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CN1670116A - Polishing composition and polishing method - Google Patents

Polishing composition and polishing method Download PDF

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Publication number
CN1670116A
CN1670116A CNA2005100592518A CN200510059251A CN1670116A CN 1670116 A CN1670116 A CN 1670116A CN A2005100592518 A CNA2005100592518 A CN A2005100592518A CN 200510059251 A CN200510059251 A CN 200510059251A CN 1670116 A CN1670116 A CN 1670116A
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Prior art keywords
polishing
composition
colloid silica
particle diameter
sub
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CNA2005100592518A
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Chinese (zh)
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CN1670116B (en
Inventor
石原直幸
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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
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B25HAND TOOLS; PORTABLE POWER-DRIVEN TOOLS; MANIPULATORS
    • B25DPERCUSSIVE TOOLS
    • B25D17/00Details of, or accessories for, portable power-driven percussive tools
    • B25D17/28Supports; Devices for holding power-driven percussive tools in working position
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B25HAND TOOLS; PORTABLE POWER-DRIVEN TOOLS; MANIPULATORS
    • B25DPERCUSSIVE TOOLS
    • B25D9/00Portable percussive tools with fluid-pressure drive, i.e. driven directly by fluids, e.g. having several percussive tool bits operated simultaneously
    • B25D9/04Portable percussive tools with fluid-pressure drive, i.e. driven directly by fluids, e.g. having several percussive tool bits operated simultaneously of the hammer piston type, i.e. in which the tool bit or anvil is hit by an impulse member
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B25HAND TOOLS; PORTABLE POWER-DRIVEN TOOLS; MANIPULATORS
    • B25DPERCUSSIVE TOOLS
    • B25D9/00Portable percussive tools with fluid-pressure drive, i.e. driven directly by fluids, e.g. having several percussive tool bits operated simultaneously
    • B25D9/06Means for driving the impulse member
    • B25D9/08Means for driving the impulse member comprising a built-in air compressor, i.e. the tool being driven by air pressure
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B25HAND TOOLS; PORTABLE POWER-DRIVEN TOOLS; MANIPULATORS
    • B25DPERCUSSIVE TOOLS
    • B25D2250/00General details of portable percussive tools; Components used in portable percussive tools
    • B25D2250/055Depth properties, e.g. tools having depth indicator or depth control

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

A polishing composition includes colloidal silica. The colloidal silica has such a particle diameter as to satisfy the relationship of the inequality: D<SUB>SA</SUB><=D<SUB>N4</SUB>, between an average primary particle diameter D<SUB>SA </SUB>of the colloidal silica calculated on the basis of a BET method and an average secondary particle diameter D<SUB>N4 </SUB>of the colloidal silica measured by a laser diffraction method. The colloidal silica has the average secondary particle diameter D<SUB>N4 </SUB>of 30 nm or smaller. The polishing composition can inhibit a polishing rate from remarkably decreasing due to clogging in a polishing pad.

Description

Composition for use in polishing and finishing method
Technical field
The invention relates to for example a kind ofly, use used composition for use in polishing in the polishing of polishing pad to substrate, and the finishing method that has used this polishing composition.
Background technology
Generally, in the polishing for substrates such as silicon chips, be accompanied by the high performance of semiconducter device and high density of integrationization and require surface quality to improve, add the increase of demand in recent years, enhancing productivity becomes important problem.For to should problem, for example Japanese patent laid-open 5-154760 communique have proposed to improving the polishing composition that polishing velocity (polishing energy rate) improves.This polishing composition contains colloidal silica sol or silica gel and piperazine, and the weight of the piperazine in the polishing composition is the 10-80% of the SiO2 weight of colloidal silica sol in the polishing composition or silica gel.Polishing pad is pressed on the silicon chip that is fixed on the ceramic block, under this state, on one side polishing composition is supplied on the polishing pad, Yi Bian make silicon chip and polishing pad rotate mutually, and thus the surface of silicon chip is carried out the mirror polish polishing of chemistry and machinery.
Use polishing pad to carry out the polishing of substrate repeatedly, blocking will appear in polishing pad soon, cause the unit time polished amount, be the decline of polishing velocity.Therefore, in order to keep the practical polishing velocity that can enhance productivity, the obstruction that reduces polishing pad is very important.
Summary of the invention
The objective of the invention is to: provide a kind of the inhibition to block the remarkable composition for use in polishing that descends of the polishing velocity that causes, and used the finishing method of this composition for use in polishing by polishing pad.
For reaching above-mentioned purpose, the invention provides a kind of polishing composition that the polishing object is polished with polishing pad that is used in.This polishing composition contains colloid silica.Satisfy inequality: DSA≤DN4 between the average offspring particle diameter DN4 of the average primary particle particle diameter DSA of the colloid silica of calculating based on the BET method and the colloid silica measured by laser inflection method.The average offspring particle diameter DN4 of colloid silica is at 30nm or following.
The present invention also provides a kind of finishing method.This finishing method comprises: the preparation process of above-mentioned polishing composition and use this polishing composition that is mixed with, with polishing pad the polishing object carried out step of polishing.
Description of drawings
Figure 1 shows that the chart that concerns between polishing number of times and polishing velocity.
Embodiment
An example of the present invention below is described.
The silicon chip that is used as the substrate of semiconducter device is made of monocrystalline silicon, its manufacturing passed through from the silicon single crystal piece downcut silicon chip operation, the surface of the silicon chip that downcuts is carried out the operation of polishing, etch etc., silicon chip surface is polished to the operation of mirror status.Polishing pad and polishing composition have been used in the polishing process of silicon chip surface.Polishing pad is made up of supatex fabric, foam, SUEDE FABRIC porous plastids such as (suede).Make this polishing pad contact with slice surfaces, to contact part supply with polishing composition on one side, make thin slice and polishing pad relatively rotate on one side, by like this silicon chip being polished.
Thin slice residue when the chip of the particle in the polishing composition, polishing pad, under cutting etc. has blocked polishing pad, and polishing velocity can significantly descend.Be to reply polishing velocity, must repair or miscellaneous operation such as replacing polishing pad, thereby cause production efficiency to descend.Therefore, in this example,, provide the following polishing composition that can reduce the polishing pad obstruction in order to suppress to block the decline of the polishing velocity that causes by polishing pad.
The necessary composition that the polishing composition of this example contains is a colloid silica.Colloid silica has played the polishing object of the polishing composition of this example of mechanical polishing---the effect of silicon chip.Colloid silica is that a kind of silicon dioxide granule is dispersed in the slurry like material in the dispersion agent.Dispersion agent is so long as liquid, and as organic solvents such as ethanol, water, surfactivity base etc., there is no particular restriction.But, from colloid silica, should not contain this viewpoint of impurity as far as possible, be preferably use and filter out ion exchanged water, distilled water of impurity etc. with strainer.
The average primary particle diameter DSA of colloid silica is the primary particle (primary particle of the silicon dioxide granule in the colloid silica, simple grain) median size calculates by specific surface area and the particle density of measuring based on the specific area measuring method (BET method) of the powder of gas adsorption.The median size of the secondary particle (agglutination particle) that the average aggregate particle size DN4 of colloid silica is the silicon dioxide granule in the colloid silica is measured by laser diffractometry.
For making the single-particle aggegation become agglutination particle, must satisfy inequality: DSA≤DN4 between the average aggregate particle size DN4 of the average primary particle diameter DSA of colloid silica and colloid silica.From avoiding the excessive agglutinative viewpoint of single-particle, it is better to satisfy inequality: DN4≤3 * DSA between average primary particle diameter DSA and the average aggregate particle size DN4.
From the viewpoint of the obstruction that reduces polishing pad, the average aggregate particle size DN4 of the colloid silica in the polishing composition must be preferably at 25nm or following at 30nm or following, is more preferably at 20nm or following.On the other hand, from guaranteeing the viewpoint of practical polishing velocity, average aggregate particle size DN4 is at 5nm or above better.In addition, practical polishing velocity refers to the polishing velocity that can finish silicon wafer polishing in production efficiency in the trouble-free time.
From the viewpoint of the obstruction that reduces polishing pad, the average primary particle diameter DSA of the colloid silica in the polishing composition is preferably at 20nm or following, is more preferably at 15nm or following, and best is at 10nm or following.On the other hand, from guaranteeing the viewpoint of practical polishing velocity, average primary particle diameter DSA is better more than 3nm.
From the viewpoint of the obstruction that reduces polishing pad, the content of silicon dioxide granule is at 50 quality % or followingly better be more preferably at 30 quality % or following in the polishing composition, and best is at 20 quality % or following.On the other hand, from guaranteeing the viewpoint of practical polishing velocity, the content of the silicon dioxide granule in the polishing composition 0.1 quality % or above better, be more preferably 1 quality % or more than, best is 10 quality % or more than.
Colloid silica contains iron, nickel, copper, calcium, chromium or metallic impurity such as their oxyhydroxide, oxide compound sometimes, these metallic impurity meetings may be attached to slice surfaces, after thermal treatment in be diffused in the thin slice, the electrical specification of thin slice is produced worse influence.From suppressing it produces baneful influence to the electrical specification of silicon chip viewpoint, if with the aqueous dispersions that is used in the colloid silica preparation colloid silica in the polishing composition, the content that makes colloid silica is the words of 20 quality %, the content of the metallic impurity in the aqueous dispersions is preferably at 300ppm or following, be more preferably at 100ppm or following, best is at 0.3ppm or following.
At the polishing composition of this example that is used for polished silicon slice, except that colloid silica, also can add at least a in alkali cpd and the sequestrant.With at least a the adding in the polishing composition in alkali cpd and the sequestrant, the dispersion agent in the colloid silica can play the function of the solvent of alkali cpd or sequestrant.
The mechanical polishing of colloid silica can be assisted and promote to alkali cpd by the chemical action of corrosion and etch, plays the effect of polishing promotor.The alkali cpd that can add in the polishing composition can be: potassium hydroxide, sodium hydroxide, saleratus, salt of wormwood, sodium bicarbonate, inorganic alkali compounds such as yellow soda ash, also can be: ammonia, or tetramethylammonium hydroxide, bicarbonate of ammonia, ammonium salts such as volatile salt, also can be: Piperazine anhydrous, piperazine six water and thing, 1-(2-aminoethyl) piperazine, N methyl piperazine, methylamine, dimethylamine, Trimethylamine 99, ethamine, diethylamine, triethylamine, quadrol, (1) thanomin, N-(β-aminoethyl) thanomin, 1, the 6-hexanediamine, diethylenetriamine, amine such as Triethylenetetramine (TETA).Wherein, potassium hydroxide, sodium hydroxide, saleratus, salt of wormwood, sodium bicarbonate, yellow soda ash, ammonia, tetramethylammonium hydroxide, bicarbonate of ammonia, volatile salt, Piperazine anhydrous, piperazine six water and thing, 1-(2-aminoethyl) piperazine and N methyl piperazine are stronger to the mechanical polishing effect that promotes colloid silica, therefore better.The kind of adding the alkali cpd in the polishing composition to can be a kind of also can be more than two kinds.
The alkali cpd of a part may combine with the metallic impurity chelating.But because combining between these alkali cpds and the metallic impurity is not strong, therefore, in the centre of using polishing composition to polish, metallic impurity may be freed from alkali cpd, pollute silicon chip.So the alkali cpd that adds in the polishing composition is more preferably the compound that can not form complex ion with metallic impurity, for example potassium hydroxide, sodium hydroxide, ammonia or tetramethylammonium hydroxide.
Cause silicon chip surface coarse and suppress the viewpoint of the gelation of polishing composition from the excess base compound that suppress to add, the content of alkali cpd is at 10 quality % or following better in the polishing composition, be more preferably at 8 quality % or following, best is at 5 quality % or following.On the other hand, from the viewpoint of the mechanical polishing of the colloid silica of making greater efforts to promote, the content of alkali cpd 0.05 quality % or above better, be more preferably 0.1 quality % or more than, best is 0.5 quality % or more than.
Sequestrant can be caught the metallic impurity in the polishing composition and be formed complex ion, suppresses the pollution of silicon chip.The sequestrant that can add in the polishing composition can be: nitrilotriacetic acid(NTA), ethylenediamine tetraacetic acid (EDTA), hydroxyethylenediamine tetracetic acid, trimethylenedinitrilo-tertraacetic acid, diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, the ethylenediamine tetraacetic ethyl phosphonic acid, ethylenediamine tetraacetic methane phosphonic acid (the four メ チ レ Application ホ ス ホ Application acid of ェ チ レ Application ジ ア ミ Application), ethylenediamine tetraacetic methane phosphonic acid (acid of ェ チ レ Application ジ ア ミ Application テ ト ラ キ ス メ チ レ Application ホ ス ホ Application), diethylenetriamine five ethyl phosphonic acids, diethylenetriamine five methane phosphonic acids, Triethylenetetramine (TETA) six ethyl phosphonic acids, Triethylenetetramine (TETA) pregnancy phosphonic acids, propylene diamine tetrem phosphonic acids, acid such as propylene diamine tetramethyl phosphonic acids also can be a kind of ammonium salts in these acid, sylvite, salt such as sodium salt and lithium salts.The kind of adding the sequestrant in the polishing composition to can be a kind of also can be more than two kinds.
From the viewpoint of the gelation that suppresses polishing composition, the content of sequestrant is at 6 quality % or followingly better be more preferably at 3 quality % or following in the polishing composition, and best is at 1 quality % or following.On the other hand, the viewpoint of the metallic impurity from more seizure polishing compositions, the content of sequestrant 0.001 quality % or above better, be more preferably 0.005 quality % or more than, best is 0.01 quality % or more than.
Can obtain following advantage according to this example.
The average aggregate particle size DN4 of colloid silica is set at greater than average primary particle diameter DSA and at 30nm or following.The single-particle diameter, the agglutination particle diameter that are the colloid silica in the polishing composition are controlled at 30nm or following all lessly.Therefore,, the obstruction of polishing pad can be reduced, the remarkable decline of the polishing velocity that causes can be suppressed to block by polishing pad by the polishing composition of this example.
Above-mentioned example also can carry out following change.
In the polishing composition of above-mentioned example, can also add the additive except that alkali cpd and sequestrant, as sanitas and tensio-active agent.In polishing composition, add anion surfactant, may reduce the obstruction of polishing pad to a greater degree.Because anion surfactant has the effect of the dispersiveness that improves electronegative colloid silica.
The polishing composition of above-mentioned example can also dilute use.From guaranteeing the viewpoint of practical polishing velocity, when the content of the silicon dioxide granule in the polishing composition under the situation of 0.1-50 quality %, dilution ratio 50 times or following better, be more preferably 40 times or below, best is 25 times or below.
The polishing composition of above-mentioned example is except being used for polished silicon slice, also can be used to polish the semiconducter device that constitutes by copper, aluminium or their alloy etc., can also be used to polish the oxide compound substrate that constitutes by the compound semiconductor substrate of the semiconductor chip of silicon-germanium etc., gallium-arsenic, indium-phosphorus etc., by lithium tantalate, Lithium niobium trioxide, sapphire etc. with Wiring construction.Perhaps also can polish the aluminium substrate and the glass substrate of the magnetic recording medium that is used for hard disk drive etc., can also polish the glass substrate and the resin substrate that are used for liquid-crystal display, OLED display etc.
Embodiments of the invention and comparative example below are described.
By in ion exchanged water, adding colloid silica, alkali cpd and sequestrant as required, make the stoste of the polishing composition of experimental example 1-16 and comparative example 1-7.The details of the colloid silica in each stoste, alkali cpd and sequestrant is as shown in table 1.By each stoste is diluted 20 times with ion exchanged water, make the polishing composition of experimental example 1-16 and comparative example 1-7.
Table 1
Colloid silica Alkali cpd Sequestrant
??DSA ??[nm] ??DN4 ??[nm] Content [wt%] Kind Content [wt%] Kind Content [wt%]
??Ex.1 ???5 ???9 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.2 ???8 ???14 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.3 ???9 ???17 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.4 ???8 ???19 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.5 ???12 ???23 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.6 ???14 ???21 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.7 ???16 ???19 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.8 ???19 ???28 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.9 ???9 ???17 ????9 ??TMAH ????2.4 ??TTHA ????0.25
??Ex.10 ???9 ???17 ????18 ??KOH ????1.3 ??TTHA ????0.25
??Ex.11 ???12 ???23 ????18 ??KOH ????1.3 ??TTHA ????0.25
??Ex.12 ???9 ???17 ????18 ??PIZ ??TMAH ????5.8 ????1.0 ??EDTPO ????0.24
??Ex.13 ???12 ???23 ????18 ??PIZ ??TMAH ????5.8 ????1.0 ??EDTPO ????0.24
??Ex.14 ???9 ???17 ????18 ??TMAH ????3.6 ??TTHA ????0.25
??Ex.15 ???9 ???17 ????18 ??TMAH ????2.4 ??- ????-
??Ex.16 ???9 ???17 ????18 ??TMAH ????2.4 ??DTPA ????0.41
??C.Ex.1 ???22 ?? 40 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??C.Ex.2 ???10 ?? 35 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??C.Ex.3 ???35 ?? 70 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??C.Ex.4 ???90 ?? 230 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??C.Ex.5 ???16 ?? 95 ????18 ??TMAH ????2.4 ??TTHA ????0.25
??C.Ex.6 ???35 ?? 70 ????18 ??KOH ????1.3 ??TTHA ????0.25
??C.Ex.7 ???35 ?? 70 ????18 ??PIZ ??TMAH ????5.8 ????1.0 ??EDTPO ????0.24
The average primary particle diameter of the colloid silica shown in " DSA " hurdle of table 1, the FlowSorbII2300 that has been to use micromeritics to produce, and on the basis of having measured specific surface area, calculate.The average aggregate particle size of the colloid silica shown in " DN4 " hurdle has been to use Beckman Coulter, and the N4 Plus Submicron Particle Sizer that Inc. produces measures." KOH " expression potassium hydroxide on " alkali cpd " hurdle, " TMAH " expression hydroxide four potassium ammoniums, " PIZ " represent Piperazine anhydrous." TTHA " expression triethylenetetraaminehexaacetic acid on " sequestrant " hurdle, " EDTPO " expression ethylenediamine tetramethylene phosphonic acid, " DTPA " represent diethylene triaminepentaacetic acid(DTPA).
Use each polishing composition, when silicon chip being polished according to following polishing condition, the thickness of mensuration thin slice centre portions before polishing and after the polishing.Then, the thickness difference before and after the polishing is calculated polishing velocity divided by polishing time (15 minutes).The value of calculating of polishing velocity during the polishing of the 5th group, the 10th group and the 15th group is shown in " polishing velocity " hurdle of table 2.In addition, this value of calculating being divided into the A-E Pyatyi estimates.Concrete, polishing velocity 1.0 μ m/ divide or above be " A ", not to 1.0 μ m/ divide and 0.9 μ m/ divide or above for " B ", not to 0.9 μ m/ divide and 0.8 μ m/ divide or above for " C ", not to 0.8 μ m/ divide and 0.7 μ m/ divide or above for " D ", not to 0.7 μ m/ divide and 0.6 μ m/ divide or above be " E ".This evaluation result is shown in table 2 " polishing velocity " hurdle.In addition, " X " in " polishing velocity " hurdle is illustrated in the 10th group or the 15th group and polishes polishing velocity before end decline to the utmost, polishing interruption afterwards.
Calculate the 10th group with the ratio (percentage) of the 5th group polishing velocity and the 15th group ratio (percentage) with the 5th group polishing velocity.This result is shown in " sustainment rate of polishing velocity " hurdle of table 2.In addition, the sustainment rate of the polishing velocity calculated being divided into the A-D level Four estimates.Concrete speed sustainment rate 90% or above be " A ", not to 90% and 80% or above for " B ", not to 80% and 70% or above for " C ", not to 70% and 60% or above be " D ".This evaluation result is shown in table 2 " sustainment rate of polishing velocity " hurdle.In addition, " X " in " sustainment rate of polishing velocity " hurdle is illustrated in the 10th group or the 15th group and polishes polishing velocity before end decline to the utmost, polishing interruption afterwards.
<polishing condition 〉
Burnishing device: possess single side polishing machine " SPM-15 " that only more mechanical industry company that 4 ceramic discs are arranged makes,
The polishing object: on each ceramic disc with each silicon chip of 46 inches of wax fixed (p-type, crystal orientation<100 〉, the resistivity 0.1 Ω cm of silicon chip or above, less than 100 Ω cm),
Polishing load: 31.5kPa,
The rotating speed of platform: 60min -1(60rpm),
The rotating speed of ceramic disc: 120min -1(120rpm),
Polishing pad: the Suba800 that Rodel company produces, do not repair all the time during use,
The behaviour in service of polishing constituent: with per minute 0.008m 3(8L) feed speed recycle,
Polishing time: per 1 group 15 minutes,
The maintenance temperature of polishing constituent: 40 ℃.
Table 2
Polishing velocity [μ m/min] The sustainment rate of polishing velocity [%]
The 5th group The 10th group The 15th group The 10th group/the 5th group The 15th group/the 5th group
The value of calculating Estimate The value of calculating Estimate The value of calculating Estimate The value of calculating Estimate The value of calculating Estimate
??Ex.1 ????1.05 ??A ???0.95 ??B ??0.90 ??B ???90 ???A ???86 ???B
??Ex.2 ????1.08 ??A ???1.00 ??A ??0.91 ??B ???93 ???A ???84 ???B
??Ex.3 ????1.07 ??A ???1.01 ??A ??0.91 ??B ???94 ???A ???85 ???B
??Ex.4 ????1.11 ??A ???1.00 ??A ??0.90 ??B ???90 ???A ???81 ???B
??Ex.5 ????1.05 ??A ???0.95 ??B ??0.87 ??C ???90 ???A ???83 ???B
??Ex.6 ????1.04 ??A ???0.96 ??B ??0.86 ??C ???92 ???A ???83 ???B
??Ex.7 ????1.04 ??A ???0.94 ??B ??0.79 ??D ???90 ???A ???76 ???C
??Ex.8 ????1.04 ??A ???0.93 ??B ??0.78 ??D ???89 ???B ???75 ???C
??Ex.9 ????1.02 ??A ???0.88 ??C ??0.75 ??D ???86 ???B ???74 ???C
??Ex.10 ????0.81 ??C ???0.81 ??C ??0.81 ??C ???100 ???A ???100 ???A
??Ex.11 ????0.81 ??C ???0.80 ??C ??0.80 ??C ???99 ???A ???99 ???A
??Ex.12 ????1.02 ??A ???0.81 ??C ??- ??X ???79 ???C ???- ???X
??Ex.13 ????1.01 ??A ???0.80 ??C ??- ??X ???79 ???C ???- ???X
??Ex.14 ????1.10 ??A ???1.01 ??A ??0.92 ??B ???92 ???A ???84 ???B
??Ex.15 ????1.07 ??A ???1.01 ??A ??0.90 ??B ???94 ???A ???84 ???B
??Ex.16 ????1.06 ??A ???1.01 ??A ??0.91 ??B ???95 ???A ???86 ???B
??C.Ex.1 ????1.06 ??A ???0.82 ??C ??0.73 ??D ???77 ???C ???69 ???D
??C.Ex.2 ????1.05 ??A ???0.80 ??C ??0.72 ??D ???76 ???C ???69 ???D
??C.Ex.3 ????1.08 ??A ???0.83 ??C ??0.74 ??D ???77 ???C ???69 ???D
??C.Ex.4 ????1.03 ??A ???0.72 ??D ??- ??X ???70 ???C ???- ???X
??C.Ex.5 ????1.01 ??A ???0.62 ??E ??- ??X ???61 ???D ???- ???X
??C.Ex.6 ????0.82 ??C ???0.80 ??C ??0.74 ??D ???98 ???A ???90 ???A
??C.Ex.7 ????1.00 ??A ???- ??X ??- ??X ???- ???X ???- ???X
As shown in table 2, compared with comparative example 1-5, the polishing velocity of embodiment 1-8 and the sustainment rate of polishing velocity have all obtained very excellent evaluation.Can know that from the result polishing constituent of embodiment 1-8 can make polishing pad be difficult to block, suppress the decline of the polishing velocity that the obstruction by polishing pad causes.In addition, can know from the result of the sustainment rate of the polishing velocity of embodiment 8 and comparative example 2, the average agglutination particle diameter DN4 of colloid silica is set in 30nm or following, the decline of the polishing velocity that causes of polishing is further suppressed repeatedly.In addition, can know that the average single-particle diameter DSA of colloid silica is set in 20nm or following, and the decline of polishing velocity has also obtained further inhibition from the result of the sustainment rate of the polishing velocity of embodiment 8 and comparative example 1.Among the embodiment 9, because the content of the colloid silica in the polishing constituent is few slightly, therefore the 15th group polishing velocity descends slightly.Compare with comparative example 6, the polishing velocity of embodiment 10,11 and the sustainment rate of polishing velocity have all obtained very excellent evaluation.Compare with comparative example 7, the polishing velocity of embodiment 12,13 and the sustainment rate of polishing velocity have all obtained very excellent evaluation.Can know from the result of embodiment 3,10 and embodiment 5,11,, further improve the sustainment rate of polishing velocity by using alkali cpd---potassium hydroxide.Can know that from the result of embodiment 3,14-16 the content and the sequestrant of the alkali cpd in the polishing constituent have or not interpolation that the sustainment rate of polishing velocity and polishing velocity be there is no too big influence.
The relation of polishing number of times of embodiment 3,8 and comparative example 3 (group number) and polishing velocity is shown in the chart of Fig. 1.As shown in Figure 1, when polishing velocity was lower than 0.60 μ m/min, the polishing number of times increased successively with the order of comparative example 3, embodiment 8, embodiment 3.Can know that from this result the average aggregate particle size DN4 of colloid silica is more little, polishing pad is difficult to block more, and the decline of being blocked the polishing velocity that causes by polishing pad is fully suppressed.

Claims (11)

1. one kind is being polished the composition for use in polishing that uses in the object polishing with polishing pad to polishing, it is characterized in that, this composition for use in polishing contains colloid silica, the average primary particle diameter DSA of the colloid silica of calculating based on the BET method and the average aggregate particle size DN4 of the colloid silica of measuring by laser diffractometry satisfy inequality: DSA≤DN4, the average aggregate particle size DN4 of colloid silica is below 30nm.
2. composition for use in polishing as claimed in claim 1 is characterized in that, the average aggregate particle size DN4 of colloid silica is below 20nm.
3. composition for use in polishing as claimed in claim 1 is characterized in that, the average aggregate particle size DN4 of colloid silica is more than 5nm.
4. composition for use in polishing as claimed in claim 1 is characterized in that, the average primary particle diameter DSA of colloid silica is below 20nm.
5. composition for use in polishing as claimed in claim 4 is characterized in that, the average primary particle diameter DSA of colloid silica is below 10nm.
6. composition for use in polishing as claimed in claim 1 is characterized in that, the average primary particle diameter DSA of colloid silica is more than 3nm.
7. composition for use in polishing as claimed in claim 1 is characterized in that, the average primary particle diameter DSA of colloid silica and average aggregate particle size DN4 satisfy inequality: DN4≤3 * DSA.
8. composition for use in polishing as claimed in claim 1 is characterized in that polishing composition also contains alkali cpd.
9. composition for use in polishing as claimed in claim 1 is characterized in that polishing composition also contains sequestrant.
10. composition for use in polishing as claimed in claim 1 is characterized in that composition for use in polishing also contains anion surfactant.
11. a finishing method is characterized in that, this finishing method has:
The preparation process of any described composition for use in polishing of preparation claim 1-10 and,
Use this composition for use in polishing that is mixed with, the polishing object is carried out step of polishing with polishing pad.
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