CN103589344B - Method for preparing alumina polishing solution - Google Patents

Method for preparing alumina polishing solution Download PDF

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Publication number
CN103589344B
CN103589344B CN201310567464.6A CN201310567464A CN103589344B CN 103589344 B CN103589344 B CN 103589344B CN 201310567464 A CN201310567464 A CN 201310567464A CN 103589344 B CN103589344 B CN 103589344B
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alumina
solution
acidic
stirring
dispersion liquid
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CN103589344A (en
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王良咏
刘卫丽
宋志棠
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Shanghai Xin'anna Electronic Technology Co ltd
Shanghai Institute of Microsystem and Information Technology of CAS
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Shanghai Xin'anna Electronic Technology Co ltd
Shanghai Institute of Microsystem and Information Technology of CAS
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Abstract

The invention relates to a method for preparing an alumina polishing solution. The method comprises the steps as follows: firstly, alumina powder is stirred to be dispersed in an acidic aqueous solution, and an acidic alumina dispersion solution is formed; then under the condition of heated stirring, a silicate aqueous solution is added dropwise, and heating is stopped after adding is finished; and the alumina polishing solution can be obtained through follow-up stirring and ageing. On the basis of the alumina dispersion solution, silicate is introduced, the unique affinity interaction between silicon and aluminum is used, and partial silicon atom substitution and charge reversals are formed on surfaces of alumina particles, so that the suspension stability of the alumina polishing solution is effectively improved, and meanwhile, the polishing performance is not affected.

Description

A kind of preparation method of alumina polishing solution
Technical field
The present invention relates to a kind of preparation method of alumina polishing solution, belong to chemical mechanical polishing liquid field.
Background technology
Aluminum oxide is because its matter is hard, physics cutting force is large, and its chemical mechanical polishing liquid is widely used in substrate material and unicircuit chemistry mechanical polishing process.For substrate material require high polishing speed to remove the certain working (machining) efficiency required by physical abuse and unicircuit mechanically resistant material, alumina polishing solution is essential.But meanwhile, alumina polishing solution free settling, easily to reunite, easily produce new scratch damage after a polish, and affect its polishing performance stability.
For this defect, conventional method introduces tensio-active agent in alumina polishing solution, make its alumina surface formed sterically hindered and increase alumina surface with electric charge, thus improve the suspension stability of alumina particle.But the fatal problem of this method is, while being introduced in of tensio-active agent improves alumina stable, usually greatly can reduces polishing speed, also can produce a large amount of foam, cause the problems such as bacterial growth.
Inventor herein is on the basis of alumina fluid dispersion, by introducing silicate, utilize affinity interaction unique between Silicified breccias, charge reversal alternative at Membranes On Alumina Particles Surface forming section Siliciumatom, thus greatly improve the suspension stability of alumina polishing solution.The method is while raising alumina polishing solution stability, and because not containing tensio-active agent, thus the polishing speed avoided existing for conventional polishing fluid improved stability method reduces, there is a large amount of foam and easily grow the problems such as bacterium.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of alumina polishing solution, can effectively improve alumina polishing solution suspension stability.
The present invention is achieved by the following technical solutions:
A preparation method for alumina polishing solution, comprises the following steps:
(1) by alumina powder through dispersed with stirring in acidic aqueous solution, form acidic alumina dispersion liquid;
(2) under condition of heating and stirring, drip aqueous silicate solution, dropwise rear stopping heating;
(3) continue stir ageing and get final product.
Wherein,
Preferably, the particle diameter of described alumina powder is 0.01-40um; Small particle size alumina particle (≤100nm), is mainly used in semiconductor film glossing, as metal W; Large stone alumina particle (100nm-40um), is mainly used in substrate glossing, as mobile phone aluminium backboard.
Preferably, described in step (1), acidic aqueous solution is the aqueous solution of pH adjusting agent, and described pH adjusting agent is selected from phosphoric acid, nitric acid, sulfuric acid, acetic acid, citric acid, hydrochloric acid and tartrate.Metallic substance in acid condition, has the feature that polishing speed is fast usually.Different pH value regulator not only affects polishing speed, also has larger impact to the stability of alumina polishing solution.
Preferably, the general formula of described silicate is M 2o.SiO 2, wherein M is Li +, Na +, K +or NH 4 +.Different silicate, its zwitterion hydration radius, ionization degree, to alumina surface aluminium atom the degree that replaces by Siliciumatom and the absorption to metallic cation, all have a great impact, thus affect the degree that alumina surface positive charge reverses to negative charge, to such an extent as to finally affect the stability of alumina polishing solution.
Preferably, described water is deionized water.
Preferably, in acidic alumina dispersion liquid described in step (1), the concentration of aluminum oxide is 0.1 ~ 40wt%, and pH value is 1 ~ 4.
Preferably, in step (2), atmospheric agitation heats and keeps boiling, then adds aqueous silicate solution with the speed of 1 ~ 200ml/min.
Preferably, in step (2), the concentration of described aqueous silicate solution is 0.1 ~ 5wt%.
Preferably, the mass ratio of described aqueous silicate solution and described acidic alumina dispersion liquid is 1:2 ~ 1:100.
Preferably, in step (3), the time of described stirring ageing is 0.5-24 hour, is preferably 24 hours.
The alumina polishing solution obtained by above-mentioned preparation method, suspension stability improves greatly.
Technique effect of the present invention and advantage are:
The present invention, by introducing silicate in alumina polishing solution, utilizes affinity interaction unique between Silicified breccias, charge reversal alternative at Membranes On Alumina Particles Surface forming section Siliciumatom, thus greatly improves the suspension stability of alumina polishing solution.The method is while raising alumina polishing solution stability, and because not containing tensio-active agent, thus the polishing speed avoided existing for conventional polishing fluid improved stability method reduces, there is a large amount of foam and easily grow the problems such as bacterium.
Embodiment
Below by way of specific specific examples, technical scheme of the present invention is described.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.And, except as otherwise noted, the numbering of various method steps is only the convenient tool differentiating various method steps, but not be ordering or the enforceable scope of restriction the present invention of restriction various method steps, the change of its relativeness or adjustment, when changing technology contents without essence, when being also considered as the enforceable category of the present invention.
Embodiment 1:
Prepare a kind of alumina polishing solution:
Get the alumina powder that particle diameter is 0.01um, through dispersed with stirring in the aqueous solution, to make alumina concentration be 20wt%, pH be 7 alumina fluid dispersion;
Alumina polishing solution stability and polishing performance result as shown in table 1.
Embodiment 2:
Prepare a kind of alumina polishing solution
(1) get the alumina powder that particle diameter is 0.01um, through dispersed with stirring in second aqueous acid, to make alumina concentration be 20wt%, pH be 4 acidic alumina dispersion liquid;
(2) heat above-mentioned acidic alumina dispersion liquid under normal pressure and maintain the temperature at more than boiling temperature, then dripping with the speed of 200ml/min the K that concentration is 0.1wt% 2siO 3the aqueous solution (K 2siO 3the aqueous solution and the mass ratio of acidic alumina dispersion liquid be 1:2), dropwise rear stopping heating;
(3) continue under normal temperature stir ageing 24 hours and get final product.Alumina polishing solution stability and polishing performance result as shown in table 1.
Embodiment 3:
Prepare a kind of alumina polishing solution:
(1) get the alumina powder that particle diameter is 0.01um, through dispersed with stirring in salt aqueous acid, to make alumina concentration be 40wt%, pH be 1 acidic alumina dispersion liquid;
(2) heat above-mentioned acidic alumina dispersion liquid under normal pressure and maintain the temperature at more than boiling temperature, then dripping with the speed of 1ml/min the Na that concentration is 3wt% 2siO 3the aqueous solution (Na 2siO 3the aqueous solution and the mass ratio of acidic alumina dispersion liquid be 1:50), dropwise rear stopping heating;
(3) continue under normal temperature stir ageing 24 hours and get final product.
Alumina polishing solution stability and polishing performance result as shown in table 1.
Embodiment 4:
Prepare a kind of alumina polishing solution:
Get the alumina powder that particle diameter is 40um, through dispersed with stirring in the aqueous solution, to make alumina concentration be 10wt%, pH be 7 alumina fluid dispersion;
Alumina polishing solution stability and polishing performance result as shown in table 1.
Embodiment 5:
Prepare a kind of alumina polishing solution:
(1) get the alumina powder that particle diameter is 40um, through dispersed with stirring in phosphorus aqueous acid, to make alumina concentration be 10wt%, pH be 4 acidic alumina dispersion liquid;
(2) heat above-mentioned acidic alumina dispersion liquid under normal pressure and maintain the temperature at more than boiling temperature, then dripping concentration for 5wt%Li with the speed of 50ml/min 2siO 3the aqueous solution (Li 2siO 3the aqueous solution and the mass ratio of acidic alumina dispersion liquid be 1:20), dropwise rear stopping heating;
(3) continue under normal temperature stir ageing 24 hours and get final product.
Alumina polishing solution stability and polishing performance result as shown in table 1.
Embodiment 6:
Prepare a kind of alumina polishing solution:
(1) get the alumina powder that particle diameter is 40um, through dispersed with stirring in the tartaric aqueous solution, to make alumina concentration be 10wt%, pH be 4 acidic alumina dispersion liquid;
(2) heat above-mentioned acidic alumina dispersion liquid under normal pressure and keep boiling, then dripping with the speed of 50ml/min the K that concentration is 5wt% 2siO 3the aqueous solution (K 2siO 3the aqueous solution and the mass ratio of acidic alumina dispersion liquid be 1:20), dropwise rear stopping heating;
(3) continue under normal temperature stir ageing 24 hours and get final product.
Alumina polishing solution stability and polishing performance result as shown in table 1.
Embodiment 7:
Prepare a kind of alumina polishing solution:
(4) get the alumina powder that particle diameter is 40um, through dispersed with stirring in lemon aqueous acid, to make alumina concentration be 10wt%, pH be 4 acidic alumina dispersion liquid;
(5) heat above-mentioned acidic alumina dispersion liquid under normal pressure and maintain the temperature at more than boiling temperature, then dripping with the speed of 50ml/min (the NH that concentration is 5wt% 4) 2siO 3the aqueous solution (NH 4) 2siO 3water-soluble
The mass ratio of liquid and acidic alumina dispersion liquid is 1:100, dropwises rear stopping heating;
(6) continue under normal temperature stir ageing 24 hours and get final product.
Alumina polishing solution stability and polishing performance result as shown in table 1.
The alumina polishing solution stability that table 1 embodiment 1-7 is obtained and polishing performance test result
As can be seen from Table 1, for the alumina polishing solution of particle diameter 0.01-40um, after silicate modified, its stability all has the raising of different amplitude; And because its dispersiveness improves, its corresponding polishing speed all has lifting.

Claims (4)

1. an alumina polishing solution, is obtained by the preparation method of described alumina polishing solution, comprises the following steps:
(1) by alumina powder through dispersed with stirring in acidic aqueous solution, form acidic alumina dispersion liquid;
The particle diameter of described alumina powder is 0.01-40 μm; In described acidic alumina dispersion liquid, the concentration of aluminum oxide is 0.1 ~ 40wt%, and pH value is 1 ~ 4;
(2) under condition of heating and stirring, drip aqueous silicate solution, dropwise rear stopping heating;
The concentration of described aqueous silicate solution is 0.1 ~ 5wt%; Atmospheric agitation heats and keeps boiling, then adds aqueous silicate solution with the speed of 1 ~ 200mL/min; The mass ratio of described aqueous silicate solution and described acidic alumina dispersion liquid is 1:2 ~ 1:100; The general formula of described silicate is M 2o.SiO 2, wherein M is Li +, Na +, K +or NH 4 +;
(3) continue stir ageing and get final product;
The time of described stirring ageing is 0.5-24 hour.
2. alumina polishing solution as claimed in claim 1, it is characterized in that, described in step (1), acidic aqueous solution is the aqueous solution of pH adjusting agent, and described pH adjusting agent is selected from phosphoric acid, nitric acid, sulfuric acid, acetic acid, citric acid, hydrochloric acid and tartrate.
3. a preparation method for alumina polishing solution, comprises the following steps:
(1) by alumina powder through dispersed with stirring in acidic aqueous solution, form acidic alumina dispersion liquid;
The particle diameter of described alumina powder is 0.01-40 μm; In described acidic alumina dispersion liquid, the concentration of aluminum oxide is 0.1 ~ 40wt%, and pH value is 1 ~ 4;
(2) under condition of heating and stirring, drip aqueous silicate solution, dropwise rear stopping heating;
The concentration of described aqueous silicate solution is 0.1 ~ 5wt%; Atmospheric agitation heats and keeps boiling, then adds aqueous silicate solution with the speed of 1 ~ 200mL/min; The mass ratio of described aqueous silicate solution and described acidic alumina dispersion liquid is 1:2 ~ 1:100; The general formula of described silicate is M 2o.SiO 2, wherein M is Li +, Na +, K +or NH 4 +;
(3) continue stir ageing and get final product;
The time of described stirring ageing is 0.5-24 hour.
4. the preparation method of a kind of alumina polishing solution as claimed in claim 3, it is characterized in that, described in step (1), acidic aqueous solution is the aqueous solution of pH adjusting agent, and described pH adjusting agent is selected from phosphoric acid, nitric acid, sulfuric acid, acetic acid, citric acid, hydrochloric acid and tartrate.
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CN106010297B (en) * 2016-06-20 2018-07-31 上海新安纳电子科技有限公司 A kind of preparation method of alumina polishing solution
CN108336218B (en) * 2018-01-29 2021-12-07 长安大学 Piezoelectric composite material for road and preparation method thereof
CN109021834A (en) * 2018-08-29 2018-12-18 德米特（苏州）电子环保材料有限公司 A kind of resin lens polishing fluid of alumina host and preparation method thereof
CN115746713B (en) * 2022-12-07 2024-05-17 安徽大学 High stability suspension Al2O3Polishing solution and preparation method thereof

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CN1850916A (en) * 2006-05-26 2006-10-25 上海大学 Method for preparing alumina/monox composite mill grain
WO2007047261A1 (en) * 2005-10-18 2007-04-26 3M Innovative Properties Company Agglomerate abrasive grains and methods of making the same
WO2007124905A2 (en) * 2006-04-28 2007-11-08 Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh Abrasive grain based on melted spherical corundum
CN101372560A (en) * 2008-10-15 2009-02-25 中国科学院上海微***与信息技术研究所 Grinding medium for chemico-mechanical polishing and preparation thereof
CN101547861A (en) * 2006-10-04 2009-09-30 纳尔科公司 Silica-coated metal oxide sols having variable metal oxide to silica ration

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Publication number Priority date Publication date Assignee Title
WO2007047261A1 (en) * 2005-10-18 2007-04-26 3M Innovative Properties Company Agglomerate abrasive grains and methods of making the same
WO2007124905A2 (en) * 2006-04-28 2007-11-08 Center For Abrasives And Refractories Research & Development C.A.R.R.D. Gmbh Abrasive grain based on melted spherical corundum
CN1850916A (en) * 2006-05-26 2006-10-25 上海大学 Method for preparing alumina/monox composite mill grain
CN101547861A (en) * 2006-10-04 2009-09-30 纳尔科公司 Silica-coated metal oxide sols having variable metal oxide to silica ration
CN101372560A (en) * 2008-10-15 2009-02-25 中国科学院上海微***与信息技术研究所 Grinding medium for chemico-mechanical polishing and preparation thereof

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