CN102391789A - Method for preparing nano diamond polishing solution - Google Patents
Method for preparing nano diamond polishing solution Download PDFInfo
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- CN102391789A CN102391789A CN2011102442417A CN201110244241A CN102391789A CN 102391789 A CN102391789 A CN 102391789A CN 2011102442417 A CN2011102442417 A CN 2011102442417A CN 201110244241 A CN201110244241 A CN 201110244241A CN 102391789 A CN102391789 A CN 102391789A
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Abstract
The invention discloses a method for preparing a nano diamond polishing solution, relating to the technical field of preparation of non rare earth polishing materials. The method comprises the following technical processes of: placing diamond micro powder, a grinding aid, a dispersing agent and deionized water into a ball mill, and carrying out wet ball milling to form initial slurry; then adding the deionized water into the initial slurry and washing diamond dispersion slurry out; adding concentrated acid to the diamond dispersion slurry for carrying out acid treatment; cleaning the diamond dispersion slurry subjected to acid treatment, then adding the dispersing agent to the diamond dispersion slurry, and carrying out classification to form the nano diamond polishing solution. The method has the characteristics that not only the aggregation problem of nano diamond can be solved, but also the nano diamond can be ensued to stably float in a water base; the process is simpler, and the like. The nano diamond polishing solution prepared by the method is suitable for precisely grinding and polishing liquid crystal conductive glass, plane optical glass, an optical sphere, optical lens glass, an optical filter, a filter window and a glass plate substrate and is particularly suitable for grinding and polishing spherical glass made of a soft material.
Description
Technical field
The present invention relates to the non-rare-earth polishing material preparing technical field in the new material technology field, be applied to the preparation method in precise finiss and polishing technology field, particularly a kind of nano diamond polishing liquid.
Background technology
Nano diamond has the dual nature of nano material and superhard material concurrently, and its excellent machinery, chemistry, light, electricity, thermal property have wide application prospect in fields such as running in oil, composite deposite, Ultraprecise polished, chemistry/medical science.The coarse grain footpath of single of Nano diamond particle is 60nm only, and median size is 8～12nm, however general commercial Nano diamond median size reach more than the 2 μ m, the most slightly reach 10 μ m, degree of aggregation is up to 200～1000.The existence of coacervate possibly be in process of cooling, to be bonded together the hard agglomeration that crystallization forms each other owing to carbon drop that the superhigh-temperature and-pressure of detonation forms, also maybe be owing to form the inferior hard agglomeration that oxo bridge key etc. forms in the aftertreatment drying and dehydrating process of detonation product between particle.The hard agglomeration of Nano diamond occupies sizable ratio, and has certain texture tendency, therefore quite is difficult to depolymerization.Hard agglomeration is restricting the application development of Nano diamond; The excellent properties of Nano diamond is almost lost; Therefore the depolymerization of hard agglomeration is the matter of utmost importance that the Nano diamond application need solves, and also is the major issue that the nano diamond polishing liquid preparation needs solution.In the prior art; To the depolymerization of the hard agglomeration of Nano diamond, adopt chemical mechanical processing that Nano diamond is carried out surface-treated usually, under the synergy of physics and chemical reagent; Through regulating the hydrophilic and hydrophobic ability of particle surface, be implemented in the purpose of stable dispersion in the water.Chinese patent (application number 200410022936.0) " a kind of water-base nano diamond polishing liquid and method of manufacture thereof ", its staple comprises: Nano diamond, properties-correcting agent, dispersion agent and/or hyper-dispersant, pH value regulator, wetting regulator, the additive with chemical action and deionized water; Its its method of manufacture mainly comprises: 1. through mechanochemical modification, the coacervate of Nano diamond is dispersed into the little aggregate that mean particle size is 20～100nm, 2. removes coarse particles and other impurity in the suspension-s; 3. add regulator (wetting agent), dispersion stabilizer, pH value regulator, additive and the deionized water of regulating workpiece and polishing fluid wetting property with chemical action, ultrasonic or/and dispersed with stirring.Chinese patent (application number 200510030024.2) " water-based diamond polishing liquid and preparation method thereof " and for example; This disclosure of the Invention a kind of water-based diamond polishing liquid, form by the component of following parts by weight: special diadust: 0.001-10, dispersion agent: 0.02-4 part, suspension agent: 0.01-5 part, suspension aids: 0.01-1 part, PH regulator: 0.1-1.5 part, sanitas: 0.1-0.5 part, deionized water: 60-99 part; The water-based diamond polishing liquid quality product of this invention preparation is consistent, good stability.
Summary of the invention
Technical problem to be solved by this invention provides a kind ofly can either solve the agglomeration traits of Nano diamond, can make the preparation method of the fairly simple nano diamond polishing liquid of its stable suspersion and technology in water base again.
The technical scheme that the present invention taked is the preparation method of a kind of nano diamond polishing liquid of invention, and its technological process is following:
A, weight share are got 100 parts of diadust 5-20 part, grinding aid 2-8 part, dispersion agent 2-8 part, the deionized waters that particle diameter is 0.1-1 μ m; Insert in the ball mill; With water is medium, carries out wet ball grinding, and the ball milling time is 1～10 hour; Drum's speed of rotation is 200～500r/min, becomes initial slurry;
B, get the deionized water of 600 parts of weight quota again, join in the initial slurry in the ball mill, clean out the diamond dispersed paste, subsequent use;
C, subsequent use diamond dispersed paste is carried out brute force stir, and in the diamond dispersed paste, add the concentrated acid liquid of 0.5-200 part weight quota while stirring, carry out s.t., the time is 30-60 minute, and temperature is 20～100 ℃;
D, adopt centrifugal settling method to clean up diamond dispersed paste after peracid treatment; The dispersion agent that adds 1-10 part weight quota again; Regulate the pH value to 9-10 with the NaOH solution of 0.1mo l/L; Carry out classification then, can obtain in water, having the nano diamond polishing liquid of height suspension stability, wherein adamantine weight percentage is 0.1～10, adamantine particle diameter is 10～100nm;
Described grinding aid can be a kind of or two kinds or several kinds or the whole combination in oleic acid, tripoly phosphate sodium STPP, polyoxyethylene glycol, the sodium lauryl sulphate; When being wherein two kinds or several kinds or whole combination, the consumption of each component is equal portions;
Described dispersion agent can be a kind of or two kinds or several kinds or the whole combination among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80; When being wherein two kinds or several kinds or whole combination, the consumption of each component is equal portions;
Described concentrated acid liquid can be the combination of a kind of of concentrated hydrochloric acid, the vitriol oil, concentrated nitric acid or two kinds or three kinds; When being the combination of wherein two kinds or three kinds, the consumption of each component is equal portions.
The particle diameter of preferred diadust is 0.3-0.5 μ m.
The preferred ball milling time is 3～6 hours.
The best ball milling time is 5 hours.
Temperature during best s.t. is 70 ℃.
Best drum's speed of rotation is 300r/min.
Above-mentioned used weight quota unit can be gram or kilogram or ton, also can be other weight unit.
The preparation method of nano diamond polishing liquid of the present invention; The method of applied chemistry treat mechanically; Adopted that ball milling is separated, pickling impurity removal and three key steps of dispersion classification; Technology is fairly simple, has both solved the agglomeration traits of Nano diamond, has obtained the nano diamond polishing liquid of Nano diamond stable suspersion in water base again.
Embodiment
Below in conjunction with embodiment, the present invention is further described.Following explanation is to adopt the mode of giving an example, but protection scope of the present invention should not be limited to this.
Embodiment one:
The preparation process of present embodiment is following:
A, weight share are got commercially available diadust 10 gram that particle diameter is 0.5 μ m, (grinding aid can adopt a kind of or two kinds or several kinds or the whole combinations in oleic acid, tripoly phosphate sodium STPP, polyoxyethylene glycol, the sodium lauryl sulphate to polyoxyethylene glycol; This example adopts polyoxyethylene glycol to make grinding aid) 5 grams, (dispersion agent can adopt a kind of or two kinds or several kinds or the whole combinations among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80 to OP-10; This example adopts OP-10 to make dispersion agent) 5 grams, deionized water 100 grams (that is: 100ml); Insert in the ball grinder of high energy ball mill; With water is medium, carries out wet ball grinding, and the ball milling time is 5 hours; Drum's speed of rotation is 300r/min, becomes initial slurry;
B, get 600 gram (that is: 600ml) deionized waters again, join in the initial slurry in the ball grinder, clean out the diamond dispersed paste, subsequent use;
C, subsequent use diamond dispersed paste is carried out brute force stir, and in the diamond dispersed paste, add 10 gram concentrated hydrochloric acids while stirring, carry out s.t., the time is 30 minutes, and temperature is 70 ℃;
D, adopt centrifugal settling method to clean up diamond dispersed paste after peracid treatment; Add again 15 the gram tripoly phosphate sodium STPP (dispersion agent can adopt a kind of or two kinds or several kinds or the whole combinations among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80; This example adopts tripoly phosphate sodium STPP to make dispersion agent); NaOH solution with 0.1mol/L is regulated pH value of slurry to 9, obtains the nano diamond polishing liquid that adamantine particle diameter is 10～100nm after the classification.
Embodiment two:
The preparation process of present embodiment is following:
A, weight share are got commercially available diadust 10 grams, polyoxyethylene glycol 5 grams, OP-10 5 grams, deionized water 100 grams (that is: 100ml) that particle diameter is 0.5 μ m; Insert in the ball grinder of high energy ball mill; With water is medium, carries out wet ball grinding, and the ball milling time is 5 hours; Drum's speed of rotation is 300r/min, becomes initial slurry;
B, get 600 gram (that is: 600ml) deionized waters again, join in the initial slurry in the ball grinder, clean out the diamond dispersed paste, subsequent use;
C, subsequent use diamond dispersed paste is carried out brute force stir, and in the diamond dispersed paste, add the 10 gram vitriol oils while stirring, carry out s.t., the time is 30 minutes, and temperature is 70 ℃;
D, the diamond dispersed paste after peracid treatment is cleaned up (centrifugal settling method cleaning); The tripoly phosphate sodium STPP that adds 15 grams; NaOH solution with 0.1mol/L is regulated pH value of slurry to 9, obtains the nano diamond polishing liquid that adamantine particle diameter is 10～100nm after the classification.
Embodiment three:
The preparation process of present embodiment is following:
A, weight share are got commercially available diadust 10 grams, polyoxyethylene glycol 5 grams, OP-10 5 grams, deionized water 100 grams (that is: 100ml) that particle diameter is 0.5 μ m; Insert in the ball grinder of high energy ball mill; With water is medium, carries out wet ball grinding, and the ball milling time is 5 hours; Drum's speed of rotation is 300r/min, becomes initial slurry;
B, get 600 gram (that is: 600ml) deionized waters again, join in the initial slurry in the ball grinder, clean out the diamond dispersed paste, subsequent use;
C, subsequent use diamond dispersed paste is carried out brute force stir, and in the diamond dispersed paste, add 10 gram concentrated nitric acids while stirring, carry out s.t., the time is 30 minutes, and temperature is 70 ℃;
D, the diamond dispersed paste after peracid treatment is cleaned up (centrifugal settling method cleaning); The tripoly phosphate sodium STPP that adds 15 grams; NaOH solution with 0.1mol/L is regulated pH value of slurry to 9, obtains the nano diamond polishing liquid that adamantine particle diameter is 10～100nm after the classification.
Use the preparation method of nano diamond polishing liquid of the present invention; The nano diamond polishing liquid of preparation; Be applicable to the precise finiss polishing of conductive liquid crystal glass, plane opticglass, optical spherical surface, optical lens glass, spectral filter, spectral window and glass disc substrate, be specially adapted to the grinding and polishing of the spherical glass of softwood matter.
Claims (6)
1. the preparation method of a nano diamond polishing liquid is characterized in that technological process is following:
A, weight share are got 100 parts of diadust 5-20 part, grinding aid 2-8 part, dispersion agent 2-8 part, the deionized waters that particle diameter is 0.1-1 μ m; Insert in the ball mill; With water is medium, carries out wet ball grinding, and the ball milling time is 1～10 hour; Drum's speed of rotation is 200～500r/min, becomes initial slurry;
B, get the deionized water of 600 parts of weight quota again, join in the initial slurry in the ball mill, clean out the diamond dispersed paste, subsequent use;
C, subsequent use diamond dispersed paste is carried out brute force stir, and in the diamond dispersed paste, add the concentrated acid liquid of 0.5-200 part weight quota while stirring, carry out s.t., the time is 30-60 minute, and temperature is 20～100 ℃;
D, adopt centrifugal settling method to clean up diamond dispersed paste after peracid treatment; The dispersion agent that adds 1-10 part weight quota again; Carry out classification; Can obtain in water, having the nano diamond polishing liquid of height suspension stability, wherein adamantine weight percentage is 0.1～10, adamantine particle diameter is 10～100nm;
Described grinding aid can be a kind of or two kinds or several kinds or the whole combination in oleic acid, tripoly phosphate sodium STPP, polyoxyethylene glycol, the sodium lauryl sulphate; When being wherein two kinds or several kinds or whole combination, the consumption of each component is equal portions;
Described dispersion agent can be a kind of or two kinds or several kinds or the whole combination among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80; When being wherein two kinds or several kinds or whole combination, the consumption of each component is equal portions;
Described concentrated acid liquid can be the combination of a kind of of concentrated hydrochloric acid, the vitriol oil, concentrated nitric acid or two kinds or three kinds; When being the combination of wherein two kinds or three kinds, the consumption of each component is equal portions.
2. the preparation method of nano diamond polishing liquid according to claim 1, it is characterized in that: the particle diameter of diadust is 0.3-0.5 μ m.
3. the preparation method of nano diamond polishing liquid according to claim 1, it is characterized in that: the ball milling time is 3～6 hours.
4. according to the preparation method of claim 1 or 3 described nano diamond polishing liquids, it is characterized in that: the ball milling time is 5 hours.
5. the preparation method of nano diamond polishing liquid according to claim 1, it is characterized in that: the temperature during s.t. is 70 ℃.
6. the preparation method of nano diamond polishing liquid according to claim 1, it is characterized in that: drum's speed of rotation is 300r/min.
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| CN103923606A (en) * | 2014-04-04 | 2014-07-16 | 湖南省美程陶瓷科技有限公司 | Steatite ceramic compound grinding aid and preparation method thereof |
| CN104059539A (en) * | 2014-06-04 | 2014-09-24 | 武汉三灵科技产业股份有限公司 | High-efficiency diamond polishing agent and preparation method thereof |
| CN104592936A (en) * | 2015-01-04 | 2015-05-06 | 和县科嘉阀门铸造有限公司 | Nano silicon carbide grinding paste for sealing surface of valve and preparation method of nano silicon dioxide grinding paste |
| CN104650741A (en) * | 2015-01-05 | 2015-05-27 | 杭州大和热磁电子有限公司 | Grinding and polishing paste for high-purity aluminum oxide ceramics |
| CN104261404B (en) * | 2014-09-29 | 2016-03-30 | 中国科学技术大学 | The preparation of the super-dispersed nano diamond water-sol |
| CN105496001A (en) * | 2015-12-22 | 2016-04-20 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Nano carbon crystal toothbrush and manufacturing method |
| CN105524558A (en) * | 2016-01-25 | 2016-04-27 | 河南省联合磨料磨具有限公司 | Polishing solution additive and preparation method thereof |
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| CN106381071A (en) * | 2016-08-31 | 2017-02-08 | 常熟市光学仪器有限责任公司 | Polishing solution used for processing optical glass |
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| 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 |
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| CN104059539A (en) * | 2014-06-04 | 2014-09-24 | 武汉三灵科技产业股份有限公司 | High-efficiency diamond polishing agent and preparation method thereof |
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| CN104592936A (en) * | 2015-01-04 | 2015-05-06 | 和县科嘉阀门铸造有限公司 | Nano silicon carbide grinding paste for sealing surface of valve and preparation method of nano silicon dioxide grinding paste |
| CN104650741A (en) * | 2015-01-05 | 2015-05-27 | 杭州大和热磁电子有限公司 | Grinding and polishing paste for high-purity aluminum oxide ceramics |
| CN105496001A (en) * | 2015-12-22 | 2016-04-20 | 郑州人造金刚石及制品工程技术研究中心有限公司 | Nano carbon crystal toothbrush and manufacturing method |
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| 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 |
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| CN107049804A (en) * | 2017-01-21 | 2017-08-18 | 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 skin care milk containing nanometer carbon crystal and preparation method thereof |
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| CN112480825A (en) * | 2020-12-10 | 2021-03-12 | 河南联合精密材料股份有限公司 | Diamond polishing solution for rough polishing of silicon carbide wafer and preparation method thereof |
| CN116005227A (en) * | 2021-10-22 | 2023-04-25 | 湖南盛强力新材料科技有限公司 | Preparation method and application of nano diamond and nickel composite coating |
| 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 |
| CN114686171A (en) * | 2022-05-19 | 2022-07-01 | 中国振华集团云科电子有限公司 | Suspensible diamond grinding fluid and preparation process thereof |
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