CN101831244A - High-precision alumina polishing solution and preparation method thereof - Google Patents
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Abstract
The invention discloses a high-precision alumina polishing solution and a preparation method thereof. The high-precision alumina polishing solution is water-base slurry and comprises the following components in part by weight: 10-25 parts of acid pH regulator, 0.1-0.8 part of dispersing agent and 74-90 parts of high-precision alumina powder; the solid content in the weight is 0.5-20 percent; the neutral position grain diameter of the high-precision alumina polishing solution in the grain size distribution is 0.2-2.0mu m, D10 is not less than 0.5D50; D90 is not more than 2D50; and the D100 is not more than 3D50. Compared with the prior art, the polishing solution has the advantages of small alumina neutral position grain diameter, narrow grain size distribution range, high wear resistance, high polishing precision for products and the like.
Description
Technical field
The present invention relates to a kind of alumina polishing solution and preparation method thereof, or rather, is little about a kind of meta particle diameter, narrow particle size distribution, alumina polishing solution that the polishing precision is high and preparation method thereof.
Background technology
(Chemical Mechanical Polishing, CMP) technology is that this method can really make whole silicon wafer surface planarization by the new technology of IBM Corporation in the mid-80 exploitation of 20th century in chemically machinery polished.The CMP technology mainly is applied to the processing of semiconductor integrated circuit electronic chemical product and the manufacturing of precision optical system.Be different from the traditional pure machinery or the finishing method of pure chemistry, CMP by chemistry with the comprehensive action of machinery, thereby shortcomings such as the polishing velocity of having avoided the surface damage that caused by simple mechanical polishing and easily having been caused by the simplification optical polishing is slow, surface finish and polishing consistence difference are the well accepted technology of the world ten big IC (Integrate Circuit) manufactories.
In the CMP technology, chemical mechanical polishing pulp is one of key factor, and the planarization effect of CMP is had very crucial influence, so the processing method of CMP all is to carry out around the development of lapping liquid basically.The CMP polishing fluid generally can be divided into two kinds of oxide cmp liquid and metal level polishing fluids, and wherein the use of oxide cmp liquid is comparatively extensive.Present CMP polishing fluid both domestic and external mainly contains: SiO
2Polishing fluid, CeO
2Polishing fluid and Al
2O
3Polishing fluid.
Alpha-alumina relies on advantages such as its high rigidity, good stability, has been widely used in the surface finish of components and parts such as unicircuit and glass substrate; As the chemically machinery polished abrasive material, the shape of Alpha-alumina, size all directly affect polishing effect.The abrasive particle particle diameter is more little, and size-grade distribution is narrow more, and promptly homogeneity is good more.Otherwise, can cause polishing unilateral on everywhere polishing speed do not wait, make polishing inhomogeneous, influence the homogeneity of rubbing paste mass transfer and the distribution of sheet upward pressure, damage to the surface in the polishing process is more serious, not only cause surfaceness bigger, also being prone to surface imperfection such as polishing cut, pit influences polishing effect.And oarse-grained existence is considered to one of root of polishing the cut generation in the polishing material.
CN1398939A has announced a kind of polishing composition, and it comprises: (a) at least a abrasive that is selected from silicon-dioxide and aluminum oxide; (b) at least a organic compound, it is selected from polyethylene oxide, poly(propylene oxide), Voranol EP 2001, polyoxypropylene alkyl oxide, polyoxyethylene polyoxy-propylene and has C-C triple-linked polyoxyalkylene addition polymer: R wherein
1-R
6Respectively be H or C
1-10Alkyl, X and Y respectively are vinyloxy group or propenyloxy group, and m and n respectively are the positive integers of 1-20; (c) at least a compound that is selected from the acceleration polishing of twisting rib acid, oxalic acid, tartrate, glycine, α-Bing Ansuan and Histidine; (d) at least a anticorrosive agent that is selected from benzotriazole, benzoglyoxaline, triazole, imidazoles and tolytriazole; (e) hydrogen peroxide; And (f) water.
CN1316477 polishing composition that is used for memory, hard disk, said composition comprises 0.1-50% (weight) at least a abrasive material of following component (a) in the polishing composition total amount at least, is selected from silicon-dioxide, aluminum oxide, cerium oxide, zirconium white, titanium oxide, silicon nitride and Manganse Dioxide.
By as can be seen above, unified understanding is that aluminum oxide is a kind of extraordinary polishing material at present, but the size-grade distribution to polishing material does not claim, and size-grade distribution is inhomogeneous, containing macrobead causes in the polishing process damage to the surface more serious, not only cause surfaceness bigger, also be prone to polishing and draw.At present the size-grade distribution of aluminum oxide is polished requirement to high precision, not a unified understanding.
WO2007/046420 has announced a kind of ceria slurry, cerium oxide polishing slurry and the method for using its polished substrate, it provides by the dispersiveness that makes cerium oxide particles and has reached the ratio that contains that maximum rating reduces oversize particle, thereby realizes reducing polishing damage and making ceria slurry, the cerium oxide polishing slurry of polishing high speed and the method for using its polished substrate.
CN1696236A has announced the method for chemical mechanical polishing slurry and polishing substrate, and it reduces coarse grained distribution by control slurry solid content.
More than two kinds of methods by improving the dispersed ratio that contains that reduces oversize particle, but can not fundamentally remove macrobead, still exist the possibility that scratches in the use.
CN 101628728A has announced a kind of production method of white alundum hyperfine abrasive micropowder, at the micro mist below 40 microns, adopts the classification of waterpower settling process for particle diameter, classification is carried out from fine to coarse, divide earlier thin level other, the back divide thick level other, finish until whole classifications.The stage division of this invention is when pulp density, settling time, siphon height are controlled in strictness, added dispersion agent efficiently, the molecule of dispersion agent interts in water between agglomerating particles, the bag be attached to all particulates that vary in size around, be subjected to the repulsion of dispersant molecule electric charge, or else particulate can be reunited together, both made the fractionated precision improve, make the finished product can keep loose condition (of surface) again.
CN 1587055A discloses a kind of low glass powder Alpha-alumina, comprises the ball milling and the hydrocyclone classification of aluminum oxide, but how classification does not describe in detail, and the product granularity that obtains simultaneously is bigger, is the 200-250 order.
As seen from the above, aluminum oxide grain size distributes the influence of polishing precision is not had unified understanding, the oarse-grained method of controlled oxidation aluminium is mainly by dilution and reduces shared ratio or the wet classification by growing up based on gravity settling of macrobead simultaneously: mixing liquid is in settling tank, the solid particulate that density is big sinks at the bottom of the pond under action of gravity lentamente, and the less relatively liquid of density is in the superiors.Yet gravity settling separation is chronic, can not satisfy the controlled requirement of industrialized production sharp separation and separating resulting.
Summary of the invention
The object of the present invention is to provide a kind of high-precision alumina polishing solution and preparation method thereof,, overcome the above-mentioned defective that prior art exists to solve the requirement of commerce to the polishing precision of increasingly stringent.
High-precision alumina polishing solution of the present invention, for a kind of water-soluble serous, feature is the component that contains following weight part:
Acidic ph modifier 10-25 part
Dispersion agent 0.1-0.8 part
High-precision alumina powder 74-90 part
The weight solid content is 0.5-20%;
Described acidic ph modifier is selected from one or more of aluminum soluble salts such as nitric acid, hydrochloric acid, acetic acid or aluminum nitrate, aluminum chloride, Tai-Ace S 150 etc., preferred aluminum soluble salt;
Described dispersion agent is selected from one or more in Macrogol 2000 0, sodium polyacrylate, Sodium hexametaphosphate 99, hexadecyl trimethyl ammonium bromide or the sodium lauryl sulphate, preferred Sodium hexametaphosphate 99;
Described high-precision alumina powder, meta particle diameter D
50Be 0.2～2.0 μ m, and satisfy: D
10〉=0.5D
50D
90≤ 2D
50D
100≤ 3D
50The granularity testing method of described polishing fluid is meant the size-grade distribution that the laser particle analyzer with the laser light scattering principle records.
The preparation method of high-precision alumina polishing solution of the present invention comprises the steps:
With raw material Alpha-alumina and water making beating, adopt the waterpower centrifugal classification then, obtain described aluminum oxide polishing powder;
Described raw material Alpha-alumina meta particle diameter D
50＜2.0 μ m, wherein, the weight percent of Alpha-alumina crystal formation accounts for more than 95%;
Concrete, comprise following concrete steps:
(1) waterpower centrifugal classification: with meta particle diameter D
50The Alpha-alumina of＜2.0 μ m mixes making beating with water, obtain slurries, and the weight solid content of described slurries is 5%～40%, adopts the waterpower centrifugal classification then, collects the slurries C ' and the slurries D ' of the Alpha-alumina that contains the different grain size distribution;
The size-grade distribution of slurries C ' is as follows: D
50=1.5 ± 0.2 μ m, D
10〉=0.5D
50, D90≤2D
50, D
100≤ 3D
50
The size-grade distribution of slurries D ' is as follows: D
50=0.5 ± 0.2 μ m, D
10〉=0.5D
50, D
90≤ 2D
50, D
100≤ 3D
50
Described waterpower centrifugal classification is the whizzer that the liquid-solid phase particles that different densities is immiscible of mat centrifugal settling speed separates.Immiscible liquid-the solid phase particles of different densities enters in the rotary drum of high speed rotating, under powerful effect of centrifugal force, and size particles subsidence rate difference, macrobead outwards moves, and accumulates in the perisporium of rotary drum, discharges from the bottom of the drum with slurries; And small-particle is got rid of from rotary drum top with slurries at internal layer.Different slurries separated deposit respectively through multiple fractionation, meet the requirements until all prods size-grade distribution, obtain the product of different stage;
Described stage equipment is general equipment, as butterfly centrifugal separating machine or horizontal spiral separating machine, as the DBS500 butterfly separating machine of the green Sheng separating machine in Nanjing company limited;
(2) drying: with the slurries collected at 100～200 ℃ of drying 6～12h;
(3) fragmentation: the product that step (2) is obtained is through comminution by gas stream, and the broken agglomerating particles that causes because of oven dry until the 500 eye mesh screens no screen overflow in back that sieves, obtains aluminum oxide polishing powder;
(4) preparation of high-precision alumina polishing solution:
Described high accuracy aluminum oxide polishing powder, acidic ph modifier, dispersion agent and water are mixed, disperse, get final product product;
Described dispersion is preferably carried out in high-speed shearing machine, and described high-speed shearing machine is a kind of general product, is the product of GFJ-2.2 and product that EHSY Western Regions model is QSJ-20 etc. as Shanghai Hua Yan Instrument and Equipment Company model; Jitter time is preferably 1-2h;
Compared with prior art, high-precision alumina polishing solution provided by the invention, it is little to have an alumina neutral position particle diameter, and particle size distribution is narrow, wear resistance height, goods precision advantages of higher.
Description of drawings
Fig. 1 is an Alpha-alumina A particle size distribution figure among the embodiment 1.
Fig. 2 is an alpha-oxidation aluminum shot B particle size distribution figure among the embodiment 1.
Fig. 3 is the particle size distribution figure of aluminum oxide polishing powder target product C among the embodiment 1.
Fig. 4 is the particle size distribution figure of aluminum oxide polishing powder target product D among the embodiment 1.
Fig. 5 is an Alpha-alumina A particle size distribution figure among the embodiment 2.
Embodiment
Among the embodiment, high-speed shearing machine is the diligent industry chemical machinery GF-250 of company limited of a Jiangyin City high speed dispersor, and micronizer mill is the OYF-400 of a Kunshan MiYou Industry Co.,Ltd micronizer mill
The granularity testing method is to adopt the laser particle analyzer of laser light scattering principle to record, and adopts Zhuhai American-European gram LS-POP (VI) type laser particle analyzer.
The preparation of high-precision alumina
(1) preparation of Alpha-alumina: (the grain size characteristic parameter is as follows: D with commercially available Alpha-alumina A
10: 2.50 μ m, D
25: 3.65 μ m, D
50: 5.42 μ m, D
75: 8.07 μ m, D
90: 12.43 μ m, D
(3,2): 4.64 μ m, D
(4,3): 6.48 μ m) through comminution by gas stream, must be suitable for fractionated alumina product B.B grain size characteristic parameter is as follows: D
10: 0.79 μ m, D
25: 1.13 μ m, D
50: 1.71 μ m, D
75: 2.61 μ m, D
90: 3.88 μ m, D
(3,2): 1.46 μ m, D
(4,3): 2.02 μ m.
(2) waterpower centrifugal classification: with B and water mechanically mixing, be made into slurries, the weight solid content is 40%, through the classification of DBS500 butterfly separating machine repeated centrifugation, obtains slurries C ' and slurries D ' that different grain size distributes respectively;
The size-grade distribution of slurries C ' is as follows: D
50=1.5 ± 0.2 μ m, D
10〉=0.5D
50, D90≤2D
50, D
100≤ 3D
50
The size-grade distribution of slurries D ' is as follows: D
50=0.5 ± 0.2 μ m, D
10〉=0.5D
50, D90≤2D
50, D
100≤ 3D
50
(3) drying: with the slurries of gained in (2) at 100 ℃ of dry 12h
(4) fragmentation: (3) step product is pulverized through the eddy current type micronizer mill, got high accuracy aluminum oxide polishing powder C and D that different grain size of the present invention distributes.
Laser particle analyzer test gained sample C size-grade distribution is seen Fig. 3, D
10: 0.78 μ m, D
25: 1.04 μ m, D
50: 1.40 μ m, D
75: 1.81 μ m, D
90: 2.16 μ m, D
100: 3.50 μ m, D
(3,2): 1.25 μ m, D
(4,3): 1.45 μ m; D
10/ D
50=0.56, D
90/ D
50=1.54, D
100/ D
50=2.50.
Laser particle analyzer test gained sample D size-grade distribution is seen Fig. 4: D
10: 0.26 μ m, D
25: 0.35 μ m, D
50: 0.47 μ m, D
75: 0.59 μ m, D
90: 0.70 μ m, D
100: 1.35 μ m, D
(3,2): 0.41 μ m, D
(4,3): 0.48 μ m; D
10/ D
50=0.55, D
90/ D
50=1.49, D
100/ D
50=2.87.
The preparation of high-precision alumina
(1) preparation of Alpha-alumina: select commercial alumina A for use, (the grain size characteristic parameter is as follows: D
10: 0.70 μ m, D
25: 0.89 μ m, D
50: 1.28 μ m, D
75: 1.85 μ m, D
90: 2.55 μ m, D
100: 13.31 μ m, D
(3,2): 1.17 μ m, D
(4,3): 1.56 μ m).See Fig. 5.
(2) waterpower centrifugal classification: it is 5% that A and water mechanically mixing are made into slurry solid content, through the classification of DBS500 butterfly separating machine repeated centrifugation, obtains slurries C ' and slurries D ' that different grain size distributes respectively;
The size-grade distribution of slurries C ' is as follows: D
50=1.5 ± 0.2 μ m, D
10〉=0.5D
50, D90≤2D
50, D
100≤ 3D
50
The size-grade distribution of slurries D ' is as follows: D
50=0.5 ± 0.2 μ m, D
10〉=0.5D
50, D90≤2D
50, D
100≤ 3D
50
(3) drying: with the slurries of gained in (2) at 200 ℃ of dry 6h;
(4) fragmentation: the product of step (3) is pulverized through the eddy current type micronizer mill, got high accuracy aluminum oxide polishing powder C and D that different grain size of the present invention distributes.
Embodiment 3
The preparation of high-precision alumina polishing solution:
74.2 products C, 25 parts of aluminum chloride among the embodiment 1 of part weight, the sodium lauryl sulphate of 0.8 part of weight, it is 0.5% slurries that water is mixed with the weight solid content, adopts high-speed shearing machine to shear and disperses 2h, obtains target product.
The preparation of high-precision alumina polishing solution:
81.5 it is 20% slurries that product D, 18 parts of acetic acid among the embodiment 1 of part weight, the sodium polyacrylate of 0.5 part of weight, water are mixed with solid content, adopts high-speed shearing machine to shear and disperses 1.5h, obtains target product.
The preparation of high-precision alumina polishing solution:
86.4 products C, 13 parts of hydrochloric acid among the embodiment 1 of part weight, the sodium lauryl sulphate of 0.6 part of weight, it is 5% slurries that water is mixed with solid content, adopts high-speed shearing machine to shear and disperses 1.5h, obtains target product.
Embodiment 6
Serves as the polishing object with embodiment 3 polishing fluid products with laser-optical disk stamper glass CD-ROM, polishes test (equipment pressure: 26Mpa, rotating speed 650r/min) through Unipol polishing trier.The roughness of polishing back product is
Do not have and scratch.
Embodiment 7
Serves as the polishing thing with embodiment 4 polishing fluid products with laser-optical disk stamper glass LD, polishes test (equipment pressure: 26Mpa, rotating speed 650r/min) through Unipol polishing trier.The roughness of polishing back product is
Do not have and scratch.
Comparative Examples 1
With commercial alumina A, 25 parts of aluminum chloride in the enforcement 2 of 74.2 parts of weight, the sodium lauryl sulphate of 0.8 part of weight, it is 0.5% slurries that water is mixed with the weight solid content, adopts high-speed shearing machine to shear and disperses 2h, obtains target product.With laser-optical disk stamper glass CD-ROM is the polishing object, polishes test (equipment pressure: 26Mpa, rotating speed 650r/min) through Unipol polishing trier.The roughness of polishing back product is
Obvious scuffing is arranged.
Claims (6)
1. high-precision alumina polishing solution is characterized in that, for a kind of water-soluble serous, contains the component of following weight part:
Acidic ph modifier 10-25 part
Dispersion agent 0.1-0.8 part
High-precision alumina powder 74-90 part
The weight solid content is 0.5-20%.
2. alumina polishing solution according to claim 1 is characterized in that described acidic ph modifier is selected from nitric acid, hydrochloric acid, acetic acid or aluminum soluble salt.
3. alumina polishing solution according to claim 2 is characterized in that described aluminum soluble salt is selected from one or more in aluminum nitrate, aluminum chloride or the Tai-Ace S 150.
4. alumina polishing solution according to claim 1 is characterized in that described dispersion agent is selected from one or more in Macrogol 2000 0, sodium polyacrylate, Sodium hexametaphosphate 99, hexadecyl trimethyl ammonium bromide or the sodium lauryl sulphate.
5. according to each described alumina polishing solution of claim 1～4, it is characterized in that described high-precision alumina powder, meta particle diameter D
50Be 0.2～2.0 μ m, and satisfy: D
10〉=0.5D
50D
90≤ 2D
50D
100≤ 3D
50
6. the preparation method of each described alumina polishing solution of claim 1～5 comprises the steps: high accuracy aluminum oxide polishing powder, acidic ph modifier, dispersion agent and water are mixed, and disperses, get final product product.
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| CN103911617A (en) * | 2014-03-13 | 2014-07-09 | 深圳市宇泰隆科技有限公司 | A silicon oxide polishing solution and a preparation method thereof |
| CN103937413A (en) * | 2014-03-21 | 2014-07-23 | 深圳市宇泰隆科技有限公司 | Aluminum oxide polishing solution for alloy polishing and preparation method thereof |
| CN103952084A (en) * | 2014-04-29 | 2014-07-30 | 德米特（苏州）电子环保材料有限公司 | Preparation method of metal polishing solution with alumina matrix |
| CN105506638A (en) * | 2015-12-21 | 2016-04-20 | 黄志华 | Polishing liquid for metallographic analysis and preparation method and application method thereof |
| CN106479371A (en) * | 2016-08-15 | 2017-03-08 | 惠州市米特仑科技有限公司 | A kind of high precision composite polishing liquid and preparation method thereof |
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| CN109867298A (en) * | 2019-04-21 | 2019-06-11 | 左海珍 | A kind of chemical mechanical polishing liquid aluminium oxide and its preparation process |
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| CN103911617A (en) * | 2014-03-13 | 2014-07-09 | 深圳市宇泰隆科技有限公司 | A silicon oxide polishing solution and a preparation method thereof |
| CN103937413A (en) * | 2014-03-21 | 2014-07-23 | 深圳市宇泰隆科技有限公司 | Aluminum oxide polishing solution for alloy polishing and preparation method thereof |
| CN103952084A (en) * | 2014-04-29 | 2014-07-30 | 德米特（苏州）电子环保材料有限公司 | Preparation method of metal polishing solution with alumina matrix |
| CN103952084B (en) * | 2014-04-29 | 2016-03-23 | 德米特（苏州）电子环保材料有限公司 | A kind of preparation method of metal-polishing liquid of alumina host |
| CN106566412A (en) * | 2015-09-25 | 2017-04-19 | 气体产品与化学公司 | Stop-on silicon containing layer additive |
| CN105506638A (en) * | 2015-12-21 | 2016-04-20 | 黄志华 | Polishing liquid for metallographic analysis and preparation method and application method thereof |
| CN105506638B (en) * | 2015-12-21 | 2018-07-06 | 黄志华 | A kind of Metallographic Analysis polishing fluid and preparation method thereof, application method |
| CN106479371A (en) * | 2016-08-15 | 2017-03-08 | 惠州市米特仑科技有限公司 | A kind of high precision composite polishing liquid and preparation method thereof |
| CN106497435A (en) * | 2016-10-21 | 2017-03-15 | 过冬 | A kind of Metallographic Analysis polishing fluid and preparation method thereof, using method |
| CN109401630A (en) * | 2017-08-18 | 2019-03-01 | 昌宏精密刀具（东莞）有限公司 | A kind of aluminium alloy anode oxide film mirror finish liquid and preparation method thereof |
| CN108034361A (en) * | 2017-12-21 | 2018-05-15 | 惠州市米特仑科技有限公司 | A kind of preparation method of acidic alumina polishing fluid |
| US11674065B2 (en) | 2018-08-10 | 2023-06-13 | Saint-Gobain Ceramics & Plastics, Inc. | Composition including a plurality of abrasive particles and method of using same |
| CN109867298A (en) * | 2019-04-21 | 2019-06-11 | 左海珍 | A kind of chemical mechanical polishing liquid aluminium oxide and its preparation process |
| CN110040737A (en) * | 2019-04-21 | 2019-07-23 | 左海珍 | A kind of preparation process for preparing aluminium oxide and aoxidizing silicon polishing raw material |
| CN109867298B (en) * | 2019-04-21 | 2021-07-30 | 湖南恒源精密陶瓷有限公司 | Alumina for chemical mechanical polishing solution and preparation process thereof |
| CN110524315A (en) * | 2019-08-07 | 2019-12-03 | 大连理工大学 | A kind of green economy environment protection chemical mechanical polishing method of optical quartz glass |
| CN115431131A (en) * | 2022-11-08 | 2022-12-06 | 德米特（苏州）电子环保材料有限公司 | Polishing method of resin lens, aluminum oxide polishing powder and preparation method of aluminum oxide polishing powder |
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Application publication date: 20100915 |