CN101050339A - Diamond polishing paste in high purity, and preparation method - Google Patents

Abstract

The invention relates to a high-purity nano-diamond polishing paste used for ultra-precision polishing of micro-holes of ceramic pins of optical fiber connectors and a preparation method thereof. A high-purity nano-diamond polishing paste is characterized in that it is prepared from diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin, and the weight percentage of each raw material is: diamond micropowder : 0.05～5%, wetting agent: 0.01～25%, surfactant: 0.1～5%, dispersion stabilizer: 0.1～50%, pH regulator: 0.1～1%, glycerin: 14～99.64%; The purity of the diamond micropowder is greater than or equal to 99.9%, and the particle size distribution is 100-200nm. The polishing paste has dual solubility, high polishing rate, good dispersion stability, moderate viscosity, and can effectively prevent the micro-hole surface of the polished ceramic pin. After testing, the insertion loss and return loss have reached the national standard Require.

Description

A kind of high-purity nano-diamond polishing paste and preparation method thereof

Technical field

The invention relates to a high-purity nano-diamond polishing paste for ultra-precision polishing on the surface of the inner hole of a ceramic ferrule of an optical fiber connector, belonging to the technical field of ultra-precision polishing on the inner surface of a microhole.

Background technique

In order to improve the surface quality of the inner hole of the ceramic ferrule of the optical fiber connector, foreign scholars, especially Japanese scholars, have conducted a lot of research on this. The current research in China mainly focuses on the ultra-fine grinding and polishing of the end face and outer surface of the optical fiber connector, while the research on the precision polishing of the inner hole of the ferrule is rarely involved. The surface finish and processing accuracy of the inner hole of the ferrule directly determine the optical performance of the fiber optic connector - insertion loss and return loss. If the flatness of the inner surface of the pin microhole does not meet the requirements or there are scratches on the surface, the optical performance of the optical fiber active connector will be significantly reduced. The key to determining the surface accuracy of the pin micro-bore is high-quality polishing paste products.

At present, general polishing products can only be used for ultra-fine grinding and polishing of the end face and outer surface of the optical fiber connector, and some manufacturers use abrasive paper or abrasive sheets to polish the end face. The inner hole processing of ceramic pins uses special equipment, which is to put many ceramic blanks on a very long steel wire with a fine tip, and the steel wire is stuck with diamond abrasives. Pass through the micropores of the green body, and gradually transition to the thick end, so as to achieve the purpose of polishing the inner hole of the ceramic pin. Therefore, the polishing paste product is required to have a certain viscosity, so as to ensure that the polishing paste adheres to the inner hole and has high efficiency; and the polishing paste is also required to have good dispersion stability and rheological properties, so that the polishing paste can be used on the ceramic pin The inner hole is evenly coated. Due to the low viscosity of the existing grinding and polishing liquid, it cannot be used for the precision machining of the inner hole of the ceramic ferrule of the optical fiber connector, and the key technology for the inner hole processing of the ceramic ferrule of the optical fiber connector is still controlled by foreign enterprises. The polishing paste used in polishing is mainly imported from Japan, and there is no related research report in China.

Therefore, it is necessary to develop a high-purity nano-diamond polishing paste with high purity, narrow particle size distribution, certain viscosity, good rheological properties, stable dispersion, high polishing efficiency, and suitable for ultra-precision polishing of the inner hole of the ceramic ferrule of the optical fiber connector.

Contents of Invention

The object of the invention is to provide a kind of high-purity nano-diamond polishing paste and preparation method thereof, the high-purity nano-diamond polishing paste obtained by the method has very high polishing rate, good dispersion stability, good rheological properties, and has Two solubility, and moderate viscosity.

In order to achieve the above object, the technical scheme of the present invention is: a kind of high-purity nano-diamond polishing paste, it is characterized in that it is prepared from diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin Components, the percentage by weight of each raw material is:

Diamond powder: 0.05~5%;

Wetting agent: 0.01～25%;

Surfactant: 0.1~5%;

Dispersion stabilizer: 0.1-50%;

pH regulator: 0.1~1%;

Glycerin: 14-99.64%;

The purity of the diamond micropowder is greater than or equal to 99.9%, and the particle size distribution is 100-200nm.

Diamond micropowder is obtained by crushing, purifying and grading diamonds synthesized by static pressure method.

The above-mentioned glycerol is proportioned by weight (14-99.64%) as an independent raw material, and it is not subordinate to the wetting agent or other dosage forms in the present invention. When glycerin is selected as the wetting agent, the total weight percentage of glycerin is the sum of 14-99.64% and 0.01-25%, and 0.01-25% by weight is used as the wetting agent.

Described wetting agent is ethanol, ethylene glycol, diethylene glycol, polyethylene glycol, 1,2 propylene glycol, 1,3 propylene glycol, 1,3 butanediol, 1,4 butanediol, glycerin , stearic acid, tartaric acid, citric acid, oxalic acid, or a mixture of any two or more (including any two), when any two or more (including any two) are mixed, it is an arbitrary proportion.

The surfactant is fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitol, polyoxyethylene fatty acid, polyoxypropylene mannitol, nonylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether , mannose, glucose, lactose or sucrose.

The dispersion stabilizer is: polyacrylic acid, polyvinyl alcohol, polyvinyl alcohol and polystyrene block copolymer, polyoxypropylene polyoxyethylene block polyether, polycarboxysiloxane polyethylene glycol two-stage Copolymer, methyl cellulose, methyl cellulose, ethyl cellulose sodium, polyethylene glycol, any one or a mixture of any two or more (including any two), any two or more (including any Two kinds) when mixing, be arbitrary proportioning.

The pH regulator is ammonia, sodium hydroxide, potassium hydroxide, ethanolamine, triethanolamine, acetic acid, oxalic acid, or a mixture of any two or more (including any two), any two or more (including When any two kinds) are mixed, it is an arbitrary proportioning.

The preparation method of above-mentioned a kind of high-purity nano-diamond polishing paste is characterized in that it comprises the steps:

1) According to the percentage by weight of each raw material: diamond powder: 0.05-5%, wetting agent: 0.01-25%, surfactant: 0.1-5%, dispersion stabilizer: 0.1-50%, pH regulator: 0.1～1%, glycerin: 14～99.64% select diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin raw material; The purity of described diamond micropowder is greater than or equal to 99.9%, and particle size distribution is 100-200nm;

2) Add nano-diamond micropowder into the wetting agent, and ultrasonicate for 5-30 minutes to fully wet;

3) Mix the wetted diamond micropowder with surfactant, add glycerin and dispersion stabilizer, ultrasonic treatment for 5-10min or mechanical stirring for 30min-60min to modify the diamond micropowder to obtain a mixed slurry;

4) Adding a pH adjuster to the mixed slurry to adjust the pH between 7 and 10, and ultrasonically or high-speed shearing to obtain a high-purity nano-diamond polishing paste.

The beneficial effects of the present invention are:

1, what the high-purity nano-diamond polishing paste of the present invention uses is that the nano-diamond micropowder with a purity of more than 99.9% is an abrasive material, and the weight percentage of nano-diamond micropowder in the high-purity nano-diamond polishing paste is 0.05～5%. If the content of the micro-powder is too small, the polishing rate will decrease; if the content of the nano-diamond micro-powder is too high, it will be difficult to disperse it evenly in the solvent, and a high-precision polishing surface cannot be obtained.

2. The particle size distribution of the nano-diamond micropowder used in the high-purity nano-diamond polishing paste of the present invention is between 100 and 200 nm. If the average particle diameter of the nano-diamond micropowder (i.e. abrasive) particles is greater than the above-mentioned range, the processed optical fiber will be connected The surface roughness of the micro-hole surface of the ceramic pin is increased, and scratches may occur.

3. The diamond micropowder is wetted by adding a wetting agent to reduce the surface tension of the micropowder, so that the diamond is easily dispersed in the paste carrier, so that the polishing paste has a self-lubricating function.

4. The high-purity nano-diamond polishing paste of the present invention has a certain viscosity (3500mpa.s～10000mpa.s), and the viscosity of the present invention is moderate; thereby ensuring that the polishing paste adheres to the inner hole of the ceramic pin and has high polishing efficiency; If the viscosity is too high, the polishing paste cannot be evenly coated on the inner wall of the micropores; if the viscosity is too small, the polishing paste cannot stay on the inner wall of the micropores for a sufficient time to reduce the polishing efficiency and cause waste of polishing paste.

5. The high-purity nano-diamond polishing paste of the present invention can be stored stably for more than 6 months. The polishing paste has good dispersion stability and rheological properties. On the one hand, the polishing paste can be evenly distributed in the inner hole of the ceramic pin, and on the other hand, it is beneficial to the storage of the polishing paste.

6. Experiments have proved that the acidity and alkalinity of the high-purity nano-diamond polishing paste of the present invention will have a greater impact on the dispersion stability of the polishing paste, and the pH value is controlled at 7-10, which has good dispersion stability.

7. The high-purity nano-diamond polishing paste of the present invention has both water and oil solubility. Its oil property makes the polishing paste have a good wetting effect on the surface of the polishing process, and its water property can reduce the polishing time, improve the polishing efficiency, and save diamond polishing paste; in addition, the polishing paste has two solubility, which is beneficial to the cleaning of the polishing surface.

Detailed ways

In order to better understand the present invention, the content of the present invention is further illustrated below in conjunction with the examples, but the content of the present invention is not limited to the following examples.

Reagents and medicines such as wetting agents, surfactants, dispersion stabilizers and pH regulators used in the method of the present invention are common reagents and medicines. The equipment used in the method of the present invention is commonly used known equipment.

Example 1:

Take 0.5g of diamond micropowder with a purity of 99.9% (particle size distribution is 100-200nm), add 5g of 1,4-butanediol, stir, ultrasonic 8min, fully wet. Add 0.3g of nonylphenol polyoxyethylene ether (OP-10) and 68.9g of glycerin to form a mixed solution. Add 25g of heated and dissolved polyethylene glycol to the mixed solution, stir it evenly, and sonicate for 10 minutes. Adjust the pH to 8 with triethanolamine, stir for 30 minutes, and then sonicate for 10 minutes to obtain a high-purity nano-diamond polishing paste. The polishing paste can be stored stably for 6 months, with a high shear viscosity of 4800mpa.s and a low shear viscosity of 8500mpa.s.

Example 2:

Take 2g of diamond micropowder with a purity of 99.9% (with a particle size distribution of 100-200nm), add 20g of ethanol, stir, and sonicate for 20 minutes to fully wet it. Add 1g of sorbitan fatty acid ester polyoxyethylene ether, add 31g of glycerin to form a mixed solution, then add 45g of polyvinyl alcohol that has been heated and dissolved, and stir while adding for 30 minutes. Add ethanolamine to adjust the pH to 9, and shear at a high speed of 10000r/min for 30min to obtain a high-purity nano-diamond polishing paste. The polishing paste can be stored stably for 6 months, with a high shear viscosity of 5800mpa.s and a low shear viscosity of 10500mpa.s.

Example 3:

Take 5g of diamond micropowder with a purity of 99.9% (with a particle size distribution of 100-200nm), add 1g of stearic acid, and ultrasonicate for 5 minutes to fully wet it. Add 0.5g of mannose and 68g of glycerin to form a mixed solution, then add 25g of polyoxypropylene polyoxyethylene block polyether, and stir for 60 minutes while adding. Add ammonia water to adjust the pH to 8, and mechanically stir for 30 minutes to obtain a high-purity nano-diamond polishing paste.

The high-purity diamond polishing paste prepared by Example 3 was stored for 6 months without sedimentation, and its high-shear viscosity was 6500mpa.s, and the low-shear viscosity was 9500mpa.s. Use this polishing paste to polish the surface of the micro inner hole of the ceramic ferrule of the optical fiber connector. There are no slip marks or black spots on the inner hole surface. After testing, the insertion loss and return loss meet the national standard requirements.

Example 4:

A kind of preparation method of above-mentioned high-purity nano-diamond polishing paste, it comprises the steps:

1) According to the percentage by weight of each raw material: diamond powder: 0.05%, wetting agent: 0.01%, surfactant: 0.1%, dispersion stabilizer: 0.1%, pH regulator: 0.1%, glycerin: 99.64% Diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin raw material; the purity of described diamond micropowder is 99.99%, and particle size distribution is 100～200nm; Described wetting agent is ethylene glycol , the surfactant is fatty alcohol polyoxyethylene ether, the dispersion stabilizer is polyacrylic acid, and the pH regulator is sodium hydroxide;

2) Add the nano-diamond micropowder into the wetting agent, stir, and ultrasonicate for 5 minutes to fully wet;

3) Mix the wetted diamond micropowder with a surfactant, add glycerin and a dispersion stabilizer, and ultrasonically treat the diamond micropowder for 5 minutes to modify the diamond micropowder to obtain a mixed slurry;

4) Add a pH adjuster to the mixed slurry to adjust the pH between 7 and 10, stir, and sonicate for 5 minutes to obtain a high-purity nano-diamond polishing paste.

Example 5:

A kind of preparation method of above-mentioned high-purity nano-diamond polishing paste, it comprises the steps:

1) According to the percentage by weight of each raw material: diamond powder: 5%, wetting agent: 25%, surfactant: 5%, dispersion stabilizer: 50%, pH regulator: 1%, glycerin: 14% Diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin raw materials; the purity of the diamond micropowder is 99.99%, and the particle size distribution is 100-200nm; the wetting agent is a Ethylene glycol, the surfactant is polyoxyethylene sorbitol, the dispersion stabilizer is: polyvinyl alcohol and polystyrene block copolymer, and the pH regulator is potassium hydroxide;

2) Add nano-diamond micropowder into the wetting agent, stir, and sonicate for 30 minutes to fully wet;

3) Mix the wetted diamond micropowder with a surfactant, add glycerin and a dispersion stabilizer, and ultrasonically treat the diamond micropowder for 10 minutes to modify the diamond micropowder to obtain a mixed slurry;

4) Add a pH adjuster to the mixed slurry to adjust the pH between 7 and 10, stir, and sonicate for 10 minutes to obtain a high-purity nano-diamond polishing paste.

Embodiment 6:

A kind of preparation method of above-mentioned high-purity nano-diamond polishing paste, it comprises the steps:

1) According to the percentage by weight of each raw material: diamond powder: 3%, wetting agent: 10%, surfactant: 2%, dispersion stabilizer: 20%, pH regulator: 0.5%, glycerin: 64.5% Diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin raw material; the purity of described diamond micropowder is greater than or equal to 99.96%, and particle size distribution is 100～200nm; Described wetting agent is poly Ethylene glycol, 1,2 propanediol, tartaric acid, citric acid and oxalic acid, polyethylene glycol, 1,2 propanediol, tartaric acid, citric acid and oxalic acid each account for 2%; the surfactant is polyoxyethylene fatty acid , the dispersion stabilizer is: polycarboxysiloxane polyethylene glycol two-stage copolymer, methyl cellulose, methyl cellulose and ethyl cellulose sodium, polycarboxysiloxane polyethylene glycol two Segment copolymer, methyl cellulose, methyl cellulose, sodium ethyl cellulose each account for 5%; the pH regulator is acetic acid, oxalic acid and sodium hydroxide, acetic acid, oxalic acid each account for 0.1%, and the hydrogen oxide Sodium at 0.3%;

2) Add nano-diamond micropowder into the wetting agent, stir, and ultrasonic for 10 minutes to fully wet;

3) Mix the wetted diamond micropowder with a surfactant, add glycerin and a dispersion stabilizer, and mechanically stir for 60 minutes to modify the diamond micropowder to obtain a mixed slurry;

4) Add a pH adjuster to the mixed slurry to adjust the pH between 7 and 10, and shear at a high speed for 10 minutes to obtain a high-purity nano-diamond polishing paste.

Claims (6)

1. a high-purity nano-diamond polishing paste is characterized in that it is prepared from diamond micropowder, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator and glycerin, and the weight percentages of each raw material are: Diamond powder: 0.05~5%; Wetting agent: 0.01～25%; Surfactant: 0.1~5%; Dispersion stabilizer: 0.1-50%; pH regulator: 0.1～1%; Glycerin: 14～99.64%; The purity of the diamond micropowder is greater than or equal to 99.9%, and the particle size distribution is 100-200nm. 2. a kind of high-purity nano-diamond polishing paste according to claim 1, is characterized in that: described wetting agent is ethanol, ethylene glycol, diethylene glycol acetal, polyethylene glycol, 1,2 Any one of propylene glycol, 1,3 propylene glycol, 1,3 butanediol, 1,4 butanediol, glycerin, stearic acid, tartaric acid, citric acid, oxalic acid or a mixture of any two or more, any two When mixing the above, it is an arbitrary proportioning ratio. 3. a kind of high-purity nano-diamond polishing paste according to claim 1, is characterized in that: described tensio-active agent is fatty alcohol polyoxyethylene ether, polyoxyethylene sorbitol, polyoxyethylene fatty acid, polyoxypropylene Mannitol, nonylphenol ethoxylates, sorbitan fatty acid ester ethoxylates, mannose, glucose, lactose or sucrose. 4. a kind of high-purity nano-diamond polishing paste according to claim 1 is characterized in that: described dispersion stabilizer is: polyacrylic acid, polyvinyl alcohol, polyvinyl alcohol and polystyrene block copolymer, polyvinyl alcohol Any one of oxypropylene polyoxyethylene block polyether, polycarboxysiloxane polyethylene glycol two-stage copolymer, methyl cellulose, methyl cellulose, ethyl cellulose sodium, polyethylene glycol A mixture of any two or more kinds, and when any two or more kinds are mixed, it is an arbitrary ratio. 5. a kind of high-purity nano-diamond polishing paste according to claim 1 is characterized in that: described pH adjuster is any in ammoniacal liquor, sodium hydroxide, potassium hydroxide, ethanolamine, triethanolamine, acetic acid, oxalic acid One or any two or more kinds of mixture, when any two or more kinds are mixed, it is an arbitrary proportion. 6. the preparation method of a kind of high-purity nano-diamond polishing paste as claimed in claim 1 is characterized in that it comprises the steps: 1) According to the percentage by weight of each raw material: diamond powder: 0.05-5%, wetting agent: 0.01-25%, surfactant: 0.1-5%, dispersion stabilizer: 0.1-50%, pH regulator: 0.1～1%, glycerin: 14～99.64% select diamond micropowder, wetting agent, surfactant, dispersion stabilizer, pH regulator and glycerin raw material; The purity of described diamond micropowder is greater than or equal to 99.9%, and particle size distribution is 100-200nm; 2) Add nano-diamond micropowder into the wetting agent, and ultrasonicate for 5-30 minutes to fully wet; 3) Mix the wetted diamond micropowder with surfactant, add glycerin and dispersion stabilizer, ultrasonic treatment for 5-10min or mechanical stirring for 30min-60min to modify the diamond micropowder to obtain a mixed slurry; 4) Adding a pH adjuster to the mixed slurry to adjust the pH between 7 and 10, and ultrasonically or high-speed shearing to obtain a high-purity nano-diamond polishing paste.