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Acidic silicon dioxide sol and its preparation method and use

A technology of silica and sol, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., can solve problems such as pollution, high metal ion content, poor stability of acidic silica gel, etc., and achieve long storage period and low copper ion content , the effect of low copper content

Inactive Publication Date: 2008-02-13
BEIJING GRISH HITECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above method, due to the limitation of the method itself or the influence of raw materials, often makes the acidic silica gel produced have the disadvantages of poor stability or high metal ion content, or it is necessary to add other additives to increase the stability of the acidic silica sol, which is harmful to silica. When the sol is used for CMP polishing in the field of electronics or semiconductors, it often produces large pollution

Method used

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  • Acidic silicon dioxide sol and its preparation method and use
  • Acidic silicon dioxide sol and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Heat 2L of high-purity water in a four-neck flask to 50°C, then add 5.0g of high-grade pure NaOH, continue heating to 70°C, add 30.0g of silicon powder while stirring, and then add 30.0g of silicon powder every half hour, and react for 7 hours Turn off heat. During the entire reaction process, the temperature was maintained at about 85°C. After the reaction solution was cooled to room temperature, it was filtered. Carry out cation exchange to the sol after filtration, the mass ratio of resin and silica gel used is 1: 1, after exchanging 2h, filter out silica gel, carry out regeneration treatment to cationic resin, regeneration solution is dilute hydrochloric acid of 1: 2, after regeneration, use Wash with high-purity water to neutrality, and perform a second exchange. After 4 hours of exchange, filter out the silica gel, and test the parameters of the obtained silica gel. The results are as follows:

[0052] Test items

Embodiment 2

[0054] Heat 500L of high-purity water in the reactor to 50°C by electric heating, then add 2.5Kg of high-grade pure NaOH, continue heating to 60°C, add 2Kg of silicon powder, start stirring, turn off heating, add 2Kg of silicon powder at 75°C After that, add 4.0Kg of silicon powder every half hour, stop feeding after 6 hours of reaction, and continue to react for 4 hours. During the reaction process, high-purity water should be replenished regularly to keep the temperature below 95°C. After the reaction solution was cooled to room temperature, it was filtered. Perform cation exchange on the filtered sol. After 4 hours of exchange, filter out the silica gel, and regenerate the cationic resin. After regeneration, wash it with high-purity water to neutrality, and perform a second exchange. Dilute hydrochloric acid is used to adjust the pH value, and each parameter is tested, and the results are as follows:

[0055] Test items

Embodiment 3

[0057] Heat 500L of high-purity water in the reactor to 60°C by electric heating, then add 2Kg of high-grade pure NaOH, continue heating to 70°C, add 2Kg of silicon powder, start stirring, turn off heating, add 2Kg of silicon powder at 75°C, and then Add 2.5Kg of silicon powder every half hour, stop feeding after 10 hours of reaction, and continue to react for 2 hours. After the reaction solution was cooled to room temperature, it was filtered. Perform cation exchange on the filtered sol. After 4 hours of exchange, filter out the silica gel, and regenerate the cationic resin. After regeneration, wash it with high-purity water to neutrality, and perform a second exchange. Adjust the pH value with dilute hydrochloric acid, test each parameter and use the silica gel to polish the GaAS wafer. The results are as follows:

[0058] Test items

Test Results

testing method

pH value

concentration

kinematic viscosity

particle size

Copper...

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Abstract

The invention provides an acidic silica sol, which is characterized in that: it comprises water and silicon dioxide colloids with a nanometer or submicron particle size dispersed in water and made of silicon powder as a raw material, and the pH value of the sol is 1.5~3.5, copper ion content ≤50ppb. The sol has the characteristics of high stability and high purity, and can be applied to chemical mechanical polishing (CMP) in the electronics industry, semiconductors, hard disks, compound crystals, precision optical devices, etc., because of its low copper content, it has advantages in the field of semiconductor polishing. The present invention also provides the preparation method and application of the above-mentioned acidic silica sol.

Description

technical field [0001] The invention relates to a silica sol-based polishing material, in particular to an acidic silica sol and its preparation method and application. Background technique [0002] With the rapid development of the information industry, the integration of electronic devices is getting higher and higher, and the planarization of the device surface is very important. The chemical mechanical polishing (CMP) technology jointly developed by IBM and Microtechnology is a manufacturing integration The preferred method of the circuit, the method can achieve overall planarization on the wafer, silica sol (such as patent TW245789B, CN1359997, CN1822325, JP2002284516, KR20040056167, JP2005159351, US6048789, CN1727431, CN1359997, CN11942883) 45 colloidal oxide or silicon coating (such as patents JP2003193038, CA2382724, US2004211337, WO2005035688, CN1543492,) the polishing liquid is the most representative polishing agent for CMP technology at present. [0003] Silica ...

Claims

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Application Information

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IPC IPC(8): C01B33/141
Inventor 许亚杰李晓冬
Owner BEIJING GRISH HITECH
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