CN103917332A - Method for producing glass substrate - Google Patents

Method for producing glass substrate Download PDF

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Publication number
CN103917332A
CN103917332A CN201280054271.4A CN201280054271A CN103917332A CN 103917332 A CN103917332 A CN 103917332A CN 201280054271 A CN201280054271 A CN 201280054271A CN 103917332 A CN103917332 A CN 103917332A
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CN
China
Prior art keywords
glass substrate
manufacture method
water
lapping liquid
quality
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CN201280054271.4A
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Chinese (zh)
Inventor
神谷广幸
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AGC Inc
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Asahi Glass Co Ltd
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Filing date
Publication date
Application filed by Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Publication of CN103917332A publication Critical patent/CN103917332A/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00Lapping machines or devices; Accessories
    • B24B37/04Lapping machines or devices; Accessories designed for working plane surfaces
    • B24B37/042Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
    • B24B37/044Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Liquid Crystal (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The present invention relates to a method for producing a glass substrate, wherein at least one main surface of a glass substrate main body is polished with a polishing liquid which is obtained by dispersing abrasive grains in a dispersion medium that is composed of a liquid medium other than water, said dispersion medium substantially containing no water or containing some water (provided that the water content in the dispersion medium is 85% by mass or less).

Description

The manufacture method of glass substrate
Technical field
The present invention relates to the manufacture method of glass substrate.More specifically, relate to manufacture method glass substrate, high-intensity glass substrate using in flat-panel monitors (FPD) such as being suitable for liquid crystal display (LCD).
Background technology
As display unit such as the information terminal such as personal computer, mobile phone, liquid crystal TV sets, use the flat-panel monitors (FPD) such as liquid crystal display (LCD).
The glass substrate of using for FPD, is accompanied by the miniaturization of equipment etc., requires lightweight, slimming.But in the time reducing the thickness of glass substrate, intensity declines, and easily cracks because falling etc.Therefore,, for glass substrate, require the glass substrate that slimming and intensity are high, can obtain good defencive function.
The glass substrate of using for FPD, for example melten glass is configured as tabular by the method for making that is called as float glass process, utilize the grinding apparatus of for example rotation and revolution to grind this glass substrate, small concavo-convex, the fluctuating on surface are removed, (for example manufacture thus the thickness of the regulation that meets the desired flatness of FPD glass substrate, 0.4~1.1mm) thin plate (for example,, with reference to patent documentation 1).
For so thin glass substrate, if surface exists concavo-convex or scar, not only poor in appearance, and easily break or crackle because external pressure produces take these positions as starting point, cannot obtain sufficient intensity.Therefore,, for so thin glass substrate, require effects on surface accurately to grind and obtain higher intensity.
For example, the method for polishing surface that the slurry that utilizes the colloidal silica agglomerate that makes to be linked with concavo-convex colloidal silica particles to be dispersed in water to form grinds glass baseplate surface is disclosed in patent documentation 1.In addition, the operation that uses grinding Liquid composition to grind glass substrate is disclosed in patent documentation 2, the silicon dioxide granule of the Area Ratio of the maximum inscribed circle area of the projected area that described grinding Liquid composition comprises silicon dioxide granule and this silicon dioxide granule in prescribed limit.
By utilizing above-mentioned method to carry out surface treatment to glass substrate, can remove to a certain extent the concavo-convex of glass baseplate surface or rise and fall, but the problem that the effect that exists the intensity of the glass substrate after grinding to improve may not be fully such.Therefore, require to improve with higher precision the method for the intensity of glass substrate.
As the enhanced processing method to glass substrate, knownly for example on glass baseplate surface, form compressive stress layer and put forward high-intensity method.Wherein, chemical enhanced facture is to flood glass substrate in the fused salt that comprises alkali metal ion, by the alkali metal ion displacement in the alkali metal ion in the glass of substrate surface and fused salt, on glass baseplate surface, form thus the method for compressive stress layer, as improve glass substrate intensity method and be widely used (for example,, with reference to patent documentation 3).
Chemical enhanced facture is not owing to needing the thickness of glass substrate self, and the intensity that is therefore particularly suitable for thin glass substrate improves, but processing required equipment becomes on a large scale, the problem that exists cost to be wanting in.
In addition, for the glass substrate of using, how forming from the teeth outwards the film of metal or metal oxide and to use for the display of liquid crystal indicator etc., when contain alkali metal in glass time, alkali metal ion spreads in film, may make membrane property deteriorated.Therefore, the glass substrate of using as display, uses and does not contain in fact alkali-metal alkali-free glass, and such glass substrate exists the problem that cannot be suitable for above-mentioned chemical enhanced facture.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2010-250915 communique
Patent documentation 2: TOHKEMY 2008-13655 communique
Patent documentation 3: TOHKEMY 2010-202514 communique
Summary of the invention
Invent problem to be solved
The present invention completes in order to address the above problem, and its object is to provide the manufacture method that can obtain having improved with high accuracy the glass substrate of the glass substrate of intensity in the glass substrate that is applicable to liquid crystal indicator etc.
For the means of dealing with problems
In the manufacture method of glass substrate of the present invention, utilize decentralized medium substantially moisture or not moisture, that comprise the liquid medium beyond water (wherein, in this decentralized medium water containing proportional be that 85 quality % are following) in be dispersed with abrasive particle lapping liquid at least one interarea of glass substrate main body is ground.
In the manufacture method of glass substrate of the present invention, in preferred described decentralized medium water containing proportional be 3~60 quality %.
In the manufacture method of glass substrate of the present invention, water containing the proportional 3 quality % that are less than in preferred described decentralized medium.
In the manufacture method of glass substrate of the present invention, the liquid medium beyond preferred described water is organic solvent.
In the manufacture method of glass substrate of the present invention, preferred described organic solvent is monohydric alcohol or polyalcohol.
In the manufacture method of glass substrate of the present invention, preferred described organic solvent is hydro carbons, ethers, ester class or ketone.
In the manufacture method of glass substrate of the present invention, the liquid medium beyond preferred described water is at least a kind that selects in the group of free methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, propane diols, n-hexane, octane, ethyl acetate, MEK, toluene and ether composition.
In the manufacture method of glass substrate of the present invention, preferred described abrasive particle is the particulate that selects at least a kind of metal oxide in the group of free silica, aluminium oxide, ceria, titanium dioxide, zirconia and manganese oxide composition.
In the manufacture method of glass substrate of the present invention, preferred described abrasive particle is that average grain diameter is the particle of 5~500nm.
In the manufacture method of glass substrate of the present invention, the abrasive particle containing in preferred described lapping liquid containing the proportional gross mass with respect to this lapping liquid be 0.1~40 quality %.
In the manufacture method of glass substrate of the present invention, preferably supply with described lapping liquid to grinding pad, the face that is polished of described glass substrate main body is contacted with described grinding pad, and by relative motion between the two, the described face that is polished is ground.
In the manufacture method of glass substrate of the present invention, preferred described glass substrate is the glass substrate that comprises alkali-free glass.
In the manufacture method of glass substrate of the present invention, the thickness of preferred described glass substrate is 0.1~5mm.
Invention effect
According to the present invention, can obtain the glass substrate to have improved intensity than in the past high precision.
Accompanying drawing explanation
Fig. 1 is the figure that represents an example of the lapping device that can use in the manufacture method of glass substrate of the present invention.
Fig. 2 is the figure that represents an example of the lapping device that can use in the manufacture method of glass substrate of the present invention.
Fig. 3 is the figure that represents the relation of the intensity containing the glass substrate obtaining after proportional and grinding of water in decentralized medium.
The specific embodiment
Below, take the FPD as LCD etc. with and the manufacture method of the glass substrate of use describes embodiments of the present invention as example.
The present invention is not limited to these embodiments, as long as aim according to the invention just comprises in the present invention.
In the manufacture method of glass substrate of the present invention, can limit lapping liquid be supplied to grinding pad, limit makes the face that is polished of glass substrate contact with grinding pad, and by relative motion between the two, the face that is polished of glass substrate is ground.
As the lapping device using, can use known lapping device in the past in above-mentioned grinding.Fig. 1 is the figure that represents an example of the lapping device that can use in the manufacture method of glass substrate of the present invention.
In lapping device 10 shown in Fig. 1, with can be around its vertical axle center C1 rotatably supported state be provided with grinding plate 1, this grinding plate 1 utilizes platform drive motor 2 to drive along the direction rotation shown in arrow in figure.Be pasted with known grinding pad 3 at the upper surface of this grinding plate 1.
On the other hand, the position of departing from from axle center C1 on grinding plate 1, is used the substrate holding structure (carrier) 5 of the grinding objects such as maintenance glass substrate such as absorption or holding frame supporting along rotation around the C2 of its axle center and the mode that can move along axle center C2 direction at lower surface.This substrate holding structure 5 is to utilize not shown artifact-driven motor or utilization to form along the mode of the direction rotation shown in arrow from the turning moment of above-mentioned grinding plate 1.At the lower surface of substrate holding structure 5, with on opposed of above-mentioned grinding pad 3 maintain as the glass substrate main body 4 of grinding object.Glass substrate main body 4 with regulation load by being pressed on grinding pad 3.
In addition, be provided with dribbling nozzle 6 etc. near of substrate holding structure 5, the lapping liquid 7 that never illustrated tank is sent is supplied on grinding plate 1.
In the time utilizing such lapping device 10 to grind, utilizing platform drive motor 2 and artifact-driven motor to make grinding plate 1 and be pasted on grinding pad 3, the substrate holding structure 5 on this grinding plate 1 and be held under the state rotariling actuate around glass substrate main body 4 axle center separately, edge of these substrate holding structure 5 lower surfaces, lapping liquid 7 is supplied to the surface of grinding pad 3 from dribbling nozzle 6 grades, and the glass substrate main body 4 being kept by substrate holding structure 5 is pressed on this grinding pad 3.Thus, the face that is polished to glass substrate main body 4, grind with the opposed face of grinding pad 3.
As lapping liquid 7, be to make abrasive particle be scattered in the pulp-like liquid that decentralized medium forms.In the present invention, as decentralized medium, use not moisture in fact or contain decentralized medium water below particular bound, that comprise the liquid medium beyond water.
By using such lapping liquid 7 to grind the face that is polished of glass substrate main body, the moisture can suppress to grind time in lapping liquid is invaded to glass substrate body interior, and can reduce the amount of moisture containing in glass substrate main body.Therefore, can improve with high accuracy the intensity of the glass substrate obtaining after grinding.
Decentralized medium is the liquid medium for abrasive particle stably being disperseed and making the described later any composition adding as required disperse, dissolve.Liquid medium in the present invention refers to organic compound or the water for liquid at normal temperatures, can be also a kind of above mixture in them.
Being organic compound as liquid medium, being not limited to be commonly called the low molecular compound of organic solvent, can be to be liquid macromolecular compound (for example, being called oily macromolecular compound) at normal temperatures.The boiling point of liquid medium is preferably more than 60 ℃, but is not limited to this.
The decentralized medium of the lapping liquid using in the present invention is not moisture or moisture in fact, comprises water liquid medium in addition, and in the case of moisture decentralized medium, in this decentralized medium, the content of water is below 85 quality %.
In the present invention, water-free in fact decentralized medium refers to the proportional decentralized medium that is less than 3 quality % that contains of water.Typically refer to and in the liquid medium beyond the water, do not add the water of substantial amount and decentralized medium while using.It should be noted that, below, unless otherwise specified, by the liquid medium beyond water referred to as liquid medium.
In the time that decentralized medium of the present invention is moisture, be preferably liquid medium and water dissolve each other separate uniform mixture.In the time that liquid medium and water do not dissolve mutually, for example, while there is undissolved water in decentralized medium, in grinding, the water capacity easily enters glass substrate inside, and the intensity of the glass substrate obtaining after grinding may not can fully raises.Even substantially in the situation of water-free decentralized medium, be also preferably dissolved in liquid medium to be less than a small amount of water that the scope of 3 quality % exists.
Water containing the proportional gross mass with respect to decentralized medium while exceeding 85 quality % in decentralized medium, even if the uniform decentralized medium that water and liquid medium dissolve mutually, in the grinding of glass substrate, water also can easily enter glass substrate inside, and the intensity of the glass substrate obtaining after grinding may not can fully improves.In the case of moisture decentralized medium, in decentralized medium, the proportional gross mass with respect to decentralized medium that contains of water is preferably below 60 quality %, more preferably below 20 quality %.
As lapping liquid 7, preferably use water for the gross mass of lapping liquid containing proportional be that 80 quality % are following, the more preferably lapping liquid below 50 quality %.
As liquid medium, preferably boiling point is 40 ℃ of above, preferred 60 ℃ of above organic solvents.
In organic solvent, hydrophilic organic solvent easily with than relatively large water mixes as uniform mixture.Therefore, hydrophilic organic solvent is suitable as the liquid medium in moisture decentralized medium.In addition, even if hydrophilic organic solvent, water-free in fact organic solvent, i.e. also can be used as water-free in fact decentralized medium containing the proportional organic solvent that is less than 3 quality % and use of water.
On the other hand, the high organic solvent of hydrophobicity is few owing to being mixed in equably amount of moisture wherein, therefore, uses usually used as the liquid medium of water-free in fact decentralized medium.
In addition, have hydrophilic organic solvent to a certain degree contain its dissolve water below tolerance and water containing proportional be 3 quality % when above, the liquid medium can be used as in moisture decentralized medium uses.In addition, when substantially not moisture, water containing proportional while being less than 3 quality %, the liquid medium can be used as in water-free in fact decentralized medium uses.
As liquid medium, preferably use the organic solvents such as such as monohydric alcohol or polyalcohol, hydro carbons, ethers, ester class, ketone.In addition, as liquid medium, also can use the mixture of the organic solvent of more than two kinds with intermiscibility.
In above-mentioned organic solvent, monohydric alcohol or the polyalcohol etc. of low carbon atom number is hydrophilic organic solvent, as mentioned above, is suitable as the liquid medium in moisture decentralized medium, water-free in fact decentralized medium.As monohydric alcohol or polyalcohol, the more preferably alkanol of carbon number below 4, single aklylene glycol or two aklylene glycols of carbon number 2~8.
On the other hand, aliphatic hydrocarbon, ester ring type hydro carbons, the hydro carbons such as aromatic hydrocarbon based are hydrophobicity, as mentioned above, are suitable as the liquid medium of water-free in fact decentralized medium.As hydro carbons, the more preferably saturated aliphatic hydrocarbon of carbon number 5~12.
As ethers, preferably alkylene glycol monoalkyl ethers or the aklylene glycol dialkyl ether of carbon number below 8, as ester class, the preferably aliphatic carboxylic acid Arrcostab of carbon number below 8.In addition the also preferred dialkyl ketone such as dialkyl ether, MEK such as aromatic hydrocarbon based, the ether such as toluene etc..
As organic solvent, particularly, for example can enumerate: methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol (following, to be called IPA), n-butanol, the tert-butyl alcohol, amylalcohol, hexanol, enanthol, octanol, decyl alcohol, the monohydric alcohol of the carbon number 1~12 of dodecanol etc., allyl alcohol, crotonyl alcohol, the unsaturated alcohols such as methyl ethylene alcohol, cyclopentanol, cyclohexanol, phenmethylol, the cyclic alcohols such as benzyl carbinol, ethylene glycol, propane diols, diethylene glycol, the dihydroxylic alcohols such as DPG, glycerine, the polyalcohol more than ternary of pentaerythrite etc., ether, propyl ether, butyl ether, ethyl vinyl ether, methyl phenyl ethers anisole, diphenyl ether, dioxane, oxolane, acetal, propylene glycol monomethyl ether, the ethers such as dihydroxypropane single-ether, Ethyl formate, methyl formate, methyl acetate, ethyl acetate, butyl acetate, benzoic ether, the ester classes such as oxalate, acetone, MEK, methyl iso-butyl ketone (MIBK), 2 pentanone, propione, methyl-n-butyl ketone, 2-HEPTANONE, cyclohexanone, the ketones such as acetophenone, pentane, hexane, heptane, octane, nonane, decane, hendecane, dodecane, methylpentane, dimethylbutane, trimethylpentane, the representative examples of saturated aliphatic hydro carbons such as isooctane, hexene, heptene, the unsaturated fatty hydrocarbons classes such as octene, pentamethylene, cyclohexane, hexahydrotoluene, cyclohexene, cyclohexyl ring hexane, the ester ring type hydro carbons such as naphthalane, benzene, toluene, dimethylbenzene, ethylbenzene, isopropylbenzene, mesitylene, detergent alkylate, naphthalene, methyl naphthalene, styrene etc. are aromatic hydrocarbon based, chloromethanes, carrene, chloroform, dichloroethanes, trichloroethanes, tetrachloro-ethylene, dichloropropane, chloropropene, chlorobutane, chlorobenzene, bromoethane, the halogenated hydrocarbons such as Bromofume, formic acid, acetic acid, propionic acid, caproic acid, the organic acids such as oleic acid, nitromethane, nitroethane, nitrobenzene, acetonitrile, methylamine, dimethylamine, ethamine, diethylamine, allylamine, aniline, dimethylaniline, toluidines, pyrroles, piperidines, pyridine, picoline, quinoline, ethylenediamine, Diethylenetriamine, formamide, NMF, dimethyl formamide, pyrrolidones, the nitrogen compound classes such as caprolactam, thiophene, the sulphur compound classes such as methyl-sulfoxide.
Wherein, from the easness of the dispersion of abrasive particle, obtain the viewpoint of good abrasive characteristic, can preferably use at least a kind of organic solvent in the group of selecting free methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, propane diols, n-hexane, octane, ethyl acetate, MEK, toluene and ether composition.
It should be noted that, as liquid medium, as long as water be not limited to organic solvent as above containing proportional low fluid, also can use the petroleum-type solvent, natural oil lipid, low polymer, silicone oil of such as benzinum, lam-oil, gasoline etc. etc.
As the abrasive particle being scattered in decentralized medium, can from known abrasive particle, suitably select.Particularly, be preferably and select free silica, aluminium oxide, ceria, zirconia, titanium dioxide, tin oxide, zinc oxide, manganese oxide, the particulate of the metal oxides such as germanium oxide, boron nitride, silicon nitride, the particulate of the nitride such as titanium nitride, carborundum, the particulate of the carbide such as boron carbide, polyethylene, polypropylene, polystyrene, acrylic resin, phenolic resins, polyester, the particulate of the resins such as organic siliconresin, gold, silver, the particulate of the metals such as copper, graphite, the particulate of the carbon such as diamond, sodium carbonate, calcium carbonate, calcium sulfate, in the group of the ultrafine particles composition of the salt such as sodium chloride and potassium chloride at least a kind.
Wherein, from obtaining high grinding precision, the viewpoint of grinding rate, can preferably use selecting the particulate of at least a kind of metal oxide in the group of free silica, aluminium oxide, ceria, zirconia, titanium dioxide and manganese oxide composition.
As silica, can use the silica that utilizes known method to manufacture.For example, can use by sol-gal process the alkyl silicate such as silester, the methyl silicate colloidal silica obtaining that is hydrolyzed.In addition, can use to the silicate such as sodium metasilicate are carried out ion-exchange and the colloidal silica that obtains, silicon tetrachloride carried out in the flame of oxygen and hydrogen to the aerosil that gas phase is synthesized into.
In addition, as silicon dioxide granule, also can use surface to there is the particle of concaveconvex shape.
Similarly, also can preferably use colloidal alumina.And, also can preferably use the ceria, zirconia, titanium dioxide, tin oxide, the zinc oxide that utilize liquid phase method, vapor phase method to manufacture.Wherein, calm particle diameter easy to control and the viewpoint that can obtain high-purity product are set out, and preferably use colloidal silica.
From the viewpoint of grinding rate, abrasive characteristic, dispersion stabilization, the average grain diameter of abrasive particle is the scope in 5~500nm preferably, more preferably the scope of 10~200nm.In the time that the average grain diameter of abrasive particle is less than 5nm, abrasive particle easily condenses in lapping liquid, possibly cannot obtain stable lapping liquid.On the other hand, in the time that the average grain diameter of abrasive particle exceedes 500nm, the infringement that the face that is polished of glass substrate is caused is large, cannot obtain the surface of level and smooth and high-quality.,, in the time that use comprises lapping liquid that average grain diameter exceedes the ceria particles of 500nm and grinds, the surface of the glass substrate after grinding easily produces scar or distortion, may can make on the contrary the intensity of the glass substrate after grinding decline.
It should be noted that, the average grain diameter of the abrasive particle in the present invention refers to the fixed average grain diameter of size distribution instrumentation of utilizing dynamic light scattering formula.In mensuration, in order to obtain suitable scattering, intensity of reflected light, will use as working sample with pure water or organic solvent diluting to the sample of the debita spissitudo scope of installing defined.As the size distribution meter of dynamic light scattering formula, particularly, use grain size analysis meter " マ イ Network ロ ト ラ ッ Network UPA-ST150 " (ProductName, NIKKISO company system), as working sample, use the sample obtaining so that its mode that reaches the debita spissitudo scope of this device defined is diluted abrasive particle pure water or organic solvent.
Contain proportional (concentration) of the abrasive particle in lapping liquid can be considered uniformity, the dispersion stabilization etc. of the grinding rate in grinding rate, glass substrate face and suitably set, but, in order to obtain sufficient abrasive characteristic, be preferably more than 0.1 quality % and below 40 quality % with respect to the gross mass of lapping liquid.Abrasive particle containing the proportional gross mass with respect to lapping liquid while being less than 0.1 quality %, cannot fully obtain the effect that improved by the intensity of grinding the glass substrate producing, while exceeding 40 quality %, dispersiveness may decline.Preferred containing proportional be 1~20 quality %, further preferred containing proportional be 5~10 quality %.
The lapping liquid using in the present invention contains aforesaid composition with the ratio of aforementioned regulation, preferably so that the abrasive particles such as colloidal silica disperse and make the mode of the admixture that composition in addition dissolves equably prepare and use equably, but can stablize in the scope of effect that obtains grinding, the each composition in lapping liquid can depart to a certain degree.Particularly, even high and there is sedimentation in lapping liquid in the situation that at the proportion of abrasive particle, if the design of the supply method by lapping liquid is supplied to abrasive particle in certain proportion grinder and can maintains the state that has certain abrasive particle on grinding pad, even if abrasive particle is not evenly dispersed in lapping liquid, sometimes also can obtain fully the effect of grinding.Mixing can adopt normally used stirring mixing method in the manufacture of lapping liquid, for example utilize the stirring mixing method of ultrasonic dispersing machine, homogenizer etc.Lapping liquid used in the present invention not necessarily needs the mixture in advance the grinding composition of formation being all obtained by mixing to be supplied to the position of grinding.Can supply with at the position to grinding time, mix the composition into lapping liquid by grinding composition.
As lapping liquid, preferably in the dispersion liquid of dispersed colloidal silica that has abrasive particle etc., coordinate organic solvent, water, suitably regulate the composition of decentralized medium to manufacture.For example, as commercially available colloidal silica, have aqueous dispersion colloidal silica, organic solvent to disperse colloidal silica, lapping liquid can disperse colloidal silica to manufacture with so commercially available aqueous dispersion colloidal silica, organic solvent.
Particularly, for example, by the method that coordinates organic solvent or disperse hydrous water in colloidal silica etc. at organic solvent in aqueous dispersion colloidal silica, can obtain being dispersed with the lapping liquid of silica abrasive grain in the decentralized medium of the water that contains ormal weight.
In addition, disperse colloidal silica for commercially available organic solvent, as required, its abrasive particle content is regulated, the lapping liquid can be used as thus in the present invention uses.Conventionally, by coordinating the organic solvent identical with the organic solvent containing in organic solvent dispersion colloidal silica to make the lapping liquid of the abrasive particle content of regulation.But the lapping liquid using is in the present invention not limited to this, also can coordinate the organic solvent different from the organic solvent containing in organic solvent dispersion colloidal silica.
Organic solvent by using aforesaid hydrophilic organic solvent to use when coordinating organic solvent to make lapping liquid in aqueous dispersion colloidal silica, this organic solvent while disperseing in colloidal silica to organic solvent that hydrous water is made lapping liquid disperse the organic solvent containing in colloidal silica, can make the decentralized medium that water and organic solvent dissolve mutually.In disperseing colloidal silica to organic solvent, coordinate kind and this organic solvent to disperse the different organic solvent of organic solvent containing in colloidal silica and make lapping liquid, above-mentioned organic solvent is preferably intermiscibility.
In the lapping liquid using in the present invention, only otherwise violate aim of the present invention, can suitably contain as required surfactant, chelating agent, reducing agent, viscosity imparting agent or viscosity modifier, anti-flocculating agent or dispersant, antirust agent etc.While stating in the use at least a kind in any composition, the total amount of above-mentioned any composition is preferably below 10 quality % with respect to lapping liquid.
Substrate holding structure 5 is not only rotated, and can carry out rectilinear motion.In addition, grinding plate 1 and grinding pad 3 can be with as grind object glass substrate main body 4 equal extent size or for the size of glass substrate main body below 4.In this case, preferably by making substrate holding structure 5 and grinding plate 1 relatively move and can grind the whole face of the face that is polished of glass substrate main body 4.In addition, grinding plate 1 and grinding pad 3 also can not be rotated, for example, can move to a direction with belt.
Grind by the face that is polished to glass substrate main body 4 like this, can obtain having improved with high accuracy the glass substrate of intensity.
In addition, lapping device 10 is that to grind object be the lapping device that the one side of glass substrate main body 4 grinds as the face of being polished, but for example also can use the two sides simultaneous grinding device that disposes the grinding pad same with lapping device 10 in the upper and lower surface of glass substrate main body 4 to grind the face that is polished (two sides) that grinds object.
The condition of utilizing such lapping device 10 to grind is not particularly limited, and by being pressed on grinding pad 3 to substrate holding structure 5 imposed loads, can improve grinding pressure, can improve grinding rate.Grinding pressure is preferably about 5kPa~about 30kPa, from be polished the grinding rate in face uniformity, flatness, prevent that cut etc. from grinding the viewpoint of defects, more preferably about 5kPa~about 15kPa.The rotating speed of grinding plate 1 and substrate holding structure 5 is preferably about 20rpm~about 100rpm, but is not limited to this.In addition, about the quantity delivered of lapping liquid 7, suitably regulate, select according to being polished composition, above-mentioned each grinding condition etc. of face constituent material, lapping liquid, for example, when the glass substrate for 50mm grinds on one side, preferably about 20cm roughly 3/ minute~about 40cm 3/ minute quantity delivered.
As grinding pad 3, can use the grinding pad that comprises common nonwoven, polyurathamc, porous resin, Non-porous resin etc.In addition, in order to promote lapping liquid 7 to accumulate a certain amount of lapping liquid 7 to the supply of grinding pad 3 or at grinding pad 3, can implement to the surface of grinding pad 3 the groove processing of clathrate, concentric circles, helical form etc.In addition, as required, can make the Surface Contact of pad conditioner and grinding pad 3, in the adjusting of carrying out grinding pad 3 surfaces, grind.
It should be noted that, in the above-described embodiment, be illustrated as example grind the release method of the lapping device that (hanging け stream) form of the what is called that is used lapping liquid all discards at every turn to use, but also can carry out in the mode of the lapping device of the formation of the so-called endless form of recovery use after the lapping liquid that is supplied to grinding pad is used in grinding.
As the lapping device of endless form, can use and for example possess as shown in Figure 2 the lapping device 20 that keeps supplying with from tank 28 to grinding pad 24 as substrate holding structure (carrier) 22, the grinding plate 23 of the glass substrate main body 21 of grinding object, the lip-deep grinding pad 24 that sticks on grinding plate 23, the tank 28 that accumulates lapping liquid 25 and use lapping liquid feed unit 27 dribbling nozzle 26 of lapping liquid 25.
Lapping device 20 becomes and has the recovery unit (not shown) that reclaims from grinding pad 24 of used lapping liquid 25 in grinding and the lapping liquid 25 reclaiming be transported to the formation of tank 28.Turn back to lapping liquid 25 in tank 28 and reuse lapping liquid feed unit 27 and be supplied to grinding pad 24 via dribbling nozzle 26, thereby recycle.
Lapping device 20 and above-mentioned lapping device 10 are similarly, can supply with lapping liquid 25 from dribbling nozzle 26 in limit, limit makes the face that is polished of the glass substrate main body 21 being kept by substrate holding structure (carrier) 22 contact with grinding pad 24, makes substrate holding structure (carrier) 22 and grinding plate 23 relatively rotatablely move and grind.
As the glass of the glass substrate main body in the present invention, can enumerate such as quartz glass, soda-lime glass, alumina silicate glass, borosilicate glass, aluminium borosilicate glass, alkali-free glass, sintered glass ceramics etc.
Especially the glass substrate that comprises alkali-free glass using for the FPD of liquid crystal display (LCD) etc., can obtain the effect improving than in the past good intensity.
In the present invention, alkali-free glass refers to the silicate Glass that is less than 2 quality % in the content based on oxide alkali metal oxide.Particularly preferably be less than borosilicate glass or the aluminium borosilicate glass of 0.5 quality % in the content based on oxide alkali metal oxide.
The thickness of glass substrate is not particularly limited, preferably 0.1~5mm.The strengthening based on grinding in the present invention can obtain the effect improving than in the past good intensity for thinner glass substrate.Thin glass substrate as a comparison, can enumerate the glass substrate of thickness 0.1~1.1mm.
It should be noted that, in the present invention, the difference of the thickness of the glass substrate preferably obtaining take the glass substrate main body before grinding and after grinding is carried out as extremely micro-mode, and as glass substrate main body, its thickness is preferably 0.1~5mm.
According to the present invention, by using the amount of moisture of decentralized medium for the lapping liquid below setting is as the lapping liquid that glass substrate main body is ground, can remove accurately small concavo-convex, the scar of glass substrate body surfaces.
In addition, by using such lapping liquid, the moisture can suppress to grind time is to the intrusion of inside glass, and can reduce the amount of moisture in the glass substrate obtaining after grinding, therefore, can improve with high accuracy the intensity of the glass substrate after grinding.
Embodiment
Below, embodiments of the invention are specifically described, but the invention is not restricted to the embodiments described.In following example, unless otherwise specified, " % " refers to quality %.
(1) preparation of lapping liquid
(1-1) colloidal silica dispersion
The organic silica > of <
Organic silica dispersions a; The EG-ST-ZL processed of Nissan Chemical Ind Ltd
(water 2 quality % are following for colloidal silica (average grain diameter 100nm) 20 quality %, ethylene glycol and water 80 quality %)
Organic silica dispersions b; The IPA-ST-ZL processed of Nissan Chemical Ind Ltd
(water 1 quality % is following for colloidal silica (average grain diameter 120nm) 20 quality %, isopropyl alcohol and water 80 quality %)
Organic silica dispersions c; The MEK-ST-ZL processed of Nissan Chemical Ind Ltd
(water 0.5 quality % is following for colloidal silica (average grain diameter 130nm) 20 quality %, MEK and water 80 quality %)
< aqueous dispersion colloidal silica >
Aqueous dispersion colloidal silica dispersion a; The コ ン processed ポ ー of Fujimart Co., Ltd. Le 80
(colloidal silica (average grain diameter 110nm) 40 quality %, water 60 quality %)
Aqueous dispersion colloidal silica dispersion b; The ST-ZL processed of Nissan Chemical Ind Ltd
(colloidal silica (average grain diameter 140nm) 40 quality %, water 60 quality %)
< organic solvent >
Ethanol: and the pure medicine system of light (reagent superfine, moisture 0.2 quality % is following)
Ethylene glycol: and the pure medicine system of light (reagent superfine, moisture 0.2 quality % is following)
Methyl alcohol: and the pure medicine system of light (reagent superfine, moisture 0.1 quality % is following)
Normal propyl alcohol: and the pure medicine system of light (reagent superfine, moisture 0.2 quality % is following)
N-butanol: and the pure medicine system of light (with light one-level, moisture 0.3 quality % is following)
Isopropyl alcohol: and the pure medicine system of light (reagent superfine, moisture 0.1 quality % is following)
N-hexane: and the pure medicine system of light (reagent superfine, moisture 0.05 quality % is following)
Ethyl acetate: and the pure medicine system of light (reagent superfine, moisture 0.1 quality % is following)
Toluene: and the pure medicine system of light (reagent superfine, moisture 0.03 quality % is following)
MEK: and the pure medicine system of light (reagent superfine, moisture 0.1 quality % is following)
It should be noted that, the average grain diameter of the abrasive particle in lapping liquid is used grain size analysis meter " マ イ Network ロ ト ラ ッ Network UPA-ST150 " (ProductName, NIKKISO company system), measures by dynamic light scattering method.For working sample, so that it reaches is definite in order to obtain suitable scattering, intensity of reflected light in the time measuring, the mode of the debita spissitudo scope of device, measure after using pure water or organic solvent to dilute.
(1-2)
With mode Preparation Example 1~21 as follows and each lapping liquid of comparative example 1~3.
[experiment A]
With mode Preparation Example 1 as follows and the lapping liquid of comparative example 1.
That is, in the each colloidal silica dispersion shown in table 1, mix above-mentioned organic solvent or the water as liquid medium in the mode that reaches the ratio shown in table 1, then fully stir, obtain the lapping liquid of embodiment 1 and comparative example 1.
Mass ratio (quality %) using mixing ratio in each lapping liquid of embodiment 1 and comparative example 1, colloidal silica dispersion, liquid medium (organic solvent) and water during as the gross mass take each lapping liquid as 100 quality % is shown in table 1.As water, use pure water.
[experiment B]
With mode Preparation Example 2~9 as follows and the lapping liquid of comparative example 2~3.
That is, in the each colloidal silica dispersion shown in table 1, mix above-mentioned organic solvent or the water as liquid medium in the mode that reaches the ratio shown in table 1, then fully stir, obtain the lapping liquid of embodiment 2~9 and comparative example 2~3.
Mass ratio (quality %) using mixing ratio in each lapping liquid of embodiment 2~9 and comparative example 2~3, colloidal silica dispersion, liquid medium (organic solvent) and water during as the gross mass take each lapping liquid as 100 quality % is shown in table 1.As water, use pure water.
[experiment C]
With the lapping liquid of mode Preparation Example 10~21 as follows.
That is, in the each colloidal silica dispersion shown in table 1, mix the above-mentioned organic solvent as liquid medium in the mode that reaches the ratio shown in table 1, then fully stir, obtain the lapping liquid of embodiment 10~21.
Mass ratio (quality %) using mixing ratio in each lapping liquid of embodiment 10~21, colloidal silica dispersion and liquid medium (organic solvent) during as the gross mass take each lapping liquid as 100 quality % is shown in table 1.As water, use pure water.
In table 1, about the lapping liquid composition of embodiment 1~21 and comparative example 1~3, by the proportional (concentration that contains with respect to lapping liquid entirety of the abrasive particle of each lapping liquid, decentralized medium (total amount) and water (comprising the water that derives from organic solvent and aqueous dispersion colloidal silica dispersion); Quality %) and water be shown in the lump table 1 for the mixing ratio containing proportional (quality %) and above-mentioned each colloidal silica etc. of decentralized medium entirety.
It should be noted that, lapping liquid composition (abrasive particle, decentralized medium and water) carrys out record with the quality % of the lapping liquid entirety with respect to preparing.In addition, water is for the proportional (concentration that contains of lapping liquid entirety; Quality %) and decentralized medium in water ratio to be the amount of moisture that contains according to above-mentioned colloidal silica dispersion and organic solvent calculate containing proportional and water shared ratio in decentralized medium entirety the value that maximum separately and minimum of a value obtain for water is shared in lapping liquid entirety.
(2) evaluation of the abrasive characteristic of lapping liquid
For the lapping liquid obtaining by embodiment 1~21 and comparative example 1~3, utilize following method to carry out the evaluation of nonferromagnetic substance.
(2-1) grinding condition
Grind and use following device, undertaken by condition shown below.
Grinder: small-sized grinder NF-300 on table (Na ノ Off ァ ク タ ー company system)
Grinding pressure: as shown in table 2.
Platen (platform) rotating speed: as shown in table 2.
Head (substrate maintaining part) rotating speed: as shown in table 2.
Lapping liquid feed speed: 40 ml/min
Grinding pad: imitative chamois leather pad H7000 (Fujiette Ai Yuan company system)
Milling time: as shown in table 2.
(2-2) grinding charge
As grinding charge, the FPD alkali-free glass AN100 (trade name, Asahi Glass company system) using at thickness 0.5mm has implemented following pretreated glass substrate.
(a) [experiment A]
Use and utilize containing cerium grinding agent (cerium concentration: 10 quality %, cerium particle diameter: 0.5 μ m) carries out grinding and the glass substrate that obtains for 3 minutes to AN100 substrate surface.
(b) [experiment B]
Use utilizes mixed liquor that aqueous dispersion colloidal silica dispersion a and pure water mix with the ratio of mass ratio 1:1 to carry out grinding for 30 minutes to AN100 substrate surface and the glass substrate that obtains.
(c) [experiment C]
Use utilizes mixed liquor that aqueous dispersion colloidal silica dispersion a and pure water mix with the ratio of mass ratio 1:1 to carry out grinding for 30 minutes to AN100 substrate surface and the glass substrate that obtains.
(2-3) evaluating characteristics of lapping liquid
The intensity of the glass substrate obtaining after grinding is evaluated by method shown below (Ball on Ring (ball) determination method).; on the platform (diameter 30mm) of ring-type; by each glass substrate of embodiment 1~21 and comparative example 1~3 to evaluate after ventricumbent mode arranges; press the rigid ball of diameter 10mm at the upper surface of glass substrate; take a speed as the 1mm/ condition imposed load of second, the load during using substrate generation breakage is as the intensity of glass substrate.
The strength detection of glass substrate uses autoplotter AG-1 (trade name, Shimadzu Seisakusho Ltd.'s system).It should be noted that, in the intensity evaluation of above-mentioned glass substrate, prepare the glass substrate of three each embodiment and comparative example, the intensity using the peak of the measured value obtaining separately as glass substrate.In addition, for the glass substrate intensity before milled processed, be set as using above-mentioned strength detection method the glass substrate of the condition processing with identical with pretreatment condition in each experiment A~C, making to be evaluated and the value that obtains.
Evaluation result is as shown in table 2.In addition, for embodiment 2~9 and comparative example 2~3 (experiment B) wherein, in the decentralized medium of lapping liquid, the relation of the intensity containing the glass substrate after proportional and grinding of water as shown in Figure 3.
As shown in Table 2, use water for the gross mass of decentralized medium containing in the comparative example 1 of the proportional lapping liquid that is 100%, the intensity of the glass substrate obtaining after grinding only obtains 690N, with respect to this, utilization make water for the gross mass of decentralized medium containing proportional be that lapping liquid below 1% carries out in the glass substrate of the embodiment 1 that milled processed obtains, obtain the intensity up to 836N, confirm the intensity that has improved glass substrate with high accuracy.
In addition, from the result of table 2 and Fig. 3, use water for the gross mass of decentralized medium containing proportional be that lapping liquid below 85 quality % grinds in the glass substrate of the embodiment 2~9 obtaining, more than the intensity of the glass substrate main body of intensity 690N is increased to 763N, confirm: along with the proportional minimizing that contains of water, can obtain higher intensity.On the other hand, grind and in the glass substrate of the comparative example 2~3 that obtains at the lapping liquid that uses water to exceed 85 quality % for the gross mass of decentralized medium, only obtain the intensity below 723N, especially in decentralized medium water containing proportional be in 100% comparative example 3, confirm: with grind before glass substrate main body compared with, intensity decline.
In addition, the kind that is coupled to the organic solvent in lapping liquid being carried out in the embodiment 10~21 of various changes, in the glass substrate obtaining, also can obtain high strength more than 747N after grinding, confirm the intensity that has improved glass substrate with high accuracy.Especially using in the embodiment 10~14 of the lapping liquid that contains ethylene glycol in decentralized medium, confirm the intensity that can obtain up to 810~840N.
The Japanese patent application 2011-240117 that the application proposed based on November 1st, 2011, and its content is incorporated in this description as reference.
Industrial applicability
According to the present invention, for the alkali-free glass substrate main body of using for glass substrate main body, especially FPD, can carry out high-precision grinding, compared with the past, can improve with high accuracy the intensity of the glass substrate obtaining after grinding.
Label declaration
1,23 ... grinding plate,
2 ... platform drive motor,
3,24 ... grinding pad,
4,21 ... glass substrate main body,
5,22 ... substrate holding structure,
6,26 ... dribbling nozzle,
7,25 ... lapping liquid,
10,20 ... lapping device,
27 ... lapping liquid feed unit,
28 ... tank

Claims (13)

1. a manufacture method for glass substrate, wherein,
Utilize the lapping liquid that is dispersed with abrasive particle in decentralized medium substantially moisture or not moisture, that comprise water liquid medium in addition to grind at least one interarea of glass substrate main body, wherein, in described decentralized medium water containing proportional be below 85 quality %.
2. the manufacture method of glass substrate according to claim 1, wherein,
In described decentralized medium water containing proportional be 3~60 quality %.
3. the manufacture method of glass substrate according to claim 1, wherein,
Water containing the proportional 3 quality % that are less than in described decentralized medium.
4. according to the manufacture method of the glass substrate described in any one in claim 1~3, wherein,
Liquid medium beyond described water is organic solvent.
5. the manufacture method of glass substrate according to claim 4, wherein,
Described organic solvent is monohydric alcohol or polyalcohol.
6. the manufacture method of glass substrate according to claim 4, wherein,
Described organic solvent is hydro carbons, ethers, ester class or ketone.
7. according to the manufacture method of the glass substrate described in any one in claim 1~4, wherein,
Liquid medium beyond described water is at least a kind that selects in the group of free methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butanol, ethylene glycol, propane diols, n-hexane, octane, ethyl acetate, MEK, toluene and ether composition.
8. according to the manufacture method of the glass substrate described in any one in claim 1~7, wherein,
Described abrasive particle is the particulate that selects at least a kind of metal oxide in the group of free silica, aluminium oxide, ceria, titanium dioxide, zirconia and manganese oxide composition.
9. according to the manufacture method of the glass substrate described in any one in claim 1~8, wherein,
Described abrasive particle is that average grain diameter is the particle of 5~500nm.
10. according to the manufacture method of the glass substrate described in any one in claim 1~9, wherein,
The abrasive particle containing in described lapping liquid containing the proportional gross mass with respect to this lapping liquid be 0.1~40 quality %.
11. according to the manufacture method of the glass substrate described in any one in claim 1~10, wherein,
Supply with described lapping liquid to grinding pad, the face that is polished of described glass substrate main body is contacted with described grinding pad, and by relative motion between the two, the described face that is polished is ground.
12. according to the manufacture method of the glass substrate described in any one in claim 1~11, wherein,
Described glass substrate is the glass substrate that comprises alkali-free glass.
13. according to the manufacture method of the glass substrate described in any one in claim 1~12, wherein,
The thickness of described glass substrate is 0.1~5mm.
CN201280054271.4A 2011-11-01 2012-10-17 Method for producing glass substrate Pending CN103917332A (en)

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