CN102391789B - Method for preparing nano diamond polishing solution - Google Patents
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- CN102391789B CN102391789B CN 201110244241 CN201110244241A CN102391789B CN 102391789 B CN102391789 B CN 102391789B CN 201110244241 CN201110244241 CN 201110244241 CN 201110244241 A CN201110244241 A CN 201110244241A CN 102391789 B CN102391789 B CN 102391789B
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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 addingthe 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 the machinery of its excellence, chemistry, light, electricity, thermal characteristics have broad application prospects 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 may be mutually to be bonded together the hard agglomeration that crystallization forms owing to carbon drop that the superhigh-temperature and-pressure of detonation forms in process of cooling, also may be owing to forming 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, so difficult is with 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 needs solution, 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, usually adopt chemical mechanical processing that Nano diamond is carried out surface modification, under the synergy of physics and chemical reagent, by regulating the hydrophilic and hydrophobic energy of particle surface, realize the purpose of stable dispersion in water.Chinese patent (application number 200410022936.0) " a kind of water-base nano diamond polishing liquid and manufacture method thereof ", its main component comprises: Nano diamond, properties-correcting agent, dispersion agent and/or hyper-dispersant, pH value conditioning agent, wetting conditioning agent, the additive with chemical action and deionized water; Its its manufacture method mainly comprises: 1. by 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; 3. add conditioning agent (wetting agent), dispersion stabilizer, pH value conditioning agent, the additive with chemical action and the deionized water of regulating workpiece and polishing fluid wetting property, 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, formed 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 conditioning agent: 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 it in the preparation method of the fairly simple nano diamond polishing liquid of water base middle stable suspersion and technique again.
The technical solution used in the present invention is the preparation method of a kind of nano diamond polishing liquid of invention, and its technological process is as follows:
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, take water as medium, carry out wet ball grinding, 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, for subsequent use;
C, diamond dispersed paste for subsequent use is carried out strong stirring, and add while stirring the concentrated acid liquid of 0.5-200 part weight quota in the diamond dispersed paste, carry out acid treatment, the time is 30-60 minute, and temperature is 20～100 ℃;
D, adopt centrifugal settling method to clean up the diamond dispersed paste after peracid treatment, the dispersion agent that adds again 1-10 part weight quota, regulate the pH value to 9-10 with the NaOH solution of 0.1mo l/L, then carry out classification, can obtain having in water 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 of several or whole combinations in oleic acid, tripoly phosphate sodium STPP, polyoxyethylene glycol, the sodium lauryl sulphate; When being several or whole combination of wherein two kinds, the consumption of each component is equal portions;
Described dispersion agent can be a kind of or two kinds of several or whole combinations among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80; When being several or whole combination of wherein two kinds, 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.
Preferred Ball-milling Time is 3～6 hours.
Best Ball-milling Time is 5 hours.
Temperature during best acid treatment 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 mechanical treatment, ball milling solution group, pickling impurity removal and three key steps of dispersion classification have been adopted, technique is fairly simple, both solve the agglomeration traits of Nano diamond, obtained again the nano diamond polishing liquid of Nano diamond at water base middle stable suspersion.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.Following explanation is to adopt the mode that exemplifies, but protection scope of the present invention should not be limited to this.
Embodiment one:
The preparation process of the present embodiment is as follows:
A, weight share is got commercially available diadust 10 grams that particle diameter is 0.5 μ m, (grinding aid can adopt oleic acid to polyoxyethylene glycol, tripoly phosphate sodium STPP, polyoxyethylene glycol, a kind of or two kinds of several or whole combinations in the sodium lauryl sulphate, this example adopts polyoxyethylene glycol to make grinding aid) 5 grams, (dispersion agent can adopt Sodium hexametaphosphate 99 to OP-10, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, a kind of or two kinds of several or whole combinations among the TW-80, 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, take water as medium, carry out wet ball grinding, 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, for subsequent use;
C, diamond dispersed paste for subsequent use is carried out strong stirring, and add 10 gram concentrated hydrochloric acids while stirring in the diamond dispersed paste, carry out acid treatment, the time is 30 minutes, and temperature is 70 ℃;
D, adopt centrifugal settling method to clean up the diamond dispersed paste after peracid treatment, (dispersion agent can adopt a kind of or two kinds of several or whole combinations among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80 to add 15 tripoly phosphate sodium STPPs that restrain again, this example adopts tripoly phosphate sodium STPP to make dispersion agent), regulate the pH value to 9 of slurry with the NaOH solution of 0.1mol/L, obtain the nano diamond polishing liquid that adamantine particle diameter is 10～100nm after the classification.
Embodiment two:
The preparation process of the present embodiment is as follows:
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, take water as medium, carry out wet ball grinding, 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, for subsequent use;
C, diamond dispersed paste for subsequent use is carried out strong stirring, and add the 10 gram vitriol oils while stirring in the diamond dispersed paste, carry out acid treatment, the time is 30 minutes, and temperature is 70 ℃;
D, the diamond dispersed paste after peracid treatment cleaned up (centrifugal settling method cleaning), the tripoly phosphate sodium STPP that adds 15 grams, regulate the pH value to 9 of slurry with the NaOH solution of 0.1mol/L, obtain the nano diamond polishing liquid that adamantine particle diameter is 10～100nm after the classification.
Embodiment three:
The preparation process of the present embodiment is as follows:
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, take water as medium, carry out wet ball grinding, 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, for subsequent use;
C, diamond dispersed paste for subsequent use is carried out strong stirring, and add 10 gram concentrated nitric acids while stirring in the diamond dispersed paste, carry out acid treatment, the time is 30 minutes, and temperature is 70 ℃;
D, the diamond dispersed paste after peracid treatment cleaned up (centrifugal settling method cleaning), the tripoly phosphate sodium STPP that adds 15 grams, regulate the pH value to 9 of slurry with the NaOH solution of 0.1mol/L, obtain 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 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 as follows:
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, take water as medium, carry out wet ball grinding, 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, for subsequent use;
C, diamond dispersed paste for subsequent use is carried out strong stirring, and add while stirring the concentrated acid liquid of 0.5-200 part weight quota in the diamond dispersed paste, carry out acid treatment, the time is 30-60 minute, and temperature is 20～100 ℃;
D, adopt centrifugal settling method to clean up the diamond dispersed paste after peracid treatment, the dispersion agent that adds again 1-10 part weight quota, regulate the pH value to 9-10 with the NaOH solution of 0.1mol/L, then carry out classification, can obtain having in water 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 is a kind of or two kinds of several or whole combinations in oleic acid, tripoly phosphate sodium STPP, polyoxyethylene glycol, the sodium lauryl sulphate; When being several or whole combination of wherein two kinds, the consumption of each component is equal portions;
Described dispersion agent is a kind of or two kinds of several or whole combinations among Sodium hexametaphosphate 99, tripoly phosphate sodium STPP, OP-10, sodium lauryl sulphate, cetyl trimethylammonium bromide, the TW-80; When being several or whole combination of wherein two kinds, the consumption of each component is equal portions;
Described concentrated acid liquid is 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: Ball-milling Time is 3～6 hours.
4. according to claim 1 or the preparation method of 3 described nano diamond polishing liquids, it is characterized in that: 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 acid treatment 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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