CN113150742B - Preparation method of abrasive for silicon-aluminum chemical mechanical polishing - Google Patents
Preparation method of abrasive for silicon-aluminum chemical mechanical polishing Download PDFInfo
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- CN113150742B CN113150742B CN202110227352.0A CN202110227352A CN113150742B CN 113150742 B CN113150742 B CN 113150742B CN 202110227352 A CN202110227352 A CN 202110227352A CN 113150742 B CN113150742 B CN 113150742B
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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Abstract
The invention discloses a preparation method of an abrasive for silicon-aluminum chemical mechanical polishing, which comprises the following steps: preparing silicon aluminum oxide by using water glass and aluminum salt solution, and keeping the pH value of the system to be neutral in the synthesis process; adding dilute sulfuric acid into the silicon aluminum oxide to enable part of aluminum species to migrate to the particle surface, aging, cooling and filtering to obtain a filter cake; washing the filter cake to reduce the content of sodium ions and sulfate radicals of the silicon dioxide in the filter cake; and re-dispersing the washed filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling and classification to obtain the abrasive for silicon-aluminum chemical mechanical polishing. According to the preparation method, liquid phase synthesis is adopted, neutral pH is adopted in the synthesis process, so that silicon-aluminum species are uniformly distributed, meanwhile, acidic treatment and washing are adopted, the surface precipitation of the aluminum species is controlled, a controllable aluminum coated silicon structure is formed, and the application range of chemical mechanical polishing of the obtained abrasive is improved.
Description
Technical Field
The invention relates to the technical field of preparation of precision polishing abrasives, in particular to a preparation method of an abrasive for silicon-aluminum chemical mechanical polishing.
Background
Chemical mechanical polishing is a process widely used in the microelectronics field, and is a very necessary process both in the polishing of substrates and in the fabrication of integrated circuits. Taking semiconductor chip fabrication as an example, integrated circuits are mass-produced by fabricating thousands of identical circuit patterns on one semiconductor wafer and then dividing these circuit patterns into identical chips. To produce integrated circuits, materials need to be modified, removed, and deposited on a semiconductor wafer. After each deposition or removal step, the surface needs to be polished by a combination of chemical and mechanical forces, known as chemical mechanical polishing, to smooth, planarize and clean the surface.
Common abrasives for chemical mechanical polishing include cerium oxide, aluminum oxide, and silicon oxide. The aluminum oxide has high Mohs hardness and high polishing speed, but is difficult to disperse into uniform spheres, and surface scratches are easily caused; the silicon oxide has lower Mohs hardness, small polishing rate, but good dispersibility and stability. In view of the harsh requirements of chemical mechanical polishing on the abrasive, the advantages and disadvantages of the alumina and silicon oxide abrasive can be utilized, the advantages and disadvantages are overcome, and various silicon-aluminum composite abrasive can be manufactured.
A method for preparing a composite abrasive of alumina coated with silica is described in patent CN 1850916. The hardness of the abrasive is reduced by coating the silica, so that scratches on the polished surfaces of hard disks and glass substrates can be reduced, but this preparation method makes it difficult to achieve uniformity of the silica in water by dispersing the alumina. Patent CN1635043 describes the use of a polishing liquid of alumina-coated silica, but does not describe the preparation method thereof. In the patent CN101490200, firstly, high-dispersion silica colloid is prepared, and then an organic or inorganic aluminum source is used for coating, so that the silicon-aluminum composite abrasive with better performance is obtained. In patent CN101372560, nano silicon oxide abrasive is used as a base material, and silicon aluminum is coated at the later stage to obtain the silicon aluminum composite abrasive, but the synthetic method is complex. In the patent CN111073518, firstly, an alumina precursor solution is prepared, ethyl orthosilicate is dripped into the alumina precursor solution, and after ageing, zinc fluoride and alumina are added for high-temperature roasting, so as to obtain the silicon-aluminum composite abrasive. For non-surface coated silica alumina composite abrasives. Patent CN104046245 describes mixing and stirring a prepared silica polishing liquid and an alumina polishing liquid uniformly for polishing sapphire. The silicon-aluminum composite abrasive is prepared directly by a combustion hydrolysis method after the silicon-aluminum precursors are mixed in the patent CN1272455, and the cost for preparing the silicon-aluminum composite abrasive is high.
In the prior art, the coated silicon-aluminum composite abrasive is mostly used, but the general preparation process of the product is complex, the control requirement on the preparation process is high, and the non-coated silicon-aluminum composite abrasive has the following problems: firstly, mechanical mixing is difficult to fully embody the advantages of the silicon-aluminum composite abrasive; and secondly, the preparation is carried out by adopting a combustion hydrolysis method, and the production cost is high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of an abrasive for silicon-aluminum chemical mechanical polishing, which adopts liquid phase synthesis, uniformly distributes silicon-aluminum species in the synthesis process through neutral pH control, and simultaneously performs acidic treatment and washing to control the surface precipitation of the aluminum species, so as to form a controllable aluminum-coated silicon structure and improve the application range of the obtained abrasive for chemical mechanical polishing.
The invention is realized by adopting the following technical scheme:
the preparation method of the abrasive for silicon-aluminum chemical mechanical polishing comprises the following steps:
s1: preparing silicon aluminum oxide by using water glass and aluminum salt solution, and keeping the pH value of the system to be neutral in the synthesis process;
s2: adding dilute sulfuric acid (the mass fraction is less than or equal to 70%) into the silicon aluminum oxide to enable part of aluminum species to migrate to the surfaces of particles, aging, cooling and filtering to obtain a filter cake;
s3: washing the filter cake to reduce the content of sodium ions and sulfate radicals of the silicon dioxide in the filter cake;
s4: and re-dispersing the washed filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling and classification to obtain the abrasive for silicon-aluminum chemical mechanical polishing.
Further, the aluminum salt solution is one or a combination of more than two of aluminum sulfate solution, aluminum nitrate solution and aluminum chloride solution.
Further, the concentration of silicon dioxide in the water glass is 10-20wt% and the modulus is 3.35.
Further, the molar ratio of aluminum in the aluminum salt solution to silicon in the water glass is 0.05-1: 1. preferably, the molar ratio of aluminum in the aluminum salt solution to silicon in the water glass is 0.40-1: 1.
further, the silicon-aluminum oxide is prepared by adopting a neutral gel method synthesis process.
Preferably, the preparation of the silicon aluminum oxide by adopting a neutral gel method synthesis process comprises the following steps:
(1) Preparing water glass with the concentration of silicon dioxide of 10-20wt% and the modulus of 3.35 for later use;
(2) Uniformly mixing an aluminum salt solution with the water glass to obtain water glass containing aluminum species;
(3) Injecting water into the reaction kettle, heating to the temperature in the step (2), simultaneously adding sodium silicate containing aluminum species and sulfuric acid solution, and keeping the pH value of the system to be neutral;
(4) And after the parallel flow is completed, heating, keeping aging at the temperature, and obtaining the silicon-aluminum oxide after aging.
Further, in the step (2), the mixing temperature of the aluminum salt solution and the water glass is 30-60 ℃; in the step (3), the parallel flow time is 30-90 min; in the step (4), the temperature is 80-100 ℃ and the aging time is 2h.
Further, in the step S2, the pH value of the solution added with the dilute sulfuric acid is 2-4, the aging time is 0.5-1.5 h, and the cooling temperature is 60-70 ℃.
Further, in step S3, the filter cake is washed with sulfuric acid and water in a concentration of 1 to 3wt% in this order.
Further, the abrasive for silicon-aluminum chemical mechanical polishing has a particle diameter of 1.5 μm to 2.0 μm.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method, liquid phase synthesis is adopted, neutral pH is adopted in the synthesis process, so that silicon-aluminum species are uniformly distributed, meanwhile, acidic treatment and washing are adopted, the surface precipitation of the aluminum species is controlled, a controllable aluminum coated silicon structure is formed, and the application range of chemical mechanical polishing of the obtained abrasive is improved.
The silicon-aluminum oxide is prepared by adopting a neutral gel method synthesis process, silicon-aluminum species are uniformly distributed, abrasive materials are easy to disperse in a water phase, and a formed colloid system is stable and is not easy to settle.
The invention uses acid treatment and washing to control the surface precipitation of aluminum species, and forms a controllable aluminum coated silicon structure, and the obtained abrasive has wider application range of chemical mechanical polishing.
The preparation method is simple, the cost is low, and the prepared abrasive has high polishing speed and low surface roughness in the application of chemical mechanical polishing.
Detailed Description
The present invention will be further described with reference to the following specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
The invention provides a preparation method of an abrasive for silicon-aluminum chemical mechanical polishing, which comprises the following preparation steps:
s1: preparing silicon aluminum oxide by using water glass and aluminum salt solution;
wherein, the preparation of the silicon aluminum oxide comprises the following steps:
(1) Preparing water glass with the concentration of silicon dioxide of 10-20wt% and the modulus of 3.35 for later use;
(2) Uniformly mixing an aluminum salt solution with the water glass at the temperature of 30-60 ℃ to obtain water glass containing aluminum species;
(3) Injecting water into the reaction kettle, heating to the temperature in the step (2), simultaneously adding sodium silicate containing aluminum species and sulfuric acid solution, and keeping the pH value of the system neutral, wherein the parallel flow time is 30-90 min;
(4) After parallel flow is completed, heating to 80-100 ℃, keeping aging for 2 hours at the temperature, and obtaining the silicon-aluminum oxide after aging;
s2: adding dilute sulfuric acid (the mass fraction is less than or equal to 70%) into the silicon aluminum oxide, regulating the pH value to be 2-4, enabling part of aluminum species to migrate to the surface of particles, aging for 0.5-1.5 h, cooling to 60-70 ℃, and filtering to obtain a filter cake;
s3: washing the filter cake with sulfuric acid and water with the concentration of 1-3 wt% in sequence to reduce the content of sodium ions and sulfate radicals in the silica in the filter cake;
s4: and re-dispersing the washed filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling and classification to obtain the silicon-aluminum chemical mechanical polishing abrasive with the particle size of 1.5-2.0 mu m.
Wherein the aluminum salt solution is one or a combination of more than two of aluminum sulfate solution, aluminum nitrate solution and aluminum chloride solution. The molar ratio of aluminum in the aluminum salt solution to silicon in the water glass is 0.05-1: 1. preferably, the molar ratio of aluminum in the aluminum salt solution to silicon in the water glass is 0.40-1: 1.
according to the preparation method, liquid phase synthesis is adopted, neutral pH is adopted in the synthesis process, so that silicon-aluminum species are uniformly distributed, meanwhile, acidic treatment and washing are adopted, the surface precipitation of aluminum species is controlled, a controllable aluminum coated silicon structure is formed, and the application range of chemical mechanical polishing of the obtained abrasive is improved.
The following are specific examples of the present invention, in which raw materials, equipment, etc. used are obtained by purchasing them, except for special restrictions.
Example 1:
45 mol of aluminum sulfate and 75 liters of 20wt% water glass were mixed uniformly at a temperature of 30 ℃. 50L of bottom water was poured into the stirred reaction vessel, the temperature was raised to 30℃and the above-mentioned sodium silicate containing aluminum salt and 30% by weight of sulfuric acid were added in parallel flow, keeping the pH of the system neutral and the parallel flow time 30 minutes. After completion of the co-current flow, the temperature was adjusted to 90℃and aged for 2 hours. After the aging is finished, dilute sulfuric acid is added to adjust the pH value to 3, the mixture is aged for 0.5 hour, then the mixture is cooled to 60 ℃, and a filter cake is obtained by filtering. Washing the filter cake with 1wt% sulfuric acid, mixing with tap water and pure water, and press filtering to obtain filter cake. And re-dispersing the filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling to obtain the product with the particle size of 1.5-2.0 microns.
Example 2:
at a temperature of 60℃15 mol of aluminium nitrate and 75 l of 20% by weight water glass are mixed homogeneously. 50L of bottom water was poured into the stirred reaction vessel, the temperature was raised to 30℃and the above-mentioned sodium silicate containing aluminum salt and 10% by weight of sulfuric acid were added in parallel flow, keeping the pH of the system neutral and the parallel flow time at 90 minutes. After completion of the co-current flow, the temperature was adjusted to 100℃and aged for 2 hours. After the aging is finished, dilute sulfuric acid is added to adjust the pH value to 2, the mixture is aged for 1.5 hours, then the mixture is cooled to 60 ℃, and a filter cake is obtained through filtration. The filter cake was washed with 3wt% sulfuric acid, and then with tap water and pure water, and press-filtered to form a filter cake. And re-dispersing the filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling to obtain the product with the particle size of 1.5-2.0 microns.
Example 3:
30 mol of aluminum chloride and 75 l of water glass with the weight percentage of 10% are mixed uniformly at a temperature of 40 ℃. 50L of bottom water was poured into the stirred reaction vessel, the temperature was raised to 30℃and the above-mentioned sodium silicate containing aluminum salt and 30% by weight of sulfuric acid were added in parallel, keeping the pH of the system neutral and the parallel flow time 60 minutes. After completion of the co-current flow, the temperature was adjusted to 80℃and aged for 2 hours. After the aging is finished, dilute sulfuric acid is added to adjust the pH value to 4, the aging is carried out for 1.0 hour, then the cooling temperature is cooled to 70 ℃, and the filter cake is obtained by filtering. Washing the filter cake with 1wt% sulfuric acid, mixing with tap water and pure water, and press filtering to obtain filter cake. And re-dispersing the filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling to obtain the product with the particle size of 1.5-2.0 microns.
Example 4:
at a temperature of 30℃15 mol of aluminium sulphate and 75 l of 20% by weight water glass are mixed homogeneously. 50L of bottom water was poured into the stirred reaction vessel, the temperature was raised to 30℃and the above-mentioned sodium silicate containing aluminum salt and 30% by weight of sulfuric acid were added in parallel flow, keeping the pH of the system neutral and the parallel flow time 30 minutes. After completion of the co-current flow, the temperature was adjusted to 90℃and aged for 2 hours. After the aging is finished, dilute sulfuric acid is added to adjust the pH value to 3, the mixture is aged for 0.5 hour, then the mixture is cooled to 70 ℃, and a filter cake is obtained through filtration. Washing the filter cake with 1wt% sulfuric acid, mixing with tap water and pure water, and press filtering to obtain filter cake. And re-dispersing the filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling to obtain the product with the particle size of 1.5-2.0 microns.
In the above embodiments, each material is not limited to the above-mentioned components, and each material may also be formed by other single components or multiple components described in the present invention, and the component parts of each material are not limited to the above-mentioned parts, and the component parts of each material may also be a combination of other component parts described in the present invention, which is not described herein.
Comparative example 1:
in comparison with example 1, the comparative example 1 was conducted in the same manner as in example 1 without adding an aluminum salt.
Comparative example 2:
in comparison with example 1, the silicon-aluminum oxide of comparative example 2 was made acidic in pH by adjusting the ratio of sulfuric acid solution to water glass containing aluminum species during synthesis, and the other operations were the same as in example 1.
Application performance detection
The performance of examples 1-4 and comparative examples 1-2 were compared.
The testing method comprises the following steps: sapphire was used as a substrate, which was polished to a polishing solution concentration of 3%, and the test results are shown in table 1:
table 1 comparative tables of application Properties of examples 1-4 and comparative examples 1-2
| Project | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Polishing rate (μm/h) | 3.6 | 2.8 | 2.6 | 3.7 | 1.4 | 1.4 |
| Surface roughness (nm) | 0.30 | 0.23 | 0.22 | 0.27 | 0.21 | 0.46 |
| Scratch, pit and orange peel | Without any means for | Without any means for | Without any means for | Without any means for | Without any means for | Has the following components |
As can be seen from Table 1, the abrasives of examples 1 to 4 were high in polishing rate, low in surface roughness, and free from scratches, pits, orange peel, and the like, as compared with comparative examples 1 to 2.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed. In addition, although specific terms are used in the present specification, these terms are for convenience of description only and do not limit the present invention in any way.
Claims (8)
1. The preparation method of the abrasive for silicon-aluminum chemical mechanical polishing is characterized by comprising the following steps:
s1: preparing silicon aluminum oxide by using water glass and aluminum salt solution, and keeping the pH value of the system to be neutral in the synthesis process;
s2: adding dilute sulfuric acid into the silicon aluminum oxide to enable part of aluminum species to migrate to the particle surface, aging, cooling and filtering to obtain a filter cake;
s3: washing the filter cake to reduce the content of sodium ions and sulfate radicals of the silicon dioxide in the filter cake;
s4: re-dispersing the washed filter cake in a small amount of water, spray-drying the slurry obtained after uniform dispersion, and carrying out jet milling and classification to obtain the abrasive for silicon-aluminum chemical mechanical polishing;
the silicon-aluminum oxide is prepared by adopting a neutral gel method synthesis process; the preparation of the silicon aluminum oxide by adopting a neutral gel method synthesis process comprises the following steps:
(1) Preparing water glass with the concentration of silicon dioxide of 10-20wt% and the modulus of 3.35 for later use;
(2) Uniformly mixing an aluminum salt solution with the water glass to obtain water glass containing aluminum species;
(3) Injecting water into the reaction kettle, heating to the temperature in the step (2), simultaneously adding sodium silicate containing aluminum species and sulfuric acid solution, and keeping the pH value of the system to be neutral;
(4) And after the parallel flow is completed, heating, keeping aging at the temperature, and obtaining the silicon-aluminum oxide after aging.
2. The method for producing an abrasive for chemical mechanical polishing of aluminum and silicon according to claim 1, wherein the aluminum salt solution is one or a combination of two or more of an aluminum sulfate solution, an aluminum nitrate solution, and an aluminum chloride solution.
3. The method for producing an abrasive for chemical mechanical polishing of silicon aluminum according to claim 1, wherein the silica concentration in the water glass is 10 to 20wt% and the modulus is 3.35.
4. The method for producing an abrasive for chemical mechanical polishing of silicon aluminum according to claim 1, wherein a molar ratio of aluminum in the aluminum salt solution to silicon in the water glass is 0.05 to 1:1.
5. the method for producing an abrasive for chemical mechanical polishing of silicon-aluminum according to claim 1, wherein in the step (2), the mixing temperature of the aluminum salt solution and the water glass is 30 to 60 ℃; in the step (3), the parallel flow time is 30-90 min; in the step (4), the temperature is 80-100 ℃ and the aging time is 2h.
6. The method according to claim 1, wherein in the step S2, the pH of the solution after adding dilute sulfuric acid is 2 to 4, the aging time is 0.5 to 1.5 hours, and the cooling temperature is 60 to 70 ℃.
7. The method for producing an abrasive for chemical mechanical polishing of silicon-aluminum according to claim 1, wherein in step S3, the cake is washed with sulfuric acid and water in the concentration of 1 to 3wt% in this order.
8. The method for producing an abrasive for silicoalumino chemical mechanical polishing according to any one of claims 1 to 7, wherein the abrasive for silicoalumino chemical mechanical polishing has a particle diameter of 1.5 μm to 2.0 μm.
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| CN111073518A (en) * | 2019-12-09 | 2020-04-28 | 湖南景翌湘台环保高新技术开发有限公司 | Preparation method of silicon-aluminum composite polishing powder |
| CN112143035A (en) * | 2020-08-19 | 2020-12-29 | 广州凌玮科技股份有限公司 | Preparation method of silicon-aluminum film opening agent and film opening agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6913634B2 (en) * | 2003-02-14 | 2005-07-05 | J. M. Huber Corporation | Abrasives for copper CMP and methods for making |
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| FR2604994A1 (en) * | 1986-10-14 | 1988-04-15 | Geopolymere France Sarl | Composite materials with inorganic matrices |
| CN1635043A (en) * | 2003-12-25 | 2005-07-06 | 长兴化学工业股份有限公司 | Grinding fluid for complanation of color photoresisting material |
| WO2008071466A1 (en) * | 2006-12-15 | 2008-06-19 | Evonik Degussa Gmbh | Process for preparing fumed silica dispersions |
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