CN106281221A - Grinding-material, composition for polishing and Ginding process - Google Patents

Grinding-material, composition for polishing and Ginding process Download PDF

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Publication number
CN106281221A
CN106281221A CN201610663520.XA CN201610663520A CN106281221A CN 106281221 A CN106281221 A CN 106281221A CN 201610663520 A CN201610663520 A CN 201610663520A CN 106281221 A CN106281221 A CN 106281221A
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grinding
acid
composition
polishing
oxide
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CN106281221B (en
Inventor
森永均
玉井诚
玉井一诚
浅井舞子
伊藤友
伊藤友一
天高恭祐
镰田透
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Fujimi Inc
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Fujimi Inc
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • 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
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/04Aqueous dispersions
    • 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
    • C09G1/06Other polishing compositions
    • C09G1/14Other polishing compositions based on non-waxy substances
    • C09G1/18Other polishing compositions based on non-waxy substances on other substances

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)

Abstract

The present invention provides a kind of grinding-material of minute surface, composition for polishing and Ginding process that the surface of alloy, metal-oxide can be ground with sufficient grinding rate and be obtained in that high-quality.Described grinding-material contain alpha-transformation degree be more than 80% and the accumulation particle diameter of volume reference distribution in the aluminium oxide that 50% particle diameter is below more than 0.15 μm and 0.35 μm.Composition for polishing contains this grinding-material and pH is less than 7.This grinding-material and composition for polishing are for the grinding grinding object containing at least one in alloy and metal-oxide.

Description

Grinding-material, composition for polishing and Ginding process
Technical field
The present invention relates to grinding-material, composition for polishing and Ginding process.
Background technology
All the time, grinding is utilized to carry out alloy, its anodic oxide coating, the minute surface polish on ceramic surface, smooth Change.But, for conventional Ginding process, the minute surface of higher quality sometimes can not be effectively obtained.
Such as in the case of alloy, owing to element and the element different from main constituent hardness of main constituent are mixed, The surface of alloy the most after grinding produces the various defects such as projection, depression, cut.Therefore, grinding is not easily passed through right Alloy carries out the minute surface polish (seeing patent documentation 1,2) of height.
It addition, in the case of anodic oxide coating, if using the existing grinding that colloidal silica is used as abrasive particle Carry out polish grinding by compositions, the most sometimes can not obtain sufficient grinding rate (seeing patent documentation 3).
Additionally, carry out minute surface polish in order to the surface of the metal-oxide as hard brittle material is ground, put down Cunningization, used the composition for polishing containing diamond abrasive grain in the past, but there are the following problems: containing the grinding of diamond abrasive grain Expensive by compositions, and easily produce cut, it is difficult to obtain the minute surface of high-quality.It addition, for colloidal silica is used Make the existing composition for polishing of abrasive particle, though not producing cut, but sometimes can not obtain sufficient grinding rate and (see patent Document 4,5).
Prior art literature
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 01-246068 publication
Patent documentation 2: Japanese Unexamined Patent Publication 11-010492 publication
Patent documentation 3: Japanese Unexamined Patent Publication 7-52030 publication
Patent documentation 4: Japanese Unexamined Patent Publication 7-179848 publication
Patent documentation 5: Japanese Unexamined Patent Publication 2008-44078 publication
Summary of the invention
The problem that invention is to be solved
Therefore, in order to solve the problem that prior art as described above has, the problem of the present invention is, it is provided that can be with Sufficiently the surface of alloy, metal-oxide is ground and is obtained in that the grinding material of minute surface of high-quality by grinding rate Material, composition for polishing and Ginding process.
For solving the scheme of problem
In order to solve aforementioned problems, the main points of the grinding-material of an embodiment of the invention are, for containing alloy With the grinding grinding object of at least one in metal-oxide, it is more than 80% and body that this grinding-material contains alpha-transformation degree The aluminium oxide that 50% particle diameter is below more than 0.15 μm and 0.35 μm in the accumulation particle diameter distribution of long-pending benchmark.
It addition, the purport of the composition for polishing of the alternate manner of the present invention is, containing grinding of said one embodiment Grind material, and pH is less than 7.
Additionally, the main points of the Ginding process of the alternate manner of the present invention are, the grinding of above-mentioned alternate manner is used to combine Grinding object containing at least one in alloy and metal-oxide is ground by thing.
The effect of invention
In accordance with the invention it is possible to the surface of alloy, metal-oxide is ground with sufficient grinding rate, it is possible to obtain Obtain the minute surface of high-quality.
Detailed description of the invention
An embodiment of the invention is described in detail.It should be noted that following embodiment illustrates One example of the present invention, the present invention is not limited to present embodiment.Furthermore it is possible to following embodiment is carried out various change More or improvement, this mode having carried out various change or improvement can also comprise in the present invention.
The grinding-material of present embodiment is for the grinding object containing at least one in alloy and metal-oxide Grinding, this grinding-material contain alpha-transformation degree be more than 80% and the accumulation particle diameter of volume reference distribution in 50% particle diameter be Aluminium oxide more than 0.15 μm and below 0.35 μm.It addition, the composition for polishing of present embodiment contains present embodiment Grinding-material and pH are less than 7.
The grinding-material of such present embodiment and composition for polishing may be used for containing alloy and metal-oxide In at least one grind object grinding.And, if using the grinding-material of present embodiment, composition for polishing pair Grinding object is ground, then can be ground the surface of alloy, metal-oxide with sufficient grinding rate, it is possible to Obtain the minute surface of high-quality.Specifically, if using the grinding-material of present embodiment, composition for polishing to grinding object Be ground, then can be with sufficient grinding rate to the grinding object containing at least one in alloy and metal-oxide Surface be ground, and improve grind object surface flatness such that it is able to obtain the defect such as high glaze and cut The minute surface of few high-quality.
Hereinafter, grinding-material and composition for polishing to present embodiment are described in detail.It should be noted that For various operations, the mensuration of physical property of following description, as long as no being particularly limited to, then it is room temperature (more than 20 DEG C and 25 DEG C Below), carry out under conditions of relative humidity more than 40% and less than 50%.
1. about grinding object
1-1 is about alloy
The grinding-material of present embodiment and composition for polishing may be used for carrying out the grinding object containing alloy The purposes ground.Alloy contains the metal species as main constituent and the metal species different from the metal species of main constituent.Right The quantity of metal species is not particularly limited, and can be 2 kinds, it is also possible to be more than 3 kinds.It addition, the method manufacturing alloy is not had It is particularly limited to, such as, can use casting, forge or roll.
The metal species of the main constituent in metal species contained in alloy be preferably selected from by aluminum, titanium, magnesium, ferrum, nickel, In the group of copper composition wantonly a kind.Preferred alloy be the metal species of main constituent be aluminum, titanium, magnesium or ferrum, further preferred Alloy be the metal species of main constituent be aluminum or ferrum.Alloy is metal species based on main constituent and names.Accordingly, as conjunction Gold, include, for example out aluminium alloy, titanium alloy, magnesium alloy, ferroalloy (such as rustless steel), nickel alloy, copper alloy etc..
Aluminium alloy is with aluminum as main constituent, as the metal species different from the metal species of main constituent, such as possibly together with choosing At least one in silicon, ferrum, copper, manganese, magnesium, zinc and chromium.The content of the metal species in addition to aluminum in aluminium alloy is for example, More than 0.1 mass %, more than more specifically 0.1 mass % and below 10 mass %.As the example of aluminium alloy, can enumerate Going out the alloy numbering 2000 described in JIS (JIS) H4000:2006, H4040:2006 and H4100:2006 is Row, 3000 series, 4000 series, 5000 series, 6000 series, 7000 series, the alloy of 8000 series.
Titanium alloy is with titanium as main constituent, as the metal species different from the metal species of main constituent, such as possibly together with choosing At least one in aluminum, ferrum and vanadium.More than content for example, 3.5 mass % of the metal species than titanium in titanium alloy And 30 below mass %.As the example of titanium alloy, the kind described in JIS (JIS) H4600:2012 can be listed The 11 of apoplexy due to endogenous wind~23 kind, 50 kinds, 60 kinds, 61 kinds and the alloy of 80 kinds.
Magnesium alloy is with magnesium as main constituent, as the metal species different from the metal species of main constituent, such as possibly together with choosing At least one in aluminum, zinc, manganese, zirconium and rare earth element.The content of the metal species beyond demagging in magnesium alloy is for example, More than 0.3 mass % and below 10 mass %.As the example of magnesium alloy, JIS (JIS) H4201 can be listed: 2011, AZ10,31,61,63,80,81,91,92 etc. described in H4203:2011 and H4204:2011.
Ferroalloy (such as rustless steel) is with ferrum as main constituent, as the metal species different from the metal species of main constituent, Such as possibly together with at least one in chromium, nickel, molybdenum and manganese.The content of the metal species in addition to ferrum in ferroalloy is such as It is below more than 10 mass % and 50 mass %.As stainless example, JIS (JIS) G4303 can be listed: SUS201 in the symbol of the kind described in 2005,303,303Se, 304,304L, 304NI, 305,305JI, 309S, 310S、316、316L、321、347、384、XM7、303F、303C、430、430F、434、410、416、420J1、420J2、 420F, 420C, 631J1 etc..
Nickel alloy is with nickel as main constituent, as the metal species different from the metal species of main constituent, such as possibly together with choosing At least one in ferrum, chromium, molybdenum and cobalt.Content for example, 20 mass % of the metal species in addition to nickel in nickel alloy with Go up and below 75 mass %.As the example of nickel alloy, can list described in JIS (JIS) H4551:2000 Alloy numbering in NCF600,601,625,750,800,800H, 825, NW0276,4400,6002,6022 etc..
Copper alloy is with copper as main constituent, as the metal species different from the metal species of main constituent, such as possibly together with choosing At least one in ferrum, lead, zinc and stannum.More than content for example, 3 mass % of the metal species beyond copper removal in copper alloy And 50 below mass %.As the example of copper alloy, the conjunction described in JIS (JIS) H3100:2006 can be listed Gold numbering in C2100,2200,2300,2400,2600,2680,2720,2801,3560,3561,3710,3713,4250, 4430,4621,4640,6140,6161,6280,6301,7060,7150,1401,2051,6711,6712 etc..
1-2 is about metal-oxide
The grinding-material of present embodiment and composition for polishing may be used for the grinding object containing metal-oxide The purposes that thing is ground.Metal-oxide is metal or semimetallic oxide or their composite oxides, such as, and can List the selected from the periodic table of elements the 3rd, 4, more than a kind metal of 13 race's elements or semimetallic oxide or they answer Close oxide.Specifically, except silicon oxide (silica), aluminium oxide (alumina), titanium oxide (titania), zirconium oxide (zirconia), beyond gallium oxide, yittrium oxide (yttria), germanium oxide, their composite oxides can also be listed.At these In metal-oxide, particularly silicon oxide, aluminium oxide (corundum etc.), zirconium oxide, yittrium oxide are applicable.
It should be noted that the metal-oxide that grinding object contains can be various metals or semimetallic oxide Mixture, can be the mixture of multiple composite oxides, it is also possible to for metal or semimetallic oxide and combined oxidation The mixture of thing.It addition, grinding the metal-oxide that contains of object can be metal or semimetallic oxide or composite oxygen The composite of the material (such as metal, carbon, pottery) of compound and the kind in addition to it.
It addition, the metal-oxide that grinding object contains can be the forms such as monocrystalline, polycrystalline, sintered body (ceramic).? In the case of metal-oxide is such form, grind the thing that object can use its entirety to be formed by metal-oxide Matter.Or, the metal-oxide that grinding object contains can be by simple metal, alloy are carried out anodic oxide coating process And the form of the anodic oxide coating formed.That is, the metal-oxide that grinding object contains can be such as simple metal, alloy That anodic oxide coating is formed at metallic surface like that, this metal autoxidation and the oxide that obtains.
In the case of metal-oxide is such form, grinds object and one part can also be used by burning The material that thing is formed and other parts are formed by other material.In the case of metal-oxide is anodic oxide coating, it is right to grind As the part including its surface of thing is formed by metal-oxide, other parts are formed by simple metal or alloy.
As the example of anodic oxide coating, the skin being made up of aluminium oxide, titanium oxide, magnesium oxide or zirconium oxide can be listed Film.
Furthermore it is possible to lead on the surface of the base material of material different types of with metal-oxide (such as metal, carbon, pottery) Cross the epitheliums such as spraying plating (such as plasma spraying, flame coating), plating, chemical vapor deposition (CVD), physical vapor deposition (PVD) to process Form epithelium, thus constitute grinding object.
As the example of the epithelium formed by spraying plating, the gold being made up of aluminium oxide, zirconium oxide or yittrium oxide can be listed Belong to oxide epithelium.
As the example of the epithelium formed by plating, can list by zinc, nickel, chromium, stannum, copper or their alloy structure The metal epithelium become.
As the example of the epithelium formed by chemical vapor deposition, can list and be made up of silicon oxide, aluminium oxide or silicon nitride Ceramic epithelium.
As the example of the epithelium formed by physical vapor deposition, can list by copper, chromium, titanium, copper alloy, nickel alloy or The metal epithelium that ferroalloy is constituted.
2. about grinding-material
The grinding-material of present embodiment contains aluminium oxide.Aluminium oxide has Alpha-alumina, beta-alumina, gama-alumina, The aluminium oxide that the crystal habits such as θ-aluminium oxide are different, it addition, there is also the aluminium compound being referred to as hydrated alumina.From grinding speed From the viewpoint of degree, preferably by the granule using Alpha-alumina as main constituent as grinding-material (abrasive particle), use containing this grinding The composition for polishing of material is ground the grinding of object.
The alpha-transformation degree of aluminium oxide can be set to more than 70%, is preferably set to more than 80%, is more preferably set to more than 90%.Oxygen The alpha-transformation degree changing aluminum can be obtained by the integrated intensity ratio of (113) face diffracted ray measured by X-ray diffraction.
It addition, the BET specific surface area of aluminium oxide can be set to 5m2/ more than g and 50m2/ below g, is preferably set to 15m2/ g with Go up and 25m2/ below g.If the BET specific surface area of aluminium oxide is too small, then has and can not remove ripple, it is impossible to obtain smooth face Worry, if excessive, then have the worry that can not obtain sufficient grinding rate.The BET specific surface area of aluminium oxide can use " the Flow Sorb II2300 " of Micromeritics company is measured.It is adsorbed in oxidation during as measurement the specific area The gas of aluminum, can list nitrogen, argon, Krypton etc..
Additionally, as aluminium oxide average aggregate particle size volume reference accumulation particle diameter distribution in 50% particle diameter (with Under be sometimes also denoted as " D50 ") be below more than 0.15 μm and 0.35 μm, more than preferably 0.16 μm and below 0.31 μm, more excellent Elect below more than 0.25 μm and 0.29 μm as, more preferably more than 0.26 μm and below 0.27 μm.
It addition, 10% particle diameter (being the most sometimes also denoted as " D10 ") in the accumulation particle diameter distribution of the volume reference of aluminium oxide Less than 50% particle diameter and be below more than 0.10 μm and 0.25 μm, preferably smaller than 50% particle diameter and be more than 0.13 μm and Below 0.23 μm, more preferably less than 50% particle diameter and be below more than 0.18 μm and 0.20 μm, it is further preferably no larger than 50% Particle diameter and be below more than 0.19 μm and 0.20 μm.
Additionally, 90% particle diameter (the most otherwise referred to as " D90 ") in the accumulation particle diameter distribution of the volume reference of aluminium oxide More than 50% particle diameter and be below more than 0.18 μm and 0.45 μm, preferably greater than 50% particle diameter and be more than 0.20 μm and Below 0.42 μm, more preferably greater than 50% particle diameter and be below more than 0.35 μm and 0.39 μm, further preferably greater than 50% Particle diameter and be below more than 0.36 μm and 0.37 μm.
If the above-mentioned particle diameter of aluminium oxide is too small, then there is the worry that can not obtain sufficient grinding rate, if excessive, then have not Ripple can be removed, the worry in smooth face cannot be obtained.
It addition, the ratio (D90/D50) that D90 is relative to D50 can be set to more than 1.1 and less than 2.5, preferably 1.1 with Upper and less than 1.7, more preferably more than 1.2 and less than 1.5.
And then, the D90 ratio (D90/D10) relative to D10 can be set to more than 1.2 and less than 6.5, preferably 1.3 with Upper and less than 2.5, more preferably more than 1.7 and less than 2.1.
And then, the D50 ratio (D50/D10) relative to D10 can be set to more than 1.1 and less than 2.0, preferably 1.1 with Upper and less than 1.8, more preferably more than 1.2 and less than 1.6.
If these ratios are too small, then there is the situation that the manufacturing cost of aluminium oxide uprises, if excessive, then have and grinding object Surface produce cut worry.
It should be noted that D10, D50, D90 refer to volume reference accumulation particle diameter be distributed in from small particle side Cumulative frequency is respectively the particle diameter of 10%, 50%, 90%.Described D10, D50, D90 can use laser diffraction/scattering formula particle diameter Distribution measurement device (" LA-950 " of such as Horiba Ltd) is measured.
Additionally, the content of the grinding-material in the composition for polishing of present embodiment can be set to more than 0.5 mass % And 40 below mass %, more than preferably 1 mass % and below 20 mass %.If the content of grinding-material is very few, then having cannot Obtain the worry of sufficient grinding rate, if too much, then have composition for polishing to become the worry of high cost.
3. about composition for polishing
Grinding-material and its pH that the composition for polishing of present embodiment contains above-mentioned present embodiment are less than 7.This The composition for polishing of embodiment is in addition to grinding-material, it is also possible to according to expectation containing liquid medium, additive.
3-1 is about liquid medium
The composition for polishing of present embodiment can containing as make grinding-material dispersion and by other composition dispersion or Dissolve disperse medium or the liquid medium of solvent and in pulp-like.As liquid medium, preferably water, from suppression to other composition Effect obstruction from the viewpoint of, do not contain the water of impurity the most as far as possible.Specifically, preferably remove with ion exchange resin After foreign ion, eliminate the pure water of foreign body, ultra-pure water or distilled water by filter.
3-2 is about pH and pH adjusting agent
The pH of the composition for polishing of present embodiment is less than 7.0, preferably less than 4.0.It addition, present embodiment The pH of composition for polishing is preferably more than 2.0.In the case of pH is in above-mentioned scope, grinding rate is excellent.It addition, by The safety of the composition for polishing in pH is in above-mentioned scope is high, therefore, it is possible to process safely.
The regulation of the pH of the composition for polishing of present embodiment can be carried out by the pH adjusting agent as additive.pH The pH of composition for polishing is adjusted by regulator, thereby, it is possible to the control grinding grinding rate of object, grinding-material Dispersibility etc..PH adjusting agent can be used alone a kind, it is also possible to is mixed with two or more.
As pH adjusting agent, it is possible to use known acid, alkali or their salt.As the acid that can serve as pH adjusting agent Concrete example, can list: the nothings such as hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., boric acid, carbonic acid, ortho phosphorous acid, phosphorous acid and phosphoric acid Machine acid;Formic acid, acetic acid, propanoic acid, butanoic acid, valeric acid, 2-Methyl Butyric Acid, n-caproic acid, 3,3-acid dimethyl, 2 Ethylbutanoic acid, 4- Methylvaleric acid, positive enanthic acid, 2 methyl caproic acid, caprylic acid, 2 ethyl hexanoic acid, benzoic acid, glycolic, salicylic acid, glyceric acid, grass Acid, malonic acid, succinic acid, 1,3-propanedicarboxylic acid, adipic acid, 1,5-pentanedicarboxylic acid., maleic acid, phthalic acid, malic acid, tartaric acid, citric acid, Lactic acid, diethyl alkyd, pyromucic acid, 2,5-furan dicarboxylic acid, 3-furancarboxylic acid, 2-oxolane carboxylic acid, 2-Methoxyacetic acid, The organic acid such as methoxyphenyl acetic acid and phenoxyacetic acid.
In the case of using mineral acid as pH adjusting agent, from the viewpoint of grinding rate improves, preferably sulfuric acid, nitre Acid, hydrochloric acid, phosphoric acid etc., in the case of using organic acid as pH adjusting agent, preferred alcohol acid, succinic acid, maleic acid, Fructus Citri Limoniae Acid, tartaric acid, malic acid, gluconic acid and itaconic acid etc..
As can act as the salt of pH adjusting agent, can list: the amine such as aliphatic amine, aromatic amine;Quaternary ammonium hydroxide etc. Organic base;The alkali-metal hydroxide such as potassium hydroxide;The hydroxide of alkaline-earth metal;And ammonia etc..In these alkali, from obtaining Obtain easiness to set out, preferably potassium hydroxide, ammonia.
Alternatively, it is also possible to use the salt such as the ammonium salt of aforementioned acid, alkali metal salt replace aforementioned acid or be applied in combination with aforementioned acid As pH adjusting agent.Particularly in the situation of the salt using weak acid and the salt of the salt of highly basic, strong acid and weak base or weak acid and weak base Under, it is possible to expect the cushioning effect of pH, and then in the case of the salt using strong acid and highly basic, it is possible to a small amount of regulation pH and Electrical conductivity.
The addition of pH adjusting agent is not particularly limited, as long as suitable adjustment makes composition for polishing be that desired pH is Can.
3-3 is about other additive
For the composition for polishing of present embodiment, in order to improve its performance, pH regulator can also be contained as required Additive beyond agent.Such as, composition for polishing can contain chelating agent, etchant, oxidant etc. and has further raising The additive of the effect of grinding rate.It addition, composition for polishing can also be containing to grinding the surface of object, grinding-material The water-soluble polymer (can be copolymer, its salt, derivant) that works of surface.And then, composition for polishing can also The easy dispersing aid of redispersion containing the aggregation making dispersant that the dispersibility of grinding-material improves, making grinding-material it The additive of class.And then, composition for polishing can also contain the known additive of preservative, antifungus agent, antirust agent etc.
Described various additive in most patent documentation etc. as generally adding in composition for polishing Material is known, and kind and addition to additive are not particularly limited.It is wherein, overall relative to composition for polishing, Addition when adding these additives is preferably respectively smaller than 1 mass %, is more preferably respectively smaller than 0.5 mass %.These add Agent can be used singly or in combination of two or more.
As the example of chelating agent, mineral acid, organic acid, aminoacid, nitrile compound and chelating agen etc. can be listed.As The concrete example of mineral acid, can list sulphuric acid, nitric acid, boric acid, carbonic acid etc., as the concrete example of organic acid, can list: first Acid, acetic acid, propanoic acid, butanoic acid, valeric acid, 2-Methyl Butyric Acid, n-caproic acid, 3,3-acid dimethyl, 2 Ethylbutanoic acid, 4-methylpent Enanthic acid sour, positive, 2 methyl caproic acid, caprylic acid, 2 ethyl hexanoic acid, benzoic acid, glycolic, salicylic acid, glyceric acid, oxalic acid, the third two Acid, succinic acid, 1,3-propanedicarboxylic acid, adipic acid, 1,5-pentanedicarboxylic acid., maleic acid, phthalic acid, malic acid, tartaric acid, citric acid, lactic acid etc.. Organic sulphuric acid such as methanesulfonic acid, ethyl sulfonic acid and hydroxyethylsulfonic acid. can also be used.The alkali gold of mineral acid or organic acid can also be used Belong to the salt such as salt replace mineral acid or organic acid or be applied in combination with mineral acid or organic acid.Among these chelating agent, the sweetest Propylhomoserin, alanine, malic acid, tartaric acid, citric acid, glycolic, hydroxyethylsulfonic acid. or their salt.
As the example of chelating agen, the carboxylic serials chelating agen such as gluconic acid can be listed;Ethylenediamine, diethylenetriamines, three The amine system chelating agen such as tetramine;Ethylenediaminetetraacetic acid, nitrilotriacetic acid(NTA), Oxyethylethylenediaminetriacetic acid, triethylene The polyamino such as four hexaacetic acids, diethylene-triamine pentaacetic acid polycarboxylic acid system chelating agen.Alternatively, it is also possible to enumerate 2-amino-ethyl Phosphonic acids, 1-hydroxy ethylidene base-1,1-di 2 ethylhexyl phosphonic acid, amino three (methylene phosphonic acid), EDTMP, diethylidene Triamine five (methylene phosphonic acid), ethane-1,1-di 2 ethylhexyl phosphonic acid, ethane-1,1,2-tri methylene phosphonic acid, methane hydroxyethylidene diphosphonic acid, 1-phosphinylidyne butane- Organic phospho acid system chelating agen, phenol derivatives, the 1,3-diketone etc. such as 2,3,4-tricarboxylic acids are as the example of chelating agen.
As the example of etchant, can list: the mineral acids such as nitric acid, sulphuric acid, hydrochloric acid, phosphoric acid, Fluohydric acid.;Acetic acid, lemon The organic acid such as lemon acid, tartaric acid, methanesulfonic acid;The inorganic bases such as potassium hydroxide, sodium hydroxide, ammonia;Amine, quaternary ammonium hydroxide etc. are organic Alkali etc..
As the example of oxidant, can list: hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, perchlorate, Persulfate, nitric acid, potassium permanganate etc..
Example as water-soluble polymer (can be copolymer, its salt, derivant), it is possible to list polyacrylate Deng polycarboxylic acids;Polyphosphonic acid;The polysulfonate acid such as polystyrolsulfon acid;The polysaccharide such as xanthan gum, sodium alginate;Hydroxyethyl cellulose, carboxylic first The cellulose derivatives such as base cellulose.Alternatively, it is also possible to enumerate Polyethylene Glycol, polyvinyl alcohol, polyvinylpyrrolidone, sorbose Alcohol acid anhydride monoleate, the oxyalkylene based polymer with one or more oxyalkylene units etc. are as the example of water-soluble polymer Son.
As the example of dispersing aid, the condensed phosphate such as pyrophosphate, hexametaphosphate etc. can be listed.As anticorrosion The example of agent, can list sodium hypochlorite etc..As the example of antifungus agent, the oxazolines such as oxazolidine-2,5-diketone can be listed Deng.
As the example of anticorrosive, can list surfactant, alcohols, macromolecule, resin, amine, pyridines, four Phenyl salt, benzotriazole, triazole type, four azoles, benzoic acid etc..
As surfactant, nonionic surfactant, anionic surfactant, cationic can be listed Surfactant, amphoteric surfactant.As nonionic surfactant, ether type, Etheric ester type, ester type can be listed, contain Nitrogen type, as anionic surfactant, can list carboxylate, sulfonate, sulfuric acid, phosphate ester salt.It addition, conduct Cationic surfactant, can list aliphatic amine salt, aliphatic quaternary ammonium salt, benzalkonium chloride, benzethonium chloride, pyridine Salt, imidazole salts, as amphoteric surfactant, can list carboxy betaine type, aminocarboxylate, imidazolinium betaine, Lecithin, alkyl amine oxide.
As the example of preservative, sodium hypochlorite etc. can be listed.It addition, as the example of antifungus agent, can list The oxazolines etc. such as oxazolidine-2,5-diketone.
4. about the manufacture method of composition for polishing
The manufacture method of the composition for polishing of present embodiment is not particularly limited, can be by by aluminium oxide and root The various additives added according to expectation stir in the liquid solvents such as water, mix and manufacture.For example, it is possible to by by oxygen Change the various additive such as aluminum and pH adjusting agent to stir in water, mix and manufacture.The most special to temperature when mixing each composition Limit, preferably more than 10 DEG C and less than 40 DEG C, can heat to improve dissolution velocity.It addition, to incorporation time also It is not particularly limited.
The composition for polishing of present embodiment can be one-pack type, it is also possible to be the multicomponent of more than two-component-type Type.During it addition, use the grinding that the lapping device of the feed path with multiple composition for polishing is ground object, can To be ground as follows.I.e., it is possible to the feedstock composition of the previously prepared multiple raw material as composition for polishing, by described Plurality of raw materials compositions is by, in feed path supply to lapping device, mixing described plurality of raw materials compositions in lapping device Close to form composition for polishing, thus be ground.
The composition for polishing of present embodiment can be prepared by the stock solution of dilute with water composition for polishing.Grinding In the case of mill compositions is bi-component, as the mixing of two kinds of feedstock compositions of raw material and the dilution of composition for polishing Order be arbitrary.For example, it is possible to after one feedstock composition being diluted with water, mix, also with another kind of feedstock composition The mixing of two kinds of feedstock compositions can be carried out simultaneously and utilize the dilution of water, or two kinds of feedstock compositions can also mixed It is diluted with water after conjunction.
5. about lapping device and Ginding process
The composition for polishing of present embodiment such as can be at the crystal formation grinding object by metal-oxide Grinding in use under normally used lapping device and grinding condition.As lapping device, it is possible to use common one side grinds Mill apparatus, double-side polishing apparatus.In the case of using single-sided grinding device to be ground, with being referred to as microscope carrier (carrier) Holding instrument keep grind object, limit supply composition for polishing, while the flat board being pasted with grinding pad is pressed against grinding The one side of object, and make flat board rotate, thus the one side grinding object is ground.Enter using double-side polishing apparatus In the case of row grinds, microscope carrier is used to keep grinding object, limit supply composition for polishing, while the flat of grinding pad will be pasted with Plate is pressed against and grinds the two-sided of object, and makes grinding pad and grinding object rotate round about, thus to grinding object The two-sided of thing is ground.When using arbitrary lapping device, all by by grinding pad and composition for polishing and grinding object Fricative physical action between thing and composition for polishing give grind the chemical action that object brings come grinding right As thing is ground.
Grinding load (when grinding to the pressure grinding object load) in grinding condition is not particularly limited, Generally grinding load the biggest, grinding-material and the frictional force ground between object are the highest.Result machining characteristics improves, and grinds Mill speed rises.Grind load and be preferably 2kPa (20gf/cm2More than) and 98kPa (1000gf/cm2) below, more preferably 3kPa(30gf/cm2More than) and 78kPa (800gf/cm2) below, more preferably 3kPa (30gf/cm2More than) and 59kPa (600gf/cm2) below.Grind load within the above range time, not only play the highest grinding rate, and can reduce Grind the breakage of object, the generation of surface defect.
It addition, the linear velocity (grinding pad during grinding and the relative velocity of grinding object) in grinding condition is generally ground Grind the impact of the quantity etc. of the rotating speed of pad, the rotating speed of microscope carrier, the size of grinding object, grinding object.When linear velocity is big, by The frequency touching grinding object in grinding-material uprises, and therefore work between grinding object and grinding-material rubs Wiping power becomes big, and the mechanical abrasive action grinding object is become big.It addition, the heat produced because of friction improves sometimes by grinding The chemical grinding effect brought by compositions.
Being not particularly limited linear velocity, preferably more than 10m/ minute and less than 300m/ minute, more preferably 30m/ are divided More than clock and less than 250m/ minute.Linear velocity within the above range time, the highest grinding rate can not only be reached, and Appropriate frictional force can be given to grinding object.On the other hand, owing to directly producing between grinding pad and grinding object Raw friction does not contributes to grind, the most minimum.
Additionally, the feed speed of the composition for polishing in grinding condition depends on grinds the kind of object, grinding dress The kind put, other grinding condition, preferably for being supplied uniformly across by composition for polishing to grinding object and grinding pad Generally sufficiently feed speed.
The kind of grinding pad is not particularly limited, it is possible to use the various grindings that the physical property such as material, thickness, hardness are different Pad.Such as can use the grinding pad of the various materials such as polyurethane-type, non-woven fabric type, suede type.Contain alternatively, it is also possible to use There are the grinding pad of abrasive particle, any number of grinding pad of the grinding pad without abrasive particle.
Additionally, the composition for polishing of present embodiment can reclaim after using in the grinding grinding object, And reuse in the grinding grinding object.As an example of the method reusing composition for polishing, can list The composition for polishing making to be finished discharged from lapping device is recycled in container so that it is again to lapping device in container Interior circulation and in grinding use method.If recycling composition for polishing, then can reduce as waste liquid discharge The amount of composition for polishing, therefore, it is possible to reduce environmental pressure.Further, since the composition for polishing of use can be reduced Amount, therefore, it is possible to the manufacturing cost needed for the grinding of object is ground in suppression.
When reusing the composition for polishing of present embodiment, can will consume because using in grinding, lose Grinding-material, additive etc. part or all add as composition regulator after reuse.Can be by with arbitrarily Blending ratio mixed grinding material, additive etc. and the mixture that obtains is used as composition regulator, it is also possible to by grinding-material, add Add agent etc. to be directly used alone as forming regulator.Add composition regulator by additional, composition for polishing can be adjusted to It is suitable for the composition reused, suitable grinding can be carried out.Form grinding-material, the concentration of additive contained in regulator It is arbitrary, is not particularly limited, suitably adjust according to size, the grinding condition of container.
(embodiment)
Embodiment described below and comparative example, more specifically the present invention will be described.
First, alumina particle, pH adjusting agent (citric acid), water-soluble polymer (sodium polyacrylate) and pure water is mixed Close, manufacture 13 kinds of composition for polishing.As described in Table 1, surplus is pure water to the content of each composition in composition for polishing.Make For alumina particle, use any one in different 7 kinds of character (alpha-transformation degree, D10, D50, D90, specific surface area).Aluminium oxide granule The alpha-transformation degree of grain, D10, D50, D90, specific surface area are as described in Table 1.It addition, the pH of each composition for polishing is as described in Table 1.
[table 1]
It should be noted that the alpha-transformation degree of alumina particle is filled by the X-ray diffraction using Rigaku Corporation The integrated intensity ratio putting (113) face diffracted ray that Ultima IV measures calculates.It addition, D10, D50, D90 of alumina particle Laser diffraction/scattering formula particle size distribution analyzer the LA-950 using Horiba Ltd measures.Additionally, oxygen The BET specific surface area changing alumina particles uses the specific area measuring device Flow Sorb II of Micromeritics company 2300 measure.
Then, use 13 kinds of composition for polishing to be ground the grinding of object, measure grinding rate, be ground face Surface roughness Rz and be ground the mist degree in face.Grind object and use the substrate (32mm on one side of 7000 series alloys Square shape), there is the substrate (square shape of 60mm on one side) of the aluminum of anodic oxide coating, the substrate of SUS304 Any one in the substrate (square shape of 45mm on one side) of (diameter 25mm's is round-shaped), SUS316L.Grinding group The combination of the kind of compound and substrate is as shown in table 1.
Grinding condition is as follows.
<grinding condition of the substrate of 7000 series alloys>
Lapping device: single-sided grinding device (diameter of flat board: 380mm)
Grinding pad: polyurethane grinding pad
Grinding load: 17.1kPa (175gf/cm2)
The rotating speed of flat board: 90min-1
Grinding rate (linear velocity): 71.5m/ minute
Milling time: 15 minutes
The feed speed of composition for polishing: 26mL/ minute
<there is the grinding condition of the substrate of the aluminum of anodic oxide coating>
Lapping device: single-sided grinding device (diameter of flat board: 65mm)
Grinding pad: polyurethane grinding pad
Grinding load: 3.7kPa (38gf/cm2)
The rotating speed of flat board: 1000min-1
Grinding rate (linear velocity): 108m/ minute
Milling time: 5 minutes
The feed speed of composition for polishing: 15mL/ minute
<grinding condition of the substrate of SUS304>
Lapping device: single-sided grinding device (diameter of flat board: 380mm)
Grinding pad: the fabric grinding pad of nonwoven
Grinding load: 16.7kPa (170gf/cm2)
The rotating speed of flat board: 90min-1
Grinding rate (linear velocity): 71.5m/ minute
Milling time: 5 minutes
The feed speed of composition for polishing: 17mL/ minute
<grinding condition of the substrate of SUS316L>
Lapping device: single-sided grinding device (diameter of flat board: 380mm)
Grinding pad: the fabric grinding pad of nonwoven
Grinding load: 27.9kPa (285gf/cm2)
The rotating speed of flat board: 72min-1
Grinding rate (linear velocity): 57.3m/ minute
Milling time: 10 minutes
The feed speed of composition for polishing: 35mL/ minute
The assay method of grinding rate, surface roughness Rz being ground face and the mist degree that is ground face is as follows.For grinding Mill speed, measures the quality of the substrate before and after grinding and is calculated by its difference.
With regard to grind object the face that is ground surface roughness Rz for, for 7000 series alloys substrate and The substrate of SUS304, surveys with the surface shape measuring instrument ZYGO New View 5032 of Zygo Corporation Fixed, for having the substrate of the aluminum of anodic oxide coating, by the contact pin type surface roughness shape of Tokyo Seimitsu Co., Ltd Shape analyzer SURFCOM 1500DX is measured, for the substrate of SUS316L, the surface manufactured with Co., Ltd.'s Keyemce Profile measuring machine VK-X200 is measured.
It is ground the mist degree in face for grinding object, under fluorescent lighting, uses the substrate after being visually confirmed to be grinding, It is evaluated as " there is no mist degree " by creating the part of the nebulousurine defect situation less than the 10% of substrate surface area, will create white The part of turbid defect is that the situation of more than the 10% of substrate surface area is evaluated as " having mist degree ".
Show the result in table 1.It should be noted that for the substrate of 7000 series alloys and the substrate of SUS304 With the substrate of SUS316L, respectively 3 substrates are ground, grinding rate and the result that surface roughness Rz is 3 substrates Meansigma methods and be shown in table 1.For having the substrate of the aluminum of anodic oxide coating, 1 substrate is ground, by this substrate Grinding rate and surface roughness Rz be shown in table 1.
Result as shown in Table 1 understands, and embodiment 1~4 has ground the surface of substrate, and table with sufficient grinding rate Surface roughness Rz and mist degree are the best.It addition, although embodiment 5 is more than the example of 7.0 for pH, but with sufficient grinding rate pair The surface of substrate is ground.On the other hand, although comparative example 1~8 grinding rate is abundant, but surface roughness Rz and mist degree In one or both bad.

Claims (9)

1. a grinding-material, it is for the grinding grinding object containing at least one in alloy and metal-oxide, Described grinding-material contain alpha-transformation degree be more than 80% and 50% particle diameter in the distribution of the accumulation particle diameter of volume reference be 0.15 μm with Aluminium oxide above and below 0.35 μm.
Grinding-material the most according to claim 1, wherein, the BET specific surface area of described aluminium oxide is 15m2/ more than g and 25m2/ below g.
Grinding-material the most according to claim 1 and 2, wherein, the accumulation particle diameter distribution of the volume reference of described aluminium oxide In 10% particle diameter less than described 50% particle diameter and be below more than 0.10 μm and 0.25 μm.
4. according to the grinding-material according to any one of claims 1 to 3, wherein, the accumulation of the volume reference of described aluminium oxide 90% particle diameter in particle diameter distribution more than described 50% particle diameter and is below more than 0.20 μm and 0.45 μm.
5. a composition for polishing, it contains the grinding-material according to any one of Claims 1 to 4, and pH is less than 7.
6. a Ginding process, it uses the composition for polishing described in claim 5 to containing in alloy and metal-oxide The grinding object of at least one be ground.
Ginding process the most according to claim 6, wherein, in described grinding object, including its surface Dividing and formed by metal-oxide, other parts are formed by alloy.
8. at least 1 during according to the Ginding process described in claim 6 or 7, wherein, described alloy contains aluminum, titanium, ferrum and magnesium Kind.
9. according to the Ginding process described in claim 6 or 7, wherein, described metal-oxide is containing silica, aluminium oxide and oxygen Change at least one in zirconium.
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