Preparation method of submicron small primary crystal alpha aluminum oxide for CMP (Chemical Mechanical Polishing) solution

A ɑ-alumina, sub-micron technology, applied in the field of sub-micron small primary crystal ɑ-alumina preparation, can solve the problems of high nano-scale ɑ-alumina, high grinding costs, and large surface damage to the polished object, reducing Difficulty in grinding and impurity removal, inhibiting the growth of original crystals, and the effect of small particle size

Pending Publication Date: 2022-06-24
中铝中州铝业有限公司 +2
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Problems solved by technology

Therefore, in the prior art, some people directly grind the industrially prepared α-alumina raw powder to produce submicron-sized α-alumina, but this method not only has high grinding costs, but also is harmful to the polished object in the application of CMP polishing fluid. Larger surface damage
However, the price of nano-sized α-alumina has been high, which has certain limitations in the application of CMP polishing fluid.

Method used

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  • Preparation method of submicron small primary crystal alpha aluminum oxide for CMP (Chemical Mechanical Polishing) solution

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preparation example Construction

[0029] A kind of preparation method of submicron-level small primary crystal ɑ aluminum oxide for CMP polishing liquid, comprising the following steps:

[0030] (1) Aluminium sulfate and sintered semen are rapidly and vigorously stirred under certain conditions to obtain a highly active ultrafine seed slurry, which is then aged for use; then the aged seed slurry is added to the sintered semen as a crystal seed for a period of time. Decompose, control the decomposition temperature to be 50°C-60°C, the seed ratio is 15%-30%, and the seed ratio is the Al in the seed slurry and the semen of the sintering method 2 O 3 Then, the slurry after the first stage of decomposition is added to the semen of the sintering method as a crystal seed, and the second stage of decomposition is carried out. For a period of decomposition slurry and sintering method of Al in semen 2 O 3 The mass ratio of D50 = 0.5μm-1.2μm, the purity of > 99.6% aluminum hydroxide;

[0031] (2) washing the aluminum...

Embodiment 1

[0043] A kind of preparation method of submicron-level small primary crystal ɑ aluminum oxide for CMP polishing liquid, comprising the following steps:

[0044](1) Under certain conditions, aluminum sulfate and sintered semen are rapidly and vigorously stirred to prepare a seed slurry, and the seed slurry is added to the sintered semen as a crystal seed, and then decomposed for a period of time, and then a segment of decomposed slurry is added to the sintered semen as a The crystal seed is decomposed in two stages, wherein the decomposition temperature is 55° C., the ratio of the first stage seed is 20%, and the ratio of the second stage seed is 6%, to prepare aluminum hydroxide with D50=1.0 μm and purity > 99.6%;

[0045] (2) washing the aluminum hydroxide decomposed in step (1) to neutrality, and then preparing the filtered cake and deionized water into aluminum hydroxide slurry with a solid content of 20%, in the slurry A dispersant is also added, and the added amount of th...

Embodiment 2

[0051] A kind of preparation method of submicron-level small primary crystal ɑ aluminum oxide for CMP polishing liquid, comprising the following steps:

[0052] (1) Under certain conditions, aluminum sulfate and sintered semen are rapidly and vigorously stirred to prepare a seed slurry, and the seed slurry is added to the sintered semen as a crystal seed, and then decomposed for a period of time, and then a segment of decomposed slurry is added to the sintered semen as a The crystal seed is decomposed in two stages, wherein the decomposition temperature is 55° C., the ratio of the first stage seed is 20%, and the ratio of the second stage seed is 8%, to prepare aluminum hydroxide with D50=0.8 μm and purity > 99.6%;

[0053] (2) washing the aluminum hydroxide decomposed in step (1) to neutrality, then preparing the filtered cake and deionized water into aluminum hydroxide slurry with a solid content of 23%, in the slurry A dispersant is also added, and the added amount of the d...

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Abstract

The invention discloses a preparation method of submicron small primary crystal alpha aluminum oxide for a CMP (chemical mechanical polishing) solution, which adopts a two-stage decomposition method to directly decompose aluminum hydroxide with the average particle size D50 of 0.5-1.2 mu m and the purity of more than 99.6%, the aluminum hydroxide is small in particle size and high in purity, and the difficulty of subsequent grinding and impurity removal is reduced; the preparation method comprises the following steps: adding a composite activator into prepared aluminum hydroxide slurry, grinding by a sand mill until the average particle size D50 is 0.3-1.0 [mu] m, activating, and carrying out spray granulation on the activated aluminum hydroxide slurry to obtain false agglomerated large particles with the average particle size D50 being 35-55 [mu] m, so that the aluminum hydroxide granulated powder and the activator can fully react in the calcining process; and hard agglomeration is reduced, so that the difficulty of airflow crushing of the alpha alumina powder after subsequent calcination is reduced. By adjusting a calcining process, the aluminum hydroxide powder after spray granulation is fed into a pushed slab kiln to be calcined at the temperature of 1100-1300 DEG C, so that the purity of the calcined aluminum oxide is greater than 99.9%, the alpha conversion rate is greater than 95%, the original grain size is 0.2-0.4 mu m, and the growth of the original crystal of the aluminum oxide can be effectively inhibited.

Description

technical field [0001] The invention belongs to the technical field of alumina preparation, and in particular relates to a preparation method of submicron-scale small primary crystal ɑ alumina used for CMP polishing liquid. Background technique [0002] Chemical Mechanical Polishing (CMP) technology is currently recognized as a global planarization precision machining technology. Through the mechanical grinding action of abrasive particles in CMP polishing solution and the chemical action of oxidants, precise and non-damaged surface machining can be achieved to meet the precision of various electronic devices. Global flattening of the product. ɑ Alumina is one of the main abrasive particles used in CMP polishing liquids, which has the characteristics of high hardness and strong cutting force. The original grain size of ɑ alumina affects the polishing accuracy and cutting rate of CMP polishing liquids. [0003] At present, the α-alumina precursor obtained by removing impurit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/441C01F7/14C09G1/02
CPCC01F7/441C01F7/144C09G1/02C01P2006/80C01P2004/62C01P2004/61
Inventor 周珊张建业李烽克李志刚卫星陆健陈向前郭俊超张燕娜白琳樊浩天王涛王琳王永平李少华张军华耿淘气周志恒苏路路孙佳莹张臻常凯田佳雯
Owner 中铝中州铝业有限公司
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