CN101050339A - Diamond polishing paste in high purity, and preparation method - Google Patents
Diamond polishing paste in high purity, and preparation method Download PDFInfo
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- CN101050339A CN101050339A CNA2007100521988A CN200710052198A CN101050339A CN 101050339 A CN101050339 A CN 101050339A CN A2007100521988 A CNA2007100521988 A CN A2007100521988A CN 200710052198 A CN200710052198 A CN 200710052198A CN 101050339 A CN101050339 A CN 101050339A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1481—Pastes, optionally in the form of blocks or sticks
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
This invention relates to a method for preparing polishing paste containing high-purity nanoscale diamond for precision polishing of the small inner pores of ceramic ferrule used in optical fiber connector. The polishing paste is prepared from: diamond micropowder 0.05-5 wt.%, wetting agent 0.01-25 wt.%, surfactant 0.1-5 wt.%, dispersion stabilizer 0.1-50 wt.%, pH regulator 0.1-1 wt.%, and glycerol 14-99.64 wt.%. The purity of the diamond micropowder is greater than or equal to 99.9%, and the particle sizes are 100-200 nm. The polishing paste is amphipathic, and has such advantages as high polishing speed, high dispersion stability, and appropriate viscosity. The polishing paste can effectively prevent the generation of small inner pores on the surface of polished ceramic ferrule.
Description
Technical field
The present invention relates to a kind of diamond polishing paste in high purity that is used for the Ultraprecise polished usefulness of joints of optical fibre ceramic contact pin bore surface, belong to the Ultraprecise polished technical field of micropore internal surface.
Background technology
In order to improve the surface quality of joints of optical fibre ceramic contact pin endoporus, external especially Japanese scholar has carried out a large amount of research to this.Domestic present research is primarily aimed at the fine abrasive and the polishing of end surface of optical fiber connector and outside surface, and precise polished research seldom relates to the contact pin endoporus.The surface smoothness of contact pin endoporus and working accuracy have directly determined the optical property of the joints of optical fibre---insert loss and return loss.If contact pin micropore internal surface planeness does not reach requirement or there is cut in the surface, the obvious decline of fiber active linker optical property.And the key of decision contact pin micro-inner-hole surface accuracy is exactly high-quality rubbing paste product.
At present, general polishing product mainly can only carry out the fine abrasive and the polishing of end surface of optical fiber connector and outside surface, and the producer that also has uses pouncing paper or abrasive sheet that end face is polished.And the endoporus of ceramic contact pin processing use is special equipment, it is that many ceramic bodies are through on the very long steel wire that has fine tip degree, be stained with diamond abrasive on the steel wire, the first micropore of its thin end by base substrate, and gradually to the butt end transition, to reach the purpose of polishing ceramic contact pin endoporus.Therefore, need the rubbing paste product to have certain viscosity, thereby guarantee that rubbing paste sticks, has higher efficient at endoporus; But also require rubbing paste that good dispersion stabilization and rheological property are arranged, make rubbing paste evenly coated at the ceramic contact pin endoporus.Existing grinding and polishing liquid is too low owing to viscosity, and can't be used for joints of optical fibre ceramic contact pin endoporus precision sizing, and the gordian technique of joints of optical fibre ceramic contact pin endoporus processing is also controlled by overseas enterprise.Polish employed rubbing paste mainly from Japanese import, the domestic correlative study report that there is no.
Therefore, develop a kind of purity height, narrow particle size distribution, have certain viscosity, good rheological property, stably dispersing, polishing efficiency height, to be fit to the Ultraprecise polished diamond polishing paste in high purity of joints of optical fibre ceramic contact pin endoporus very necessary.
Summary of the invention
The purpose of this invention is to provide a kind of diamond polishing paste in high purity and preparation method thereof, the diamond polishing paste in high purity that this method obtains have very high polishing speed, good dispersion stabilization, preferably rheological property, have two dissolubilities and modest viscosity.
To achieve these goals, technical scheme of the present invention is: a kind of diamond polishing paste in high purity, it is characterized in that it is that feedstock production forms by diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine, the shared weight percent of each raw material is:
Diadust: 0.05～5%;
Wetting agent: 0.01～25%;
Tensio-active agent: 0.1～5%;
Dispersion stabilizer: 0.1～50%;
PH regulator agent: 0.1～1%;
Glycerine: 14～99.64%;
The purity of described diadust is more than or equal to 99.9%, and size-grade distribution is 100～200nm.
Diadust is with gained after the fragmentation of static pressure method synthetic diamond process, purification, the stage treatment.
Above-mentioned glycerine is to carry out weight percent proportioning (14～99.64%) by a kind of independently raw material, and it is not subordinated to wetting agent or other formulation in the present invention.When selecting glycerine to make wetting agent as wetting agent, then the total shared weight percent of add-on of glycerine is 14～99.64% and 0.01～25% sum, and shared weight percent 0.01～25% is as wetting agent.
Described wetting agent is ethanol, ethylene glycol, glycol ether, polyoxyethylene glycol, 1,2 propylene glycol, 1,3 propylene glycol, 1,3 butyleneglycols, 1, in 4 butyleneglycols, glycerine, stearic acid, oilstone acid, citric acid, the oxalic acid any one or any mixing that (contains any two kinds) more than two kinds, any when (containing any two kinds) more than two kinds and mixing, be any proportioning.
Described tensio-active agent is fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitol, polyoxyethylene fatty acid, polyoxypropylene N.F,USP MANNITOL, polyoxyethylene nonylphenol ether, sorbitan fatty acid ester Soxylat A 25-7, seminose, glucose, lactose or sucrose.
Described dispersion stabilizer is: any one in polyacrylic acid, polyvinyl alcohol, polyvinyl alcohol and polystyrene block copolymer, polyoxyethylene polyoxypropylene block type polyethers, poly-carboxyl siloxanes polyoxyethylene glycol two sections multipolymers, methylcellulose gum, the methylcellulose gum that contracts, ethyl cellulose sodium, the polyoxyethylene glycol or any mixing of (containing any two kinds) more than two kinds, any when (containing any two kinds) more than two kinds and mixing, be any proportioning.
Described pH regulator agent is any one or any mixing that (contains any two kinds) more than two kinds in ammoniacal liquor, sodium hydroxide, potassium hydroxide, thanomin, trolamine, acetate, the oxalic acid, any when (containing any two kinds) more than two kinds and mixing, be any proportioning.
The preparation method of above-mentioned a kind of diamond polishing paste in high purity is characterized in that it comprises the steps:
1) by the shared weight percent of each raw material be: diadust: 0.05～5%, wetting agent: 0.01～25%, tensio-active agent: 0.1～5%, dispersion stabilizer: 0.1～50%, pH regulator agent: 0.1～1%, glycerine: 14～99.64% choose diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine raw material; The purity of described diadust is more than or equal to 99.9%, and size-grade distribution is 100～200nm;
2) the Nano diamond micro mist is joined in the wetting agent, ultrasonic 5～30min, fully wetting;
3) diadust of getting after wetting mixes with tensio-active agent, adds glycerine and dispersion stabilizer, and ultrasonication 5～10min or mechanical stirring 30min～60min make the diadust modification, obtain mixed pulp;
4) add pH value conditioning agent in mixed pulp and regulate pH between 7～10, ultrasonic or high speed shear gets diamond polishing paste in high purity.
The invention has the beneficial effects as follows:
1, diamond polishing paste in high purity of the present invention uses is that purity is that Nano diamond micro mist more than 99.9% is abrasive material, the weight percentage of Nano diamond micro mist is 0.05～5% in the diamond polishing paste in high purity, if the Nano diamond powder content is very few, polishing speed will reduce; If the Nano diamond powder content is too high, be difficult to it is evenly dispersed in the solvent, can not get high-precision polished surface.
2, the employed Nano diamond micro mist of diamond polishing paste in high purity of the present invention size-grade distribution is between 100～200nm, if Nano diamond micro mist (being abrasive material) particulate median size is greater than above-mentioned scope, the surfaceness on processed joints of optical fibre ceramic contact pin micro-inner-hole surface is strengthened, and might produce cut.
3, diadust is wetting by adding wetting agent, reduces the surface tension of micro mist, and diamond is dispersed in the paste carrier easily, makes rubbing paste have self-lubricating function.
4, diamond polishing paste in high purity of the present invention has certain viscosity (3500mpa.s～10000mpa.s), modest viscosity of the present invention; Thereby guarantee that rubbing paste sticks, has very high polishing efficiency at the ceramic contact pin endoporus; Viscosity is too big, and rubbing paste can't be evenly coated at the micropore inwall; Viscosity is too little, and rubbing paste can't stop time enough and reduce polishing efficiency at the micropore inwall, causes the rubbing paste waste.
5, diamond polishing paste in high purity of the present invention can be stablized and deposits more than 6 months.Rubbing paste has good dispersion stabilization and rheological property, makes rubbing paste at ceramic contact pin endoporus uniform distribution on the one hand, helps depositing of rubbing paste in addition.
6, the acid-basicity that experiment showed, diamond polishing paste in high purity of the present invention can produce bigger influence to the dispersion stabilization of rubbing paste, and the pH value is controlled at 7～10, has good dispersion stabilization.
7, diamond polishing paste in high purity of the present invention has water-based, oiliness two dissolubilities.Its oiliness can make rubbing paste polishing tabulation mask that good immersional wetting is arranged, and its water-based can reduce polishing time, improve polishing efficiency, saves diamond polishing cream; In addition, rubbing paste has the cleaning that two dissolubilities help glazed surface.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Reagent such as used wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and medicine are common reagent, medicine in the method for the present invention.The used equipment of method of the present invention all is known devices of using always.
Embodiment 1:
(size-grade distribution is 100～200nm), and adding 5g 1,4 butyleneglycol stirs, and ultrasonic 8min is fully wetting to get 0.5g purity 99.9% diadust.Add 0.3g polyoxyethylene nonylphenol ether (OP-10), add glycerine 68.9g, be made into mixed solution, with the 25g heating for dissolving polyoxyethylene glycol join in the mixed solution, mechanical stirring mixes, ultrasonic 10min.Trolamine is regulated pH to 8, stirs 30min, ultrasonic then 10min, get final product diamond polishing paste in high purity.This rubbing paste can be stablized and deposits 6 months, shear viscosity 4800mpa.s, low-shear viscosity 8500mpa.s.
Embodiment 2:
(size-grade distribution is 100～200nm), and the ethanol of adding 20g stirs, and ultrasonic 20min is fully wetting to get 2g purity 99.9% diadust.Add 1g sorbitan fatty acid ester Soxylat A 25-7, add glycerine 31g, be made into mixed solution, add the 45g heating for dissolving then polyvinyl alcohol, the limit edged stirs, time 30min.Add thanomin and regulate pH to 9, high speed shear 30min obtains diamond polishing paste in high purity under the 10000r/min.This rubbing paste can be stablized and deposits 6 months, shear viscosity 5800mpa.s, low-shear viscosity 10500mpa.s.
Embodiment 3:
(size-grade distribution is 100～200nm), adds the stearic acid of 1g, and ultrasonic 5min is fully wetting to get 5g purity 99.9% diadust.Add the 0.5g seminose, add glycerine 68g, be made into mixed solution, add 25g polyoxyethylene polyoxypropylene block type polyethers then, the limit edged stirs 60min.Add ammoniacal liquor and regulate pH to 8, mechanical stirring 30min obtains diamond polishing paste in high purity.
Depositing by the high purity diamond polishing cream of embodiment 3 preparation did not have sedimentation in 6 months, its shear viscosity 6500mpa.s, low-shear viscosity 9500mpa.s.With this rubbing paste polishing fiber junctor ceramic contact pin micro-inner-hole surface, bore surface does not have slide mark or stain to occur, and after testing, inserts loss and return loss and all reaches the GB requirement.
Embodiment 4:
The preparation method of above-mentioned a kind of diamond polishing paste in high purity, it comprises the steps:
1) by the shared weight percent of each raw material be: diadust: wetting agent 0.05%: tensio-active agent 0.01%: dispersion stabilizer 0.1%: pH regulator agent 0.1%: glycerine 0.1%: 99.64% chooses diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine raw material; The purity of described diadust is 99.99%, and size-grade distribution is 100～200nm; Described wetting agent is an ethylene glycol, and described tensio-active agent is a fatty alcohol-polyoxyethylene ether, and described dispersion stabilizer is: polyacrylic acid, and described pH regulator agent is a sodium hydroxide;
2) the Nano diamond micro mist is joined in the wetting agent, stir, ultrasonic 5min, fully wetting;
3) diadust of getting after wetting mixes with tensio-active agent, adds glycerine and dispersion stabilizer, and ultrasonication 5min makes the diadust modification, obtains mixed pulp;
4) add pH value conditioning agent in mixed pulp and regulate pH between 7～10, stir, ultrasonic 5min gets diamond polishing paste in high purity.
Embodiment 5:
The preparation method of above-mentioned a kind of diamond polishing paste in high purity, it comprises the steps:
1) by the shared weight percent of each raw material be: diadust: wetting agent 5%: tensio-active agent 25%: dispersion stabilizer 5%: pH regulator agent 50%: glycerine 1%: 14% chooses diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine raw material; The purity of described diadust is 99.99%, and size-grade distribution is 100～200nm; Described wetting agent is a glycol ether, and described tensio-active agent is a polyoxyethylene sorbitol, and described dispersion stabilizer is: polyvinyl alcohol and polystyrene block copolymer, and described pH regulator agent is a potassium hydroxide;
2) the Nano diamond micro mist is joined in the wetting agent, stir, ultrasonic 30min, fully wetting;
3) diadust of getting after wetting mixes with tensio-active agent, adds glycerine and dispersion stabilizer, and ultrasonication 10min makes the diadust modification, obtains mixed pulp;
4) add pH value conditioning agent in mixed pulp and regulate pH between 7～10, stir, ultrasonic 10min gets diamond polishing paste in high purity.
Embodiment 6:
The preparation method of above-mentioned a kind of diamond polishing paste in high purity, it comprises the steps:
1) by the shared weight percent of each raw material be: diadust: wetting agent 3%: tensio-active agent 10%: dispersion stabilizer 2%: pH regulator agent 20%: glycerine 0.5%: 64.5% chooses diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine raw material; The purity of described diadust is more than or equal to 99.96%, and size-grade distribution is 100～200nm; Described wetting agent is polyoxyethylene glycol, 1,2 propylene glycol, oilstone acid, citric acid and oxalic acid, and polyoxyethylene glycol, 1,2 propylene glycol, oilstone acid, citric acid, oxalic acid respectively account for 2%; Described tensio-active agent is a polyoxyethylene fatty acid, described dispersion stabilizer is: poly-carboxyl siloxanes polyoxyethylene glycol two sections multipolymers, methylcellulose gum, contract methylcellulose gum and ethyl cellulose sodium, and poly-carboxyl siloxanes polyoxyethylene glycol two sections multipolymers, methylcellulose gum, the methylcellulose gum that contracts, ethyl cellulose sodium respectively account for 5%; Described pH regulator agent is acetate, oxalic acid and sodium hydroxide, and acetate, oxalic acid respectively account for 0.1%, and sodium hydroxide accounts for 0.3%;
2) the Nano diamond micro mist is joined in the wetting agent, stir, ultrasonic 10min, fully wetting;
3) diadust of getting after wetting mixes with tensio-active agent, adds glycerine and dispersion stabilizer, and mechanical stirring 60min makes the diadust modification, obtains mixed pulp;
4) add pH value conditioning agent in mixed pulp and regulate pH between 7～10, high speed shear 10min gets diamond polishing paste in high purity.
Claims (6)
1. a diamond polishing paste in high purity is characterized in that it is that feedstock production forms by diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine, and the shared weight percent of each raw material is:
Diadust: 0.05～5%;
Wetting agent: 0.01～25%;
Tensio-active agent: 0.1～5%;
Dispersion stabilizer: 0.1～50%;
PH regulator agent: 0.1～1%;
Glycerine: 14～99.64%;
The purity of described diadust is more than or equal to 99.9%, and size-grade distribution is 100～200nm.
2. a kind of diamond polishing paste in high purity according to claim 1, it is characterized in that: described wetting agent be ethanol, ethylene glycol ,-diglycol ethylene, polyoxyethylene glycol, 1,2 propylene glycol, 1,3 propylene glycol, 1,3 butyleneglycols, 1, in 4 butyleneglycols, glycerine, stearic acid, oilstone acid, citric acid, the oxalic acid any one or any mixing more than two kinds, any when mixing more than two kinds, be any proportioning.
3. a kind of diamond polishing paste in high purity according to claim 1 is characterized in that: described tensio-active agent is fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitol, polyoxyethylene fatty acid, polyoxypropylene N.F,USP MANNITOL, polyoxyethylene nonylphenol ether, sorbitan fatty acid ester Soxylat A 25-7, seminose, glucose, lactose or sucrose.
4. a kind of diamond polishing paste in high purity according to claim 1, it is characterized in that: described dispersion stabilizer is: any one in polyacrylic acid, polyvinyl alcohol, polyvinyl alcohol and polystyrene block copolymer, polyoxyethylene polyoxypropylene block type polyethers, poly-carboxyl siloxanes polyoxyethylene glycol two sections multipolymers, methylcellulose gum, the methylcellulose gum that contracts, ethyl cellulose sodium, the polyoxyethylene glycol or any mixing more than two kinds, any when mixing more than two kinds, be any proportioning.
5. a kind of diamond polishing paste in high purity according to claim 1, it is characterized in that: described pH regulator agent is any one or any mixing more than two kinds in ammoniacal liquor, sodium hydroxide, potassium hydroxide, thanomin, trolamine, acetate, the oxalic acid, any when mixing more than two kinds, be any proportioning.
6. the preparation method of a kind of diamond polishing paste in high purity as claimed in claim 1 is characterized in that it comprises the steps:
1) by the shared weight percent of each raw material be: diadust: 0.05～5%, wetting agent: 0.01～25%, tensio-active agent: 0.1～5%, dispersion stabilizer: 0.1～50%, pH regulator agent: 0.1～1%, glycerine: 14～99.64% choose diadust, wetting agent, tensio-active agent, dispersion stabilizer, pH regulator agent and glycerine raw material; The purity of described diadust is more than or equal to 99.9%, and size-grade distribution is 100～200nm;
2) the Nano diamond micro mist is joined in the wetting agent, ultrasonic 5～30min, fully wetting;
3) diadust of getting after wetting mixes with tensio-active agent, adds glycerine and dispersion stabilizer, and ultrasonication 5～10min or mechanical stirring 30min～60min make the diadust modification, obtain mixed pulp;
4) add pH value conditioning agent in mixed pulp and regulate pH between 7～10, ultrasonic or high speed shear gets diamond polishing paste in high purity.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100521988A CN100535070C (en) | 2007-05-17 | 2007-05-17 | Diamond polishing paste in high purity, and preparation method |
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| CNB2007100521988A CN100535070C (en) | 2007-05-17 | 2007-05-17 | Diamond polishing paste in high purity, and preparation method |
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| CN101050339A true CN101050339A (en) | 2007-10-10 |
| CN100535070C CN100535070C (en) | 2009-09-02 |
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| CN102191118A (en) * | 2011-04-07 | 2011-09-21 | 大连理工大学 | Oil-based suspended base liquid of nano diamond powder and preparation process thereof |
| CN102504705A (en) * | 2011-10-17 | 2012-06-20 | 刘玉林 | Polishing solution used for precision machining of optical communication ZrO2 ceramic stub and preparation method thereof |
| CN102898952A (en) * | 2012-10-12 | 2013-01-30 | 浙江汉威阀门制造有限公司 | Metallic grinding and polishing agent for valves and preparation method thereof |
| CN103013345A (en) * | 2012-12-21 | 2013-04-03 | 清华大学 | Oily diamond grinding liquid and preparation method thereof |
| CN103897606A (en) * | 2013-11-11 | 2014-07-02 | 东南大学 | High-purity nano-diamond polishing solution and preparation method thereof |
| CN104017499A (en) * | 2014-05-19 | 2014-09-03 | 贵州荣清工具有限公司 | Diamond grinding paste |
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