 2015-09-25 | 2016-01-27 | 郑州华晶金刚石股份有限公司 | Preparation process of nano carbon crystals |
| CN105293469A (en) * | 2015-09-25 | 2016-02-03 | 郑州华晶金刚石股份有限公司 | Process for preparing nanometer diamond alkene |
| CN105419308A (en) * | 2015-12-08 | 2016-03-23 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Diamond-alkene reinforced and toughened PA6 modified plastic and preparation method thereof |
| CN105692609A (en) * | 2016-03-10 | 2016-06-22 | 天津迪麦爱科科技有限公司 | Preparation method of nano-diamond with relatively good liquid suspension stability |
| CN105969481A (en) * | 2016-04-29 | 2016-09-28 | 中国科学院宁波材料技术与工程研究所 | Carbon nanomaterial-containing lubricating oil additive and preparation method thereof |
| CN106147617A (en) * | 2015-04-28 | 2016-11-23 | 天津诺邦科技有限公司 | A kind of water base polishing fluid of polycrystalline diamond and preparation method thereof |
| WO2017050263A1 (en) * | 2015-09-25 | 2017-03-30 | 郑州华晶金刚石股份有限公司 | Novel nanocarbon crystal |
| CN106607180A (en) * | 2016-12-30 | 2017-05-03 | 广东工业大学 | Separation method of nanoparticles |
| CN106905754A (en) * | 2017-03-20 | 2017-06-30 | 河南省联合磨料磨具有限公司 | A kind of super hydrophobic coating anti-wear additive and preparation method thereof, super-hydrophobic wear-resistant paint and super-hydrophobic transparent coating |
| CN107001049A (en) * | 2014-11-26 | 2017-08-01 | 纳米资源有限公司 | The separation method of detonation Nano diamond |
| CN107505239A (en) * | 2017-08-28 | 2017-12-22 | 河南克拉钻石有限公司 | A kind of detection method of Nano diamond granularity |
| CN108126808A (en) * | 2017-11-21 | 2018-06-08 | 包头稀土研究院 | High pressure liquid stream fuel pulverizing plant and its milling method |
| CN108219678A (en) * | 2016-12-21 | 2018-06-29 | 蓝思科技（长沙）有限公司 | A kind of diamond grinding fluid and preparation method thereof |
| CN109108524A (en) * | 2018-08-30 | 2019-01-01 | 桂林电子科技大学 | A kind of diamond-nano mattisolda Heat Conduction Material and preparation method thereof |
| CN110684959A (en) * | 2019-10-30 | 2020-01-14 | 中国科学院深圳先进技术研究院 | Diamond gradient coating and its preparation method and application |
| CN110713820A (en) * | 2019-10-29 | 2020-01-21 | 河南联合精密材料股份有限公司 | Preparation method of hydrophobic modified diamond abrasive |
| CN111926351A (en) * | 2020-08-07 | 2020-11-13 | 浙江集工阀门有限公司 | Composite plating process for ball valve |
| CN111962052A (en) * | 2020-08-07 | 2020-11-20 | 浙江集工阀门有限公司 | Composite plating process for nickel-based alloy |
| CN113717691A (en) * | 2021-08-31 | 2021-11-30 | 昆山捷纳电子材料有限公司 | Preparation method and application of polyethylene polyamine modified diamond composite abrasive particles |
| CN114590807A (en) * | 2020-12-03 | 2022-06-07 | 深圳先进技术研究院 | Preparation method of nano-diamond dispersed aqueous solution with small particle size |
| CN114806501A (en) * | 2022-04-28 | 2022-07-29 | 浙江奥首材料科技有限公司 | Modified diamond powder, preparation method and application thereof, and polishing solution containing modified diamond powder |
| CN116589928A (en) * | 2023-05-17 | 2023-08-15 | 耐博检测技术(武汉)有限公司 | Super-dispersed diamond suspension and preparation method thereof |
-
2002
- 2002-11-18 CN CN 02139764 patent/CN1203915C/en not_active Expired - Lifetime
Cited By (74)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331581C (en) * | 2004-05-14 | 2007-08-15 | 深圳市金刚源新材料发展有限公司 | Surface treatment method for Nano diamond fine particles added to lubricant |
| CN1957253B (en) * | 2004-05-20 | 2011-06-01 | 清美化学股份有限公司 | Method for evaluating quality of abrasive particles, method for polishing glass and abrasive composition for polishing glass |
| CN101813692B (en) * | 2004-05-20 | 2012-08-29 | 清美化学股份有限公司 | Method for polishing glass and abrasive composition for polishing glass |
| CN100388967C (en) * | 2004-12-02 | 2008-05-21 | 鸿富锦精密工业（深圳）有限公司 | Particle dispersing method and its device |
| CN101007252B (en) * | 2006-01-24 | 2010-11-10 | 河南省联合磨料磨具有限公司 | Apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond and its producing method |
| CN101489928B (en) * | 2006-06-05 | 2012-05-23 | 中央硝子株式会社 | Preparation method of fluorinated nano-diamond dispersion liquid |
| US20090283718A1 (en) * | 2006-06-05 | 2009-11-19 | Central Glass Co., Ltd. | Method for preparing fluorinated nanodiamond liquid dispersion |
| US8790541B2 (en) * | 2006-06-05 | 2014-07-29 | Central Glass Co., Ltd. | Method for preparing fluorinated nanodiamond liquid dispersion |
| US20110232199A1 (en) * | 2007-10-15 | 2011-09-29 | Central Glass Company, Limited | Process for Production of Dispersion of Fluorinated Nano Diamond |
| US8961631B2 (en) * | 2007-10-15 | 2015-02-24 | Central Glass Company, Limited | Process for production of dispersion of fluorinated nano diamond |
| CN101433786B (en) * | 2007-11-15 | 2012-08-29 | 赢创德固赛有限责任公司 | Method of fractionating oxidic nanoparticles by crossflow membrane filtration |
| CN101628728B (en) * | 2009-01-17 | 2011-04-06 | 汉寿金诚研磨材有限公司 | White alundum hyperfine abrasive micropowder preparation method |
| CN102753734B (en) * | 2010-01-22 | 2015-02-11 | 爱德有限公司 | Composite plating solution having diamond fine particles dispersed therein and method for producing same |
| CN102753734A (en) * | 2010-01-22 | 2012-10-24 | 爱德有限公司 | Composite plating solution having diamond fine particles dispersed therein and method for producing same |
| US8609188B2 (en) | 2010-07-01 | 2013-12-17 | Industrial Technology Research Institute | Surface modification of nano-diamonds and manufacturing method thereof |
| CN101898761B (en) * | 2010-07-13 | 2012-06-27 | 天津大学 | Method for dispersing detonation method nano-diamond in liquid phase |
| CN101898761A (en) * | 2010-07-13 | 2010-12-01 | 天津大学 | Method for Dispersing Detonation Nanodiamonds in Liquid Phase |
| CN102344135A (en) * | 2010-08-03 | 2012-02-08 | 财团法人工业技术研究院 | Surface modified nanodiamond and method of forming the same |
| US8658578B2 (en) | 2010-12-29 | 2014-02-25 | Industrial Technology Research Institute | Lubricating oil composition and method for manufacturing the same |
| CN102321396A (en) * | 2011-06-02 | 2012-01-18 | 杭州正博新型建筑材料有限公司 | Process for depolymerizing and purifying high-performance and environment-friendly phenylalanine ammonia lyase (PAL) flame-retardant material |
| CN102391789A (en) * | 2011-08-19 | 2012-03-28 | 永州皓志稀土材料有限公司 | A kind of preparation method of nano-diamond polishing liquid |
| CN102391789B (en) * | 2011-08-19 | 2013-10-16 | 湖南皓志新材料股份有限公司 | A kind of preparation method of nano-diamond polishing liquid |
| CN102320565A (en) * | 2011-09-08 | 2012-01-18 | 苏州衡业新材料科技有限公司 | Single preparation technology who disperses the complex component nano material with universality |
| CN102489383A (en) * | 2011-12-02 | 2012-06-13 | 宝丰恒瑞新材料有限公司 | Dispersing agent used for silicon carbide micro powder water overflow grading and application method thereof |
| CN102601745B (en) * | 2012-03-22 | 2014-06-11 | 湖南大学 | Preparation method of resin binder diamond abrasive product used for accurate grinding |
| CN102601745A (en) * | 2012-03-22 | 2012-07-25 | 湖南大学 | Preparation method of resin binder diamond abrasive product used for accurate grinding |
| GB2503643A (en) * | 2012-04-27 | 2014-01-08 | Univ Newcastle | Method for separation of diamond particle clusters |
| CN102744399A (en) * | 2012-06-20 | 2012-10-24 | 兰州理工大学 | Dispersing method for nanometer copper powder aggregates |
| CN102744399B (en) * | 2012-06-20 | 2014-08-13 | 兰州理工大学 | Dispersing method for nanometer copper powder aggregates |
| CN104031560A (en) * | 2013-03-07 | 2014-09-10 | 天津市乾宇超硬科技有限公司 | Water-based diamond polishing solution used for crystal processing |
| CN104031560B (en) * | 2013-03-07 | 2015-11-25 | 天津市乾宇超硬科技有限公司 | For the water-based diamond polishing liquid of crystal pro cessing |
| CN103254799A (en) * | 2013-05-29 | 2013-08-21 | 陈玉祥 | Hydrophilic diamond-suspended grinding and polishing solution and preparation method thereof |
| CN104031724A (en) * | 2014-05-30 | 2014-09-10 | 成都天成鑫钻纳米科技股份有限公司 | Lithium-based lubricating grease containing nano-diamond and preparation method of lubricating grease |
| CN104031724B (en) * | 2014-05-30 | 2016-02-17 | 成都天成鑫钻纳米科技股份有限公司 | Containing the lithium soap grease and preparation method thereof of Nano diamond |
| CN104059716A (en) * | 2014-07-02 | 2014-09-24 | 宝捷润滑油镇江有限公司 | Anti-oxidation automobile lubricating oil and preparation method thereof |
| CN104128096A (en) * | 2014-07-15 | 2014-11-05 | 江苏凯孚碳素科技有限公司 | Ultrasound-assisted method and device for extracting nano-particles from nano-powder organic solvent suspension liquid |
| CN104085888A (en) * | 2014-07-17 | 2014-10-08 | 长沙矿冶研究院有限责任公司 | Method for preparing detonation nanometer diamond dispersion |
| CN104085888B (en) * | 2014-07-17 | 2016-05-11 | 长沙矿冶研究院有限责任公司 | The preparation method of detonation nanodiamond liquid dispersion |
| CN104388996A (en) * | 2014-10-30 | 2015-03-04 | 苏州禾川化学技术服务有限公司 | Black hole liquid and preparation method thereof |
| CN107001049B (en) * | 2014-11-26 | 2019-11-22 | 纳米资源有限公司 | The separation method of detonation Nano diamond |
| CN107001049A (en) * | 2014-11-26 | 2017-08-01 | 纳米资源有限公司 | The separation method of detonation Nano diamond |
| CN104532016A (en) * | 2014-12-23 | 2015-04-22 | 西安石油大学 | Cobalt leaching method of cobalt-leached composite acid based on synthetic polycrystalline diamond composite sheet |
| CN106147617A (en) * | 2015-04-28 | 2016-11-23 | 天津诺邦科技有限公司 | A kind of water base polishing fluid of polycrystalline diamond and preparation method thereof |
| CN105153942A (en) * | 2015-07-28 | 2015-12-16 | 郑州磨料磨具磨削研究所有限公司 | Control method for grain size of abrasive material in nano diamond polishing solution |
| CN105293469A (en) * | 2015-09-25 | 2016-02-03 | 郑州华晶金刚石股份有限公司 | Process for preparing nanometer diamond alkene |
| CN105271173A (en) * | 2015-09-25 | 2016-01-27 | 郑州华晶金刚石股份有限公司 | Preparation process of nano carbon crystals |
| CN105271173B (en) * | 2015-09-25 | 2017-12-12 | 郑州华晶金刚石股份有限公司 | A kind of preparation technology of nanometer carbon crystal |
| WO2017050263A1 (en) * | 2015-09-25 | 2017-03-30 | 郑州华晶金刚石股份有限公司 | Novel nanocarbon crystal |
| CN105419308A (en) * | 2015-12-08 | 2016-03-23 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Diamond-alkene reinforced and toughened PA6 modified plastic and preparation method thereof |
| CN105419308B (en) * | 2015-12-08 | 2018-01-30 | 郑州人造金刚石及制品工程技术研究中心有限公司 | A kind of diamond alkene activeness and quietness PA6 modified plastics and preparation method thereof |
| CN105692609B (en) * | 2016-03-10 | 2019-10-25 | 天津迪麦爱科科技有限公司 | The method of the preferable Nano diamond preparation of liquid suspension stability |
| CN105692609A (en) * | 2016-03-10 | 2016-06-22 | 天津迪麦爱科科技有限公司 | Preparation method of nano-diamond with relatively good liquid suspension stability |
| CN105969481A (en) * | 2016-04-29 | 2016-09-28 | 中国科学院宁波材料技术与工程研究所 | Carbon nanomaterial-containing lubricating oil additive and preparation method thereof |
| CN105969481B (en) * | 2016-04-29 | 2019-01-11 | 中国科学院宁波材料技术与工程研究所 | Lube oil additive and preparation method thereof containing nano-carbon material |
| CN108219678A (en) * | 2016-12-21 | 2018-06-29 | 蓝思科技（长沙）有限公司 | A kind of diamond grinding fluid and preparation method thereof |
| CN108219678B (en) * | 2016-12-21 | 2020-09-04 | 蓝思科技（长沙）有限公司 | Diamond grinding fluid and preparation method thereof |
| CN106607180B (en) * | 2016-12-30 | 2019-02-22 | 广东工业大学 | A kind of separation method of nanoparticles |
| CN106607180A (en) * | 2016-12-30 | 2017-05-03 | 广东工业大学 | Separation method of nanoparticles |
| CN106905754A (en) * | 2017-03-20 | 2017-06-30 | 河南省联合磨料磨具有限公司 | A kind of super hydrophobic coating anti-wear additive and preparation method thereof, super-hydrophobic wear-resistant paint and super-hydrophobic transparent coating |
| CN107505239A (en) * | 2017-08-28 | 2017-12-22 | 河南克拉钻石有限公司 | A kind of detection method of Nano diamond granularity |
| CN108126808A (en) * | 2017-11-21 | 2018-06-08 | 包头稀土研究院 | High pressure liquid stream fuel pulverizing plant and its milling method |
| CN109108524A (en) * | 2018-08-30 | 2019-01-01 | 桂林电子科技大学 | A kind of diamond-nano mattisolda Heat Conduction Material and preparation method thereof |
| CN110713820B (en) * | 2019-10-29 | 2021-02-09 | 河南联合精密材料股份有限公司 | Preparation method of hydrophobic modified diamond abrasive |
| CN110713820A (en) * | 2019-10-29 | 2020-01-21 | 河南联合精密材料股份有限公司 | Preparation method of hydrophobic modified diamond abrasive |
| CN110684959B (en) * | 2019-10-30 | 2022-02-15 | 中国科学院深圳先进技术研究院 | Diamond gradient coating and preparation method and application thereof |
| CN110684959A (en) * | 2019-10-30 | 2020-01-14 | 中国科学院深圳先进技术研究院 | Diamond gradient coating and its preparation method and application |
| CN111962052A (en) * | 2020-08-07 | 2020-11-20 | 浙江集工阀门有限公司 | Composite plating process for nickel-based alloy |
| CN111926351A (en) * | 2020-08-07 | 2020-11-13 | 浙江集工阀门有限公司 | Composite plating process for ball valve |
| CN111962052B (en) * | 2020-08-07 | 2022-09-02 | 浙江集工阀门有限公司 | Composite plating process for nickel-based alloy |
| CN114590807A (en) * | 2020-12-03 | 2022-06-07 | 深圳先进技术研究院 | Preparation method of nano-diamond dispersed aqueous solution with small particle size |
| CN113717691A (en) * | 2021-08-31 | 2021-11-30 | 昆山捷纳电子材料有限公司 | Preparation method and application of polyethylene polyamine modified diamond composite abrasive particles |
| CN114806501A (en) * | 2022-04-28 | 2022-07-29 | 浙江奥首材料科技有限公司 | Modified diamond powder, preparation method and application thereof, and polishing solution containing modified diamond powder |
| CN114806501B (en) * | 2022-04-28 | 2023-04-28 | 浙江奥首材料科技有限公司 | Modified diamond powder, preparation method, application and polishing solution containing modified diamond powder |
| CN116589928A (en) * | 2023-05-17 | 2023-08-15 | 耐博检测技术(武汉)有限公司 | Super-dispersed diamond suspension and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1203915C (en) | 2005-06-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1203915C (en) | Nano-diamond deagglomeration and grading method | |
| CN1560161A (en) | Water-based nano diamond polishing solution and preparation method thereof | |
| CN101230210A (en) | Preparation method of organically modified silicate mineral clay | |
| CN101654862B (en) | Preparation method of waterborne nano slurry | |
| CN104085888A (en) | Method for preparing detonation nanometer diamond dispersion | |
| CN110713820B (en) | Preparation method of hydrophobic modified diamond abrasive | |
| CN101891972B (en) | Method for producing chemical fiber titanium dioxide by surface coating of common titanium dioxide (TiO2) in solvent phase | |
| CN115449417B (en) | Naphthalene compound dispersing agent, activated nano-primary pulp containing naphthalene compound dispersing agent and preparation method of naphthalene compound dispersing agent | |
| CN108822579A (en) | A kind of modification shell powder preparation method with good dispersion | |
| CN111253790B (en) | Preparation method of thin composite nano flake coating | |
| CN113549345A (en) | Preparation method and system of titanium dioxide for plastics | |
| CN113956048B (en) | Preparation method for silicon carbide ceramic powder by slip casting, injection and extrusion molding | |
| CN112127211B (en) | Stone paper, calcium carbonate slurry and preparation method thereof | |
| CN117089223A (en) | Barite powder and preparation method and application thereof | |
| CN115572625B (en) | Compound dispersing agent, activated nano-primary pulp containing compound dispersing agent and preparation method of activated nano-primary pulp | |
| CN110773301A (en) | Special ground calcium carbonate powder for stone paper, preparation method and stone paper | |
| CN115584287B (en) | Naphthalene dispersant for preparing nano hydrocarbon fuel and application thereof | |
| CN114426781B (en) | Superfine heavy calcium carbonate and preparation method thereof | |
| CN111777987B (en) | A kind of grinding suspending agent and its preparation method and application, grinding agent | |
| CN112552708A (en) | Dispersible barium sulfate composite powder for water-based paint and preparation method thereof | |
| CN113321282B (en) | Concrete mixing plant water circulation system and water treatment method thereof | |
| CN1273383C (en) | Synthesis method of single dispersing nano-cerium ion modified mesoporous silicon oxide material | |
| CN1297613C (en) | Surface modified nano calcium carbonate for corrosion resistance paint | |
| CN111808438B (en) | Grinding aid special for calcium carbonate powder and using method thereof | |
| CN115259735A (en) | Viscosity-reducing phase-change material for concrete and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: KINGRAY NEW MATERIALS SCIENCE AND TECHNOLOGY Co.,Ltd. Assignor: Changsha Research Institute of Mining and Metallurgy Contract fulfillment period: 2007.12.6 to 2022.11.17 Contract record no.: 2008430000021 Denomination of invention: Method for sorting and disgregating nano diamonds Granted publication date: 20050601 License type: Exclusive license Record date: 20081113 |
|
| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.12.6 TO 2022.11.17; CHANGE OF CONTRACT Name of requester: KINGRAY NEW MATERIAL SCIENCE + TECHNOLOGY CO., LTD Effective date: 20081113 |
|
| EC01 | Cancellation of recordation of patent licensing contract |
Assignee: KINGRAY NEW MATERIALS SCIENCE AND TECHNOLOGY Co.,Ltd. Assignor: Changsha Research Institute of Mining and Metallurgy Contract record no.: 2008430000021 Date of cancellation: 20131121 |
|
| LICC | Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20030903 Assignee: CHENGDU TIANCHENG XINZUAN NANO TECHNOLOGY CO.,LTD. Assignor: CHANGSHA RESEARCH INSTITUTE OF MINING AND METALLURGY Co.,Ltd. Contract record no.: 2014430000001 Denomination of invention: Method for sorting and disgregating nano diamonds Granted publication date: 20050601 License type: Exclusive License Record date: 20140120 |
|
| EE01 | Entry into force of recordation of patent licensing contract | ||
| CX01 | Expiry of patent term |
Granted publication date: 20050601 |
|
| CX01 | Expiry of patent term |