CN104946202A - Iron-doped silica sol composite abrasive grain, and polishing solution composition and preparation method thereof - Google Patents
Iron-doped silica sol composite abrasive grain, and polishing solution composition and preparation method thereof Download PDFInfo
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- CN104946202A CN104946202A CN201510276371.7A CN201510276371A CN104946202A CN 104946202 A CN104946202 A CN 104946202A CN 201510276371 A CN201510276371 A CN 201510276371A CN 104946202 A CN104946202 A CN 104946202A
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Abstract
The invention relates to an iron-doped silica sol composite abrasive grain, and a polishing solution composition and a preparation method thereof. The preparation method of the composite abrasive grain comprises the following steps: adding a 0.29 wt% ferric chloride solution and a 2-3 wt% dilute silicic acid solution in a mass ratio of 1:1 into a silica crystal seed under certain reaction conditions, and doping the iron element into the silica sol abrasive grain in the silica sol growth process to form the uniform stable iron-doped silica sol composite abrasive grain, wherein the doping mass percent is 0.1-5.0%. The physical structure of the composite abrasive grain is nano spherical. The chemical composition of the abrasive grain contains the iron element capable of performing chemical actions with the sapphire and silicon chip surface, thereby enhancing the polishing rate. When being used for polishing the sapphire substrate and silicon chip, the polishing solution provided by the invention can effectively lower the surface roughness and microroughness of the sapphire and silicon chip and enhance the polishing rate of the sapphire and silicon chip.
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 preparation method of ferro element doped silicon colloidal sol Compostie abrasive particles and starting 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, photodiode (LED) has the simple advantage such as low-work voltage, reduce power consumption, high-level efficiency, long lifetime, solidification, fast-response speed and driving circuit, is acknowledged as one of 21 century high-tech sector most with prospects.Sapphire because it has good high-temperature stability and mechanical property, and as the substrate material of LED.Sapphire surface quality has very important impact to LED component Performance and quality, requires ultra-smooth, zero defect and roughness is less than 0.2nm at present.Therefore the requirement of last one polishing of sapphire is very high, becomes most important processing procedure.
At present, chemically machinery polished (CMP) technology is generally adopted to carry out precise polished to sapphire device surface.Abrasive particle is the main component in chemical mechanical polishing liquid, the abrasive grain normally conventional inorganic such as silicon oxide, the aluminum oxide particle extensively adopted in current reality.And silicon oxide abrasive particle is better to sapphire polishing effect, but mainly in CMP polishing process there are some problems, as low in polishing speed and cause production efficiency low, surface quality needs to continue to improve.Therefore we improve clearance by changing abrasive particle characteristic in polishing fluid.
Summary of the invention
An object of the present invention there are provided a kind of ferro element doped silicon colloidal sol Compostie abrasive particles.
Two of object of the present invention is to provide the polishing fluid composition adopting this Compostie abrasive particles.
For achieving the above object, the present invention adopts following technical scheme.
A kind of ferro element doped silicon of the present invention colloidal sol Compostie abrasive particles, is characterized in that having following composition
Ferro element compound (ironic hydroxide) 0.1-5 wt.%;
Silica sol 99.9-95 wt.%.
The preparation method of a kind of ferro element doped silicon oxide of the present invention colloidal sol Compostie abrasive particles, is characterized in that having following process and step:
A. by massfraction be 8.0 % water glass by Zeo-karb, when the pH value of the liquid flowed out is between 2.5-3.5 receive flow out liquid, then obtaining massfraction is 2.0-3.0% active silicic acid solution;
B. at 100 DEG C and under stirring, be 0.29% ferric chloride Solution and 750-3000 gram mass mark by 750-3000 gram mass mark be 2.0-3.0% active silicic acid solution, joining 3000 gram mass marks is in the crystal seed silica solution of 10%, drip massfraction is the sodium hydroxide solution of 0.4% simultaneously, control rate of addition, keep the liquid level of silicon oxide crystal seed mother liquor to keep substantially constant, and control pH scope is between 9.0-11.0;
C. control to drip and moisture velocity of evaporation, make the liquid level of mother liquor keep substantially constant, until mixed solution drips off, reaction turns off well heater after half an hour, stirs and cools to room temperature; Namely the Compostie abrasive particles of ferro element doped silicon oxide colloidal sol is obtained.
A kind of polishing fluid composition of the present invention, is characterized in that having following composition:
A. ferro element doped silicon oxide colloidal sol Compostie abrasive particles 6-6.12 wt.%,
B. sodium hexametaphosphate dispersant 2 wt.%,
C. deionized water surplus;
D. the mass percentage sum of above each composition is 100 wt.%.
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 ferro element doped silicon oxide colloidal sol Compostie abrasive particles solution is passed through 350 object screens, removing macrobead;
B. the solution that deionized water is mixed with 5 liters is added wherein;
C. add 100 grams of sodium hexametaphosphate dispersants more wherein, stir; Namely polishing fluid composition is obtained.
The physical structure of Compostie abrasive particles of the present invention is nanometer spherical, and containing ferro element in the chemical constitution of this abrasive particle, ferro element can improve the chemical action of abrasive particle.Chemical action can improve the polishing speed of abrasive particle, improves the removal speed of material.
Adopt polishing fluid provided by the invention to carry out polishing to sapphire substrate, silicon chip, effectively can reduce the roughness of sapphire, silicon chip surface, improve the removal speed of sapphire, silicon chip surface.
Embodiment
Now specific embodiments of the invention are summarized in rear.
Embodiment 1
Ferro element doped silicon oxide colloidal sol Compostie abrasive particles of the present invention can adopt coprecipitation method to prepare.Preparation process is: be doped in silica sol particle by the method for co-precipitation by ferro element in the process of Production of Silica Sol by Ion-Exchange.By massfraction be 8.0 % water glass by Zeo-karb, when the pH value of the liquid flowed out is between 2.5-3.5 receive flow out liquid, then obtaining massfraction is 2.0-3.0% active silicic acid solution; At 100 DEG C and under stirring, be 0.29% ferric chloride Solution and 750 gram mass marks by 750 gram mass marks be 2.0-3.0% active silicic acid solution, joining 3000 gram mass marks is in the crystal seed silica solution of 10%, drip massfraction is the sodium hydroxide solution of 0.4% simultaneously, control rate of addition, keep the liquid level of silicon oxide crystal seed mother liquor to keep substantially constant, and control pH scope is between 9.0-11.0.Reaction is carried out always, until after the mixed solution of iron ion and active silicic acid drips, reaction terminates, and stops heating, continues to be stirred to solution to room temperature, then pour in beaker the Compostie abrasive particles solution that can obtain ferro element doped silicon oxide colloidal sol into.Before polishing, Compostie abrasive particles solution is considered sieve through 350 objects, adds the polishing fluid that deionized water is mixed with 5 liters, then add 100g sodium hexametaphosphate dispersant, stir.The polishing fluid of the solution of gained to be namely doping mass ratio the be ferro element doped silicon oxide colloidal sol Compostie abrasive particles of 0.48%.
Doping mass ratio is that the composition of 0.48 % Fe2O3 doping colloidal silica composite abrasive grain polishing solution and mass percent are as follows:
Ferro element doped silicon oxide colloidal sol Compostie abrasive particles 6.02 wt.%
Sodium hexametaphosphate dispersant 2 wt.%
Deionized water 91.98 wt.%
Embodiment 2
Adopt 1500g massfraction be 0.29% ferric chloride Solution and 1500g massfraction be 2.0-3.0% active silicic acid solution.Finally obtain the polishing fluid of the ferro element doped silicon oxide colloidal sol Compostie abrasive particles of doping mass ratio 0.96%.
Doping mass ratio is that the composition of 0.96 % Fe2O3 doping colloidal silica composite abrasive grain polishing solution and mass percent are as follows:
Ferro element doped silicon oxide colloidal sol Compostie abrasive particles 6.06 wt.%
Sodium hexametaphosphate dispersant 2 wt.%
Deionized water 91.94 wt.%
Embodiment 3
Adopt 3000g massfraction be 0.29% ferric chloride Solution be that 2.0-3.0% active silicic acid solution mixes with 3000g massfraction.Finally obtain the polishing fluid of the ferro element doped silicon oxide colloidal sol Compostie abrasive particles of doping mass ratio 1.91%.
Doping mass ratio is that the composition of 1.91 % Fe2O3 doping colloidal silica composite abrasive grain polishing solutions and mass percent are as follows:
Ferro element doped silicon oxide colloidal sol Compostie abrasive particles 6.12 wt.%
Sodium hexametaphosphate dispersant 2 wt.%
Deionized water 91.88 wt.%
Comparative example 1
Unadulterated pure silica sol polishing fluid.Namely do not drip ferric chloride Solution in reaction process, obtain the pure silica colloidal sol polishing fluid of non-doping iron.
Composition and the mass percent of pure colloidal silica abrasive grain polishing solution are as follows:
Silica sol Compostie abrasive particles 6.0 wt.% of non-doping iron element
Sodium hexametaphosphate dispersant 2 wt.%
Deionized water 92 wt.%
Polishing experiments
Use above-mentioned polishing fluid to carry out polishing experiments to sapphire substrate, silicon chip under certain polishing condition, polishing condition is as follows:
Polishing machine: UNIPOL-1502 single side polishing machine
Polishing workpiece: diameter is the sapphire substrate of 50.8nm, diameter is the silicon chip of 50.8nm
Polishing pad: polyurethane material, RODEL produce
Polish pressure: sapphire is finished to 6 kilograms, silicon wafer polishing is 4 kilograms
Lower wall rotating speed: 60rpm
Polishing time: sapphire is finished to 3 hours, silicon wafer polishing is 1 hour
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 dust.Test specification is 93.5 microns × 93.5 microns.Substrate weight analytical balance weighs, and before and after polishing, divided by substrate surface, long-pending and polishing time is polishing speed to weight difference.
Each embodiment polishing fluid is visible in table 1. respectively to sapphire polishing effect, compared with comparative example 1 pure silica abrasive grain polishing solution, after iron content element doping silica sol Compostie abrasive particles (embodiment 1,2,3) carries out polishing to sapphire substrate, all reduce roughness (Ra) and the microroughness (RMS) on sapphire substrate surface, and improve the clearance on sapphire substrate surface.
Each embodiment polishing fluid is visible in table 2. respectively to the polishing effect of silicon chip, the silicon oxide abrasive grain polishing solution pure with comparative example 1() compared with, after iron content element doping silica sol Compostie abrasive particles (embodiment 1,2,3) carries out polishing to silicon chip, all reduce roughness (Ra) and the microroughness (RMS) of silicon chip surface, and substantially increase clearance.
Claims (4)
1. a Compostie abrasive particles for ferro element doped silicon oxide colloidal sol, is characterized in that having following composition:
A. ferro element compound (iron(ic) chloride) 0.1-5 wt.%;
B. silica sol 99.9-95 wt.%.
2. a preparation method for ferro element doped silicon oxide colloidal sol Compostie abrasive particles, is characterized in that having following process and step:
A. by massfraction be 8.0 % water glass by Zeo-karb, when the pH value of the liquid flowed out is between 2.5-3.5 receive flow out liquid, then obtaining massfraction is 2.0-3.0% active silicic acid solution;
B. at 100 DEG C and under stirring, be 0.29% ferric chloride Solution and 750-3000 gram mass mark by 750-3000 gram mass mark be 2.0-3.0% active silicic acid solution, joining 3000 gram mass marks is in the crystal seed silica solution of 10%, drip massfraction is the sodium hydroxide solution of 0.4% simultaneously, control rate of addition, keep the liquid level of silicon oxide crystal seed mother liquor to keep substantially constant, and control pH scope is between 9.0-11.0;
C. control to drip and moisture velocity of evaporation, make the liquid level of mother liquor keep substantially constant, until mixed solution drips off, reaction turns off well heater after half an hour, stirs and cools to room temperature; Namely the Compostie abrasive particles of ferro element doped silicon oxide colloidal sol is obtained.
3. a polishing fluid composition, is characterized in that having following composition:
Ferro element doped silicon oxide colloidal sol Compostie abrasive particles 6-6.12 wt.%,
Sodium hexametaphosphate dispersant 2 wt.%,
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 ferro element doped silicon oxide colloidal sol Compostie abrasive particles solution is by 350 object screens, removing macrobead;
B. the solution that deionized water is mixed with 5 liters is added wherein;
C. add 100 grams of sodium hexametaphosphate dispersants more wherein, stir; Obtain polishing fluid composition.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105238354A (en) * | 2015-11-04 | 2016-01-13 | 华侨大学 | Hard-core soft-shell composite abrasive, and preparation method and application thereof |
| 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 |
| CN105885790A (en) * | 2016-05-17 | 2016-08-24 | 江苏天恒纳米科技股份有限公司 | Titanium element doped silicon oxide sol composite abrasive grains, as well as polishing solution and preparation method thereof |
| CN105907371A (en) * | 2016-05-17 | 2016-08-31 | 江苏天恒纳米科技股份有限公司 | Composite abrasive particle containing copper element doped silica sol as well as polishing liquid composition and preparation method of composite abrasive particle |
| CN110551454A (en) * | 2018-06-01 | 2019-12-10 | 凯斯科技股份有限公司 | Polishing slurry composition |
| 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 |
| CN114525108A (en) * | 2022-02-18 | 2022-05-24 | 太仓硅源纳米材料有限公司 | Silica sol active abrasive particles for chemical mechanical polishing and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424373A (en) * | 2001-12-14 | 2003-06-18 | 长兴化学工业股份有限公司 | Composite abradant and composition and preparation thereof |
| CN102127373A (en) * | 2011-01-06 | 2011-07-20 | 清华大学 | Chemical and mechanical polishing composition for high-removal and low-scratch silicon chip and preparation method thereof |
| CN102408871A (en) * | 2011-09-28 | 2012-04-11 | 上海大学 | Porous nano composite abrasive particle containing polishing active elements, polishing solution composition and preparation method thereof |
| CN103450813A (en) * | 2013-01-10 | 2013-12-18 | 湖南皓志新材料股份有限公司 | Preparation method of iron-doped zirconium oxide polishing solution |
| CN104046245A (en) * | 2014-06-11 | 2014-09-17 | 泰安麦丰新材料科技有限公司 | Manufacturing method of silicon-aluminum composite polishing solution |
-
2015
- 2015-05-26 CN CN201510276371.7A patent/CN104946202A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424373A (en) * | 2001-12-14 | 2003-06-18 | 长兴化学工业股份有限公司 | Composite abradant and composition and preparation thereof |
| CN102127373A (en) * | 2011-01-06 | 2011-07-20 | 清华大学 | Chemical and mechanical polishing composition for high-removal and low-scratch silicon chip and preparation method thereof |
| CN102408871A (en) * | 2011-09-28 | 2012-04-11 | 上海大学 | Porous nano composite abrasive particle containing polishing active elements, polishing solution composition and preparation method thereof |
| CN103450813A (en) * | 2013-01-10 | 2013-12-18 | 湖南皓志新材料股份有限公司 | Preparation method of iron-doped zirconium oxide polishing solution |
| CN104046245A (en) * | 2014-06-11 | 2014-09-17 | 泰安麦丰新材料科技有限公司 | Manufacturing method of silicon-aluminum composite polishing solution |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105238354A (en) * | 2015-11-04 | 2016-01-13 | 华侨大学 | Hard-core soft-shell composite abrasive, and preparation method and application thereof |
| 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 |
| CN105885790A (en) * | 2016-05-17 | 2016-08-24 | 江苏天恒纳米科技股份有限公司 | Titanium element doped silicon oxide sol composite abrasive grains, as well as polishing solution and preparation method thereof |
| CN105907371A (en) * | 2016-05-17 | 2016-08-31 | 江苏天恒纳米科技股份有限公司 | Composite abrasive particle containing copper element doped silica sol as well as polishing liquid composition and preparation method of composite abrasive particle |
| CN110551454A (en) * | 2018-06-01 | 2019-12-10 | 凯斯科技股份有限公司 | Polishing slurry composition |
| CN110551454B (en) * | 2018-06-01 | 2022-04-19 | 凯斯科技股份有限公司 | Polishing slurry composition |
| 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 |
| CN114525108A (en) * | 2022-02-18 | 2022-05-24 | 太仓硅源纳米材料有限公司 | Silica sol active abrasive particles for chemical mechanical polishing and preparation method thereof |
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