CN104877633A - Magnesium-element-doped silicon dioxide sol compound abrasive grains, polishing solution and preparation method thereof - Google Patents
Magnesium-element-doped silicon dioxide sol compound abrasive grains, polishing solution and preparation method thereof Download PDFInfo
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- CN104877633A CN104877633A CN201510276373.6A CN201510276373A CN104877633A CN 104877633 A CN104877633 A CN 104877633A CN 201510276373 A CN201510276373 A CN 201510276373A CN 104877633 A CN104877633 A CN 104877633A
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Abstract
The invention relates to magnesium-element-doped silicon dioxide sol compound abrasive grains, a polishing solution and a preparation method thereof. The preparation method of the compound abrasive grain comprises the following steps: mixing a magnesium nitrate solution and a silicic acid solution of which the mass fractions are respectively 1.1 wt% and 2.5 wt% according to the mass ratio of 1: 1; depositing the mixture on silicon dioxide seed crystals through coprecipitation. Compound particles in the sol are uniformly spherical, and the doping amount of magnesium hydroxide relative to silicon dioxide is 0.1 wt%-5 wt%. The polishing solution is prepared from the compound abrasive grains. The magnesium element is doped into the silicon dioxide particles in the format of magnesium hydroxide and conducts chemical reaction with the surface layer of sapphire in the polishing process, so that the polishing rate is increased. The compound abrasive grains in the sol are uniformly spherical, and the spherical structures can reduce scratching and cutting of sapphire substrates in the polishing process to keep the surfaces smooth. When the polishing solution is adopted to polish the sapphire substrates, the removal rate of the sapphire substrates can be effectively improved and the surface roughness of sapphire is reduced.
Description
Technical field
The present invention relates to a kind of polishing abrasive particle, polishing fluid and preparation method thereof, particularly a kind of Compostie abrasive particles, polishing fluid and preparation method thereof of magnesium elements doping silicon dioxide colloidal sol.
Background technology
Monocrystalline sapphire has excellent optics, electricity, mechanics, chemical physical property.Good light transmission and mechanical property make it be paid attention in aerospace and national defence, the glasses for infrared use window made with sapphire single-crystal and nose cone, be widely used in airborne, spaceborne, boat carry and dive carry, continental rise optoelectronic device.It is worth mentioning that monocrystalline sapphire c (0001) face because with the lattice CTE mismatch rate of semi-conductor GaN is less, physical strength is high, low price etc. become photodiode main substrate material and be used as substrate sapphire surface sufficiently the smooth zero defect that could meet GaN grow.But monocrystalline sapphire is because its hardness is high, and the features such as chemical stability is good propose new challenge to precise polished.
At present, chemically machinery polished (CMP) is because the low polishing velocity of its cost is widely used in the precise polished of device surface soon.Polishing fluid is topmost key element in chemically machinery polished, and the factor such as abrasive grain type, dispersiveness in polishing fluid has a great impact polishing effect.At present in the practical application of sapphire polishing, usually adopt the conventional inorganic such as silicon oxide, aluminum oxide abrasive particle, it is low to sapphire polishing speed, and polishing speed and surfaceness are not well positioned to meet industrial requirement.The Compostie abrasive particles reported also be all mostly dissolved again by high-temperature calcination after obtain composite oxides abrasive particle, and in calcining redispersion process, particle can form erose aggregate, thus increases the surfaceness of polishing substrate.The Compostie abrasive particles of conventional inorganic grain surface grafting organism nucleocapsid structure, can reduce the hardness of inorganic polishing particles like this, but because surface organic matter is inertia system, well and substrate surface generation chemical reaction, thus can not reduce polishing speed.
Summary of the invention
An object of the present invention is Compostie abrasive particles providing magnesium doping silicon dioxide colloidal sol and preparation method thereof.
Two of object of the present invention is to provide the polishing fluid containing Compostie abrasive particles.
For achieving the above object, the present invention adopts following technical scheme:
The Compostie abrasive particles of a kind of magnesium elements doped silicon oxide of the present invention colloidal sol, is characterized in that having following composition:
Magnesium elements compound (magnesium hydroxide) 0.1-5 wt.%;
Silica sol 99.9-95 wt.%.
The preparation method of a kind of magnesium elements doped silicon oxide of the present invention colloidal sol Compostie abrasive particles, is characterized in that having following process and step:
A. first preparing pH value with base exchange method is 2.5, and massfraction is the silicic acid of 2.5 %;
B., under 100 DEG C of agitation conditions, be the silicic acid of 2.5 % by massfraction, massfraction is the Mg (NO of 1.1 %
3)
2it is in the silica-seed of 10% that solution and 1 wt% sodium hydroxide add 750g massfraction respectively; Sodium hydroxide controls whole sol system pH value and remains on 10.5, and the rate of addition controlling magnesium nitrate and silicate mixture keeps velocity of evaporation and rate of addition in sol system to balance each other; The mass ratio of described silicate solution and described magnesium nitrate solution is 1:1.
C. drip 120 minutes respectively, 240 minutes, 360 minutes, obtained magnesium doping is 0.5 wt%, the composite particles sol system of 1.0 wt%, 1.5 wt%, i.e. a kind of magnesium elements doped silicon oxide colloidal sol Compostie abrasive particles.
A kind of polishing fluid composition of the present invention, is characterized in that having following composition:
Magnesium doped silicon oxide Compostie abrasive particles 10-10.5%,
Pentasodium triphosphate of dispersing agent 0.2-3%,
Surfactant sodium dodecyl base benzene sulfonic acid sodium salt 0.01-1%,
Deionized water surplus;
The mass percentage sum of each composition is 100 wt % above.
The preparation method of a kind of polishing fluid composition of the present invention, is characterized in that having following process and step:
A. above-mentioned magnesium elements doped silicon oxide colloidal sol Compostie abrasive particles solution is passed through 350 object screens, removing macrobead;
B. use sodium hydroxide adjust ph to 10.5;
C. add 0.2-3% pentasodium triphosphate of dispersing agent, 0.01-1% surfactant sodium dodecyl base benzene sulfonic acid sodium salt, namely Homogeneous phase mixing obtains polishing fluid composition.
The structure of Compostie abrasive particles of the present invention is inner is pure silica-seed, and the part that skin is grown up is the part of magnesium hydroxide together with silica-doped.The aluminum oxide generation chemical reaction on outer magnesium hydroxide and sapphire top layer, thus improve sapphire clearance.Magnesium hydroxide hardness ratio silicon oxide is little simultaneously, can reduce the wearing and tearing to sapphire surface, reduces surfaceness.The abrasive particle of such design can reach the object of " two-forty, low roughness " polishing simultaneously.
Adopt polishing fluid provided by the invention to carry out polishing to sapphire substrate, can effectively improve sapphire surface clearance, reduce the roughness of sapphire surface.
Embodiment
With some examples, embodiment of the present invention are described further below.、
Embodiment.
The compounded abrasive colloidal sol of magnesium doped silicon oxide of the present invention adopts coprecipitation method preparation.Preparation process is: first preparing pH value with base exchange method is 2.5, and massfraction is the silicic acid of 2.5 wt %.Under 100 DEG C of agitation conditions, the Mg (NO that the silicic acid 620g that massfraction is 2.5 %, massfraction are 1.1 %
3)
2solution 620g and massfraction are that to add 750g massfraction be respectively in the silica-seed of 10% to the sodium hydroxide of 1 %.Sodium hydroxide controls whole sol system pH value and remains on 10.5, and the rate of addition controlling magnesium nitrate and silicate mixture keeps velocity of evaporation and rate of addition in sol system to balance each other.Obtained magnesium doping is the composite particles sol system of 0.5 wt%.The Compostie abrasive particles particle diameter of magnesium doping silicon dioxide is 101 nanometers, and colloidal sol final ph is 10.5.After filtering with 350 object screens, add 1.0% pentasodium triphosphate of dispersing agent, 0.5% surfactant sodium dodecyl base benzene sulfonic acid sodium salt, obtain polishing fluid.
Composition and the mass percent of magnesium doped silicon oxide composite abrasive grain polishing solution are as follows:
Magnesium doped silicon oxide Compostie abrasive particles 10.05%
Pentasodium triphosphate of dispersing agent 1.0%
Surfactant sodium dodecyl base benzene sulfonic acid sodium salt 0.5%,
Deionized water 88.45%;
Embodiment 2.
The compounded abrasive colloidal sol of magnesium doped silicon oxide of the present invention adopts coprecipitation method preparation.Preparation process is: first preparing pH value with base exchange method is 2.5, and massfraction is the silicic acid of 2.5 wt %.Under 100 DEG C of agitation conditions, the Mg (NO that the silicic acid 1239g that massfraction is 2.5 %, massfraction are 1.1 %
3)
2solution 1239g and massfraction are that to add 750g massfraction be respectively in the silica-seed of 10% to the sodium hydroxide of 1 %.Sodium hydroxide controls whole sol system pH value and remains on 10.5, and the rate of addition controlling magnesium nitrate and silicate mixture keeps velocity of evaporation and rate of addition in sol system to balance each other.Obtained magnesium doping is the composite particles sol system of 1.0 wt%.The Compostie abrasive particles particle diameter of magnesium doping silicon dioxide is 105 nanometers, and colloidal sol final ph is 10.5.After filtering with 350 object screens, add 1.0% pentasodium triphosphate of dispersing agent, 0.5% surfactant sodium dodecyl base benzene sulfonic acid sodium salt, both obtained polishing fluid.
Composition and the mass percent of magnesium doped silicon oxide composite abrasive grain polishing solution are as follows:
Magnesium doped silicon oxide Compostie abrasive particles 10.1%
Pentasodium triphosphate of dispersing agent 1.0%
Surfactant sodium dodecyl base benzene sulfonic acid sodium salt 0.5%,
Deionized water 88.4%;
Embodiment 3.
The compounded abrasive colloidal sol of magnesium doped silicon oxide of the present invention adopts coprecipitation method preparation.Preparation process is: first preparing pH value with base exchange method is 2.5, and massfraction is the silicic acid of 2.5 wt %.Under 100 DEG C of agitation conditions, the Mg (NO that the silicic acid 1860g that massfraction is 2.5 %, massfraction are 1.1 %
3)
2solution 1860g and massfraction are that to add 750g massfraction be respectively in the silica-seed of 10% to the sodium hydroxide of 1 %.Sodium hydroxide controls whole sol system pH value and remains on 10.5, and the rate of addition controlling magnesium nitrate and silicate mixture keeps velocity of evaporation and rate of addition in sol system to balance each other.Obtained magnesium doping is the composite particles sol system of 1.5 wt%.The Compostie abrasive particles particle diameter of magnesium doping silicon dioxide is 129 nanometers, and colloidal sol final ph is 10.5.After filtering with 350 object screens, add 1.0% pentasodium triphosphate of dispersing agent, 0.5% surfactant sodium dodecyl base benzene sulfonic acid sodium salt, both obtained polishing fluid.
Composition and the mass percent of magnesium doped silicon oxide composite abrasive grain polishing solution are as follows:
Magnesium doped silicon oxide Compostie abrasive particles 10.15%
Pentasodium triphosphate of dispersing agent 1.0%
Surfactant sodium dodecyl base benzene sulfonic acid sodium salt 0.5%,
Deionized water 88.35%;
Comparative example 1.
The pure silica colloidal sol polishing fluid of not magnesium-doped element; Namely in preparation process, magnesium nitrate solution is not added; Particle is 95 nanometers, and adjust ph is 10.5.After filtering with 350 object screens, add 1.0% pentasodium triphosphate of dispersing agent, 0.5% surfactant sodium dodecyl base benzene sulfonic acid sodium salt, obtain not magnesium-doped pure silica colloidal sol polishing fluid.
Composition and the mass percent of silica abrasive grain polishing fluid are as follows:
Silica abrasive grain 10%
Pentasodium triphosphate of dispersing agent 1.0%
Surfactant sodium dodecyl base benzene sulfonic acid sodium salt 0.5%,
Deionized water 88.5%;
Polishing is tested: use above-mentioned each polishing fluid to carry out polishing test to sapphire substrate under certain polishing condition.Polishing condition is as follows:
Polishing machine: UNIPOL-1502 single side polishing machine
Workpiece: diameter is sapphire c (0001) face of 50.8 mm
Polishing pad: polyurethane material, RODEL produce
Polish pressure: 6 kilograms
Lower wall rotating speed: 60 rpm
Polishing time: 120 minutes
After polishing, then washing and dry substrate, then measure the surface appearance feature of substrate.Surface average roughness (Ra) Ambios XI-100 surface topographic apparatus fo test, its resolving power is 0.1 dust.Test specification is 93.5 μm ' 93.5 μm.Substrate weight analytical balance weighs, and before and after polishing, weight difference is polishing speed divided by polishing time.
The polishing effect of each embodiment polishing fluid is respectively in table 1.Visible, with comparative example 1(pure silicon colloidal sol) compared with, the colloidal sol (embodiment 1,2,3) mixing Compostie abrasive particles containing magnesium, to after sapphire substrate polishing, all improves polishing velocity, and reduces the roughness of sapphire surface.
The each embodiment polishing fluid of table 1 is to the polishing effect of sapphire substrate
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| Polishing speed mg/h | 3.70 | 4.95 | 4.80 | 3.00 |
| Ra，nm | 1.775 | 1.695 | 1.104 | 2.654 |
Claims (4)
1. a Compostie abrasive particles for magnesium elements doped silicon oxide colloidal sol, is characterized in that having following composition:
A. magnesium elements compound (magnesium nitrate) 0.1-5 wt.%;
B. silica sol 99.9-95 wt.%.
2. a preparation method for magnesium elements doped silicon oxide colloidal sol Compostie abrasive particles, is characterized in that having following process and step:
A. first preparing pH value with base exchange method is 2.5, and massfraction is the silicic acid of 2.5 %,
B., under 100 DEG C of agitation conditions, be the silicic acid of 2.5 % by massfraction, massfraction is the Mg (NO of 1.1 %
3)
2solution and massfraction are that to add 750g massfraction be respectively in the silica-seed of 10 % to 1 % sodium hydroxide,
Sodium hydroxide controls whole sol system pH value and remains on 10.5, the rate of addition controlling magnesium nitrate and silicate mixture keeps velocity of evaporation and rate of addition in sol system to balance each other, the mass ratio of described silicate solution and described magnesium nitrate solution is 1:1
C. by dripping the magnesium nitrate solution of different amount, obtained magnesium doping is 0.5 wt%, the composite particles sol system of 1.0 wt%, 1.5 wt%, i.e. a kind of magnesium elements doped silicon oxide colloidal sol Compostie abrasive particles.
3. a polishing fluid composition, is characterized in that having following composition:
Magnesium doped silicon oxide Compostie abrasive particles 10-10.5%
Pentasodium triphosphate of dispersing agent 0.2-3%
Surfactant sodium dodecyl base benzene sulfonic acid sodium salt 0.01-1%,
Deionized water surplus;
The mass percentage sum of each composition is 100 wt % above.
4. a preparation method for polishing fluid composition, is characterized in that having following process and step:
A. above-mentioned magnesium elements doped silicon oxide colloidal sol Compostie abrasive particles solution sodium hydroxide adjust ph is to 10.5;
B. by 350 object screens, removing macrobead;
C. add 0.2-3% pentasodium triphosphate of dispersing agent, 0.01-1% surfactant sodium dodecyl base benzene sulfonic acid sodium salt, namely Homogeneous phase mixing obtains polishing fluid composition.
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Cited By (7)
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| CN105647478A (en) * | 2016-03-08 | 2016-06-08 | 上海大学 | Nickel element doped silicon dioxide composite abrasive particle, polishing solution composition and preparation method of polishing solution composition |
| CN105694811A (en) * | 2016-03-08 | 2016-06-22 | 上海大学 | Zinc doped silica sol composite abrasive particles, polishing agent composition and preparation method of polishing agent composition |
| CN108359384A (en) * | 2018-03-21 | 2018-08-03 | 合肥师范学院 | A kind of sapphire polishing liquid and preparation method thereof |
| 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 |
| CN111748318A (en) * | 2020-07-28 | 2020-10-09 | 上海大学 | Popcorn-like silica sol, preparation method and application thereof |
| CN115322594A (en) * | 2022-07-14 | 2022-11-11 | 中国科学院上海硅酸盐研究所 | High-infrared-radiation magnesium-doped silicon dioxide coating and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105647478A (en) * | 2016-03-08 | 2016-06-08 | 上海大学 | Nickel element doped silicon dioxide composite abrasive particle, polishing solution composition and preparation method of polishing solution composition |
| CN105694811A (en) * | 2016-03-08 | 2016-06-22 | 上海大学 | Zinc doped silica sol composite abrasive particles, polishing agent composition and preparation method of polishing agent composition |
| CN108359384A (en) * | 2018-03-21 | 2018-08-03 | 合肥师范学院 | A kind of sapphire polishing liquid and preparation method thereof |
| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
| 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 |
| CN111253910B (en) * | 2020-03-18 | 2021-07-16 | 昆山捷纳电子材料有限公司 | Preparation method of inorganic polyelectrolyte-silicon oxide composite polishing abrasive particles |
| CN111748318A (en) * | 2020-07-28 | 2020-10-09 | 上海大学 | Popcorn-like silica sol, preparation method and application thereof |
| CN115322594A (en) * | 2022-07-14 | 2022-11-11 | 中国科学院上海硅酸盐研究所 | High-infrared-radiation magnesium-doped silicon dioxide coating and preparation method thereof |
| CN115322594B (en) * | 2022-07-14 | 2023-04-07 | 中国科学院上海硅酸盐研究所 | High-infrared-radiation magnesium-doped silicon dioxide coating and preparation method thereof |
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Inventor after: Lei Hong Inventor after: Ma Pan Inventor after: Gu Qian Inventor after: Tong Kaiyu Inventor after: Liu Tingting Inventor after: Chen Ruling Inventor after: Huang Liqin Inventor after: Zhang Baichun Inventor before: Lei Hong Inventor before: Chen Ruling Inventor before: Ma Pan Inventor before: Gu Qian Inventor before: Tong Kaiyu Inventor before: Huang Liqin Inventor before: Zhang Baichun |
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Application publication date: 20150902 |