CN105907371A - Composite abrasive particle containing copper element doped silica sol as well as polishing liquid composition and preparation method of composite abrasive particle - Google Patents
Composite abrasive particle containing copper element doped silica sol as well as polishing liquid composition and preparation method of composite abrasive particle Download PDFInfo
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- CN105907371A CN105907371A CN201610328093.XA CN201610328093A CN105907371A CN 105907371 A CN105907371 A CN 105907371A CN 201610328093 A CN201610328093 A CN 201610328093A CN 105907371 A CN105907371 A CN 105907371A
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- copper
- silicon oxide
- abrasive particles
- doped silicon
- colloidal sol
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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
- C09K3/1436—Composite particles, e.g. coated particles
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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)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention provides a composite abrasive particle containing copper element doped silica sol as well as a polishing liquid composition and a preparation method of the composite abrasive particle. The composite abrasive particle comprises the following components in percentage by weight: 0.1wt%-5wt% of copper-containing compound and 95wt%-99.9wt% of silica sol. The composite abrasive particle is of a nanometer spherical physical structure, and the composite abrasive particle contains copper element capable of improving the chemical action of the abrasive particle in chemical composition, so that the polishing velocity of the abrasive particle can be increased, and the removal velocity of a material can be increased. By polishing a sapphire substrate by virtue of polishing liquid provided by the invention, the roughness of the surface of a sapphire can be effectively reduced, and the removal velocity of the surface of the sapphire can be effectively 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 copper doping
The preparation method of Ludox Compostie abrasive particles and raw material surface grinding and polishing technical field.
Background technology
Sapphire material due to its higher Mohs' hardness and preferable chemical stability, be widely used in electricity,
The fields such as optics.In optoelectronic areas, light emitting diode (LED) have low-work voltage, low-power consumption, high efficiency, the long-life,
The simple advantage such as solidification, fast-response speed and drive circuit, is acknowledged as 21 century high-tech sector most with prospects
One of.Sapphire has good high-temperature stability and mechanical property because of it, and as the backing material of LED.Sapphire table
Face quality has very important impact to LED component performance and quality, currently requires that ultra-smooth, zero defect and roughness are less than
0.2nm.Therefore the requirement of last one polishing of sapphire is the highest, becomes most important processing procedure.
At present, sapphire device surface is carried out precise polished by commonly used chemically mechanical polishing (CMP) technology.Abrasive particle is
Main component in chemical mechanical polishing liquid, abrasive grains widely used in current reality is typically silicon oxide, aluminium oxide etc. and passes
System inorganic particulate.And silicon oxide abrasive particle is preferable to sapphire polishing effect, but during CMP planarization, it is primarily present some asks
Topic, as low in polishing speed and cause production efficiency low, surface quality needs to continue to improve.Therefore we are by changing in polishing fluid
Abrasive particle characteristic improves clearance.
Patent application " 201110298605.X ", entitled " containing the polishing porous nano composite abrasive of active element, polishing
Liquid compositions and preparation method thereof ", this patent is traditional co-precipitation-sintering-ball milling method, lives although this method introduces
Property element improve the efficiency of polishing fluid, but be difficult to keep the good homogeneity of granule, and store, dispersive property relatively
Difference.
Summary of the invention
In place of solving the deficiencies in the prior art, the present invention prepares composite mill by growing method in aqueous solution
Grain, in preparation process, abrasive particle is in water solution system, favorable dispersibility, and is collosol state, improves polishing fluid polishing efficiency
While, also make Compostie abrasive particles be uniformly dispersed, be difficult to coagulation.
An object of the present invention there are provided a kind of copper doped silicon oxide colloidal sol Compostie abrasive particles.
The two of the purpose of the present invention are the polishing fluid combination provided containing copper doped silicon oxide colloidal sol Compostie abrasive particles
Thing.
The copper doped silicon oxide colloidal sol Compostie abrasive particles of the present invention, described Compostie abrasive particles, according to percetage by weight by
Following component forms:
Copper-containing compound 0.1-5%
Silica sol 95-99.9%.
Preferably,
Described Compostie abrasive particles consists of the following composition according to percetage by weight:
Copper-containing compound 1-2%
Silica sol 98-99%
Described copper-containing compound is Copper hydrate.
The preparation method of the copper doped silicon oxide colloidal sol Compostie abrasive particles of the present invention, comprises the steps:
1) by waterglass by cation exchange resin, when the pH value of the liquid flowed out is between 2.0-3.5, stream is received
The liquid gone out, then obtain active silicic acid solution；
2) under 100 DEG C and stirring, by copper nitrate solution and step 1) the active silicic acid solution of gained, join crystal seed oxygen
In SiClx solution, it is simultaneously added dropwise sodium hydroxide solution, controls rate of addition, keep the liquid level of silicon oxide crystal seed mother solution to keep basic
Constant, and control pH scope between 8.5-10.5；
3) control dropping and moisture evaporation rate, make the liquid level of mother solution keep being basically unchanged, until mixed liquor drips off, turn off
Heater, stirring cools to room temperature；I.e. obtain the Compostie abrasive particles of copper doped silicon oxide colloidal sol.
Described step 1) in, the mass fraction of waterglass is 8%；The mass fraction of described active silicic acid solution is 2-
3%.
Described step 2) in, the mass fraction of copper nitrate solution is 0.3%；The quality of described crystal seed silica solution
Mark is 10%.
Containing the polishing fluid composition of copper doped silicon oxide colloidal sol Compostie abrasive particles, described polishing fluid composition according to
Percetage by weight consists of the following composition:
Copper doped silicon oxide colloidal sol Compostie abrasive particles 10.06-10.12wt.%,
Sodium hexametaphosphate dispersant 6.67wt.%,
Deionized water surplus,
The weight/mass percentage composition sum of each component is 100%.
The preparation method of described polishing fluid composition, comprises the steps:
1) the above-mentioned copper doped silicon oxide colloidal sol Compostie abrasive particles solution screen by 350 mesh, removes bulky grain；
2) it is added thereto to sodium hexametaphosphate dispersant, stirs；Obtain polishing fluid composition.
The physical arrangement of the Compostie abrasive particles of the present invention is nanometer spherical, containing copper in the chemical composition of this abrasive particle, and copper
Element can improve the chemical action of abrasive particle.Chemical action can improve the polishing speed of abrasive particle, improves the removal rate of material.
Sapphire substrate is polished by the polishing fluid using the present invention to provide, and can be effectively reduced sapphire surface
Roughness, improves the removal rate of sapphire surface.
Detailed description of the invention
Now the specific embodiment of the present invention is summarized in rear.
Embodiment 1
The copper doped silicon oxide colloidal sol Compostie abrasive particles of the present embodiment can use coprecipitation to prepare.Preparation process is:
During Production of Silica Sol by Ion-Exchange, copper is doped in silica sol granule by the method for co-precipitation.
Specifically comprise the following steps that
1) being 8.0% waterglass by cation exchange resin by mass fraction, the pH value of liquid to be flowed out is at 2.0-
Receive the liquid flowed out time between 3.5, then obtaining mass fraction is 2.7% active silicic acid solution；
2) under 100 DEG C and stirring, it is 0.30% copper nitrate solution and 1954 grams of steps 1 by 1954 gram mass marks) institute
The mass fraction obtained is 2.7% active silicic acid solution, joins in the crystal seed silica solution that 3000 gram mass marks are 10%,
It is simultaneously added dropwise the sodium hydroxide solution that mass fraction is 0.5%, controls rate of addition, keep the liquid level of silicon oxide crystal seed mother solution to protect
Hold and be basically unchanged, and control pH scope between 8.5-10.5.
3) controlling dropping and moisture evaporation rate, make the liquid level of mother solution keep being basically unchanged, reaction is carried out always, until copper
After the mixed liquor of ion and active silicic acid drips, turning off heater after reacting 7 hours, stirring cools to room temperature；It is subsequently poured into
Beaker i.e. can get the Compostie abrasive particles of copper doped silicon oxide colloidal sol.
MCu(OH)2It it is the molal weight of Copper hydrate；
MCu(NO3)2It it is the molal weight of copper nitrate；
mCu(NO3)2It it is the inventory of copper nitrate；
mCu(NO3)2Inventory × 0.3% of=copper nitrate solution；
mCompostie abrasive particles solid contentFor the solid content that Compostie abrasive particles is total；
In embodiment 1 Copper hydrate content be (1954 × 0.3% × 98/187.56)/(3000 × 10%+1954 ×
0.3% × 98/187.56)=1%
Therefore, Compostie abrasive particles contains Copper hydrate and the silica sol granule of 99%w/w of 1%w/w.
During use, making polishing fluid composition, composition and the mass percent of polishing fluid composition are as follows:
Copper doped silicon oxide colloidal sol Compostie abrasive particles 10.06wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water surplus
The weight/mass percentage composition sum of each component is 100%.
The preparation method of polishing fluid composition:
1) the above-mentioned copper doped silicon oxide colloidal sol Compostie abrasive particles solution screen by 350 mesh, removes bulky grain；
2) it is added thereto to sodium hexametaphosphate dispersant, stirs；Obtain polishing fluid composition.
Embodiment 2
The copper doped silicon oxide colloidal sol Compostie abrasive particles of the present embodiment, preparation process is as follows: use 2931 gram masses to divide
Number be 0.30% copper nitrate solution and 2931 gram mass marks be 2.7% active silicic acid solution, other steps are with embodiment 1.
Obtain the Compostie abrasive particles of copper doped silicon oxide colloidal sol.
In embodiment 2 Copper hydrate content be (2931 × 0.3% × 98/187.56)/(3000 × 10%+2931 ×
0.3% × 98/187.56)=1.5%
Therefore, Compostie abrasive particles contains Copper hydrate and the silica sol granule of 98.5%w/w of 1.5%w/w.
During use, making polishing fluid composition, composition and the mass percent of polishing fluid composition are as follows:
Copper doped silicon oxide colloidal sol Compostie abrasive particles 10.09wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water surplus
The weight/mass percentage composition sum of each component is 100%.
The preparation method of polishing fluid composition is with embodiment 1.
Embodiment 3
The copper doped silicon oxide colloidal sol Compostie abrasive particles of the present embodiment, preparation process is as follows: use 3909 gram masses to divide
Number be 0.30% copper nitrate solution and 3909 gram mass marks be 2.7% active silicic acid solution, other steps are with embodiment 1.
Obtain the Compostie abrasive particles of copper doped silicon oxide colloidal sol.
In embodiment 3 Copper hydrate content be (3909 × 0.3% × 98/187.56)/(3000 × 10%+3909 ×
0.3% × 98/187.56)=2%
Therefore, Compostie abrasive particles contains Copper hydrate and the silica sol granule of 98%w/w of 2%w/w.
During use, making polishing fluid composition, composition and the mass percent of polishing fluid composition are as follows:
Copper doped silicon oxide colloidal sol Compostie abrasive particles 10.12wt.%
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water surplus
The weight/mass percentage composition sum of each component is 100%.
The preparation method of polishing fluid composition is with embodiment 1.
Comparative example 1
Unadulterated pure silica sol polishing fluid.Course of reaction does not i.e. drip copper nitrate solution, obtains undoped p
The pure silica colloidal sol polishing fluid of copper.
Composition and the mass percent of pure colloidal silica abrasive grain polishing solution are as follows:
The silica sol Compostie abrasive particles 10.00wt.% of undoped p copper
Sodium hexametaphosphate dispersant 6.67wt.%
Deionized water 83.33wt.%
Embodiment 4 polishing experiments
Using above-mentioned polishing fluid that sapphire substrate is polished under certain polishing condition experiment, polishing condition is as follows:
Buffing machine: UNIPOL-1502 single side polishing machine
Polishing workpiece: the sapphire substrate of a diameter 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 wash and be dried substrate, then measuring the surface appearance feature of substrate.Surface average roughness
(Ra) using AmbiosXI-100 surface topographic apparatus fo with microroughness (RMS), its resolving power is 0.1 angstrom.Test scope is 93.5 micro-
Rice × 93.5 microns.Substrate weight analytical balance weighs, and before and after polishing, weight difference divided by substrate surface area and polishing time is
Polishing speed.
It is visible, with comparative example 1 pure silica abrasive particle that each embodiment polishing fluid is shown in Table 1. respectively to sapphire polishing effect
Polishing fluid is compared, after sapphire substrate is polished by cupric element doping silica sol Compostie abrasive particles (embodiment 1,2,3),
All reduce roughness (Ra) and the microroughness (RMS) on sapphire substrate surface, and improve going of sapphire substrate surface
Except rate.
The table 1 various polishing fluid polishing effect to sapphire substrate
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| Clearance mg/h | 6.4 | 6.65 | 5.85 | 4.4 |
| Ra/nm | 1.350 | 1.227 | 1.199 | 2.281 |
| RMS/nm | 1.682 | 1.518 | 1.493 | 2.822 |
Claims (7)
1. a copper doped silicon oxide colloidal sol Compostie abrasive particles, it is characterised in that described Compostie abrasive particles is according to weight percent
Number consists of the following composition:
Copper-containing compound 0.1-5%
Silica sol 95-99.9%.
2. according to the copper doped silicon oxide colloidal sol Compostie abrasive particles described in claim 1, it is characterised in that described composite mill
Grain consists of the following composition according to percetage by weight:
Copper-containing compound 1-2%
Silica sol 98-99%
Described copper-containing compound is Copper hydrate.
3. the preparation method of copper doped silicon oxide colloidal sol Compostie abrasive particles as claimed in claim 1 or 2, it is characterised in that
Comprise the steps:
1) by waterglass by cation exchange resin, when the pH value of the liquid flowed out is between 2.0-3.5, outflow is received
Liquid, then obtain active silicic acid solution；
2) under 100 DEG C and stirring, by copper nitrate solution and step 1) the active silicic acid solution of gained, join crystal seed silicon oxide
In solution, it is simultaneously added dropwise sodium hydroxide solution, controls rate of addition, keep the liquid level of silicon oxide crystal seed mother solution to keep the most not
Become, and control pH scope between 8.5-10.5；
3) control dropping and moisture evaporation rate, make the liquid level of mother solution keep being basically unchanged, until mixed liquor drips off, turn off heating
Device, stirring cools to room temperature；I.e. obtain the Compostie abrasive particles of copper doped silicon oxide colloidal sol.
The preparation method of copper doped silicon oxide colloidal sol Compostie abrasive particles the most according to claim 3, it is characterised in that institute
The step 1 stated) in, the mass fraction of waterglass is 8%；The mass fraction of described active silicic acid solution is 2-3%.
The preparation method of copper doped silicon oxide colloidal sol Compostie abrasive particles the most according to claim 3, it is characterised in that institute
The step 2 stated) in, the mass fraction of copper nitrate solution is 0.3%；The mass fraction of described crystal seed silica solution is
10%.
6. the polishing fluid containing the copper doped silicon oxide colloidal sol Compostie abrasive particles as described in claim 1-2 any one combines
Thing, it is characterised in that described polishing fluid composition consists of the following composition according to percetage by weight:
Copper doped silicon oxide colloidal sol Compostie abrasive particles 10.06-10.12wt.%,
Sodium hexametaphosphate dispersant 6.67wt.%,
Deionized water surplus,
The weight/mass percentage composition sum of each component is 100%.
7. the preparation method of polishing fluid composition as claimed in claim 6, it is characterised in that comprise the steps:
1) the above-mentioned copper doped silicon oxide colloidal sol Compostie abrasive particles solution screen by 350 mesh, removes bulky grain；
2) it is added thereto to sodium hexametaphosphate dispersant, stirs；Obtain polishing fluid composition.
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| CN201610328093.XA CN105907371A (en) | 2016-05-17 | 2016-05-17 | Composite abrasive particle containing copper element doped silica sol as well as polishing liquid composition and preparation method of composite abrasive particle |
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| CN201610328093.XA CN105907371A (en) | 2016-05-17 | 2016-05-17 | Composite abrasive particle containing copper element doped silica sol as well as polishing liquid composition and preparation method of composite abrasive particle |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269695A (en) * | 2020-02-29 | 2020-06-12 | 上海大学 | Peanut-shaped silicon oxide abrasive particles and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104694081A (en) * | 2015-03-23 | 2015-06-10 | 江苏天恒纳米科技股份有限公司 | Cobalt-containing doped silicon dioxide nano-composite abrasive grain sol and preparation method thereof, and polishing solution and preparation method thereof |
| CN104745146A (en) * | 2015-03-23 | 2015-07-01 | 江苏天恒纳米科技股份有限公司 | Nano-composite abrasive particle sol containing cerium-doped silicon dioxide, polishing agent and preparation method thereof |
| CN104946202A (en) * | 2015-05-26 | 2015-09-30 | 上海大学 | Iron-doped silica sol composite abrasive grain, and polishing solution composition and preparation method thereof |
-
2016
- 2016-05-17 CN CN201610328093.XA patent/CN105907371A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104694081A (en) * | 2015-03-23 | 2015-06-10 | 江苏天恒纳米科技股份有限公司 | Cobalt-containing doped silicon dioxide nano-composite abrasive grain sol and preparation method thereof, and polishing solution and preparation method thereof |
| CN104745146A (en) * | 2015-03-23 | 2015-07-01 | 江苏天恒纳米科技股份有限公司 | Nano-composite abrasive particle sol containing cerium-doped silicon dioxide, polishing agent and preparation method thereof |
| CN104946202A (en) * | 2015-05-26 | 2015-09-30 | 上海大学 | Iron-doped silica sol composite abrasive grain, and polishing solution composition and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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