CN100460478C - Polishing composition for magnetic disk - Google Patents

Polishing composition for magnetic disk Download PDF

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Publication number
CN100460478C
CN100460478C CNB2004100562306A CN200410056230A CN100460478C CN 100460478 C CN100460478 C CN 100460478C CN B2004100562306 A CNB2004100562306 A CN B2004100562306A CN 200410056230 A CN200410056230 A CN 200410056230A CN 100460478 C CN100460478 C CN 100460478C
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China
Prior art keywords
acid
substrate
liquid composition
grinding
weight
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Expired - Fee Related
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CNB2004100562306A
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CN1580173A (en
Inventor
北山博昭
藤井滋夫
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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
    • C09K3/1409Abrasive particles per se
    • 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

Abstract

A polishing composition for a magnetic disk, comprising alumina, water, a peroxide and an organic acid; a polishing process for a substrate to be polished, comprising the step of polishing the substrate to be polished with the polishing composition; and a process for manufacturing a substrate, comprising the step of polishing a substrate to be polished with the polishing composition. The polishing composition can be suitably used for the manufacture of a magnetic disk substrate for high-quality hard disks and the like.

Description

The disk grinding Liquid composition
Technical field
The present invention relates to disk with grinding Liquid composition and the manufacture method of using the Ginding process and the substrate of this grinding Liquid composition.
Background technology
Hard disk requires to reduce the float-amount of magnetic head and prevents surface imperfection (surface is dirty) in order to reduce the smallest record area, to advance high capacity.In order to reduce the float-amount of this magnetic head, need to reduce short wavelength's external waviness (external wavinesses of wavelength 50~500 μ m) and long wavelength's external waviness (external waviness that wavelength 0.5mm is above) in the grinding step of hard disk substrate, and prevent that from there is residue on the surface.Here said " external waviness " is meant the long concave-convex surface of specific surface roughness ripple, can be the mensuration such as optical metrological instrument of representative in order to " Zygo " that Canon vendor company makes.In order to make the substrate of this external waviness, surperficial dirty minimizing, 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 method by grinding Liquid composition.The spy opens the 2003-14733 communique and discloses the grinding Liquid composition that contains oxygenant, inorganic phosphor-contained acid and other mineral acid; Te Kaiping 11-246849 communique discloses the grinding step slip that contains polishing particles, hydrogen peroxide, metal nitrate and nitric acid.But, by the method for these grinding Liquid compositions, reduce, and prevent to see on the dirty viewpoint in surface and can not say so fully from having required grinding rate of practicability and external waviness simultaneously.
Summary of the invention
That is, the present invention relates to
(1) contains aluminum oxide, water, superoxide and organic acid disk grinding Liquid composition;
(2) comprise that the quilt that uses above-mentioned (1) described grinding Liquid composition to grind the operation of being ground substrate grinds the Ginding process of substrate; And
(3) comprise the manufacture method of using above-mentioned (1) described grinding Liquid composition to grind the substrate of the operation of being ground substrate.
Embodiment
The present invention relates to have high grinding rate, and can reduce the grinding Liquid composition of external waviness.The invention still further relates to and use this grinding Liquid composition, for example make the Ginding process of the external waviness minimizing of being ground substrate, and the manufacture method of using the substrate of this grinding Liquid composition.
These and other advantage of the present invention may be clearer by following explanation.
By grinding Liquid composition of the present invention being used for disk, can reach high grinding rate, the external waviness of minimizing grinding charge, and generation makes base board defect, the particularly effect of the dirty minimizing of substrate with grinding.Also obtain using this grinding Liquid composition to make by the Ginding process of the external waviness minimizing of grinding substrate and the manufacture method of substrate.
One big feature of grinding Liquid composition of the present invention is, the grinding promotor of using the grinding Liquid composition of aluminum oxide as abrasive substance, and with organic acid and superoxide.The grinding Liquid composition that discovery has this feature by use, the external waviness that can reach high grinding rate, is ground substrate effectively reduces and base board defect, the particularly unusual effect of the dirty minimizing of substrate such as scratch, pit.
The details of the mechanism of the grinding when using grinding Liquid composition of the present invention it be unclear that.Supposition is that grinding rate improves more because the pH of the grinding Liquid composition in the grinding is descended more, and the hydrogen ion that is generated by acid grinds being promoted by the corrosive effect of abrasive substance, is not limited thereto.Therefore, strength of acid is high more, and grinding rate is high more.In addition, in order to give full play to the grinding effect of aluminum oxide, superoxide changes the grinding charge surface, and above-mentioned corrosive nature is strengthened.External waviness when the result can reduce the process velocity of actual production level.Infer reinforced effects that the combination of this organic acid and superoxide obtains simultaneously and reduce base board defect, it is dirty relevant particularly to reduce substrate, is not limited thereto.
Grinding Liquid composition of the present invention contains aluminum oxide as abrasive substance.From reducing external waviness, reduce surfaceness, improve grinding rate and preventing the viewpoint of surface imperfection, aluminum oxide as the present invention's use, be preferably purity in aluminum oxide and be the aluminum oxide more than 95%, be more preferably more than 97%, be more preferably the aluminum oxide more than 99%.In addition, from the viewpoint of grinding rate, preferred Alpha-alumina; From the viewpoint of surface texture and minimizing external waviness, intermediate aluminas such as preferred gama-alumina, δ-aluminum oxide, θ-aluminum oxide, η-aluminum oxide, κ-aluminum oxide.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.In these intermediate aluminas, from improving the viewpoint of grinding rate and minimizing external waviness, preferred gama-alumina, δ-aluminum oxide, θ-aluminum oxide and their mixture are more preferably gama-alumina and θ-aluminum oxide.
The median size of the primary particle of aluminum oxide, from reducing the viewpoint of external waviness, the median size of primary particle is more preferably 0.005~0.8 μ m, be more preferably 0.01~0.4 μ m, the median size of offspring is more preferably 0.01~2 μ m, be more preferably 0.05~1.0 μ m, be more preferably 0.1~0.5 μ m.Can carry out image analysis by with sem observation (preferred 3000~30000 times) or transmission electron microscope observation (preferred 10000~300000 times), measure the median size that particle diameter is obtained the primary particle of abrasive substance.In addition, available laser diffractometry is measured the median size of offspring as volume average particle size.
Especially, when aluminum oxide was intermediate alumina, the specific surface area of measuring with the BET method was preferably 30~300m 2/ g is more preferably 50~200m 2/ g.
From improving the viewpoint of grinding rate and minimizing external waviness, the content of aluminum oxide is preferably more than the 0.05 weight % in the grinding Liquid composition, is 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 %.In addition, from the viewpoint of surface quality and economy, this content is preferably below the 40 weight % in the grinding Liquid composition, is more preferably below the 30 weight %, is more preferably below the 25 weight %, is more preferably below the 20 weight %.That is, the content of the aluminum oxide in the grinding Liquid composition is preferably 0.05~40 weight %, is more preferably 0.1~30 weight %, is preferably 0.5~25 weight % especially, is more preferably 1~20 weight %.
From improving the viewpoint of advantages such as grinding rate and minimizing external waviness, grinding Liquid composition of the present invention should contain superoxide.Superoxide of the present invention can roughly be divided into inorganic peroxide and organo-peroxide by its structure.The object lesson of these superoxide is as follows.As inorganic peroxide, can use hydrogen peroxide, also has 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, halogen-containing oxygen acid or derivatives thereof such as sodium iodate class.As organo-peroxide, can use percarboxylic acids such as peracetic acid, peroxyformic acid, peroxybenzoic acid, peroxides such as tert-butyl peroxide, cumene hydroperoxide thing.Wherein, in order to improve grinding rate and being easy to get property, usability such as water-soluble, preferred inorganic peroxide.And, consider from the aspect of environmental problem, preferably do not contain the inorganic peroxide of heavy metal.Viewpoint from above is more preferably inorganic peroxide, and particularly hydrogen peroxide, persulfuric acid salt, halogen-containing oxygen acid or its salt are more preferably hydrogen peroxide.In addition, 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 superoxide is preferably more than the 0.002 weight % in the grinding Liquid composition, be 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 %.In addition, from the viewpoint of surface quality and economy, this content is preferably below the 20 weight % in the grinding Liquid composition, is more preferably below the 15 weight %, is more preferably below the 10 weight %, is more preferably below the 5 weight %.That is, the content of superoxide is preferably 0.002~20 weight % in the grinding Liquid composition, is 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, in the grinding Liquid composition of the present invention, outside alumina, the superoxide, also should contain organic acid.From the viewpoint of raising grinding rate and minimizing external waviness, the organic acid that the present invention uses, its pK1 is less than 7, is more preferably below 5, is more preferably below 4, is more preferably below 2.The logarithmic value of the inverse of first acid ionization constant when here, pK1 represents 25 ℃.The pK1 of each compound is on the books in 4 editions (basis a piece of writing) II, pp316~325 (Japanization association volumes) etc. are changed in chemical brief guide.
As the appropriate organic among the present invention, from improving grinding rate, reduce external waviness and prevent the viewpoint that the surface is dirty, preferred sulfur-bearing organic acid, carboxylic acid and phosphorous organic acid.Its object lesson is as follows.Formic acid is for example arranged; acetate; oxyacetic acid; lactic acid; propionic acid; hydroxy-propionic acid; butyric acid; phenylformic acid; monocarboxylic acids 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 acids such as ethylenediamine tetraacetic acid (EDTA); methylsulfonic acid; sulfur-bearing organic acids such as tosic acid; etherophosphoric acid; butyl phosphate; lauryl phosphate; HPAA; hydroxy ethylene-1, the 1-di 2 ethylhexyl phosphonic acid; the phosphinylidyne butane tricarboxylic acid; phosphorous organic acid such as ethylenediamine tetramethylene phosphonic acid etc.Wherein, from improving the viewpoint of grinding rate and minimizing external waviness, preferred sulfur-bearing organic acid and phosphorous organic acid are more preferably organic sulfonic acid class and organic phosphine acids, preferred especially organic sulfonic acid class.In addition, from the viewpoint that prevents that grinding charge is dirty, preferred sulfur-bearing organic acid and carboxylic acid are more preferably organic sulfonic acid class and polycarboxylic acid class.
These compounds can be used alone, but also also mix together.
From improving the viewpoint of grinding rate and minimizing external waviness, organic acid content is preferably more than the 0.002 weight % in the grinding Liquid composition, be 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 %.In addition, from the viewpoint of surface quality and economy, this content is preferably below the 20 weight % in the grinding Liquid composition, is more preferably below the 15 weight %, is more preferably below the 10 weight %, is more preferably below the 5 weight %.That is, the content of acid is preferably 0.002~20 weight % in the grinding Liquid composition, is more preferably 0.005~15 weight %, is more preferably 0.007~10 weight %, is more preferably 0.01~5 weight %.
Water in the grinding Liquid composition of the present invention is as medium.From the viewpoint of effective grinding grinding charge, the content of water is preferably 55~99 weight %, is more preferably 60~97 weight %, is more preferably 70~95 weight %.
From further raising grinding rate and reduce the viewpoint of external waviness, in the grinding Liquid composition of the present invention, preferred and use mineral acid.As mineral acid, nitrogenous mineral acids such as nitric acid, nitrous acid are for example arranged, sulfur-bearing mineral acids such as sulfuric acid, sulfurous acid, thionamic acid, inorganic phosphor-contained acid such as phosphoric acid, tetra-sodium, Tripyrophosphoric acid, phosphonic acids etc.Wherein, from improving the viewpoint of grinding rate, preferred nitric acid, nitrous acid, sulfuric acid, sulfurous acid and thionamic acid are more preferably sulfuric acid, sulfurous acid and thionamic acid, are more preferably sulfuric acid.And when using mineral acid, its content is preferably more than the 0.002 weight % in the grinding Liquid composition, is more preferably more than the 0.005 weight %, is more preferably more than the 0.007 weight %, is more preferably more than the 0.01 weight %.In addition, from the viewpoint of surface quality and economy, this content is preferably below the 20 weight % in the grinding Liquid composition, is more preferably below the 15 weight %, is preferably especially below the 10 weight %, is more preferably below the 5 weight %.That is, the content of mineral acid is preferably 0.002~20 weight % in the grinding Liquid composition, is more preferably 0.005~15 weight %, is preferably 0.007~10 weight % especially, is more preferably 0.01~5 weight %.
In addition, as required, can cooperate other compositions such as inorganic salt, thickening material, rust-preventive agent, alkaline matter in the grinding Liquid composition of the present invention.Especially, inorganic salt such as ammonium nitrate, ammonium sulfate, vitriolate of tartar, single nickel salt, Tai-Ace S 150, Ammonium sulfamate have auxiliaring effect to improving grinding rate.These other compositions may be used alone, can also be two or more kinds in combination.In addition, from the viewpoint of economy, its content is preferably 0.05~20 weight % in the grinding Liquid composition, is more preferably 0.05~10 weight %, is more preferably 0.05~5 weight %.
And,, as required, can cooperate sterilant and antiseptic-germicide etc. as other compositions.From the performance functional point of view and to the influence of nonferromagnetic substance and the viewpoint of economy, the content of these sterilant, antiseptic-germicide is preferably 0.0001~0.1 weight % in the grinding Liquid composition, be more preferably 0.001~0.05 weight %, be preferably 0.002~0.02 weight % especially.
Moreover, 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 occasions are that the form with concentrated solution prepares composition, before using or when using its dilution are used.
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 quality etc. suitably to determine.From improving the viewpoint of grinding rate, minimizing external waviness, pH is low more good more, but viewpoint from the preservative property of processor and operator's security, pH is preferably near 7, therefore during both additions, pH is preferably more than 0.1 and less than 6, is more preferably more than 0.5 and less than 5, be more preferably more than 1 and, be more preferably more than 1 and less than 3 less than 4.The pH of grinding Liquid composition can be by suitably cooperating aequum organic acid such as mineral acid, hydroxycarboxylic acid, polycarboxylic acid, aminopolycarboxylic, amino acid such as nitric acid, sulfuric acid and alkaline matter such as metal-salt, ammonium salt, ammoniacal liquor, sodium hydroxide, potassium hydroxide, amine thereof adjust.
The manufacture method of substrate of the present invention comprises with above-mentioned grinding Liquid composition and grinds the operation of being ground substrate.
The substrate disk substrate that ground as object of the present invention is used the substrate of medium as magnetic recording.As the object lesson of magnetic disc substrate, representational is the aluminium alloy base plate of plating Ni-P alloy, can also list, and replaces the aluminium alloy plating with the substrate of Ni-P or the substrate that replaces plating Ni-P to coat by plating and the various metallic compounds of evaporation with glass and vitreous carbon.
In the above-mentioned grinding step,,, make abrasive disk and substrate rotating when exerting pressure, can grind and be ground substrate the abrasive surface of grinding Liquid composition supplying substrate of the present invention with posting the abrasive disk clamping substrate that porous matter organic polymer is an abrasive cloth etc.Therefore, the present invention relates to comprise the Ginding process that is ground substrate that grinds the operation of being ground substrate with above-mentioned grinding Liquid composition.Other conditions (feed rate of the kind of shredder, grinding temperature, grinding rate, lapping liquid etc.) when grinding are not particularly limited.
Grinding Liquid composition of the present invention produces effect in polishing process especially, but equally also applicable to other grinding steps, for example polishes operation etc.
Embodiment
Further specify, disclose mode of the present invention below by embodiment.These embodiment just illustrate of the present invention, do not represent to have any qualification.
Embodiment 1~6, comparative example 1~2
1, preparation grinding Liquid composition
Mix, stir aluminum oxide (median size of offspring is 0.2 μ m, purity about 99.9%), superoxide, organic acid and other additives etc. of the specified rate shown in the table 1, surplus is an ion exchanged water, the preparation grinding Liquid composition.
2, Ginding process
The surface of the substrate that the aluminium alloy of the plating Ni-P of thickness 1.27mm, diameter 3.5 inches (95mm) is constituted (the short wavelength's external waviness 3.8nm, the long wavelength's external waviness 1.6nm that measure with " Zygo New View 200 "), use two side machining apparatus, polishing under the imposing a condition of following two side machining apparatus obtains as the grinding charge of magnetic recording media with the aluminium alloy base plate of the plating Ni-P of substrate.
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: 4 minutes
The piece number of the substrate that drops into: 10
3, evaluation method
(1) 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 and comparative example with the grinding rate of comparative example 1.
Weight minimizing 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) * 1000000
(2) external waviness
Measure each substrate after grinding under the following conditions.
Machine: Zygo New-View 200 (Canon manufacturing)
Object lens: 2.5 times of Michelson
Zoom ratio: 0.5
Shift out: cylinder
Wave filter: FFT fixed band is logical
-short wavelength external waviness: the high wavelength 50 μ m of wave filter
Wave filter hangs down wavelength 50 μ m
-short wavelength external waviness: the high wavelength 0.5mm of wave filter
Wave filter hangs down wavelength 5mm
Area: 4.33mm * 5.77mm
(3) surface is dirty
By 300 times of surfaces of observing each substrate after grinding, carry out following 5 grades of evaluations with polarizing microscope.1,2 grades can not be practical.
5: the surface is not observed aluminum oxide residue and lapping rejects etc. fully
4: only observe very trace
3: observe a small amount of
2: observe volume
1: observe very many
The result is as shown in table 1.
Figure C200410056230D00131
As shown in Table 1, the grinding Liquid composition that embodiment 1~6 obtains with comparing that comparative example 1~2 obtains, has high grinding rate, and short wavelength's external waviness, long wavelength's external waviness all reduce, and the surperficial dirty of substrate also significantly reduces.
Grinding Liquid composition of the present invention goes for making the magnetic disc substrate of high-quality hard disk etc.
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, all changes that those skilled in the art did all are included in the technical scope of appended claim.

Claims (12)

1. disk grinding Liquid composition, it contains aluminum oxide, water, superoxide, organic acid and mineral acid, wherein this mineral acid be selected from nitric acid, nitrous acid, sulfuric acid, sulfurous acid and the thionamic acid more than a kind.
2. the described grinding Liquid composition of claim 1, wherein, organic acid is for being selected from sulfur-bearing organic acid, carboxylic acid and phosphorous organic acid more than a kind.
3. the described grinding Liquid composition of claim 1, wherein, composition pH is more than 0.1 and less than 6.
4. the described grinding Liquid composition of claim 2, wherein, composition pH is more than 0.1 and less than 6.
5. ground the Ginding process of substrate, it comprises the operation of using the described grinding Liquid composition grinding of claim 1 to be ground substrate.
6. ground the Ginding process of substrate, it comprises the operation of using the described grinding Liquid composition grinding of claim 2 to be ground substrate.
7. the described method of claim 5 is wherein ground the aluminium alloy base plate of substrate for plating Ni-P alloy.
8. the described method of claim 6 is wherein ground the aluminium alloy base plate of substrate for plating Ni-P alloy.
9. the manufacture method of substrate, it comprises and uses the described grinding Liquid composition of claim 1 to grind the operation of being ground substrate.
10. the manufacture method of substrate, it comprises and uses the described grinding Liquid composition of claim 2 to grind the operation of being ground substrate.
11. the described manufacture method of claim 9 is wherein ground the aluminium alloy base plate of substrate for plating Ni-P alloy.
12. the described manufacture method of claim 10 is wherein ground the aluminium alloy base plate of substrate for plating Ni-P alloy.
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