CN102504705A - 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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- CN102504705A CN102504705A CN201110314587XA CN201110314587A CN102504705A CN 102504705 A CN102504705 A CN 102504705A CN 201110314587X A CN201110314587X A CN 201110314587XA CN 201110314587 A CN201110314587 A CN 201110314587A CN 102504705 A CN102504705 A CN 102504705A
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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 19
- 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 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000004064 cosurfactant Substances 0.000 claims abstract description 12
- 239000003381 stabilizer Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 7
- 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 76
- 238000003756 stirring Methods 0.000 claims description 38
- 238000003780 insertion Methods 0.000 claims description 29
- 230000037431 insertion Effects 0.000 claims description 29
- 238000004513 sizing Methods 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 17
- 229910052684 Cerium Inorganic materials 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 12
- 229960004418 trolamine Drugs 0.000 claims description 12
- -1 USP Kosher Chemical compound 0.000 claims description 11
- 238000009736 wetting Methods 0.000 claims description 11
- 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
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical group O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 8
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 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
- 239000002994 raw material Substances 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
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 2
- 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
- 239000001384 succinic acid Substances 0.000 claims description 2
- 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 7
- 230000000694 effects Effects 0.000 abstract description 14
- 229910000420 cerium oxide Inorganic materials 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract 3
- 206010003591 Ataxia Diseases 0.000 abstract 1
- 206010010947 Coordination abnormal Diseases 0.000 abstract 1
- 239000000654 additive Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 208000016290 incoordination Diseases 0.000 abstract 1
- 239000003643 water by type Substances 0.000 description 20
- 239000003595 mist Substances 0.000 description 17
- 238000005516 engineering process Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 15
- 239000007787 solid Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-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
- 238000012545 processing Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 210000001503 joint Anatomy 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
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- 239000000835 fiber Substances 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 239000006260 foam Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Landscapes
- 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 the ceramic insertion core precision sizing is used and preparation method thereof.
Background technology
Optical communication undergoes an unusual development rapidly in recent years, and the direction towards ultra-high speed, large vol, long distance develops on the one hand; On the other hand, the fiber optic local area network custom system is developed energetically, and full optical communication is the inevitable direction of optical communication development.In the modern optical fiber communications industry joints of optical fibre be consumption at most, optical passive component that the transmission quality of optical-fibre communications is had the greatest impact; Its effect is the accurate butt joint of two end faces of optical fiber; The luminous energy of launching fiber output is coupled in the reception optical fiber to greatest extent, and guarantees 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 big to the influence of junctor, and the safety insertion loss lower with acquisition in order to guarantee lock pin effectively suppresses the light loss in the communication network, guarantees 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 surpass finishing polish to its end face and process.
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 processing is a 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 big, complex process, should technology be monopolized the ZrO that particularly Japanese injection moulding is produced by the U.S., Japan for many years always
2Lock pin is monopolizing technology such as starting material, technology and molding device at the international level.Domestic main ZrO
2In the ceramic insertion core manufacturing enterprise, a part of enterprise is that the 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 carries out a series of precision sizing again, also is follow-up precision machined important step to the ceramic surface planarization wherein.
According to reported in literature, states such as U.S.A, day 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 is combined by the chemical corrosion and the mechanical mill of IBM Corporation's exploitation in 1992 the earliest; Be called for short the CMP technology, being acknowledged as at present almost is unique leveling technology, and its range of application enlarges just day by day.The ultimate principle of CMP technology be with polished workpiece in the presence of certain pressure and polishing fluid; Polishing pad rotates relatively; Mechanical grinding and chemical oxidation corrosive nature by abrasive material in the polishing fluid are accomplished the removal to the workpiece surface material, to obtain smooth, bright and clean surface.Polishing fluid is one of key element of most critical in the CMP technology, and the performance of polishing fluid directly has influence on the quality of polishing back workpiece surface.For ZrO
2The ceramic insertion core surface finishing is with the prescription of polishing fluid, and abroad always as secret of the trade, the document of publishing is less, and disclosed polishing fluid, its abrasive mainly are ultra-fine SiO
2, Al
2O
3, micro mist such as diamond or core/shell type structure Compostie abrasive particles etc.
At present, domesticly meet device ZrO for optical fiber
2Mechanical milling tech is mainly adopted in the processing of ceramic insertion core flattening surface, and this processing mode is cut by abrasive substance with abrasive grains; And the form of impelling its fragility to burst apart realizes the removal of material; Finished surface is prone to form tiny crack, and surface quality is not good, can not satisfy user's needs.
Summary of the invention
The technical problem that the present invention will solve: the deficiency that overcomes prior art; A kind of polishing fluid that contains cerium oxide and alumina powder compound abrasive is provided; Solved and used single inorganic abradant polishing efficiency and the inharmonic problem of polishing precision in the traditional C MP technology; 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 that price is low, Mohs' hardness and ZrO
2The Al that ceramic hardness is approaching
2O
3(Mohs' hardness is 9) ultra-fine micropowder polishes test as the abrasive of polishing fluid.Scheme two: select the relatively low CeO of Mohs' hardness
2(Mohs' hardness is 6) ultra-fine micropowder polishes test as the abrasive of polishing fluid.
Through simultaneous test, the polishing efficiency of scheme one is higher, but at ZrO
2A small amount of cut often appears in the ceramic insertion core surface; The polishing precision of scheme two is high, polishing back workpiece surface no marking and damage, 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 the polishing characteristics, selects CeO for use
2And Al
2O
3Micro mist mixes with certain mass ratio, and mixed abrasive material is as the abrasive of polishing fluid; Add wetting regulator, dispersion agent, dispersion stabilizer, cosurfactant and deionized water; Through mechanical stirring and ultra-sonic dispersion, form uniform suspension-s, this suspension-s is as Zr0
2The ceramic insertion core surface accurate adds uses polishing fluid.
Technical scheme of the present invention:
A kind of optical communication Zr0
2The ceramic insertion core precision sizing is used polishing fluid; Represent with weight percent; Raw material is: the oxide compound 0.5～12% of cerium, aluminum oxide 0.1～4%, wetting regulator 0.01～0.1%, dispersion agent 0.05～2%, dispersion stabilizer 0.01～4%, cosurfactant 0.005～0.5%, surplus are deionized water.
Said raw material is preferably: oxide compound 1.0～9 % of cerium, aluminum oxide 0.3～3%, wetting regulator 0.01～0.05%, dispersion agent 0.1～1.5%, dispersion stabilizer 0.01～1.5%, cosurfactant 0.01～0.1%, surplus are deionized water.
The oxide compound of said cerium is cerium dioxide or cerous oxide, and aluminum oxide is an 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; The aluminum oxide median size is 0.1～6.0 μ m.
The preferred cerium dioxide of the oxide compound of said cerium, the weight ratio of cerium dioxide and aluminum oxide are 3:1, and 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.
Said wetting regulator is a kind of in aluminum nitrate, Hydrocerol A, acetic acid, hydrochloric acid, Succinic Acid and the nitric acid, or wherein two or more; Said dispersion agent is a kind of in trolamine, USP Kosher, Ucar 35 and the 1.4-butyleneglycol.
Said dispersion stabilizer is a kind of in W 166, ZX-I, Z 150PH and the polyvinyl alcohol derivative; Cosurfactant is TX10 or AEO.
The preparation method of said polishing fluid: the oxide compound and the aluminum oxide of cerium are joined in the dispersed with stirring device, add part deionized water and wetting regulator earlier, after dispersed with stirring is even; Add dispersion agent, dispersion stabilizer and cosurfactant again, stir, add balance of deionized water again; Continue to stir and obtain the uniform slurry of dispersion and emulsion; Add pH value regulator then, regulate pH value of slurry to 2～5, after ultrasonic dispersing, sieve; Form uniform suspension-s, promptly obtain said Zr0
2The ceramic insertion core surface accurate adds uses polishing fluid.
Said pH value regulator is a kind of in thanomin, diethylolamine, the trolamine, and the amount of part deionized water is meant the half the water yield that is lower than the deionized water total amount.
Technical requirements of the present invention and explanation:
1, selects in the test, in the abrasive material proportioning when polish abrasive is only used CeO
2The time, polishing efficiency is lower, but surface effect better (roughness Ra reaches 10nm); Along with Al
2O
3Consumption increases, and polishing efficiency improves thereupon, and surfaceness increases thereupon; When polish abrasive is only used Al
2O
3The time, polishing efficiency is high, and surfaceness is also higher, reaches more than the 50nm, and promptly surface effect is relatively poor.Take all factors into consideration, select the abrasive of two component compound abrasives of cerium oxide and aluminum oxide for use, CeO as polishing fluid
2And Al
2O
3Weight ratio between 5-1:1, optimum ratio 3:1.
2, select in the test at the particle diameter of abrasive material, the median size of cerium oxide micro mist is selected 0.1～6.0 μ m for use, preferred 0.5～4.0 μ m; The median size of alumina powder is selected 0.1～6.0 μ m for use, preferred 0.5～3.0 μ m.Particle diameter exceeds above-mentioned scope, and glazed surface is coarse bigger, can produce scratch, depression etc.; If grain size of micropowder is less, then polishing efficiency is too low, can not satisfy needs of production.
3, select in the test in concentration, find that the solid content of polishing fluid is low excessively, polishing efficiency is just low; Solid content is too high, and the dispersion stability of polishing fluid is relatively poor, disperses inhomogeneously, influences the surface finish precision.Solid content when polishing fluid>15% the time, polishing efficiency is better, reach more than the 280nm/min, but surfaceness increases to more than the 50nm; When polishing fluid solid content≤0.5%, can obtain surface effect preferably, but polishing efficiency is reduced to below the 20nm/min.Take all factors into consideration polishing efficiency and surfaceness index, combined process requirement, the present invention select the solid content of polishing fluid between 1%～15%, and polishing efficiency is more than 75nm/min at this moment, and surfaceness is less than 50nm.The polishing fluid solid content here mainly is micron power CeO
2, Al
2O
3Content.
4, the wetting regulator in the component plays the moistened surface effect to abrasive particle, helps the dispersion of ultra-fine micropowder particle agglomeration.Micro mist powder specific surface area is bigger, and in dispersion medium such as empty G&W, reuniting easily forms macrobead, so dispersion medium selection deionized water, adds wetting regulator simultaneously, can improve the wettability of abrasive material powder, is convenient to the dispersion treatment of micro mist.
5, the dispersion agent in the component is to playing the surface-treated effect than small agglomerates and primary partical in the suspension-s.Be easy to generate reunion, sedimentation phenomenon than small agglomerates and primary partical in the dispersion-s, add dispersion agent and can stop and scatteredly reunite once more than small-particle.
6, the dispersion stabilizer in the component is a kind of polymeric surface active agent, and polishing fluid is played the stably dispersing effect, can improve the gravity settling property of dispersion system, makes polishing fluid have high density, LV and high dispersion stability.The add-on of dispersion stabilizer is 0.01～4%, and is preferred 0.01～1.5%, and this moment, the viscosity of polishing fluid was lower, and dispersion effect is better.Add-on exceeds above-mentioned scope, and discrete particles can produce reunion in the suspension-s, influences the stability of polishing fluid.
7, the cosurfactant in the component is TX10, AEO etc., and add-on is 0.005～0.5t%, preferred 0.01～0.1t%; Add-on is lower than above-mentioned scope, influences the erasable of surface of polished, and add-on is higher than above-mentioned scope, and foam is more in the course of processing, influences 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 the polishing processing, even also influential to the cleaning after polishing, and stability is good more; Size distribution is even more, and polishing effect is just good more.The pH value of polishing fluid is closely related with stability, and when total variation tendency showed as polishing fluid and from acidity to alkalescence, changes, its stability reduced gradually.Adopt laser particle size analyzer to test different pH value agglomerating particles size-grade distribution situation, confirmed stable variation tendency with the pH value from the variation of agglomerating particles median size.When the pH value 2～5 the time, agglomeration is less, even particle distribution, particle diameter are minimum, this moment the polishing fluid dispersion-s stability better.
Positive beneficial effect of the present invention:
1, the present invention is different with the 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 abrasive as polishing fluid; Solved and used single inorganic abradant polishing efficiency and the inharmonic contradiction of polishing precision in the traditional C MP technology; Reach the single abrasive material polishing effect that is beyond one's reach, not only improved polishing efficiency, improved the polishing precision simultaneously.Polishing fluid polishing efficiency of the present invention reaches more than the 75nm/min, and the surface roughness Ra value has the excellent application performance ability less than 50nm.Test-results is referring to table 1.
2, polishing fluid of the present invention has improved the erasable of polishing fluid through adding cosurfactant, the element surface light after the polishing, the easy cleaning; Through selecting suitable pH value, the polishing fluid agglomeration that obtains is less, and even particle distribution, particle diameter are less, and the stability of polishing fluid dispersion system 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 erasable, and polishing efficiency is high, and surfaceness is low; Simultaneously, this polishing fluid also can be used for the precision polishing processing of electronic component with industries such as sytull, semiconductor wafer, opticglass, precision dies, and polishing effect reaches import like product level.
Embodiment
Instance 1Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 51.2 gram CeO
2(median size is 0.78 μ m) and 12.8 gram Al
2O
3(median size is 0.5 μ m) micro mist; Add 300 gram deionized waters and 0.32 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine adds 1.6 gram USP Kosher, 2.4 gram polyvinyl alcohol derivatives, 0.16 gram polyoxyethylene nonylphenol and 431 gram deionized waters; Continue dispersed with stirring 2.0h; Add trolamine and regulate pH value to 4.5,, obtain solid content (CeO after sieving through ultrasonic dispersing 20min
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.
Instance 2Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 48 gram CeO
2(median size is 0.78 μ m) and 16 gram Al
2O
3(median size is 0.5 μ m) micro mist adds 300 gram deionized waters and 0.32 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.6 gram USP Kosher, 2.4 gram Z 150PH, 0.16 gram polyoxyethylene nonylphenol and 431 gram deionized waters, continue dispersed with stirring 2.0h, regulate pH value to 4.5 with trolamine; Through ultrasonic dispersing 20min; Obtain the aaerosol solution of solid content 8.0%wt after sieving, dispersion liquid viscosity 0.016Pa.s is polishing fluid of the present invention.
Instance 3Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 42.6 gram CeO
2(median size is 0.78 μ m) and 21.4 gram Al
2O
3(median size is 0.5 μ m) micro mist adds 300 gram deionized waters and 0.32 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.6 gram USP Kosher, 2.4 gram Z 150PH, 0.16 gram polyoxyethylene nonylphenol and 431 gram deionized waters, continue dispersed with stirring 2.0h, regulate pH value to 4.5 with trolamine; Through ultrasonic dispersing 20min; Obtain the aaerosol solution of solid content 8.0%wt after sieving, dispersion liquid viscosity 0.015Pa.s is polishing fluid of the present invention.
Instance 4Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 32 gram CeO
2(median size is 0.78 μ m) and 32 gram Al
2O
3(median size is 0.5 μ m) micro mist adds 300 gram deionized waters and 0.32 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.6 gram USP Kosher, 2.4 gram Z 150PH, 0.16 gram AEO and 431 gram deionized waters, continue dispersed with stirring 2.0h, regulate pH value to 4.5 with thanomin; Through ultrasonic dispersing 20min; Obtain the aaerosol solution of solid content 8.0%wt after sieving, dispersion liquid viscosity 0.016Pa.s is polishing fluid of the present invention.
Instance 5Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 90 gram CeO
2(median size is 0.78 μ m) and 30 gram Al
2O
3(median size is 0.5 μ m) micro mist adds 300 gram deionized waters and 0.40 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 2.8 gram 1.4-butyleneglycols, 3.2 gram W 166s, 0.16 gram polyoxyethylene nonylphenol and 373 gram deionized waters, continue dispersed with stirring 2.5h, regulate pH value to 4.5 with diethylolamine; Through ultrasonic dispersing 20min; Sieve back aaerosol solution to solid content 15.0%wt, dispersion liquid viscosity 0.025Pa.s is polishing fluid of the present invention.
Instance 6Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 36 gram CeO
2(median size is 0.78 μ m) and 12 gram Al
2O
3(median size is 0.5 μ m) micro mist adds 250 gram deionized waters and 0.50 gram hydrochloric acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.25 gram trolamines, 2.0 gram Z 150PH, 0.16 gram polyoxyethylene nonylphenol and 498 gram deionized waters, continue dispersed with stirring 2.0h, regulate pH value to 4.5 with trolamine; Through ultrasonic dispersing 20min; Obtain the aaerosol solution of 6.0%wt after sieving, dispersion liquid viscosity 0.015Pa.s is polishing fluid of the present invention.
Instance 7Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 9 gram CeO
2(median size is 0.78 μ m) and 3 gram Al
2O
3(median size is 0.5 μ m) micro mist adds 450 gram deionized waters and 0.15 gram acetic acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.2 gram 1.4-butyleneglycols, 1.5 gram polyvinyl alcohol derivatives, 0.24 gram polyoxyethylene nonylphenol and 735 gram deionized waters, continue dispersed with stirring 1.5h, regulate pH value to 4.5 with trolamine; Through ultrasonic dispersing 20min; Obtain the aaerosol solution of solid content 1.0%wt after sieving, dispersion liquid viscosity 0.006Pa.s is polishing fluid of the present invention.
Instance 8Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 48 gram CeO
2(median size is 1.50 μ m) and 16 gram Al
2O
3(median size is 1.0 μ m) micro mist; Add 300 gram deionized waters, 0.16 gram aluminum nitrate and 0.16 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine adds 1.6 gram Ucar 35,2.4 gram Z 150PH, 0.16 gram polyoxyethylene nonylphenol and 431 gram deionized waters again; Continue dispersed with stirring 2.0h; Regulate pH value to 4.5 with trolamine,, obtain the aaerosol solution of solid content 8.0%wt after sieving through ultrasonic dispersing 20min; Dispersion liquid viscosity 0.014Pa.s is polishing fluid of the present invention.
Instance 9Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 48 gram Ce
2O
3(median size is 2.50 μ m) and 16 gram Al
2O
3(median size is 2.0 μ m) micro mist adds 300 gram deionized waters, 0.12 gram Hydrocerol A and 0.2 gram nitric acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.6 grams 1; 4-butyleneglycol, 2.4 gram ZX-Is, 0.16 gram polyoxyethylene nonylphenol and 431 gram deionized waters continue dispersed with stirring 2.0h, regulate pH value to 4.5 with trolamine; Through ultrasonic dispersing 20min; Obtain the aaerosol solution of solid content 8.0%wt after sieving, dispersion liquid viscosity 0.015Pa.s is polishing fluid of the present invention.
Instance 10Optical communication Zr0
2The ceramic insertion core precision sizing is with polishing fluid and preparation method thereof
Get 48 gram Ce
2O
3(median size is 2.0 μ m) and 16 gram Al
2O
3(median size is 1.50 μ m) micro mist adds 300 gram deionized waters and 0.32 gram Succinic Acid, dispersed with stirring 0.5h in stirring dispersion machine; Add 1.6 gram USP Kosher, 2.4 gram polyvinyl alcohol derivatives, 0.16 gram polyoxyethylene nonylphenol and 431 gram deionized waters, continue dispersed with stirring 2.0h, regulate pH value to 4.5 with trolamine; Through ultrasonic dispersing 20min; Get the aaerosol solution of solid content 8.0%wt after sieving, dispersion liquid viscosity 0.014Pa.s is polishing fluid of the present invention.
Instance 11The polishing test
With optical communication Zr0 of the present invention
2The ceramic insertion core precision sizing is polished application test with polishing fluid, and polished object is joints of optical fibre ZrO
2Ferrule endface, polishing are tested and are divided into thick throwing and smart throwing, and thick throwing and essence cast and all use Hefei section brilliant UNIPOL-1202 type precise grinding polisher fully.
The thick throwing selects that to grind particle diameter be that the diamond lap paper of 60 μ m, 45 μ m, 30 μ m grinds for use, through thick throw grind after, ZrO
2The ferrule endface roughness is still bigger, uses the polishing fluid in the above-mentioned instance then, on UNIPOL-1202 type precise grinding polisher, carries out precise polished test.Polishing pad is selected polyurethane polishing pad (Shore hardness 20～50D) for use.
Polishing condition: polish pressure 0.85kg/cm
2, 30 ℃ of polish temperatures, polishing disk rotating speed 120r/min, the polishing fluid input speed is 160ml/min, test-results sees the following form 1:
Can know by above-mentioned polishing test; Polishing fluid polishing efficiency of the present invention reaches more than the 75nm/min; Surfaceness is less than 50nm, and median size can reach 0.68 μ m, and viscosity is less than 0.03 Pa.s; Cave in the surface, the scratch aspect is respond well, reached the coordinating and unifying of polishing efficiency with the polishing precision.
Claims (10)
1. optical communication Zr0
2The ceramic insertion core precision sizing is used polishing fluid; It is characterized in that: represent with weight percent; Raw material is: the oxide compound 0.5～12% of cerium, aluminum oxide 0.1～4%, wetting regulator 0.01～0.1%, dispersion agent 0.05～2%, dispersion stabilizer 0.01～4%, cosurfactant 0.005～0.5%, surplus are deionized water.
2. polishing fluid according to claim 1; It is characterized in that: said raw material is: oxide compound 1.0～9 % of cerium, aluminum oxide 0.3～3%, wetting regulator 0.01～0.05%, dispersion agent 0.1～1.5%, dispersion stabilizer 0.01～1.5%, cosurfactant 0.01～0.1%, surplus are deionized water.
3. polishing fluid according to claim 1 is characterized in that: the oxide compound of said cerium is cerium dioxide or cerous oxide, and aluminum oxide is an Alpha-alumina.
4. polishing fluid according to claim 1 is characterized in that: the oxide compound of said 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; The aluminum oxide median size is 0.1～6.0 μ m.
5. polishing fluid according to claim 1 is characterized in that: the oxide compound of said cerium is a cerium dioxide, and the weight ratio of cerium dioxide and aluminum oxide is 3:1, and 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.
6. polishing fluid according to claim 1 is characterized in that: said wetting regulator is a kind of in aluminum nitrate, Hydrocerol A, acetic acid, hydrochloric acid, Succinic Acid and the nitric acid, or wherein two or more; Said dispersion agent is a kind of in trolamine, USP Kosher, Ucar 35 and the 1.4-butyleneglycol.
7. according to each described polishing fluid of claim 1-6, it is characterized in that: said dispersion stabilizer is a kind of in W 166, ZX-I, Z 150PH and the polyvinyl alcohol derivative; Said cosurfactant is TX10 or AEO.
8. the preparation method of the said polishing fluid of claim 1 is characterized in that: said method comprising the steps of: the oxide compound and the aluminum oxide of cerium are joined in the dispersed with stirring device, add part deionized water and wetting regulator earlier; After dispersed with stirring is even, add dispersion agent, dispersion stabilizer and cosurfactant again, stir; Add balance of deionized water again, continue stirring and obtain the uniform slurry of dispersion and emulsion, add the pH regulator agent then; Regulate pH value of slurry to 2～5; After ultrasonic dispersing, sieve, form uniform suspension-s, promptly obtain said Zr0
2The ceramic insertion core surface accurate adds uses polishing fluid.
9. preparation method according to claim 8 is characterized in that: said pH regulator agent is a kind of in thanomin, diethylolamine, the trolamine.
10. it is characterized in that according to Claim 8 or 9 described preparing methods: the amount of said part deionized water is lower than the half the of deionized water total amount.
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