CN104559798B - A kind of alumina base chemical mechanical polishing liquid - Google Patents
A kind of alumina base chemical mechanical polishing liquid Download PDFInfo
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- CN104559798B CN104559798B CN201410837824.4A CN201410837824A CN104559798B CN 104559798 B CN104559798 B CN 104559798B CN 201410837824 A CN201410837824 A CN 201410837824A CN 104559798 B CN104559798 B CN 104559798B
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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
Abstract
A kind of alumina base chemical mechanical polishing liquid, in terms of the gross mass of the chemical mechanical polishing liquid, the chemical mechanical polishing liquid includes following components and percentage composition：0.1 ~ 30wt% of polishing particles, 0.01 ~ 10wt% of surfactant, surplus are pH adjusting agent and aqueous medium.The chemical mechanical polishing pulp that the present invention is provided can be controlled in 50nm/min to 200nm/min to the polishing speed of saphire substrate material, while surface roughness is reduced to less than 15.It can be realized to saphire substrate material controllable-rate, surface low damnification and the polishing of noresidue using above-mentioned polishing fluid.
Description
Technical field
The present invention relates to a kind of polishing fluid, and in particular to a kind of alumina base chemical mechanical polishing liquid.
Background technology
Sapphire, also known as white stone, are constituted as α-A12O3, it is transparent, there is identical optical characteristics and power with natural gemstone
Performance is learned, has good thermal characteristics, fabulous electrical characteristic and dielectric property, and anti-chemical corrosion, to infrared light transmission
Height, wearability is good, and hardness is only second to diamond, up to 9 grades of Mohs, still has preferable stability at high temperature, fusing point is 2030
DEG C, it is widely used in the field such as industry, national defence, scientific research, civilian, is increasingly being used as Solid State Laser, infrared window, semiconductor
The manufacture material of part in the high-tech sectors such as substrate slice, light emitting diode substrate piece, the accurate anti-friction bearing of chip.Sapphire
Because its hardness is high and fragility is big, machining is difficult.Especially to the sapphire substrate sheet precision processing technology for GaN growth
It is more complicated, it is the problem of current primary study.With developing rapidly for photoelectric technology, photovoltaic is to saphire substrate material
The increasingly increase of demand, while with the continuous expansion of LED element, sapphire have become most important backing material it
One, with great domestic and international market demand.
In the CMP process of sapphire crystal, polishing fluid, which is undoubtedly, determines its quality of finish polishing efficiency
The species of key, wherein abrasive material, the size of particle diameter and content have to the speed of polishing and the roughness flatness of polished surface etc.
Very big influence.Abrasive material used in current sapphire polishing liquids mainly has three kinds：Diamond powder, silicon dioxide gel and
α-Al2O3The nano dispersion fluid of (corundum aluminum oxide).The hardness of diamond is big, high polishing speed is can guarantee that, even if particle is big
It is small to reach nano level diamond powder, sapphire polished surface damage is will also result in seriously, because the hardness mistake of diamond
Height, in the polishing process on sapphire surface, substantially mechanical process, in addition, the use cost of diamond is than all
Other abrasive materials will be high, at present, and diamond liquid is used mainly as sapphire rough polishing or grinding.Sapphire final chemistry
It is most popular in mechanical polishing process to be alkaline silicon dioxide sol solution, sapphire chemically mechanical polishing Ludox
Silicon dioxide granule be usually 100 DEG C or so low temperature synthesize, hardness is well below sapphire crystal, and granular size is general
In 100nm or so, the general scope in 10-20% of polishing concentration.Due to being that low temperature is synthesized, the polishing fluid is not contained typically
Large granule, be difficult scuffing sapphire crystal is polished surface, and its suspension is good in addition, easy to use, and polishing fluid is in itself
It is cheap, but the disadvantage of Ludox polishing fluid is that polishing efficiency is low, and polishing time is tediously long；In addition, Ludox is thrown
Light liquid heated easy gel during glossing, and easily air-dried in sapphire surface, follow-up cleaning is unsuitable for,
Although the price of Ludox polishing fluid in itself is relatively low, the processing cost that it is integrated is still high, and low efficiency is that silica sol is thrown
The disadvantage of light liquid.
Alpha-alumina (α-Al2O3) be most stable of crystal phase in numerous alumina crystalline phases, it by other crystalline phases oxidation
Aluminium changes at high temperature to be formed, and is hardness very high material in native oxide crystal, and hardness is only second to diamond, is far longer than
Silica sol particles, it is in a kind of conventional polishing abrasive material, the polishing for being widely used in many hard materials.
Alpha-alumina (α-Al2O3) it is atomic arrangement mould in same material or material, material structure with sapphire in fact
Formula is identical, except that the difference of polycrystal and monocrystal.So, from hardness, Alpha-alumina (α-Al2O3) receive
Ground rice body is suitable with the hardness of sapphire crystal, can be used for polishing sapphire crystal.α-Al2O3Powder can be prepared into average
Granular size from 10nm to 1000nm more than different polishing fluids, for the rough polishing of sapphire crystal, the different processes that essence is thrown
In.But, up to the present, α-Al2O3Alumina polishing solution is not used in sapphire polishing on a large scale.α-
Al2O3Alumina particle needs the high temperature sintering by more than 1000 DEG C in preparation process, trigger transitional alumina to α-
Al2O3Phase in version, in the process, Al2O3Particle is easy to reunite, and these aggregate hard and compacts, it is difficult to effectively
Disperseed in polishing fluid.As a result, the alumina particle reunited easily produces cut scuffing in polishing process.Separately
Outside, aluminum oxide also easily sedimentation in polishing fluid, forms hard lump, it is necessary to maintain in use in the bottom of container
Stirring.These shortcomings, seriously hinder application of the alumina polishing solution on sapphire is precise polished.
The content of the invention
It is an object of the invention to provide a kind of alumina base chemical mechanical polishing liquid, polished in the prior art for overcoming
Liquid disperses uneven, and essence throws of poor quality, the problem of there are flaw and cut in surface.
The further object of the present invention is to provide a kind of preparation method of chemical mechanical polishing liquid as described above.
The further object of the present invention is to provide a kind of application of above-mentioned chemical mechanical polishing liquid.
To achieve the above object, the present invention is to take what following concrete technical scheme was realized：
A kind of alumina base chemical mechanical polishing liquid, in terms of the gross mass of the chemical mechanical polishing liquid, the chemical machine
Tool polishing fluid includes following components and percentage composition：
0.1~30wt% of polishing particles
0.01~10wt% of surfactant
Surplus is pH adjusting agent and aqueous medium.
Preferably, the polishing particles are selected from nano aluminium oxide, and the particle diameter of the polishing particles is 10~1500nm.
Preferably, the particle diameter of the polishing particles is 30~200nm.
Preferably, the polishing particles be shaped as it is spherical.
Preferably, the surfactant be selected from polyoxyethylene sodium sulphate, Sodium Polyacrylate, polyoxyethylene ether phosphate,
Alkylol polyoxyethylene base ether, cetyl trimethylammonium bromide, ammonium polyacrylate and one kind in polyvinylpyrrolidone or
It is a variety of.
It is highly preferred that the surfactant is selected from Sodium Polyacrylate, polyoxyethylene sodium sulphate, cetyl trimethyl bromine
Change the one or more in ammonium, polyoxyethylene ether phosphate and alkylol polyoxyethylene base ether
Preferably, the pH adjusting agent is in nitric acid, phosphoric acid, potassium hydroxide, ethoxy second diamino and tetramethyl hydrogen ammonia
One or more.
Preferably, the pH value range of the chemical mechanical polishing liquid is 1~11.
Preferably, the content of the surfactant is 0.05~2wt%.
Preferably, the content of the polishing particles is 0.5~25wt%.
It is highly preferred that the content of the polishing particles is 5~25wt%.
Preferably, the aqueous medium is deionized water.
The invention also discloses application of the chemical mechanical polishing liquid as described above in the CMP of Sapphire Substrate.
Oxide cmp particle is included provided by the present invention for the chemical mechanical polishing liquid of Sapphire Substrate.Polished
Cheng Zhong, polishing particles general action is can then to pass through its rigidity and external mechanical power with being polished materials chemistry crosslinking
Remove cross-linking products and taken away by liquid.This process moves in circles, so as to ensure that being carried out continuously for polishing process.It is wide at present
The oxide cmp particle of general application has titanium oxide, cerium oxide, colloidal silica, zirconium oxide, aluminum oxide etc., and their Mohs is hard
Degree is followed successively by 5~6,7,7,8.5,9.It is polished from the hard nano aluminium oxide of matter, chemical action is weaker in polishing process, it is main
The polishing to saphire substrate material higher rate can be achieved based on mechanical removal.
The chemical mechanical polishing pulp that the present invention is provided can be controlled in 50nm/ to the polishing speed of saphire substrate material
Min to 200nm/min, while surface roughness is reduced toBelow.Realized using above-mentioned polishing fluid section and sapphire is served as a contrast
Bottom material controllable-rate, surface low damnification and the polishing of noresidue.
Chemical mechanical polishing liquid in the present invention overcomes many disadvantages of the prior art and creative.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
In following examples, when sapphire substrate material polishing is tested the instrument that uses and parameter for：
A. instrument：CMP tester(CETR CP-4)
B. condition：Pressure (Down Force)：10psi
Polishing pad rotating speed (Pad Speed):150rpm
Rubbing head rotating speed (Carrier Speed):150rpm
Temperature：25℃
Polish flow velocity (Feed Rate)：125ml/min
C. polishing fluid：Polishing fluid obtained by Example is tested.
After being polished using the CP-4 polishing machines of U.S. CE TR companies to Sapphire Substrate, AFM atomic force microscopies are utilized
The roughness RMS (Root Mean Square) in the 5 μm of regions of μ m of mirror test saphire substrate material surface 5.
Embodiment 1
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 30
The parts by weight of surfactant 4
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 150nm；PH adjusting agent is salpeter solution；Table
Face activating agent is Sodium Polyacrylate.
The pH of chemical mechanical polishing liquid is 3.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 2
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 20
The parts by weight of surfactant 0.5
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 150nm；PH adjusting agent is salpeter solution；Table
Face activating agent is polyoxyethylene sodium sulphate.
The pH of chemical mechanical polishing liquid is 5.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 3
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 10
The parts by weight of surfactant 0.5
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 200nm；PH adjusting agent is potassium hydroxide；Table
Face activating agent is polyoxyethylene sodium sulphate.
The pH of chemical mechanical polishing liquid is 11.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 4
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 5
The parts by weight of surfactant 0.3
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 100nm；PH adjusting agent is phosphoric acid；Live on surface
Property agent be polyoxyethylene ether phosphate.
The pH of chemical mechanical polishing liquid is 1.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 5
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 30
The parts by weight of surfactant 0.01
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 1000nm；PH adjusting agent is nitric acid；Live on surface
Property agent be Sodium Polyacrylate.
The pH of chemical mechanical polishing liquid is 4.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 6
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 10
The parts by weight of surfactant 0.3
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 200nm；PH adjusting agent is phosphoric acid；Live on surface
Property agent be polyoxyethylene ether phosphate.
The pH of chemical mechanical polishing liquid is 3.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 7
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 15
The parts by weight of surfactant 0.5
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 300nm；PH adjusting agent is phosphoric acid；Live on surface
Property agent be polyoxyethylene sodium sulphate.
The pH of chemical mechanical polishing liquid is 2.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 8
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 15
The parts by weight of surfactant 1
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 1000nm；PH adjusting agent is tetramethyl hydrogen ammonia；
Surfactant is Sodium Polyacrylate.
The pH of chemical mechanical polishing liquid is 10.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Embodiment 9
In the present embodiment, the chemical mechanical polishing liquid is 100 parts by weight, wherein containing following raw material components and weight
Part：
The parts by weight of polishing particles 10
The parts by weight of surfactant 0.3
Surplus is water and pH adjusting agent.
Polishing particles described in the present embodiment are alumina particle；Particle diameter is 400nm；PH adjusting agent is ethoxy second two
Ammonia；Surfactant is polyoxyethylene ether phosphate.
The pH of chemical mechanical polishing liquid is 9.
Above-mentioned each raw material components are stirred and produce chemical mechanical polishing liquid.
It is as shown in table 1 that it polishes test result.
Table 1
As can be seen from Table 1, polishing speed of the chemical mechanical polishing pulp that the present invention is provided to saphire substrate material
50nm/min to 200nm/min is can be controlled in, while surface roughness is reduced toBelow.It is real using above-mentioned polishing fluid section
Now to saphire substrate material controllable-rate, surface low damnification and the polishing of noresidue.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (5)
1. a kind of alumina base chemical mechanical polishing liquid for Sapphire Substrate, it is characterised in that thrown with the chemical machinery
The gross mass meter of light liquid, the chemical mechanical polishing liquid includes following components and percentage composition：
0.1~30wt% of polishing particles
0.01~10wt% of surfactant
Surplus is pH adjusting agent and aqueous medium；
The polishing particles are selected from nano aluminium oxide, and the particle diameter of the polishing particles is 30~200nm；The shape of the polishing particles
Shape is spherical；
The surfactant is selected from polyoxyethylene sodium sulphate, Sodium Polyacrylate, polyoxyethylene ether phosphate, alkylol polyoxy second
One or more in alkene ether, cetyl trimethylammonium bromide, ammonium polyacrylate and polyvinylpyrrolidone；The chemistry
The pH value range of machine polishing liquor is 1~11.
2. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the pH adjusting agent is selected from nitric acid, phosphoric acid, hydrogen-oxygen
Change the one or more in potassium, AEEA.
3. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the content of the surfactant is 0.05~
2wt%.
4. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the content of the polishing particles is 0.5~
25wt%.
5. application of the chemical mechanical polishing liquid in the CMP of Sapphire Substrate as described in Claims 1 to 4 is any.
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| CN106010297B (en) * | 2016-06-20 | 2018-07-31 | 上海新安纳电子科技有限公司 | A kind of preparation method of alumina polishing solution |
| CN108239484B (en) * | 2016-12-23 | 2020-09-25 | 蓝思科技（长沙）有限公司 | Alumina polishing solution for sapphire polishing and preparation method thereof |
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| CN107083192A (en) * | 2017-04-17 | 2017-08-22 | 黄美香 | A kind of preparation method of alumina polishing solution |
| US20190085205A1 (en) * | 2017-09-15 | 2019-03-21 | Cabot Microelectronics Corporation | NITRIDE INHIBITORS FOR HIGH SELECTIVITY OF TiN-SiN CMP APPLICATIONS |
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| CN108485532A (en) * | 2018-04-23 | 2018-09-04 | 江苏金琥珀光学科技股份有限公司 | The sapphire polishing liquid and its polishing process of high surface smoothness |
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| CN111378385B (en) * | 2018-12-28 | 2023-08-08 | 安集微电子（上海）有限公司 | Application of alpha alumina abrasive in PI material polishing |
| CN109732462A (en) * | 2018-12-28 | 2019-05-10 | 江苏澳洋顺昌集成电路股份有限公司 | A kind of processing method of large-sized wafer |
| CN109807695A (en) * | 2019-03-29 | 2019-05-28 | 苏州恒嘉晶体材料有限公司 | A kind of sapphire substrate sheet polishing method |
| CN110272685A (en) * | 2019-06-10 | 2019-09-24 | 青海圣诺光电科技有限公司 | A kind of sapphire polishing liquid and preparation method thereof |
| CN110669439A (en) * | 2019-09-12 | 2020-01-10 | 江苏吉星新材料有限公司 | Coarse grinding fluid for sapphire grinding |
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