CN105694811A - Zinc doped silica sol composite abrasive particles, polishing agent composition and preparation method of polishing agent composition - Google Patents
Zinc doped silica sol composite abrasive particles, polishing agent composition and preparation method of polishing agent composition Download PDFInfo
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- CN105694811A CN105694811A CN201610129751.2A CN201610129751A CN105694811A CN 105694811 A CN105694811 A CN 105694811A CN 201610129751 A CN201610129751 A CN 201610129751A CN 105694811 A CN105694811 A CN 105694811A
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- abrasive particles
- silicon oxide
- sol
- doped silicon
- zinc element
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- C—CHEMISTRY; METALLURGY
- 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
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention discloses zinc doped silica sol composite abrasive particles, polishing agent composition and a preparation method of the polishing agent composition. The preparation method of the polishing agent composition comprises the following steps: a, a zinc doped silica sol composite particle sol system is processed by a 350-mesh filter sieve and filtered, and large particles in the system are removed; b, 6.67% by mass of a dispersing agent sodium hexametaphosphate is added to the filtered composite particle sol system and stirred uniformly, and the polishing agent composition of the zinc doped silica sol composite abrasive particles is obtained. The composite abrasive particles adopt a nano-spherical physical structure and chemically comprise zinc which can improve the chemical action of the abrasive particles, and by means of the chemical action, the polishing rate of the abrasive particles can be increased and the removal rate of a material can be increased. When a polishing agent is used for polishing a sapphire substrate, the roughness of a sapphire silicon wafer can be reduced effectively, and the removal rate for the sapphire surface is increased.
Description
Technical field
The present invention relates to a kind of polishing abrasive particle, polishing fluid composition and preparation method thereof, particularly a kind of zinc element doped silicon oxide colloidal sol Compostie abrasive particles, polishing fluid composition and preparation method thereof, belong to material surface grinding and polishing technical field。
Background technology
Sapphire material, due to its higher Mohs' hardness and good chemical stability, is widely used in the field such as electricity, optics。In optoelectronic areas, light emitting diode (LED) has the simple advantage such as low-work voltage, low-power consumption, high efficiency, long-life, solidification, fast-response speed and drive circuit。Sapphire material is because it has good high-temperature stability and mechanical property, and as the backing material of LED, LED component performance and quality are had very important impact by sapphire material surface quality, and current sapphire material requires ultra-smooth, zero defect, and roughness is less than 0.2nm。
At present, it is common to adopting chemically mechanical polishing (CMP) technology to carry out precise polished to sapphire device surface, wherein abrasive particle is a composition in chemical mechanical polishing liquid, actual widely used abrasive grains is the inorganic polishing particles such as silicon oxide, aluminium oxide。And wherein silicon oxide abrasive particle is better to sapphire polishing effect, but the problem being primarily present in chemically mechanical polishing CMP planarization process is, causes that owing to polishing speed is low production efficiency is low, and surface roughness needs to continue to improve。
Summary of the invention
An object of the present invention is in that to provide a kind of zinc element doped silicon oxide colloidal sol Compostie abrasive particles。
The two of the purpose of the present invention are in that the preparation method providing a kind of zinc element doped silicon oxide colloidal sol Compostie abrasive particles。
The three of the purpose of the present invention are in that to provide a kind of zinc element doped silicon oxide colloidal sol Compostie abrasive particles, polishing fluid composition and preparation method thereof。
For achieving the above object, the present invention adopts the following technical scheme that
One zinc element doped silicon oxide colloidal sol Compostie abrasive particles of the present invention, it is characterised in that described Compostie abrasive particles forms and mass percentage content is:
Zinc element compound (zinc hydroxide) 0.1-2wt.%；
Silica sol 99.9-95wt.%。The preparation method of a kind of zinc element doped silicon oxide Compostie abrasive particles of the present invention, it is characterised in that there is following process and step:
A. the waterglass that mass fraction is 8.0% being passed through cation exchange resin, obtaining mass fraction is 2.0-3.0% active silicic acid solution, and the pH value of described silicate solution is 2.5-3.5；
B. it is that 2.0-3.0% active silicic acid solution stirring mixes by zinc nitrate aqueous solution that mass fraction is 0.29% with mass fraction, forms mixed solution；The sodium hydroxide solution that mixed mixed solution and mass fraction are 0.5% is simultaneously added dropwise temperature be 100 DEG C, mass fraction be 10% crystal seed silica solution in, form sol system, obtain polishing fluid；Control rate of addition is 1-2ml/min, and this rate of addition is identical with the evaporation rate of sol system, and the liquid level keeping sol system is constant；The pH value keeping sol system is 8.5-10.5, until mixed solution drips；Stirring is cooled to room temperature, namely obtains the Compostie abrasive particles sol system of zinc element doped silicon oxide colloidal sol, the Compostie abrasive particles sol system of above-mentioned zinc element doped silicon oxide is sent into the 350 overanxious sieves of order, filters, removes bulky grain therein；Adding mass percent to the Compostie abrasive particles sol system after above-mentioned filtration is the sodium hexametaphosphate dispersant of 6.67%, stirs, obtains the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles。
The polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles of the present invention, it is characterised in that the composition of described polishing fluid composition and mass percentage content be:
Zinc element doped silicon oxide colloidal sol Compostie abrasive particles 10-10.12wt.%,
Sodium hexametaphosphate dispersant 6.67wt.%,
Deionized water surplus；
The mass percentage content sum of each composition is 100wt.% above。The preparation method of the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles of the present invention, it is characterised in that there is following process and step:
A. above-mentioned zinc element doped silicon oxide Compostie abrasive particles sol system is sent into 350 order sieves, filter, remove bulky grain therein；
B. adding mass percent to the Compostie abrasive particles sol system after above-mentioned filtration is the sodium hexametaphosphate dispersant of 6.67%, stirs, namely obtains polishing fluid composition。
The physical arrangement of the Compostie abrasive particles of the present invention is nanometer spherical, and containing zinc element in the chemical composition of this abrasive particle, zinc element can improve the chemical action of abrasive particle, and chemical action can improve the polishing speed of abrasive particle, improves the removal rate of material。
Adopt polishing fluid provided by the invention that sapphire substrate is polished, it is possible to be effectively reduced the roughness on silicon on sapphire surface, improve the removal rate of sapphire surface。
Detailed description of the invention
Now specific embodiments of the invention are summarized in rear。
The zinc element doped silicon oxide colloidal sol Compostie abrasive particles preparation process of embodiment 1 present invention is:
Being that 8.0% waterglass passes through cation exchange resin by mass fraction, obtaining mass fraction is 2.0-3.0% active silicic acid solution, and the pH value of described silicate solution is 2.5-3.5；The zinc nitrate aqueous solution (987g) that mass fraction is 0.29% is mixed with active silicic acid solution (987g) stirring that mass fraction is 2.0-3.0%, forms mixed solution；The sodium hydroxide solution that mixed mixed solution and mass fraction are 0.5% is simultaneously added dropwise temperature be 100 DEG C, mass fraction be in 10% crystal seed silica solution (3000g), form sol system, obtain polishing fluid；Control rate of addition is 1-2ml/min, and this rate of addition is identical with the evaporation rate of sol system, and the liquid level keeping sol system is constant；The pH value keeping sol system is 8.5-10.5, until mixed solution drips；Stirring is cooled to room temperature, namely obtains the Compostie abrasive particles sol system of zinc element doped silicon oxide；The Compostie abrasive particles sol system of above-mentioned zinc element doped silicon oxide is sent into the 350 overanxious sieves of order, filters, remove bulky grain therein；Adding mass percent to the Compostie abrasive particles sol system after above-mentioned filtration is the sodium hexametaphosphate dispersant of 6.67%, stirs, obtains the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles, and wherein, zinc element doping mass fraction is 0.5%。Composition and the mass percentage content of the described zinc doping colloidal silica Ludox composite abrasive grain polishing solution compositions that doping mass fraction is 0.5% are as follows:
Zinc element doped silicon oxide colloidal sol Compostie abrasive particles 10.03wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water 83.3t.%。
Embodiment 2
The zinc nitrate aqueous solution (1974g) adopting mass fraction to be 0.29% is 2.0-3.0% active silicic acid solution (1974g) with mass fraction, other steps are with embodiment 1, finally obtain the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles, wherein, zinc element doping mass fraction is 1.0%。
Composition and the mass percentage content of the described zinc doping colloidal silica Ludox composite abrasive grain polishing solution compositions that doping mass fraction is 1.0% are as follows:
Zinc element doped silicon oxide colloidal sol Compostie abrasive particles 10.06wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water 83.27wt.%。
Embodiment 3
The zinc nitrate aqueous solution (2961g) adopting mass fraction to be 0.29% is 2.0-3.0% active silicic acid solution (2961g) with mass fraction, other steps are with embodiment 1, finally obtain the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles, wherein, zinc element doping mass fraction is 1.5%。
Composition and the mass percentage content of the described zinc doping colloidal silica Ludox composite abrasive grain polishing solution compositions that doping mass fraction is 1.5% are as follows:
Zinc element doped silicon oxide colloidal sol Compostie abrasive particles 10.09wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water 83.24wt.%。
Embodiment 4
The zinc nitrate aqueous solution (3948g) adopting mass fraction to be 0.29% is 2.0-3.0% active silicic acid solution (3948g) with mass fraction, other steps are with embodiment 1, finally obtain the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles, wherein, zinc element doping mass fraction is 2.0%。
Composition and the mass percentage content of the described zinc doping colloidal silica Ludox composite abrasive grain polishing solution compositions that doping mass fraction is 2.0% are as follows:
Zinc element doped silicon oxide colloidal sol Compostie abrasive particles 10.12wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water 83.21wt.%。
Comparative example 1:
With composition and the step of embodiment 1, simply unadulterated pure silica sol polishing fluid, does not namely drip zinc nitrate solution in preparation process, obtains the pure silica colloidal sol polishing fluid of undoped p zinc。
Composition and the mass percentage content of described pure colloidal silica Abrasive Polishing fluid composition are as follows:
The silica sol Compostie abrasive particles 10.0wt.% of undoped p zinc element
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water 83.33wt.%
Polishing experiments
Using above-mentioned polishing fluid, under certain polishing condition, sapphire substrate, silicon chip are polished experiment, polishing condition is as follows:
Buffing machine: UNIPOL-1502 single side polishing machine
Polishing workpiece: diameter is the sapphire substrate of 50.8nm
Polishing pad: polyurethane material, RODEL produce
Polish pressure: sapphire is finished to 6 kilograms
Lower wall rotating speed: 60rpm
Polishing time: sapphire is finished to 2 hours
After polishing, then washing and dry substrate, then measure the surface appearance feature of substrate；Surface average roughness (Ra) and microroughness (RMS) use AmbiosXI-100 surface topographic apparatus fo, and its resolving power is 0.1 angstrom；Test ranges for 93.5 microns × 93.5 microns。Substrate weight analytical balance weighs, and before and after polishing, weight difference is polishing speed divided by substrate surface area and polishing time。
Each embodiment polishing fluid is visible in Table 1. to sapphire polishing effect, compared with comparative example 1 pure silica abrasive grain polishing solution, after sapphire substrate is polished by (embodiment 1,2,3,4) containing zinc element doped silicon oxide colloidal sol Compostie abrasive particles, all reduce roughness (Ra) and the microroughness (RMS) on sapphire substrate surface；For the clearance of sapphire surface, embodiment 1,2 improves its clearance, and embodiment 3,4 does not improve its clearance, that is the doping mass ratio zinc doping colloidal silica Compostie abrasive particles lower than 1.5% can improve the clearance of sapphire surface。
Claims (4)
1. a zinc element doped silicon oxide colloidal sol Compostie abrasive particles, it is characterised in that described Compostie abrasive particles forms and mass percentage content is:
Zinc element compound (zinc hydroxide) 0.1-2wt.%；
Silica sol 99.9-95wt.%。
2. the preparation method of a zinc element doped silicon oxide colloidal sol Compostie abrasive particles, it is characterised in that the method has following steps:
A. the waterglass that mass fraction is 8.0% being passed through cation exchange resin, obtaining mass fraction is 2.0-3.0% active silicic acid solution, and the pH value of described silicate solution is 2.5-3.5；
B. it is that 2.0-3.0% active silicic acid solution stirring mixes by zinc nitrate aqueous solution that mass fraction is 0.29% with mass fraction, forms mixed solution；The sodium hydroxide solution that mixed mixed solution and mass fraction are 0.5% is simultaneously added dropwise temperature be 100 DEG C, mass fraction be 10% crystal seed silica solution in, form sol system, obtain polishing fluid；Control rate of addition is 1-2ml/min, and this rate of addition is identical with the evaporation rate of sol system, and the liquid level keeping sol system is constant；The pH value keeping sol system is 8.5-10.5, until mixed solution drips, stirring is cooled to room temperature, namely the Compostie abrasive particles sol system of zinc element doped silicon oxide colloidal sol is obtained, the Compostie abrasive particles sol system of above-mentioned zinc element doped silicon oxide is sent into the 350 overanxious sieves of order, filter, remove bulky grain therein；Adding mass percent to the Compostie abrasive particles sol system after above-mentioned filtration is the sodium hexametaphosphate dispersant of 6.67%, stirs, obtains the polishing fluid composition of zinc element doped silicon oxide colloidal sol Compostie abrasive particles。
3. the polishing fluid composition of a zinc element doped silicon oxide colloidal sol Compostie abrasive particles, it is characterised in that the composition of described polishing fluid composition and mass percentage content be:
Zinc element doped silicon oxide colloidal sol Compostie abrasive particles 10-10.12wt.%,
Sodium hexametaphosphate dispersant 6.67wt.%,
Deionized water surplus；
The mass percentage content sum of each composition is 100wt.% above。
4. the preparation method of the polishing fluid composition preparing zinc element doped silicon oxide colloidal sol Compostie abrasive particles according to claim 3, it is characterised in that there is following process and step:
A. above-mentioned zinc element doped silicon oxide colloidal sol Compostie abrasive particles sol system is sent into 350 order sieves, filter, remove bulky grain therein；
B. adding mass percent to the Compostie abrasive particles sol system after above-mentioned filtration is the sodium hexametaphosphate dispersant of 6.67%, stirs, namely obtains polishing fluid composition。
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Cited By (3)
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| CN111253910A (en) * | 2020-03-18 | 2020-06-09 | 昆山捷纳电子材料有限公司 | Preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles |
| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
| CN114591684A (en) * | 2022-02-18 | 2022-06-07 | 浙江开化元通硅业有限公司 | Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof |
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| CN105176492A (en) * | 2015-09-02 | 2015-12-23 | 上海大学 | Lanthanum-doped silicon dioxide sol composite abrasive particles, polishing solution composition and preparation methods of lanthanum-doped silicon dioxide sol composite abrasive particles and polishing solution composition |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
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| CN114591684A (en) * | 2022-02-18 | 2022-06-07 | 浙江开化元通硅业有限公司 | Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof |
| CN114591684B (en) * | 2022-02-18 | 2024-01-30 | 浙江开化元通硅业有限公司 | Environment-friendly chemical mechanical polishing solution based on high-purity spherical silica sol, and preparation method and polishing method thereof |
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