CN102504705B - Polishing solution used for precision machining of optical communication ZrO2 ceramic stub and preparation method thereof - Google Patents
Polishing solution used for precision machining of optical communication ZrO2 ceramic stub and preparation method thereof Download PDFInfo
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- 238000005498 polishing Methods 0.000 title claims abstract description 129
- 239000000919 ceramic Substances 0.000 title claims abstract description 33
- 238000004891 communication Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000003287 optical effect Effects 0.000 title claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title abstract 4
- 238000003754 machining Methods 0.000 title abstract 2
- 239000006185 dispersion Substances 0.000 claims abstract description 52
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000004064 cosurfactant Substances 0.000 claims abstract description 11
- 239000003381 stabilizer Substances 0.000 claims abstract description 11
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012530 fluid Substances 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 38
- 238000003780 insertion Methods 0.000 claims description 29
- 230000037431 insertion Effects 0.000 claims description 29
- 239000003795 chemical substances by application Substances 0.000 claims description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 238000004513 sizing Methods 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 15
- 229910052684 Cerium Inorganic materials 0.000 claims description 14
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 12
- 230000003750 conditioning effect Effects 0.000 claims description 12
- -1 polyoxyethylene Polymers 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 229960004418 trolamine Drugs 0.000 claims description 12
- 238000009736 wetting Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 239000000725 suspension Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical group [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical group O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 5
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 5
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 239000002002 slurry Substances 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 claims description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 229910000421 cerium(III) oxide Inorganic materials 0.000 claims description 2
- 239000000839 emulsion Substances 0.000 claims description 2
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 claims description 2
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 2
- 239000001384 succinic acid Substances 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 6
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- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 5
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- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 9
- 239000013307 optical fiber Substances 0.000 description 9
- 238000007873 sieving Methods 0.000 description 9
- 239000003082 abrasive agent Substances 0.000 description 8
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- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
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- 239000002612 dispersion medium Substances 0.000 description 2
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- 230000003746 surface roughness Effects 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
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- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses a polishing solution used for precision machining of an optical communication ZrO2 ceramic stub and a preparation method thereof. The polishing solution is composed of 0.5 to 12% of cerium oxides, 0.1 to 4% of aluminum oxide, 0.01 to 0.1% of moisture regulators, 0.05 to 2% of dispersants, 0.01 to 4% of dispersion stabilizers, 0.005 to 0.5% of cosurfactants and the balance of deionized water. The preparation method comprises the following steps of: loading cerium oxides and aluminum oxide into a mixing disperser, adding a part of deionized water and a part of moisture regulators, thoroughly mixing, adding the rest additives and the rest deionized water, mixing again, adjusting pH to 2 to 5, and ultrasonically dispersing. The invention solves the problem of incoordination between polishing efficiency and polishing precision in the conventional CMP process using single inorganic grinding material, achieves the polishing effect which can not be reached by single inorganic grinding material, can not only increase polishing efficiency but also improve polishing precision, and has good application performances.
Description
Technical field
The present invention relates to the polishing fluid that a kind of precision sizing is used, particularly relate to a kind of optical communication Zr0
2polishing fluid that ceramic insertion core precision sizing is used and preparation method thereof.
Background technology
Optical communication undergoes an unusual development rapidly in recent years, and one side is towards the future development of ultra-high speed, large capacity, long distance; On the other hand, fiber optic local area network custom system obtains Devoting Major Efforts To Developing, and full optical communication is the inevitable direction of optical communication development.In modern optical-fibre communications industry, the joints of optical fibre are optical passive components that consumption is maximum, the transmission quality of optical-fibre communications is had the greatest impact, its effect is accurate two end faces of optical fiber docking, the luminous energy of launching fiber output is coupled in reception optical fiber to greatest extent, and ensures transmission quality.The core of the joints of optical fibre and basic device are ZrO
2ceramic insertion core, plays the instrumentality of connection, conversion, data transmission.As the core of junctor, ZrO
2the processing quality of ceramic insertion core is very large on the impact of junctor, in order to ensure the reliability of lock pin and to obtain lower insertion loss, effectively suppresses the light loss in communication network, ensures the transmission quality of optical communication, to optical fiber and ZrO
2have relatively high expectations in the accurately machined of ferrule endface, particularly ZrO
2that the end face of lock pin requires is very smooth, smooth, no marking, not damaged, surface roughness Ra≤50nm, otherwise, can have a strong impact on the transmission quality of optical communication, therefore, must carry out superfinishing polishing to its end face.
ZrO
2ceramic insertion core is a kind of by nano level ZrO
2material is through a series of high precision special cermacis elements that process, and the junctor of making is fiber active linker detachable, classification, makes the connection of optical channel, conversion dispatch more flexible.ZrO
2the manufacturing technology difficulty of ceramic insertion core is large, complex process, and this technology is monopolized by the U.S., Japan always for many years, the ZrO that particularly Japanese injection moulding is produced
2lock pin, is monopolizing the technology such as starting material, technique and molding device at the international level.Domestic main ZrO
2in ceramic insertion core manufacturing enterprise, a part of enterprise is that starting material and the molding device of import Japan produced ZrO
2ceramic insertion core, most of enterprise is the ZrO of import Japan
2blank of cored ceramics, then carry out a series of precision sizing, be wherein also follow-up precision machined important step to ceramic surface planarization.
According to reported in literature, U.S., Deng state are at ZrO
2in the follow-up precision sizing of ceramic insertion core, the main CMP technology that adopts of flattening surface processing, this technology is the polishing technology that the chemical corrosion of being developed by IBM Corporation for 1992 and mechanical mill combine the earliest, be called for short CMP technology, being acknowledged as is at present almost unique leveling technology, the positive expanding day of its range of application.The ultimate principle of CMP technique be by polished workpiece under certain pressure and polishing fluid exist, polishing pad rotates relatively, mechanical grinding and chemical oxidation corrosive nature by abrasive material in polishing fluid complete the removal to workpiece surface material, to obtain smooth, bright and clean surface.In CMP technology, polishing fluid is one of key element of most critical, and the performance of polishing fluid directly has influence on the quality of workpiece surface after polishing.For ZrO
2the formula of polishing fluid for ceramic insertion core surface finishing, abroad always as secret of the trade, the document of publishing is less, disclosed polishing fluid, its abrasive is mainly ultra-fine SiO
2, Al
2o
3, the micro mist such as diamond or core/shell type structure Compostie abrasive particles etc.
At present, domesticly meet device ZrO for optical fiber
2the processing of ceramic insertion core flattening surface, mainly adopts mechanical milling tech, and this processing mode is polished material with abrasive grains incision, and impel form that its fragility is burst apart to realize the removal of material, finished surface easily forms tiny crack, and surface quality is not good, can not meet user's needs.
Summary of the invention
The technical problem to be solved in the present invention: overcome the deficiencies in the prior art, a kind of polishing fluid that contains cerium oxide and alumina powder compound abrasive is provided, solve and in traditional C MP technology, used single inorganic abradant polishing efficiency and the inharmonic problem of polishing precision, reach the single abrasive material polishing effect that is beyond one's reach, the present invention also provides the preparation method of this polishing fluid.
Conception plans of the present invention:
Scheme one, selects low, the Mohs' hardness of price and ZrO
2the Al that ceramic hardness is approaching
2o
3(Mohs' hardness is 9) ultra-fine micropowder, as the abrasive of polishing fluid, carries out polishing test.Scheme two: select the relatively low CeO of Mohs' hardness
2(Mohs' hardness is 6) ultra-fine micropowder, as the abrasive of polishing fluid, carries out polishing test.
By simultaneous test, the polishing efficiency of scheme one is higher, but at ZrO
2often there is a small amount of cut in ceramic insertion core surface; The polishing precision of scheme two is high, workpiece surface no marking and damage after polishing, but polishing efficiency is lower.
The present invention is the deficiency that overcomes above-mentioned technology, according to CeO
2and Al
2o
3the Mohs' hardness of micro mist is different with polishing feature, selects CeO
2and Al
2o
3micro mist, mixes with certain mass ratio, and mixed abrasive material is as the abrasive of polishing fluid, add wetting conditioning agent, dispersion agent, dispersion stabilizer, cosurfactant and deionized water, through mechanical stirring and ultrasonic dispersion, form uniform suspension, this suspension is as Zr0
2ceramic insertion core surface accurate adds uses polishing fluid.
technical scheme of the present invention:
A kind of optical communication Zr0
2ceramic insertion core precision sizing polishing fluid, represent with weight percent, raw material is: the oxide compound 0.5～12% of cerium, aluminum oxide 0.1～4%, wetting conditioning agent 0.01～0.1%, dispersion agent 0.05～2%, dispersion stabilizer 0.01～4%, cosurfactant 0.005～0.5%, surplus is deionized water.
Described raw material is preferably: oxide compound 1.0～9 % of cerium, aluminum oxide 0.3～3%, wetting conditioning agent 0.01～0.05%, dispersion agent 0.1～1.5%, dispersion stabilizer 0.01～1.5%, cosurfactant 0.01～0.1%, surplus is deionized water.
The oxide compound of described cerium is cerium dioxide or cerous oxide, and aluminum oxide is Alpha-alumina, and the oxide compound of cerium and the weight ratio of aluminum oxide are 5-1:1; The oxide compound median size of cerium is 0.1～6.0 μ m; Aluminum oxide median size is 0.1～6.0 μ m.
The preferred cerium dioxide of oxide compound of described cerium, the weight ratio of cerium dioxide and aluminum oxide is 3:1, the median size of cerium dioxide is 0.5～4.0 μ m; The median size of aluminum oxide is 0.5～3.0 μ m.
Described wetting conditioning agent is the one in aluminum nitrate, citric acid, acetic acid, hydrochloric acid, succinic acid and nitric acid, or wherein two or more; Described dispersion agent is the one in trolamine, glycerol, propylene glycol and 1.4-butyleneglycol.
Described dispersion stabilizer is the one in polypropylene glycol, sodium polyacrylate, polyvinyl alcohol and polyvinyl alcohol derivative; Cosurfactant is alkylphenol polyoxyethylene or fatty alcohol-polyoxyethylene ether.
The preparation method of described polishing fluid: the oxide compound of cerium and aluminum oxide are joined in dispersed with stirring device, first add part deionized water and wetting conditioning agent, after dispersed with stirring is even, add again dispersion agent, dispersion stabilizer and cosurfactant, stir, add again the deionized water of surplus, continue to stir and obtain the uniform slurry of dispersion and emulsion, then add pH value conditioning agent, regulate pH value to 2～5 of slurry, after ultrasonic wave is disperseed, sieve, form uniform suspension, obtain described Zr0
2ceramic insertion core surface accurate adds uses polishing fluid.
Described pH value conditioning agent is the one in thanomin, diethanolamine, trolamine, and the amount of part deionized water refers to the water yield lower than the half of deionized water total amount.
technical requirements of the present invention and explanation:
1, select in test, when polish abrasive is only used CeO in abrasive material proportioning
2time, polishing efficiency is lower, but better (roughness Ra reaches 10nm) of surface effect; Along with Al
2o
3consumption increases, and polishing efficiency improves thereupon, and surfaceness increases thereupon; When polish abrasive is only used Al
2o
3time, polishing efficiency is high, and surfaceness is also higher, and more than reaching 50nm, surface effect is poor.Consider, select two component compound abrasives of cerium oxide and aluminum oxide as the abrasive of polishing fluid, CeO
2and Al
2o
3weight ratio between 5-1:1, optimum ratio 3:1.
2, select in test at the particle diameter of abrasive material, the median size of cerium oxide micro mist is selected 0.1～6.0 μ m, preferably 0.5～4.0 μ m; The median size of alumina powder is selected 0.1～6.0 μ m, preferably 0.5～3.0 μ m.Particle diameter exceeds above-mentioned scope, and glazed surface is coarse larger, can produce scratch, depression etc.; If grain size of micropowder is less, polishing efficiency is too low, can not meet needs of production.
3, select in test in concentration, find that the solid content of polishing fluid is too low, polishing efficiency is just low; Solid content is too high, and the dispersion stability of polishing fluid is poor, disperses inhomogeneously, affects surface finish precision.In the time of the solid content >15% of polishing fluid, polishing efficiency is better, more than reaching 280nm/min, but more than surfaceness increases to 50nm; In the time of polishing fluid solid content≤0.5%, can obtain good surface effect, but polishing efficiency is down to below 20nm/min.Consider polishing efficiency and surfaceness index, combined process requirement, the present invention selects the solid content of polishing fluid between 1%～15%, and now polishing efficiency is more than 75nm/min, and surfaceness is less than 50nm.The polishing fluid solid content is here mainly micron power CeO
2, Al
2o
3content.
4, the wetting conditioning agent in component plays moistened surface effect to abrasive particle, contributes to the dispersion of ultra-fine micropowder particle agglomeration.Micro mist powder specific-surface area detection is larger, in the dispersion medium such as empty G&W, easily reunites and forms macrobead, and therefore dispersion medium is selected deionized water, adds wetting conditioning agent simultaneously, can improve the wettability of abrasive material powder, is convenient to the dispersion treatment of micro mist.
5, the dispersion agent in component is to playing surface modification effect compared with small agglomerates and primary partical in suspension.In dispersion, easily produce reunion, sedimentation phenomenon compared with small agglomerates and primary partical, add dispersion agent to stop and scatteredly again reunite compared with small-particle.
6, the dispersion stabilizer in component is a kind of polymeric surface active agent, and polishing fluid is played to stably dispersing effect, can improve the gravity settling of dispersion system, makes polishing fluid have high density, low viscosity and high dispersion stability.The add-on of dispersion stabilizer is 0.01～4%, preferably 0.01～1.5%, and now the viscosity of polishing fluid is lower, and dispersion effect is better.Add-on exceeds above-mentioned scope, and in suspension, discrete particles can produce reunion, affects the stability of polishing fluid.
7, the cosurfactant in component is alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether etc., and add-on is 0.005～0.5t%, preferably 0.01～0.1t%; Add-on, lower than above-mentioned scope, affects the erasability of surface of polished, and add-on is higher than above-mentioned scope, and in the course of processing, foam is more, affects polishing effect.
8, the stability of the suspension property of polishing fluid reaction polishing fluid, the stability of polishing fluid relates to the formation of workpiece surface cut and spot corrosion in polishing, even the cleaning after polishing is also had to impact, and stability is better, size distribution is more even, and polishing effect is just better.PH value and the stability of polishing fluid are closely related, and when total variation tendency shows as polishing fluid and changes from acidity to alkalescence, its stability reduces gradually.Adopt laser particle size analyzer to test different pH value agglomerating particles size-grade distribution situations, confirmed the variation tendency of stability with pH value from the variation of agglomerating particles median size.When pH value is 2～5 time, agglomeration is less, even particle distribution, particle diameter minimum, and now the stability of polishing fluid dispersion is better.
positive beneficial effect of the present invention:
1, the present invention is different with polishing characteristic according to the Mohs' hardness of the oxide compound of cerium and alumina powder, adopt the oxide compound, aluminum oxide two-pack compound abrasive of cerium as the abrasive of polishing fluid, solve and in traditional C MP technology, used single inorganic abradant polishing efficiency and the inharmonic contradiction of polishing precision, reach the single abrasive material polishing effect that is beyond one's reach, not only improve polishing efficiency, improved polishing precision simultaneously.More than polishing fluid polishing efficiency of the present invention reaches 75nm/min, surface roughness Ra value is less than 50nm, has good application performance.Test-results is referring to table 1.
2, polishing fluid of the present invention, by adding cosurfactant, has improved the erasability of polishing fluid, the element surface light after polishing, easy cleaning; By selecting suitable pH value, the polishing fluid agglomeration obtaining is less, and even particle distribution, particle diameter are less, and the stability of polishing fluid dispersion system is better.
3, polishing fluid of the present invention is at ZrO
2respond well in the practical application of lock pin surface finishing, glazed surface seldom causes depression, scratch, has good erasability, and polishing efficiency is high, and surfaceness is low; Meanwhile, this polishing fluid also can be used for the precision polishing of the industries such as devitrified glass for electronic component, semiconductor wafer, opticglass, precision die, and polishing effect reaches import like product level.
Embodiment
example 1optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
?get 51.2 grams of CeO
2(median size is m) He 12.8 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 300 grams of deionized waters and 0.32 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.6 grams of glycerol, 2.4 grams of polyvinyl alcohol derivatives, 0.16 gram of polyoxyethylene nonylphenol ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, add trolamine to regulate pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain solid content (CeO
2, Al
2o
3micro mist) be the aaerosol solution of 8.0%wt, dispersion liquid viscosity is 0.015Pa.s, is polishing fluid of the present invention.
example 2optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 48 grams of CeO
2(median size is m) He 16 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 300 grams of deionized waters and 0.32 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.6 grams of glycerol, 2.4 grams of polyvinyl alcohol, 0.16 gram of polyoxyethylene nonylphenol ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of solid content 8.0%wt, dispersion liquid viscosity 0.016Pa.s, is polishing fluid of the present invention.
example 3optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 42.6 grams of CeO
2(median size is m) He 21.4 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 300 grams of deionized waters and 0.32 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.6 grams of glycerol, 2.4 grams of polyvinyl alcohol, 0.16 gram of polyoxyethylene nonylphenol ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of solid content 8.0%wt, dispersion liquid viscosity 0.015Pa.s, is polishing fluid of the present invention.
example 4optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 32 grams of CeO
2(median size is m) He 32 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 300 grams of deionized waters and 0.32 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.6 grams of glycerol, 2.4 grams of polyvinyl alcohol, 0.16 gram of fatty alcohol-polyoxyethylene ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, by thanomin adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of solid content 8.0%wt, dispersion liquid viscosity 0.016Pa.s, is polishing fluid of the present invention.
example 5optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 90 grams of CeO
2(median size is m) He 30 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 300 grams of deionized waters and 0.40 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 2.8 grams of 1.4-butyleneglycols, 3.2 grams of polypropylene glycols, 0.16 gram of polyoxyethylene nonylphenol ether and 373 grams of deionized waters, continue dispersed with stirring 2.5h, by diethanolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, sieve to obtain the rear aaerosol solution to solid content 15.0%wt, dispersion liquid viscosity 0.025Pa.s, is polishing fluid of the present invention.
example 6optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 36 grams of CeO
2(median size is m) He 12 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 250 grams of deionized waters and 0.50 gram of hydrochloric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.25 grams of trolamines, 2.0 grams of polyvinyl alcohol, 0.16 gram of polyoxyethylene nonylphenol ether and 498 grams of deionized waters, continue dispersed with stirring 2.0h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of 6.0%wt, dispersion liquid viscosity 0.015Pa.s, is polishing fluid of the present invention.
example 7optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 9 grams of CeO
2(median size is m) He 3 grams of Al of 0.78 μ
2o
3(median size is m) micro mist of 0.5 μ, add 450 grams of deionized waters and 0.15 gram of acetic acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.2 grams of 1.4-butyleneglycols, 1.5 grams of polyvinyl alcohol derivatives, 0.24 gram of polyoxyethylene nonylphenol ether and 735 grams of deionized waters, continue dispersed with stirring 1.5h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of solid content 1.0%wt, dispersion liquid viscosity 0.006Pa.s, is polishing fluid of the present invention.
example 8optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 48 grams of CeO
2(median size is m) He 16 grams of Al of 1.50 μ
2o
3(median size is m) micro mists of 1.0 μ, add 300 grams of deionized waters, 0.16 gram of aluminum nitrate and 0.16 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add again 1.6 grams of propylene glycol, 2.4 grams of polyvinyl alcohol, 0.16 gram of polyoxyethylene nonylphenol ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of solid content 8.0%wt, dispersion liquid viscosity 0.014Pa.s, is polishing fluid of the present invention.
example 9optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 48 grams of Ce
2o
3(median size is m) He 16 grams of Al of 2.50 μ
2o
3(median size is m) micro mists of 2.0 μ, add 300 grams of deionized waters, 0.12 gram of citric acid and 0.2 gram of nitric acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.6 gram 1,4-butyleneglycol, 2.4 grams of sodium polyacrylates, 0.16 gram of polyoxyethylene nonylphenol ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, after sieving, obtain the aaerosol solution of solid content 8.0%wt, dispersion liquid viscosity 0.015Pa.s, is polishing fluid of the present invention.
example 10optical communication Zr0
2polishing fluid and preparation method thereof for ceramic insertion core precision sizing
Get 48 grams of Ce
2o
3(median size is m) He 16 grams of Al of 2.0 μ
2o
3(median size is m) micro mists of 1.50 μ, add 300 grams of deionized waters and 0.32 gram of succinic acid, dispersed with stirring 0.5h in stirring dispersion machine, add 1.6 grams of glycerol, 2.4 grams of polyvinyl alcohol derivatives, 0.16 gram of polyoxyethylene nonylphenol ether and 431 grams of deionized waters, continue dispersed with stirring 2.0h, by trolamine adjusting pH value to 4.5, disperse 20min through ultrasonic wave, the aaerosol solution that obtains solid content 8.0%wt after sieving, dispersion liquid viscosity 0.014Pa.s, is polishing fluid of the present invention.
example 11polishing test
With optical communication Zr0 of the present invention
2ceramic insertion core precision sizing is carried out polishing application test with polishing fluid, and polished object is joints of optical fibre ZrO
2ferrule endface, polishing test is divided into rough polishing and essence is thrown, and rough polishing and essence cast the standby Hefei section brilliant UNIPOL-1202 type precise grinding polisher that all uses.
Rough polishing is selected and ground particle diameter is that the diamond lap paper of 60 μ m, 45 μ m, 30 μ m grinds, after rough polishing is ground, and ZrO
2ferrule endface roughness is still larger, then uses the polishing fluid in above-mentioned example, on UNIPOL-1202 type precise grinding polisher, carries out precise polished test.Polishing pad is selected polyurethane polishing pad (Shore hardness 20～50D).
Polishing condition: polish pressure 0.85kg/cm
2, 30 DEG C of polish temperatures, polishing disk rotating speed 120r/min, polishing fluid input speed is 160ml/min, test-results sees the following form 1:
From above-mentioned polishing test, more than polishing fluid polishing efficiency of the present invention reaches 75nm/min, surfaceness is less than 50nm, median size can reach 0.68 μ m, viscosity is less than 0.03 Pa.s, cave in surface, scratch aspect is respond well, reached the coordinating and unifying of polishing efficiency and polishing precision.
Claims (1)
1. an optical communication Zr0
2ceramic insertion core precision sizing polishing fluid, it is characterized in that: by following weight percent: oxide compound 1.0～9 % of cerium, aluminum oxide 0.3～3%, wetting conditioning agent 0.01～0.05%, dispersion agent 0.1～1.5%, dispersion stabilizer 0.01～1.5%, cosurfactant 0.01～0.1%, surplus is that deionized water is made, preparation method comprises the following steps: the oxide compound of cerium and aluminum oxide are joined in dispersed with stirring device, first add part deionized water and wetting conditioning agent, after dispersed with stirring is even, add again dispersion agent, dispersion stabilizer and cosurfactant, stir, add again the deionized water of surplus, continue to stir and obtain the uniform slurry of dispersion and emulsion, then add pH adjusting agent, regulate pH value to 2～5 of slurry, after disperseing, ultrasonic wave sieves, form uniform suspension, obtain described Zr0
2ceramic insertion core surface accurate processing polishing fluid, described pH adjusting agent is the one in thanomin, diethanolamine, trolamine, the amount of described part deionized water is lower than the half of deionized water total amount,
The oxide compound of described cerium is cerium dioxide or cerous oxide, and aluminum oxide is Alpha-alumina;
The oxide compound of described cerium and the weight ratio of aluminum oxide are 5-1:1; The oxide compound median size of cerium is 0.1～6.0 μ m; Aluminum oxide median size is 0.1～6.0 μ m;
Described wetting conditioning agent is the one in aluminum nitrate, citric acid, acetic acid, hydrochloric acid, succinic acid and nitric acid, or wherein two or more; Described dispersion agent is the one in trolamine, glycerol, propylene glycol and 1.4-butyleneglycol;
Described dispersion stabilizer is the one in polypropylene glycol, sodium polyacrylate, polyvinyl alcohol and polyvinyl alcohol derivative; Described cosurfactant is alkylphenol polyoxyethylene or fatty alcohol-polyoxyethylene ether.
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