CN1330733C - Abrasive slurry having high dispersion stability and manufacturing method for a substrate - Google Patents

Abrasive slurry having high dispersion stability and manufacturing method for a substrate Download PDF

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Publication number
CN1330733C
CN1330733C CNB2004100055621A CN200410005562A CN1330733C CN 1330733 C CN1330733 C CN 1330733C CN B2004100055621 A CNB2004100055621 A CN B2004100055621A CN 200410005562 A CN200410005562 A CN 200410005562A CN 1330733 C CN1330733 C CN 1330733C
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abrasive
substrate
abrasive slurry
colloidal
slurry
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CN1550537A (en
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长俊连
岩城彰
麻生敏明
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AMA CHEMICALS Co Ltd
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AMA CHEMICALS Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C19/00Surface treatment of glass, not in the form of fibres or filaments, by mechanical means
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Mechanical Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Silicon Compounds (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention provides an abrasive slurry having high dispersion stability, including: abrasive fine particles made of one or more kinds of oxides; colloidal fine particles made of colloidal oxide with an average particle size smaller than an average particle size of the abrasive fine particles; and a dispersion medium in which the abrasive fine particles and the colloidal fine particles are dispersed, and a manufacturing method for a substrate as an inorganic substrate, including polishing the substrate using the abrasive slurry. An abrasive slurry according to the present invention keeps high dispersion stability for a long time and shows a satisfactory redispersion property, which can eliminate a problem about precipitation/aggregation as much as possible and can be used as a dispersant-free abrasive containing absolutely no organic dispersant. In particular, by using the abrasive slurry, it is possible to manufacture a substrate such as a silicon substrate used in a semiconductor manufacturing process or an aluminum substrate used in an electrostatic chuck manufacturing process through CMP with industrial advantage.

Description

The abrasive slurry that dispersion stabilization is good and the manufacture method of substrate
Technical field
The present invention relates to the good abrasive slurry of dispersion stabilization, though there is no particular limitation, but relating more specifically to be preferred for the surface grinding of carrying out in semi-conductor manufacturing process and electrostatic chuck manufacturing process that is used for the substrate surface planarization is the purposes of cmp (ChemicalMechanical Polishing is hereinafter referred to as " CMP ") representative, that extensively adopted by the grinding of abrasive surface at photomask blanks, glass disc, optical lens etc.
Background technology
For example, for silicon substrate that in semiconductor fabrication process, adopts and the substrates such as aluminium base that in electrostatic chuck manufacturing process, adopt, the flatness that needs very high degree of precision, as making conduct by the technology of the substrate surface planarization of abrasive surface, adopt following such technology, the CMP that promptly utilizes the mechanical mill that will be undertaken by abrasive particles and the chemical grinding that is undertaken by etching solution to combine does not make the substrate surface high planarization to substrate surface with causing damage.
And as the abrasive that adopts in such planarization, usually, corresponding to the kind of the grinding object that constitutes and the needed process velocity of technology of planarization etc., employing will have the cerium oxide (CeO of all size (median size) 2), Manganse Dioxide (MnO 2) wait Si oxide (SiO such as metal oxide and precipitated silica, fumed silica (fumed silica), colloidal silica 2) and aluminum oxide (Al such as vapor phase process aluminum oxide (fumed alumina), colloidal alumina 2O 3) wait various abrasive particles to be distributed to the slurry that obtains in the dispersion medium such as water.
Yet, these abrasive particles, make dispersion stabilization variation in the dispersion medium according to its kind and size, for example, under the situation of cerium oxide particles, owing to have bigger proportion, so when cerium oxide particles is distributed in the dispersion medium, during the modulation abrasive slurry, though the temporary transient homodisperse in modulation back, in the after this short time, its cerium oxide particles begins to separate, precipitation then causes the cohesion of particle soon, and its particle diameter increases, cause size-grade distribution such precipitation that broadens, coagulation problems, process velocity changed along with the time, and, produce problems such as substrate surface damage.
Thereby, in the past, for the precipitation that solves such abrasive slurry, the problem of cohesion, for example, be implemented in to use at once stir before the abrasive slurry so that abrasive particles once more the dispersive redispersion handle or to cohesion and become bigger unusual aggregated particle and filter and the separation that separates removal is removed and handled etc. than regulation particle diameter, the burden in the planarization operation of substrate etc. becomes big.
Therefore, the past has just proposed several be used to the solve precipitation of abrasive slurry, the problems of cohesion.
That is, propose a kind of cerium oxide abrasive, wherein, contained the multipolymer and the water of cerium oxide particle, vinylformic acid ammonium salt and methyl acrylate, be difficult to sedimentation, can be not to SiO 2The abrasive (opening 2000-17 with reference to the spy, No. 195 communiques) of the cerium oxide that grinds at a high speed of insulating film etc. with being caused damage by abrasive surface.
And, a kind of cerium oxide abrasive has also been proposed, wherein, contain at least a compound of from water soluble organic polymer, water soluble anionic surfactant, water soluble nonionic surfactant and water-soluble amine, selecting as dispersion agent, maximum settlement speed is below 1 μ m/s, sedimentation is little, is easy to carry out homogenizing by stirring, can not damage SiO 2Insulating films etc. are ground (opening 2001-138 with reference to the spy, No. 214 communiques) at a high speed by abrasive surface ground.
And then, a kind of cerium oxide abrasive has also been proposed, wherein, comprise cerium oxide particles, utilize ammonia to neutralize surpassing 90% first polyacrylate, utilizing ammonia neutralized 15~50% second polyacrylate and water of polyacrylic whole carboxyls of polyacrylic whole carboxyls, the total content of first polyacrylate and second polyacrylate is 0.15~1 weight %, have good stability, can not cause that two separate or coagulative precipitation are fixed, viscosity changes (holding 2002-353 with reference to the spy, No. 175 communiques).
But, even for the cerium oxide abrasive that contains these dispersion agents, in the long term more than one month or one month, eliminated the problem of precipitation, cohesion, but be difficult to keep the good order and condition of redispersibility, and in manufacturing process, confirmation can take place because the interior situations such as obstruction that install pipes that the abrasive of cohesion causes may not necessarily address these problems fully.
And, any cerium oxide abrasive among these, the organic compound such as water soluble organic polymer, water soluble anion surfacant, water soluble nonionic surfactant, water-soluble amine that contains more amount (0.1~5 weight %) as dispersion agent, in the waste liquid after milled processed, be mixed with the organic substance of the inorganic substance of cerium oxide particles and dispersion agent etc., in this liquid waste disposal, there are very trouble and the high problem of cost.
In addition, in such abrasive slurry, from the viewpoint that reduces manufacturing cost as much as possible and carry cost, then wish during fabrication, make the slurry of high density as far as possible, be diluted to normality in use and use, still, high density then is easy to generate the problem of precipitation, cohesion more, wishes further to develop the good abrasive slurry of dispersion stabilization.
Summary of the invention
At this, the inventor etc. are for good except dispersion stabilization in long-time and redispersibility is good, can eliminate precipitation, the coagulation problems as much as possible, the abrasive slurry that can use in the dispersion agent slurry that does not use organic class dispersion agent is fully conscientiously studied, found that, as the colloidal oxide compound, have the gluey particulate of the median size littler by interpolation, can suppress precipitation, the cohesion of abrasive particles as much as possible, realized the present invention than abrasive particles.
Thereby, the purpose of this invention is to provide a kind of abrasive slurry, this slurry except the dispersion stabilization in long-time good and redispersibility well, can eliminate as much as possible precipitation, the coagulation problems, can in the dispersion agent slurry that does not use organic class dispersion agent fully, use.
And, another object of the present invention provides a kind of manufacture method of substrate, this method adopts this abrasive slurry, is used for utilizing CMP advantageously to be manufactured on used substrates such as aluminium base in silicon substrate that semi-conductor manufacturing process uses and the electrostatic chuck manufacturing process industrial.
Promptly, the present invention is the good abrasive slurry of a kind of dispersion stabilization, comprises: the abrasive particles that constitutes by one or more oxide compound, as gluey oxide compound have the median size littler than above-mentioned abrasive particles colloidal particulate, make these abrasive particles and colloidal particulate dispersive dispersion medium.
And the present invention is the manufacture method of substrate, is to comprise the manufacture of substrates that adopts the grinding step that above-mentioned abrasive slurry grinds substrate.
In the present invention, the oxide compound as abrasive particles can use existing various abrasive particles in the same old way, particularly, can have for example: cerium oxide (CeO 2), Manganse Dioxide (MnO 2) wait Si oxide (SiO such as metal oxide and precipitated silica, fumed silica, colloidal silica 2) and aluminum oxide (Al such as vapor phase process aluminum oxide, colloidal alumina 2O 3) etc.Except can only using wherein a kind of separately, also can mix two or more the use.
Among these oxide compounds, being preferably for example has as abrasive particles use aspect among the present invention: it is higher or median size is bigger to resemble cerium oxide particles, aluminium oxide particles etc. and so on proportion, self be easy to cause the particle of precipitation, cohesion, effective especially for such polishing particles.
Median size (Dp) for the abrasive particles that adopts in the present invention has no particular limits, and is in addition, also different according to different its median sizes of kind, under the situation of cerium oxide particles, be generally 100~5,000nm, be preferably 500~2,000nm is according to the kind of abrasive particles, when median size (Dp) than 100nm hour, existence can not be given full play to the situation of mill capacity, on the contrary, and when greater than 5, during 000nm, exist abrasive surface to be easy to produce the problem of damage.
In addition,, for example can enumerate gluey oxide compounds such as colloidal silica, colloidal alumina for the colloidal particulate that uses with this abrasive particles, except can only use individually wherein a kind of, also can mix use two or more.
And, median size (Dc) for this colloidal particulate, have at least necessary less than above-mentioned abrasive particles, also can there be difference according to kind, comprising the colloidal silica situation in most cases, be generally 10~300nm, be preferably 20~200nm, the particle diameter ratio (Dc/Dp) of the median size (Dc) of the median size of above-mentioned abrasive particles (Dp) and its colloidal particulate is below 10, preferably about 0.01~3.When the median size (Dc) of this colloidal particulate than 10nm hour, instability during manufacturing is easy to gelation, on the contrary, when greater than 300nm, be easy to produce uneven at particle diameter, and when particle diameter ratio (Dc/Dp) surpassed 10, abrasive particles was too small as a result, can not give full play to mill capacity.
And then, for the dispersion medium that constitutes abrasive slurry, the dispersion medium that can in this abrasive slurry, use in the former state employing past, have no particular limits, the purposes of this abrasive slurry for example has: the CMP abrasive slurry of using in the substrate planarization of the aluminium base that uses in silicon substrate that uses in semiconductor fabrication process or the electrostatic chuck manufacturing process etc., also can be photomask blanks, glass disc, the CMP abrasive slurry that optical lens etc. are used in the grinding of abrasive surface, and then, can be in other common abrasive slurry of using in by the grinding of abrasive surface etc., can suit to select, but, preferably adopt water, or with water main component, contain methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, alcohols such as the trimethyl carbinol, ketone, the ester class, the aqueous dispersion medium of water-soluble solvents such as ethers.And, the same with the situation in past in this dispersion medium, when CMP, also can add the etching solution that is used to carry out chemical grinding as required.
And, particle concentration (Cp) for the above-mentioned abrasive particles that constitutes abrasive slurry of the present invention, according to the kind of abrasive particles and difference, under the situation of cerium oxide particles, be generally 5~40 weight %, be preferably 5~30 weight %, 5~10 weight % more preferably, and, for the particle concentration (Cc) of colloidal particulate, in the situation that comprises colloidal silica in most cases, be generally 0.1~5 weight %, be preferably 0.5~2 weight %, and then, the mixing ratio by weight of above-mentioned abrasive particles and colloidal particulate (Cc/Cp) is preferably below 0.5 below 1.With such particle concentration (Cp) and (Cc) synthetic abrasive slurry, with the particle concentration (Cp) of former state with (Cc) or as required be diluted to the particle concentration (Cp) of regulation and (Cc), be used in during CMP etc. grinds with dispersion agent.When the particle concentration (Cp) of abrasive particles was lower than 5 weight %, the mill capacity deficiency on the contrary, when being higher than 40 weight %, had problems aspect solvability.And when the particle concentration (Cc) of colloidal particulate was lower than 0.1 weight %, the effect that suppresses precipitation, cohesion descended, and on the contrary, when being higher than 5 weight %, is easy to produce coacervation conversely.And then, when the weight proportion (Cc/Cp) of abrasive particles and colloidal particulate surpasses 1, be easy to produce coacervation.
Abrasive slurry of the present invention, even particularly do not add organic class dispersion agents such as water soluble organic polymer, water soluble anionic surfactant, water soluble nonionic surfactant and water-soluble amine, also can keep good dispersion stabilization for a long time, and, redispersibility is good, can eliminate precipitation, coagulation problems as much as possible.
And, in the present invention, method to the modulation abrasive slurry, as long as adopt abrasive particles, colloidal particulate and the dispersion medium uniform mixing make as its constituent, abrasive particles and colloidal particulate evenly spread to slurry in the dispersion medium, have no particular limits, except adopting common stirrer modulates, as required, also can adopt wet type dispersion machines such as ultrasonic dispersing machine, homogenizing device, ball mill, vibromill, planetary ball mill, media-agitation type grinding machine.
Abrasive slurry of the present invention, be of use not only in the substrate leveling of silicon substrate that uses in the semi-conductor manufacturing process and the aluminium base that in electrostatic chuck manufacturing process, uses etc., also be used for the oxide film of silicon oxide insulating film etc. on wiring board, forming with regulation distribution, glass, inorganic insulating membranes such as silicon nitride, photomask, lens, opticglass such as prism, inorganic conductive films such as ITO, the optic integrated circuit that constitutes by glass and crystalline material, switching element, light-guide wave path, the end face of fiber optics, optics such as scintillator single crystal, the Solid State Laser single crystal, the LED sapphire substrate that blue laser is used, SiC, GaP, monocrystal semiconductors such as GaAS, glass substrate for disc, magnetic heads etc. grind.
For example, at the semiconductor substrate in the stage that has formed loop element and aluminum oxide distribution or formed on the substrate of semiconductor substrate etc. in loop element stage and formed in the substrate of oxide films such as silicon oxide insulating film, under the situation of the CMP of the leveling that is used to eliminate its oxide film concave-convex surface, employing is furnished with keeper that keeps substrate and the common grinding device that is pasted with the rotating disk of abrasive cloth (pad), utilize a certain amount of abrasive slurry of the present invention of each supply on abrasive cloth continuously such as pump, can and add to depress at the revolution of regulation and grind.
And, the same to the substrate after grind finishing with the situation of common subsequent disposal, after in mobile water, fully cleaning, adopt rotatory drier (spin direr) etc. to wipe attached to the water droplet on the substrate, make its drying then.
The waste liquid that substrate was discharged when grinding owing to be the dispersion agent monomer that does not adopt organic class dispersion agent fully, so with compare in the past, can carry out liquid waste disposal very economically.
Embodiment
Below, according to embodiment and comparative example, specify the preferred embodiment of the present invention.
Embodiment 1~27
[modulation of colloidal silica (20nm)]
Is being furnished with the 1m that liquid distillates the band cover of mouth, grasshopper and stirrer 3In the container, add methyl silicate 32kg, methyl alcohol 100kg and pure water 768kg, be mixed and made into A liquid.
And, be furnished with the 3m of stirrer 3In the container, add the ammoniacal liquor 12kg of methyl silicate 368kg, methyl alcohol 100kg, pure water 1840g and 28wt%, be mixed and made into B liquid.
Secondly, to adding the container steam heating of A liquid, distillate the mixed solution of first alcohol and water, when beginning from A liquid, to distillate liquid, add B liquid so that the liquid level of A liquid keeps certain, till B liquid is all added, and then, add the pure water of 240kg so that the liquid level of A liquid keeps certain, make its reaction.
After reaction finishes, take out reaction product in the container that has added A liquid and analyze, the result is the silica colloidal product (colloidal silica (20nm)) of 20 weight %, median size 20nm for silica concentration.
[modulation of colloidal silica (70nm)]
3m at the band cover of being furnished with stirrer 3In the container, add the ammoniacal liquor 88.4kg of methyl alcohol 1721.7kg, pure water 306.3kg and 28wt%, after the mixing, the liquid temperature is adjusted to 23 ± 1 ℃, then, Yi Bian the liquid temperature is remained on 23 ± 1 ℃, with the methyl silicate that under agitation added 404.4kg in 2~2.5 hours, make its reaction on one side.
After reaction finishes, the raw product of the reaction mixture that obtained is transferred to be furnished with that liquid distillates mouthful, the 1m of the band cover of grasshopper and stirrer 3In the container, to the container steam heating, distillate the mixed solution of methyl alcohol, water and ammonia, begin distillating liquid from container, add remaining reaction mixture so that liquid level keeps certain, till reaction mixture is all added, and then, add pure water so that liquid level keeps constant, add the liquid temperature of pure water in container and reach 100 ℃.
When the liquid temperature arrives 100 ℃, finish heating, cool off, add the ammoniacal liquor of an amount of 28wt% when the liquid temperature reaches 70 ℃, and then after stirring, mixing, take out reaction product from container as intermediate.
The reaction product that is obtained is that silica concentration is that 30 weight % and median size are the silica colloidal product (colloidal silica (70nm) of 70nm.
[modulation of colloidal silica (170nm)]
At the 1.8m that is furnished with stirrer, band cover 3In the container, add the ammoniacal liquor 113.25kg of methyl alcohol 885.1kg, pure water 63.1kg and 28wt%, after mixing temperature is adjusted to 23 ± 1 ℃, then, the liquid temperature is maintained 23 ± 1 ℃ on one side, on one side the lasting methyl silicate that under agitation added 171.1kg in 3 hours, react.
After reaction finishes, the raw product of the reaction mixture that obtained transferred to be furnished with that liquid distillates mouthful, the 1m of the band cover of grasshopper and stirrer 3In the container, to the container steam heating, distillate the mixed solution of methyl alcohol, water and ammonia, begin distillating liquid from container, add residual reaction mixture so that liquid level keeps certain, when reaction mixture is all added, and then, add pure water so that liquid level keeps certain, add the liquid temperature of pure water in container always and reach 100 ℃.
When the liquid temperature reaches 100 ℃, finish heating, cool off, when the liquid temperature reaches 70 ℃, add the ammoniacal liquor of an amount of 28wt% as intermediate, and then, after stirring and mixing, take out reaction product from container.
The reaction product that obtains is that silica concentration is the silica colloidal product (colloidal silica (170nm)) of 22 weight % and median size 170nm.
[modulation of abrasive slurry]
Adopt cerium oxide particles (the SEIMICHEMICAL society system of median size 1.1 μ m and maximum particle diameter 8 μ m as abrasive particles, trade(brand)name: TE-508), adopt 3 kinds of colloidal silicas pressing above-mentioned acquisition as colloidal particulate, adopt pure water as dispersion medium, ratio with expression in the table 1 cooperates, mix with stirrer, modulate the abrasive slurry of each embodiment 1~27.
[evaluation of precipitation, state of aggregation and redispersibility]
For the abrasive slurry of each embodiment 1~27 that is obtained, the slurry of 50ml is joined 100ml in vitro, after leaving standstill 1 month, the state of visual observation precipitation, cohesion.
And, the abrasive slurry of 50ml is joined in the polyethylene container made of 100ml, leave standstill 1 month time.Then, the redispersibility that visual observation is vibrated with hand, and, its traverse (is gone into the Jiang Shanghuishe system: the V-1M type) in desktop ball milling stirrer, at mixing speed is that 100rpm, churning time are to stir under 10 minutes the condition, the redispersibility that visual observation is obtained by stirrer.
Divide 4 grades of results that estimate above-mentioned precipitation, state of aggregation and redispersibility:
◎: precipitation portion is all softening, can redispersion with the hand vibration in the several seconds, and in addition, utilize the stirrer can redispersion within 5 minutes,
Zero: have solid-state part in precipitation portion, realized redispersion in about 30 seconds with hand vibration needs, in addition, utilizing stirrer to carry out redispersion needs about 10 minutes,
△: have solid-state part in precipitation portion, need to realize redispersion more than 2 minutes with the hand vibration, in addition, utilizing stirrer to carry out redispersion needs about 10 minutes,
*: the whole completely solidified of precipitation portion, can not redispersion with hand vibration 10 minutes, in addition, utilizing stirrer to carry out redispersion needs more than 10 minutes.
The result is illustrated in the table 1.
[quartz base plate grinding rate]
In addition, abrasive slurry is diluted to 3 times with ultrapure water, adopt the CMP be furnished with abrasive cloth with shredder (Nanofactor society system: FACT-200), at revolution 200rpm, tonnage 500g/cm 2, and the abrasive slurry supply rate be under the condition of 10ml/min, sample (quartz base plate of width 3.3cm * 2.6cm, thickness 1.15mm) was ground 10 minutes, utilize micrometer to measure the sample thickness that grinds front and back, obtain for quartz base plate (SiO by the sample thickness before and after grinding 2) grinding rate (μ m/10min).
The result is illustrated in the table 1.
Comparative example 1~15
Adopt polyvinylpyrrolidone (PVP) as organic class dispersion agent, the same with the situation of the foregoing description 1~27, the abrasive slurry of modulation comparative example 1~15, abrasive for each comparative example 1~15 that is obtained, the same with the situation of each embodiment 1~27, estimate precipitation, state of aggregation and redispersibility, and, obtain for quartz base plate (SiO 2) grinding rate (μ m/10min).
The result is illustrated in the table 1 with the various embodiments described above 1~27.
[table 1]
Embodiment No. 1 2 3 4 5 6 7 8 9
Abrasive is formed (wt%) Cerium oxide particles (CeO 2) 5 15 30 5 15 30 5 15 30
Colloidal silica (20nm) 1 1 1 2 2 2 5 5 5
Dispersion agent - - - - - - - - -
The evaluation of precipitation curdled appearance and redispersibility
Quartz base plate grinding rate (3 times of diluents: μ m/10min) 10 10 10 10 10 10 10 10 10
Embodiment No. 10 11 12 13 14 15 16 17 18
Abrasive is formed (wt%) Cerium oxide particles (CeO2) 5 15 30 5 15 30 5 15 30
Colloidal silica (70nm) 1 1 1 2 2 2 5 5 5
Dispersion agent - - - - - - - - -
The evaluation of precipitation curdled appearance and redispersibility
Quartz base plate grinding rate (3 times of diluents: μ m/10min) 10 10 10 10 10 10 10 10 10
Embodiment No. 19 20 21 22 23 24 25 26 27
Abrasive is formed (wt%) Cerium oxide particles (CeO 2) 5 15 30 5 15 30 5 15 30
Colloidal silica (170nm) 1 1 1 2 2 2 5 5 5
Dispersion agent - - - - - - - - -
The evaluation of precipitation curdled appearance and redispersibility
Quartz base plate grinding rate (3 times of diluents: μ m/10min) 10 10 10 10 10 10 10 10 10
Comparative example No. 1 2 3 4 5 6 7 8 9
Abrasive is formed (wt%) Cerium oxide particles (CeO 2) 5 15 30 5 15 30 5 15 30
Colloidal silica - - - - - - - - -
Dispersion agent - - - 1 1 1 3 3 3
The evaluation of precipitation curdled appearance and redispersibility × × × × × ×
Quartz base plate grinding rate (3 times of diluents: μ m/10min) - - - 10 10 10 10 10 10
Comparative example No. 10 11 12 13 14 15
Abrasive is formed (wt%) Cerium oxide particles (CeO 2) 5 15 30 5 15 30
Colloidal silica - - - - - -
Dispersion agent 1 1 1 3 3 3
The evaluation of precipitation curdled appearance and redispersibility
Quartz base plate grinding rate (3 times of diluents: μ m/10min) 10 10 10 10 10 10
As the result from table 1 shows, any precipitation with the abrasive slurry of various embodiments of the present invention 1~27, the evaluation of state of aggregation and redispersibility, and the performance excellent properties is relative in the quartz base plate grinding rate, do not add the abrasive slurry of the comparative example 1~3 of any colloidal particulate and dispersion agent, can not realize redispersion, can not measure grinding rate, in addition, the abrasive slurry of comparative example 4~15 of only adding the dispersion agent of 1 weight % or 3 weight % needs for a long time when redispersion, show that abrasive slurry of the present invention is especially in precipitation, state of aggregation and redispersibility aspect have excellent characteristic.
Adopt the present invention, a kind of abrasive slurry is provided, its dispersion stabilization in long-time is good, in addition, redispersibility is good, can eliminate the problem of precipitation, cohesion as much as possible, and, can in the dispersion agent monomer that does not adopt organic class dispersion agent fully, use.
And, utilize abrasive slurry of the present invention, can utilize CMP at the industrial substrate that advantageously is manufactured on silicon substrate that uses in the semi-conductor manufacturing process or the aluminium base that in the electrostatic chuck manufacturing process, uses etc.

Claims (7)

1, the abrasive slurry that a kind of dispersion stabilization is good, comprise: the abrasive particles that constitutes by one or more oxide compound, for gluey oxide compound has the colloidal particulate of the median size littler than above-mentioned abrasive particles and makes these abrasive particles and colloidal particulate dispersive dispersion medium, the median size Dp of abrasive particles is 100~5,000nm, the median size Dc of colloidal particulate is 10~300nm, the particle diameter ratio Dc/Dp of the median size Dp of above-mentioned abrasive particles and the median size Dc of colloidal particulate is below 10, the particle concentration Cp of abrasive particles is 5~30 weight %, the particle concentration Cc of colloidal particulate is 0.1~5 weight %, and the mixing ratio by weight Cc/Cp of above-mentioned abrasive particles and colloidal particulate is below 1.
2, the good abrasive slurry of dispersion stabilization as claimed in claim 1 wherein, does not contain organic dispersing agent.
3, the good abrasive slurry of dispersion stabilization as claimed in claim 1 or 2, wherein, dispersion medium is water or is the aqueous dispersion medium of main component with water.
4, the good abrasive slurry of dispersion stabilization as claimed in claim 1 or 2, wherein, abrasive particles is a cerium oxide particles.
5, the good abrasive slurry of dispersion stabilization as claimed in claim 1 or 2, wherein, colloidal particulate is a colloidal silica.
6, a kind of manufacture of substrates is characterized in that, is the method for making the inorganics substrate, comprises the grinding step that adopts any one described abrasive slurry of claim 1~5 to grind aforesaid substrate.
7, manufacture of substrates as claimed in claim 6 wherein, has oxide film on the surface of substrate.
CNB2004100055621A 2003-05-09 2004-02-18 Abrasive slurry having high dispersion stability and manufacturing method for a substrate Expired - Lifetime CN1330733C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP131025/2003 2003-05-09
JP2003131025A JP2004331852A (en) 2003-05-09 2003-05-09 Abrasive slurry excellent in dispersion stability, and manufacturing method for substrate

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Families Citing this family (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005244123A (en) * 2004-02-27 2005-09-08 Fujimi Inc Polishing composition
US7056192B2 (en) * 2004-09-14 2006-06-06 International Business Machines Corporation Ceria-based polish processes, and ceria-based slurries
JP2006086462A (en) * 2004-09-17 2006-03-30 Fujimi Inc Polishing composition and manufacturing method of wiring structure using the same
KR100497413B1 (en) * 2004-11-26 2005-06-23 에이스하이텍 주식회사 Slurry for tungsten-chemical mechanical polishing and method for manufacturing of the same
US7294044B2 (en) * 2005-04-08 2007-11-13 Ferro Corporation Slurry composition and method for polishing organic polymer-based ophthalmic substrates
US7467988B2 (en) * 2005-04-08 2008-12-23 Ferro Corporation Slurry composition and method for polishing organic polymer-based ophthalmic substrates
JP2007103463A (en) * 2005-09-30 2007-04-19 Sumitomo Electric Ind Ltd POLISHING SLURRY, SURFACE TREATMENT METHOD OF GaxIn1-xAsyP1-y CRYSTAL, AND GaxIn1-xAsyP1-y CRYSTAL SUBSTRATE
JP4983603B2 (en) 2005-10-19 2012-07-25 日立化成工業株式会社 Cerium oxide slurry, cerium oxide polishing liquid, and substrate polishing method using the same
WO2007055278A1 (en) * 2005-11-11 2007-05-18 Hitachi Chemical Co., Ltd. Polishing agent for silicon oxide, liquid additive, and method of polishing
TWI414811B (en) * 2006-03-23 2013-11-11 Sumitomo Chemical Co Method for producing a layered material containing a layer of inorganic particles
JP4731384B2 (en) * 2006-04-04 2011-07-20 多摩化学工業株式会社 Method for producing acidic and stable colloidal silica
US20100062287A1 (en) * 2008-09-10 2010-03-11 Seagate Technology Llc Method of polishing amorphous/crystalline glass to achieve a low rq & wq
US20100243670A1 (en) * 2009-03-24 2010-09-30 Ferro Corporation Methods and products for replenishing a polishing slurry in a polishing apparatus
US9368367B2 (en) * 2009-04-13 2016-06-14 Sinmat, Inc. Chemical mechanical polishing of silicon carbide comprising surfaces
CN103282160A (en) * 2010-12-29 2013-09-04 Hoya株式会社 Manufacturing method for glass substrate for magnetic disk, and manufacturing method for magnetic disk
WO2013065491A1 (en) * 2011-11-01 2013-05-10 旭硝子株式会社 Method for producing glass substrate
CN102709523A (en) * 2012-06-13 2012-10-03 湖南丰源业翔晶科新能源股份有限公司 Process for dispersing carbon nanotubes in electroconductive adhesive of lithium ion battery
KR101727848B1 (en) * 2013-03-13 2017-04-17 가부시키가이샤 후지미인코퍼레이티드 Slurry for thermal spraying, thermal sprayed coating, and method for forming thermal sprayed coating
KR20150123939A (en) 2013-03-13 2015-11-04 가부시키가이샤 후지미인코퍼레이티드 Slurry for thermal spraying, thermal spraying film, and formation method for thermal spraying film
JP6484894B2 (en) 2014-03-28 2019-03-20 山口精研工業株式会社 Abrasive composition and method for polishing magnetic disk substrate
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4462188A (en) * 1982-06-21 1984-07-31 Nalco Chemical Company Silica sol compositions for polishing silicon wafers
CN1077974A (en) * 1992-04-27 1993-11-03 罗德尔公司 Composition and method that polishing and planarizing surfaces are used
CN1288920A (en) * 1999-09-21 2001-03-28 不二见株式会社 Polishing composition

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4113282B2 (en) * 1998-05-07 2008-07-09 スピードファム株式会社 Polishing composition and edge polishing method using the same
US6428392B1 (en) * 1999-03-23 2002-08-06 Seimi Chemical Co., Ltd. Abrasive
US6261476B1 (en) 2000-03-21 2001-07-17 Praxair S. T. Technology, Inc. Hybrid polishing slurry
CN1200066C (en) * 2000-05-12 2005-05-04 日产化学工业株式会社 Polishing composition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4462188A (en) * 1982-06-21 1984-07-31 Nalco Chemical Company Silica sol compositions for polishing silicon wafers
CN1077974A (en) * 1992-04-27 1993-11-03 罗德尔公司 Composition and method that polishing and planarizing surfaces are used
CN1288920A (en) * 1999-09-21 2001-03-28 不二见株式会社 Polishing composition

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