CN1320078C - Polishing composition - Google Patents

Polishing composition Download PDF

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Publication number
CN1320078C
CN1320078C CNB2004100619164A CN200410061916A CN1320078C CN 1320078 C CN1320078 C CN 1320078C CN B2004100619164 A CNB2004100619164 A CN B2004100619164A CN 200410061916 A CN200410061916 A CN 200410061916A CN 1320078 C CN1320078 C CN 1320078C
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China
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acid
grinding
liquid composition
alumina
grinding liquid
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CN1576346A (en
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藤井滋夫
北山博昭
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Kao Corp
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Kao Corp
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    • 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
    • C09K3/1454Abrasive powders, suspensions and pastes for polishing
    • C09K3/1463Aqueous liquid suspensions

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Manufacturing Of Magnetic Record Carriers (AREA)
  • Manufacturing Optical Record Carriers (AREA)

Abstract

A polishing composition containing an alpha-alumina, an intermediate alumina, an oxidizing agent and water; a method for reducing waviness of a substrate to be polished, including the step of applying the polishing composition to the substrate to be polished; and a method for manufacturing a substrate, including the step of polishing a substrate to be polished with the polishing composition. The polishing composition is suitable for polishing substrates for precision parts such as substrates for magnetic recording media for magnetic discs, optical discs, opto-magnetic discs, and the like; photomask substrates; glass for liquid crystals; optical lenses; optical mirrors; optical prisms; and semiconductor substrates.

Description

Grinding Liquid composition
Technical field
The present invention relates to have high grinding rate, can reduce by the grinding Liquid composition of the external waviness of grinding substrate.Further, the present invention relates to use this grinding Liquid composition to reduce by the method for the external waviness of grinding substrate and the manufacture method of substrate.
Background technology
Hard disk requires to reduce the amount of floating of magnetic head in order to reduce the smallest record area, to advance high capacity.In order to reduce the amount of floating of magnetic head, the short wavelength's external waviness (external wavinesses of wavelength 50~500 μ m) in the grinding step of needs minimizing hard disk substrate and long wavelength's external waviness (external waviness that wavelength 0.5mm is above).Here said " external waviness " is meant the long concave-convex surface of specific surface roughness ripple.In order to make the substrate that this external waviness reduces, the grinding load when aperture control, Hardness Control, the grinding of having discussed grinding pad and these mechanical conditionss of control of rotating speed.But,, can't say so fully though these mechanical conditionss produce effect.On the other hand, also discussed and reduced external waviness by grinding Liquid composition.Te Kaiping 3-115383 communique has been discussed the grinding Liquid composition that contains Alpha-alumina, water-soluble peroxide and boehmite; The spy opens 2001-260005 communique (US 6261476 B1) and has discussed the grinding Liquid composition that contains polishing particles once, disperses micelle and oxygenant; The spy opens 2002-327170 communique (US 2002194789 A1) and discloses the grinding Liquid composition that contains colloidal silica, oxygenant and organic phospho acid; The spy opens 2003-41239 communique (US 2003041526 A1) and discloses the grinding Liquid composition that uses intermediate alumina.But these grinding Liquid compositions can not be said so from this viewpoint of minimizing with the external waviness on the required grinding rate basis of practicability fully.
Summary of the invention
That is, main points of the present invention relate to
(1) contains the grinding Liquid composition of Alpha-alumina, intermediate alumina, oxygenant and water;
(2) grinding Liquid composition of being put down in writing with above-mentioned (1) reduces the method for the external waviness that is ground substrate; And
(3) has the manufacture method that the grinding Liquid composition of being put down in writing with above-mentioned (1) grinds the substrate of the operation of being ground substrate.
Embodiment
The present invention relates to have high grinding rate, can reduce by the grinding Liquid composition of the external waviness of grinding substrate, also relate to and use this grinding Liquid composition to reduce, and use this grinding Liquid composition to make the manufacture method of the high-quality substrate of external waviness minimizing by the method for the external waviness of grinding substrate.
These and other advantage of the present invention may be clearer by following explanation.
Grinding Liquid composition of the present invention, the big feature of one is abrasive substance and uses Alpha-alumina and intermediate alumina, grind promotor and use oxygenant, discovery is by the grinding Liquid composition that use has this feature, the grinding rate that can reach high arranged and can significantly reduce the unusual effect of the external waviness that is ground substrate.
By also using Alpha-alumina and intermediate alumina, obtain the effect that grinding rate improves and external waviness reduces, about its mechanism of action, supposition is owing to mutually different particle diameter particle and because the hardness difference, the filling raising, grind the physical force useful effect in the grinding charge surface, be limited to this but have more than.
Grinding Liquid composition of the present invention contains the Alpha-alumina as abrasive substance.As Alpha-alumina, be preferably the aluminum oxide that gibbsite, bayerite, nordstrandite (nordstrandite), diaspore, boehmite, pseudobochmite, alumina gel, gama-alumina and θ-aluminum oxide etc. are burnt till under the temperature more than 1100 ℃ by well-established law.From reducing external waviness, reduce surfaceness, improve grinding rate and prevent the viewpoint of surface imperfection, it is aluminum oxide more than 95% that Alpha-alumina is preferably in aluminum oxide purity, more preferably more than 97%, is more preferably more than 99%.
The median size of the primary particle of Alpha-alumina from reducing the viewpoint of external waviness, is preferably 0.005~0.8 μ m, 0.01~0.4 μ m more preferably, the median size of offspring is preferably 0.01~2 μ m, and more preferably 0.05~1.0 μ m is more preferably 0.1~0.5 μ m.The median size of the primary particle of abrasive substance, with sem observation (preferred 3000~30000 times) or transmission electron microscope observation (preferred 10000~300000 times), and carry out image analysis, can obtain as the quantity median size by the mean value of major diameter and minor axis.The median size of offspring can be measured as volume average particle size with laser diffractometry.
From improving grinding rate and reduce the viewpoint of external waviness, be preferably 0.1~50m with the specific surface area of the Alpha-alumina of BET method mensuration 2/ g, more preferably 1~40m 2/ g is more preferably 2~20m 2/ g.
From improving the viewpoint of grinding rate and minimizing external waviness, the content of the Alpha-alumina in the grinding Liquid composition is preferably more than the 0.05 weight %, more preferably more than the 0.1 weight %, is more preferably more than the 0.5 weight %, is more preferably more than the 1 weight %.From the viewpoint of surface quality and economy, be preferably below the 40 weight %, more preferably below the 30 weight %, be more preferably below the 25 weight %, be more preferably below the 20 weight %.That is, the content of the Alpha-alumina in the grinding Liquid composition is preferably 0.05~40 weight %, and more preferably 0.1~30 weight % is more preferably 0.5~25 weight %, is more preferably 1~20 weight %.
From improving the viewpoint of grinding rate and minimizing external waviness, grinding Liquid composition of the present invention should contain intermediate alumina.Intermediate alumina of the present invention is the general name of the aluminium oxide particles beyond the alpha-alumina particle, and concrete example is if any gama-alumina particle, δ-aluminium oxide particles, θ-aluminium oxide particles, η-aluminium oxide particles, κ-aluminium oxide particles and their mixture etc.Wherein, from improving the viewpoint of grinding rate and minimizing external waviness, be preferably following intermediate alumina.Its crystal type is preferably gama-alumina, δ-aluminum oxide, θ-aluminum oxide and their mixture, more preferably gama-alumina, θ-aluminum oxide.The specific surface area of measuring with the BET method is preferably 30~300m 2/ g, more preferably 50~200m 2/ g.From reducing the viewpoint of external waviness, the median size of the offspring of intermediate alumina is preferably 0.01~5 μ m, and more preferably 0.01~2 μ m is more preferably 0.05~1 μ m, is more preferably 0.1~0.5 μ m.This median size for example can be made made " LA-920 " this laser diffractometry with the hole field and be measured as volume average particle size.
The content of basic metal and alkaline-earth metal in the intermediate alumina is preferably below the 0.1 weight %, more preferably below the 0.05 weight %, is more preferably below the 0.01 weight %.For example, when the poor aluminium hydroxide of, basic metal bigger with specific surface area and alkaline-earth metal was raw material, because the welding of the intermediate alumina of making is few, particle intensity was also little, so, can effectively reduce the surface imperfection of grinding charge.
As the aluminium hydroxide of the raw material of intermediate alumina, the specific surface area of measuring with the BET method is preferably 10~500m 2/ g, more preferably 30~400m 2/ g is more preferably 50~300m 2/ g.The basic metal in the aluminium hydroxide and the content of alkaline-earth metal are preferably below the 0.1 weight %, more preferably below the 0.05 weight %, are more preferably below the 0.01 weight %.When making intermediate alumina, feed dry air or nitrogen during heating, can effectively prevent the surface imperfection of grinding charge by the aluminium hydroxide thermal dehydration.Above-mentioned thermal dehydration is handled and can be undertaken by well-established law.These intermediate aluminas for example can carry out wet type or dry type pulverizing by pulverizers such as ball mill, ball mill, high-pressure homogenizer, jet mills as required, are adjusted into the particle diameter of regulation.
Aluminium hydroxide is chemical formula Al (OH) 3, AlOOH, AlOOHnH 2O or Al 2O 3NH 2The compound of O (n is 1~3) expression, so long as the compound of can thermal dehydration making intermediate alumina all can, not special the qualification.Object lesson for example has gibbsite, bayerite, nordstrandite, diaspore, boehmite, pseudobochmite, alumina gel etc.
The details of the mechanism of action when this intermediate alumina grinds is unclear, but thinks and compare with the independent intermediate alumina that uses with independent use Alpha-alumina that grinding rate improved when both mixed, and therefore grinding charge Surface Physical power was increased.
From improving the viewpoint of grinding rate and minimizing external waviness, the content of the intermediate alumina in the grinding Liquid composition is preferably more than the 0.05 weight %, more preferably more than the 0.1 weight %, is more preferably more than the 0.5 weight %, is more preferably more than the 1 weight %.From the viewpoint of surface quality and economy, be preferably below the 40 weight %, more preferably below the 30 weight %, be more preferably below the 25 weight %, be more preferably below the 20 weight %.That is, the content of the intermediate alumina in the grinding Liquid composition is preferably 0.05~40 weight %, and more preferably 0.1~30 weight % is more preferably 0.5~25 weight %, is more preferably 1~20 weight %.
From improving the viewpoint of grinding rate and minimizing external waviness, the weight ratio of Alpha-alumina and intermediate alumina (Alpha-alumina/intermediate alumina) is preferably 99/1~30/70, more preferably 97/3~40/60, be more preferably 95/5~50/50, be more preferably 93/7~55/45.
In order effectively to improve grinding rate and to reduce external waviness, the total amount of Alpha-alumina and intermediate alumina is preferably 0.1~45 weight %, and more preferably 0.2~35 weight % is more preferably 1~30 weight %, is more preferably 2~25 weight %.
From improving the viewpoint of grinding rate and minimizing external waviness, should contain oxygenant in the grinding Liquid composition of the present invention.It is unclear that about the mechanism of grinding, but infer it is to act on by abrasive substance, become the state of the grinding effectiveness that can give full play to aluminum oxide by oxygenant.The oxygenant that the present invention uses for example has the metal-salt of the peroxy acid of superoxide, metal or its salt, oxygen acid or its salt, nitrate, vitriol, acid etc.Can roughly divide into inorganic oxidizer and organic oxidizing agent by its structure in the oxygenant.The object lesson of these oxygenants is as follows.As inorganic oxidizer, can use hydrogen peroxide, and sodium peroxide, Potassium peroxide, calcium peroxide, barium peroxide, basic metal such as Magnesium peroxide, or the peroxide of alkaline-earth metal, SPC-D, percarbonic acid salts such as antihypo, ammonium peroxydisulfate, Sodium persulfate, Potassium Persulfate, persulfuric acid or its esters such as permonosulphuric acid, peroxy-nitric acid, peroxy-nitric acid sodium, peroxy-nitric acid or its esters such as potassium per nitrate, peroxophosphoric acid sodium, potassium superphosphate, peroxophosphoric acid or its esters such as ammonium superphosphate, Sodium peroxoborate, peroxyboric acid salts such as potassium per(oxy)borate, potassium perchromate, peroxychromic acid salts such as sodium peroxy-chromate, potassium permanganate, the contour manganate of sodium permanganate, sodium perchlorate, potassium perchlorate, chloric acid, clorox, sodium periodate, potassium periodate, acid iodide, hydracid or derivatives thereof classes such as sodium iodate, iron(ic) chloride (III), ferric sulfate mineral acid metal-salts such as (III).As organic oxidizing agent, can use peroxide, ironic citrates (III) such as percarboxylic acids such as peracetic acid, peroxyformic acid, peroxybenzoic acid, tert-butyl peroxide, cumene peroxide.Wherein, when relatively grinding rate improves property, being easy to get property, usability such as water-soluble, preferably use inorganic oxidizer.From the viewpoint of environmental problem, preferably do not contain the inorganic peroxide of heavy metal.From preventing to be ground the surperficial dirty viewpoint of substrate, more preferably hydrogen peroxide, persulfuric acid salt, hydracid or derivatives thereof are more preferably hydrogen peroxide.These superoxide can use a kind, also can mix use more than 2 kinds.
From improving the viewpoint of grinding rate and minimizing external waviness, the content of oxygenant is preferably more than the 0.002 weight % in the grinding Liquid composition, more preferably more than the 0.005 weight %, be more preferably more than the 0.007 weight %, be more preferably more than the 0.01 weight %.From the viewpoint of surface quality and economy, be preferably below the 20 weight %, more preferably below the 15 weight %, be more preferably below the 10 weight %, be more preferably below the 5 weight %.That is, the content of oxygenant is preferably 0.002~20 weight % in the grinding Liquid composition, and more preferably 0.005~15 weight % is more preferably 0.007~10 weight %, is more preferably 0.01~5 weight %.
From improving the viewpoint of grinding rate and minimizing external waviness, further contain acid in the preferred grinding Liquid composition of the present invention.
From improving the viewpoint of grinding rate and minimizing external waviness, its pK1 of acid that the present invention uses is preferably below 7, more preferably below 5, is more preferably below 3, is more preferably below 2.Here, when the logarithmic value of the inverse of acid ionization constant (25 ℃) was expressed as pKa, pK1 was the logarithmic value of the inverse of first acid ionization constant wherein.The pK1 of each compound is for example on the books in 4 editions (a basis piece of writing) II, pp 316~325 (Japanization association volume) etc. are changed in chemical brief guide.
The object lesson of the acid that the present invention uses is as follows.As mineral compound nitric acid, hydrochloric acid, perchloric acid, acid amides sulfuric acid multi-element, inorganic acids such as monobasic inorganic acids, sulfuric acid, sulfurous acid, phosphoric acid, tetra-sodium, Tripyrophosphoric acid, phosphonic acids, phospho acid such as (amide sulfuric acid) are for example arranged.As organic compound formic acid is for example arranged; acetate; oxyacetic acid; lactic acid; propionic acid; hydroxy-propionic acid; butyric acid; phenylformic acid; monocarboxylic acid classes such as glycine; oxalic acid; succsinic acid; pentanedioic acid; hexanodioic acid; toxilic acid; fumaric acid; methylene-succinic acid; oxysuccinic acid; tartrate; citric acid; isocitric acid; phthalic acid; nitrotrimethylolmethane acetate; polycarboxylic acid classes such as ethylenediamine tetraacetic acid (EDTA); methylsulfonic acid; alkylsulphonic acid classes such as tosic acid; ethyl phosphonic acid; alkylphosphonic acid carboxylic acid classes such as butyl phosphoric acid; the phosphono oxyacetic acid; hydroxy ethylene diphosphonic acid; the phosphinylidyne butane tricarboxylic acid; organic phosphine acids such as ethylenediamine tetramethylene phosphonic acid.Wherein, from the viewpoint of raising grinding rate and minimizing external waviness, preferred polyprotonic acid, more preferably multi-element, inorganic acid, polynary organic carboxyl acid and polynary organic phospho acid are more preferably multi-element, inorganic acid and polynary organic carboxyl acid.Here, polyprotonic acid is meant that intramolecularly has acid more than two, that can produce hydrionic hydrogen atom.From preventing to be ground the surperficial dirty viewpoint of substrate, preferred nitric acid, sulfuric acid, phosphonic acids and carboxylic acid.
Above-mentioned acid can be used separately, but preferred the mixing more than 2 kinds uses.Wherein, when grinding the such metallic surface of nickel plating-phosphorus (Ni-P) substrate, the metal ion stripping of grinding charge in process of lapping, the pH of grinding Liquid composition rises, when can not get high grinding rate, change in order to reduce pH, preferred pK1 is the combination of the acid more than 2.5 less than 2.5 acid and pK1, and the acid and the pK1 that are more preferably pK1 and are below 1.5 are the combination of the acid more than 2.5.When containing such sour more than 2 kinds, from improving grinding rate and reducing external waviness, and the viewpoint of the being easy to get property of acid, pK1 preferably uses mineral acid and organic phospho acids such as nitric acid, sulfuric acid, phosphoric acid, Tripyrophosphoric acid less than in 2.5 the acid.On the other hand, pK1 is in the acid more than 2.5, from same viewpoint, and organic carboxyl acids such as preferred acetate, succsinic acid, oxysuccinic acid, tartrate, citric acid.
From improving the viewpoint of grinding rate and minimizing external waviness, the total content of above-mentioned acid is preferably more than the 0.002 weight % in the grinding Liquid composition, more preferably more than the 0.005 weight %, be more preferably more than the 0.007 weight %, be more preferably more than the 0.01 weight %.From the viewpoint of surface quality and economy, above-mentioned total content is preferably below the 20 weight %, more preferably below the 15 weight %, is more preferably below the 10 weight %, is more preferably below the 5 weight %.That is, the total content of acid is preferably 0.002~20 weight % in the grinding Liquid composition, and more preferably 0.005~15 weight % is more preferably 0.007~10 weight %, is more preferably 0.01~5 weight %.From improving the viewpoint of grinding rate, the weight ratio that pK1 is the acid more than 2.5 less than 2.5 acid and pK1 (pK1 is acid more than 2.5 less than acid/pK1 of 2.5) is preferably 9/1~1/9, and more preferably 7/1~1/7, be more preferably 5/1~1/5.
Water in the grinding Liquid composition of the present invention uses as medium, and from the viewpoint of effective grinding grinding charge, its content is preferably 50~99 weight %, and more preferably 60~97 weight % are more preferably 70~95 weight %.
From improving grinding rate, reduce external waviness, reaching purpose according to other, can further cooperate other compositions in the grinding Liquid composition of the present invention, as other compositions inorganic salt, thickening material, rust-preventive agent, alkaline matter etc. are for example arranged.As inorganic salt ammonium nitrate, ammonium sulfate, vitriolate of tartar, single nickel salt, aluminum nitrate, Tai-Ace S 150, Ammonium sulfamate etc. are for example arranged.These other compositions may be used alone, can also be two or more kinds in combination.From the viewpoint of economy, its content is preferably 0.05~20 weight % in the grinding Liquid composition, and more preferably 0.05~10 weight % is more preferably 0.05~5 weight %.
As other compositions, can further cooperate sterilant, antiseptic-germicide etc. as required.From bring into play its functional point of view, to the influence of nonferromagnetic substance, the viewpoint of economy, the content of these sterilant, antiseptic-germicide is preferably 0.0001~0.1 weight % in the grinding Liquid composition, more preferably 0.001~0.05 weight % is more preferably 0.002~0.02 weight %.
The preferred concentration of the concentration of each composition of grinding Liquid composition of the present invention when grinding, but also can be the concentration of said composition when preparing.Usually, most cases is that the form with concentrated solution prepares composition, before using or when using it is diluted.
In addition, grinding Liquid composition can adopt arbitrary method interpolation, the required one-tenth of mixing to assign to prepare.
The pH of grinding Liquid composition is preferably according to the kind of grinding charge and require suitably decision such as quality.For example, from improve grinding rate, reduce the viewpoint of external waviness, from the viewpoint of the preservative property of processor, operator's security, the pH of grinding Liquid composition is preferably less than 7, more preferably 0.1~6, be more preferably 0.5~5, be more preferably 1~4, be more preferably 1~3.As required, alkaline matter such as organic acid such as mineral acid, hydroxy acid, polycarboxylic acid, aminopolycarboxylic, amino acid such as the nitric acid that this pH can be by suitably cooperating aequum, sulfuric acid or its metal-salt, ammonium salt, ammoniacal liquor, sodium hydroxide, potassium hydroxide, amine is regulated.
The manufacture method of substrate of the present invention has with above-mentioned grinding Liquid composition grinds the operation of being ground substrate.
Grind the material of the grinding charge of substrate representative as the quilt of object of the present invention, metal or metalloids such as silicon, aluminium, nickel, tungsten, copper, tantalum, titanium for example being arranged, reach with these metals is the alloy of principal constituent, glassy mass such as glass, vitreous carbon, decolorizing carbon, stupaliths such as aluminum oxide, silicon-dioxide, silicon nitride, tantalum nitride, titanium carbide, resins such as polyimide resin etc.Wherein, preferably, metal such as aluminium, nickel, tungsten, copper and be that the alloy of principal constituent is a grinding charge with these metals, or the semiconductor substrates such as semiconductor element that contain these metals are grinding charges.Particularly, when the substrate that the aluminium alloy of plating Ni-P constitutes used grinding Liquid composition of the present invention, external waviness can significantly reduce, so preferred.The shape of grinding charge is not particularly limited, and for example plate-like, sheet, tabular, prism-shaped etc. have the shape of planar section and lens etc. that the shape of curvature portion is arranged, and all are the objects that grinds with grinding Liquid composition of the present invention.Wherein, good especially to the grinding of plate-like grinding charge.
The invention further relates to and reduce above-mentioned method of being ground the external waviness of substrate.In the method for the external waviness that is ground substrate of minimizing use grinding Liquid composition of the present invention, the grinding Liquid composition of the application of the invention grinds the above-mentioned quilt grinding substrate of enumerating, and can significantly reduce external waviness.For example,, supply with grinding Liquid composition of the present invention, make abrasive disk and substrate rotating when exerting pressure, can make the high quality substrate that external waviness reduces to abrasive surface with posting the abrasive disk clamping substrate that porous matter organic polymer is an abrasive cloth etc.
Grinding Liquid composition of the present invention is applicable to and grinds the precise part substrate.For example be applicable to the substrate, photomask base plate, optical lens, optical mirror, optical prism, semiconductor substrate of magnetic recording medias such as grinding disk, CD, photomagneto disk etc.The grinding of semiconductor substrate for example has formation operation, the planarization operation of interlayer dielectric, the formation operation of embed type metal wiring, the buried capacitors of polishing process at silicon wafer (naked wafer), embed type element isolation film to form the grinding of carrying out in the operation etc.Grinding Liquid composition of the present invention produces effect in polishing process especially, but equally also applicable to other grinding steps, for example polishing (lapping) operation etc.Grinding Liquid composition of the present invention is specially adapted to grind the disk substrate.
Embodiment
To the further write up explanation of mode of the present invention, these embodiment are openly the present invention just by following embodiment, and not representing has any qualification.
Embodiment 1~17, comparative example 1~5
[lapping liquid compound method]
(median size of primary particle is 0.07 μ m, and the median size of offspring is 0.3 μ m, and specific surface area is 15m to mix the Alpha-alumina of the specified rate shown in table 1~3 2/ g, purity is 99.9%), (median size of offspring is 0.2 μ m to θ-aluminum oxide, and specific surface area is 120m 2/ g, purity is 99.9%), oxygenant, acid and other additives, surplus is an ion exchanged water, regulates pH with ammoniacal liquor, grinding Liquid composition.
[Ginding process]
(stylus tip size: 25 μ m * 25 μ m, by-pass filter: 80 μ m, measured length: 0.64mm) the center line average roughness Ra of Ce Dinging is 0.2 μ m to the Talystep that will make with Rank Taylor Hobson company, thickness is 1.27mm, diameter is that polish under the imposing a condition of following two side machining apparatus with two side machining apparatus on the surface of the substrate that constitutes of the aluminium alloy of the plating Ni-P of 3.5 inches (95.0mm), obtains as the abrasive material of magnetic recording media with the aluminium alloy base plate of the plating Ni-P of substrate use.
Imposing a condition of two side machining apparatus is as follows.
Imposing a condition of<two side machining apparatus 〉
Two side machining apparatus: Speedfam company makes, 9B type two side machining apparatus
Tonnage: 9.8kPa
Grinding pad: " H9900S " (trade(brand)name) that Fujibo company makes
Price fixing rotating speed: 50r/ minute
Grinding Liquid composition supply flow rate: 100ml/ minute
Milling time: 5 minutes
The substrate block number that drops into: 10
[grinding rate]
Grind the weight of each substrate of front and back with balance (" BP-210S " that Sartorius company makes) mensuration, obtain the changes in weight of each substrate, as reduction, its value divided by milling time is reduced speed as weight with 10 mean values.Weight minimizing speed is imported following formula, be transformed into grinding rate (μ m/ minute).As benchmark value 1, obtain the relative value (speed of relative movement) of the grinding rate of each embodiment or comparative example with the grinding rate of comparative example 1.
Weight reduces speed (g/ minute)={ weight (g) after weight (the g)-grinding before grinding }
/ milling time (minute)
Grinding rate (μ m/ minute)=weight reduces speed (g/ minute)/substrate single face area (mm 2)
/ Ni-P plating density (g/cm 3) * 10 6
[external waviness]
Each substrate after the grinding is got 2 points (amount to 4 points) every 180 °, measures short wavelength's external waviness and long wavelength's external waviness under the following conditions.
Machine: " Zygo New View200 "
Object lens: 2.5 times " Michelson "
Zoom ratio: 0.5
Shift out: cylinder
Wave filter: FFT fixed band leads to (Band Pass)
Measure wavelength:
Short wavelength's external waviness: the high wavelength 50 μ m of wave filter
Wave filter hangs down wavelength 500 μ m
Long wavelength's external waviness: the high wavelength 0.5mm of wave filter
Wave filter hangs down wavelength 5mm
Area: 4.33mm * 5.77mm
[surface is dirty]
Each substrate after the grinding by 300 times of observations, carries out 4 grade evaluations to the surface is dirty with polarizing microscope in piece leaf formula scrubber after the detergent water washing and ion-exchange water washing through having used PVA (polyvinyl acetate) section.
◎: the surface does not have aluminum oxide residue and lapping rejects fully.
Zero: the surface does not almost have aluminum oxide residue and lapping rejects.
△: there are aluminum oxide residue and lapping rejects in some places, surface.
*: there are a lot of aluminum oxide residues and lapping rejects in the surface.
The result is shown in table 1,2.The value of grinding rate and external waviness is with the value of comparative example 1 relative value as benchmark value 1.Hence one can see that, compares with comparative example, contain that grinding Liquid composition grinding rate that the embodiment 1~12 of Alpha-alumina, intermediate alumina, oxygenant obtains improves and external waviness to reduce by two performances all very good.Particularly, when adding acid, its effect is remarkable.And the grinding Liquid composition that embodiment 1~12 obtains prevents to be ground the dirty effect of substrate in addition.
Table 1
Alpha-alumina (%) θ-aluminum oxide (%) Oxygenant (%) Acid (%) pH Grinding rate External waviness (relative value) Substrate is dirty
Relative value The short wavelength The long wavelength
Embodiment 1 3 1 Hydrogen peroxide 0.6 - - 4.1 2.5 0.59 0.77
Embodiment 2 3.5 0.5 Hydrogen peroxide 0.6 Citric acid 3.0 2.0 29 0.24 0.43
Embodiment 3 2 2 Hydrogen peroxide 0.6 Citric acid 3.0 2.0 28 0.23 0.38
Embodiment 4 1 3 Hydrogen peroxide 0.6 Citric acid 3.0 2.0 20 0.21 0.34
Embodiment 5 3 1 Hydrogen peroxide 0.6 Citric acid 3.0 2.0 42 0.26 0.25
Embodiment 6 3 1 Hydrogen peroxide 0.6 Nitric acid 1.1 0.8 36 0.27 0.42
Embodiment 7 3 1 Hydrogen peroxide 0.6 Sulfuric acid 1.7 0.8 53 0.26 0.21
Embodiment 8 3 1 Hydrogen peroxide 1.8 Sulfuric acid 5.1 0.5 63 0.25 0.19
Embodiment 9 3 1 Hydrogen peroxide 0.6 Methylsulfonic acid 1.7 0.8 41 0.26 0.30
Embodiment 10 3 1 Hydrogen peroxide 0.6 Phosphoric acid 1.7 1.4 34 0.27 0.35
Embodiment 11 3 1 Hydrogen peroxide 0.6 Hydroxy ethylene diphosphonic acid 1.8 1.2 44 0.26 0.22
Embodiment 12 3 1 Hydrogen peroxide 0.6 Tripyrophosphoric acid 1.4 1.4 37 0.25 0.27
Comparative example 1 3 1 - - - - 4.1 1 1 1 ×
In the table, % represents weight %.
Table 2
Alpha-alumina (%) θ-aluminum oxide (%) Oxygenant (%) Acid and other additives (%) pH Grinding rate External waviness (relative value) Substrate is dirty
Relative value The short wavelength The long wavelength
Comparative example 1 3 1 - - - - 4.1 1 1 1 ×
Comparative example 2 3 0 Hydrogen peroxide 0.6 Boehmite 1.0 4.1 1.1 0.91 0.92
Comparative example 3 3 0 Aluminum nitrate 0.6 Colloidal silica *) 1.0 4.1 2.0 0.59 0.77
Comparative example 4 3 1 Citric acid 0.5 3.0 2.3 0.72 0.85
Comparative example 5 0 0 Hydrogen peroxide 0.6 Colloidal silica *)Hydroxy ethylene diphosphonic acid 4.0 1.8 1.2 1.5 0.27 0.92
In the table, % represents weight %.
*): median size 0.05 μ m, purity 99.9%.
Table 3 expression is considered to the security of human body with to the corrodibility of machinery, result when pH is higher than table 1.As can be known, the grinding Liquid composition that embodiment 13~17 obtains is compared with comparative example 1, and grinding rate improves and external waviness reduces all good.In addition, compare with the situation (embodiment 13,14) of using independent acid, when embodiment 15~17 also for example also used carboxylic-acid and mineral acid sulfuric acid with 2 kinds of acid, the effect that grinding rate improves and external waviness reduces further improved.And the grinding Liquid composition that embodiment 13~17 obtains all prevents to be ground the dirty effect of substrate in addition.
In addition we know, because the external waviness that embodiment 1~17 estimates is small external waviness, so the grinding Liquid composition that embodiment 1~17 obtains all has the effect of the small external waviness of remarkable minimizing.
Table 3
Alpha-alumina (%) θ-aluminum oxide (%) Oxygenant (%) Acid *) (%) (%) pH Grinding rate External waviness (relative value) Substrate is dirty
Relative value The short wavelength The long wavelength
Embodiment 13 3 1 Hydrogen peroxide 0.6 Citric acid 1.0 - - 2.2 35 0.29 0.37
Embodiment 14 3 1 Hydrogen peroxide 0.6 - - Sulfuric acid 1.1 2.1 20 0.29 0.40
Embodiment 15 3 1 Hydrogen peroxide 0.6 Citric acid 1.0 Sulfuric acid 1.1 2.1 49 0.25 0.19
Embodiment 16 3 1 Hydrogen peroxide 0.6 Tartrate 1.0 Sulfuric acid 1.1 2.1 40 0.27 0.22
Embodiment 17 3 1 Hydrogen peroxide 0.6 Acetate 1.0 Sulfuric acid 1.1 2.1 41 0.26 0.20
Comparative example 1 3 1 - - - - - - 4.1 1 1 1 ×
In the table, % represents weight %.
*): citric acid pK1=2.9, tartrate pK1=2.8, acetate pK1=4.6, sulfuric acid pK1<0.
Grinding Liquid composition of the present invention is applicable to grinding the precise part substrate, for example is applicable to the substrate, photomask base plate, optical lens, optical mirror, optical prism, semiconductor substrate of magnetic recording medias such as grinding disk, CD, photomagneto disk etc.
Grinding Liquid composition of the present invention is by being used to grind precise part with substrate etc., the effect that can obtain high grinding rate and the external waviness of grinding charge is reduced.Wherein, the external waviness that is made of long wavelength's external waviness of short wavelength's external waviness of wavelength 50~500 μ m and wavelength 0.5~5mm is called small external waviness, and the present invention has the effect of this small external waviness of remarkable minimizing.
And because that the abrasive material that obtains adheres to lapping rejects etc. is dirty few, the washing after the grinding can be carried out easily, so have the effect that can make the high quality substrate that external waviness reduces economically.
Obviously, there is the form of many same scopes in aforesaid the present invention.Think that this species diversity does not break away from the spirit and scope of invention, be construed as all changes that those skilled in the art does and all comprise within the scope of the claims.

Claims (18)

1, the grinding Liquid composition that contains Alpha-alumina, intermediate alumina, hydrogen peroxide, water and acid.
2, grinding Liquid composition according to claim 1, its pH is less than 7.
3, grinding Liquid composition according to claim 1, wherein the weight ratio of Alpha-alumina and intermediate alumina (Alpha-alumina/intermediate alumina) is 99/1~30/70.
4, grinding Liquid composition according to claim 2, wherein the weight ratio of Alpha-alumina and intermediate alumina (Alpha-alumina/intermediate alumina) is 99/1~30/70.
5, grinding Liquid composition according to claim 1, wherein the median size of the offspring of Alpha-alumina is 0.01~2 μ m, and specific surface area is 0.1~50m 2/ g, the median size of the offspring of intermediate alumina is 0.01~5 μ m, and specific surface area is 30~300m 2/ g.
6, grinding Liquid composition according to claim 2, wherein the median size of the offspring of Alpha-alumina is 0.01~2 μ m, and specific surface area is 0.1~50m 2/ g, the median size of the offspring of intermediate alumina is 0.01~5 μ m, and specific surface area is 30~300m 2/ g.
7, grinding Liquid composition according to claim 3, wherein the median size of the offspring of Alpha-alumina is 0.01~2 μ m, and specific surface area is 0.1~50m 2/ g, the median size of the offspring of intermediate alumina is 0.01~5 μ m, and specific surface area is 30~300m 2/ g.
8, grinding Liquid composition according to claim 1, wherein acid is polyprotonic acid.
9, grinding Liquid composition according to claim 2, wherein acid is polyprotonic acid.
10, grinding Liquid composition according to claim 3, wherein acid is polyprotonic acid.
11, grinding Liquid composition according to claim 5, wherein acid is polyprotonic acid.
12, grinding Liquid composition according to claim 1, it contains pK1 is acid more than 2.5 less than 2.5 acid and pK1.
13, grinding Liquid composition according to claim 2, it contains pK1 is acid more than 2.5 less than 2.5 acid and pK1.
14, grinding Liquid composition according to claim 3, it contains pK1 is acid more than 2.5 less than 2.5 acid and pK1.
15, grinding Liquid composition according to claim 5, it contains pK1 is acid more than 2.5 less than 2.5 acid and pK1.
16, grinding Liquid composition according to claim 8, it contains pK1 is acid more than 2.5 less than 2.5 acid and pK1.
17, reduce the method for the external waviness that is ground substrate, it has the operation of being ground substrate with the described grinding Liquid composition grinding of claim 1.
18, the manufacture method of substrate, it has the operation of grinding quilt grinding substrate with the described grinding Liquid composition of claim 1.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI752013B (en) * 2016-03-25 2022-01-11 日商福吉米股份有限公司 Polishing composition for polishing object having metal-containing layer, method for producing polishing composition, method for polishing, and method for producing substrate

Families Citing this family (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI506621B (en) * 2005-12-22 2015-11-01 Kao Corp Polishing composition for hard disk substrate
JP4753710B2 (en) * 2005-12-22 2011-08-24 花王株式会社 Polishing liquid composition for hard disk substrate
JP2007257810A (en) 2006-03-24 2007-10-04 Hoya Corp Method of manufacturing glass substrate for magnetic disk, and method of manufacturing magnetic disk
JP5283249B2 (en) * 2006-12-27 2013-09-04 花王株式会社 Method for producing polishing composition
JP5461772B2 (en) * 2007-12-14 2014-04-02 花王株式会社 Polishing liquid composition
US7922926B2 (en) 2008-01-08 2011-04-12 Cabot Microelectronics Corporation Composition and method for polishing nickel-phosphorous-coated aluminum hard disks
JP5049249B2 (en) * 2008-10-31 2012-10-17 花王株式会社 Polishing liquid composition
US8226841B2 (en) 2009-02-03 2012-07-24 Cabot Microelectronics Corporation Polishing composition for nickel-phosphorous memory disks
JP5536433B2 (en) * 2009-12-11 2014-07-02 花王株式会社 Polishing liquid composition for hard disk substrate
KR101396232B1 (en) * 2010-02-05 2014-05-19 한양대학교 산학협력단 Slurry for polishing phase change material and method for patterning polishing phase change material using the same
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
US9039914B2 (en) 2012-05-23 2015-05-26 Cabot Microelectronics Corporation Polishing composition for nickel-phosphorous-coated memory disks
JP6734018B2 (en) * 2014-09-17 2020-08-05 株式会社フジミインコーポレーテッド Abrasive material, polishing composition, and polishing method
WO2016042744A1 (en) * 2014-09-17 2016-03-24 株式会社フジミインコーポレーテッド Polishing material, composition for polishing, and polishing method
JP6622991B2 (en) * 2015-06-30 2019-12-18 株式会社フジミインコーポレーテッド Polishing composition
EP3775076A4 (en) * 2018-03-28 2021-12-22 FUJIFILM Electronic Materials U.S.A, Inc. Barrier ruthenium chemical mechanical polishing slurry
CN109233644B (en) * 2018-09-19 2021-03-12 广州亦盛环保科技有限公司 Fine polishing solution and preparation method thereof
JP7457586B2 (en) * 2020-06-18 2024-03-28 株式会社フジミインコーポレーテッド Concentrated solution of polishing composition and polishing method using the same

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002006418A1 (en) * 2000-07-19 2002-01-24 Kao Corporation Polishing fluid composition
CN1366247A (en) * 2001-01-18 2002-08-28 深圳市中兴集成电路设计有限责任公司 PCI bridge with improved structure
CN1414925A (en) * 1999-12-27 2003-04-30 昭和电工株式会社 Alumina Particles, method for producing the same, composition comprising the same and alumina slurry for polishing

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5693239A (en) * 1995-10-10 1997-12-02 Rodel, Inc. Polishing slurries comprising two abrasive components and methods for their use
JP3507628B2 (en) * 1996-08-06 2004-03-15 昭和電工株式会社 Polishing composition for chemical mechanical polishing
KR19980019046A (en) * 1996-08-29 1998-06-05 고사이 아키오 Abrasive composition and use of the same
WO2000032712A1 (en) * 1998-11-27 2000-06-08 Kao Corporation Abrasive fluid compositions
JP4053165B2 (en) * 1998-12-01 2008-02-27 株式会社フジミインコーポレーテッド Polishing composition and polishing method using the same
TW572979B (en) * 2000-02-02 2004-01-21 Rodel Inc Polishing composition
US6261476B1 (en) * 2000-03-21 2001-07-17 Praxair S. T. Technology, Inc. Hybrid polishing slurry
US6569215B2 (en) * 2000-04-17 2003-05-27 Showa Denko Kabushiki Kaisha Composition for polishing magnetic disk substrate
TWI268286B (en) * 2000-04-28 2006-12-11 Kao Corp Roll-off reducing agent
US6468913B1 (en) * 2000-07-08 2002-10-22 Arch Specialty Chemicals, Inc. Ready-to-use stable chemical-mechanical polishing slurries
JP4009986B2 (en) * 2000-11-29 2007-11-21 株式会社フジミインコーポレーテッド Polishing composition and polishing method for polishing memory hard disk using the same
JP4231632B2 (en) * 2001-04-27 2009-03-04 花王株式会社 Polishing liquid composition
CN100378145C (en) * 2001-06-21 2008-04-02 花王株式会社 Grinding liquid composition
GB2393186B (en) * 2002-07-31 2006-02-22 Kao Corp Polishing composition
GB2393447B (en) * 2002-08-07 2006-04-19 Kao Corp Polishing composition

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1414925A (en) * 1999-12-27 2003-04-30 昭和电工株式会社 Alumina Particles, method for producing the same, composition comprising the same and alumina slurry for polishing
WO2002006418A1 (en) * 2000-07-19 2002-01-24 Kao Corporation Polishing fluid composition
CN1366247A (en) * 2001-01-18 2002-08-28 深圳市中兴集成电路设计有限责任公司 PCI bridge with improved structure

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI752013B (en) * 2016-03-25 2022-01-11 日商福吉米股份有限公司 Polishing composition for polishing object having metal-containing layer, method for producing polishing composition, method for polishing, and method for producing substrate

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