CN101338082A - Modified silicon dioxide sol, preparation method and application thereof - Google Patents
Modified silicon dioxide sol, preparation method and application thereof Download PDFInfo
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- CN101338082A CN101338082A CNA2007100435569A CN200710043556A CN101338082A CN 101338082 A CN101338082 A CN 101338082A CN A2007100435569 A CNA2007100435569 A CN A2007100435569A CN 200710043556 A CN200710043556 A CN 200710043556A CN 101338082 A CN101338082 A CN 101338082A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/146—After-treatment of sols
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
- C09C1/30—Silicic acid
- C09C1/3081—Treatment with organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
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- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention discloses modified silica sol and a preparation method thereof, and polishing solution which contains the modified silica sol. The silicon dioxide surface of the modified silica sol is bonded with silane coupling agent which contains epoxy group. The silica sol, surface active agent and the silane coupling agent which contains epoxy group are mixed, and the product is obtained through modification reaction. In the modified silica sol of the invention, the silicon dioxide particle surface is grafted with epoxy group, which changes the hydrophilicity of the silicon dioxide particle on the one hand and the mutual effect of the silicon dioxide particle and wafer and polishing pad surfaces on the other hand. Based on the improvement of the two properties, the CMP polishing solution prepared with the modified silica sol of the invention has quite high TEOS and BD polishing rate, and has no significant impact on Ta and Cu polishing.
Description
Technical field
The present invention relates to a kind of modified silicon dioxide sol and preparation method thereof, and the application in polishing fluid.
Background technology
As its name suggests, the polishing fluid of chemically machinery polished (CMP) to the polishing mechanism of semiconducter device is: each component in the polishing fluid is removed metal in the semiconducter device and nonmetal by the chemical machinery effect, thereby further plays the effect of planarization.The CMP polishing fluid mainly is made up of three parts: abrasive material, chemical reagent and dispersion medium.Common dispersion medium is water or alcohols material, as ethanol, methyl alcohol, glycerine etc.Chemical reagent is an of paramount importance component in the CMP polishing fluid, and these chemical reagent can be divided into complexing agent (or speed increases auxiliary agent), inhibiter, oxygenant, tensio-active agent, rheology control agent and pH value conditioning agent etc. according to function.Another important component of CMP polishing fluid is an abrasive material, and these abrasive materials are inorganic particulate and organic polymer particles.
Can have a variety ofly as the abrasive material of CMP polishing fluid, mostly be oxide particle or organic granular greatly, for example silicon-dioxide, aluminum oxide, zirconium dioxide, cerium oxide, ferric oxide, granules of polystyrene and/or their mixture etc.These particles have different hardness and surface chemistry, thereby the polishing effect of each base material of semiconducter device is also had nothing in common with each other, and wherein aluminum oxide and silicon-dioxide are to use maximum polish abrasives.
Silicon-dioxide can be divided into aerosil, sedimentation type silicon-dioxide and silicon dioxide gel according to the preparation method.Aerosil and sedimentation type silicon-dioxide mostly are the aggregate of silicon dioxide granule, and its product mostly is SiO 2 powder, when these two kinds of silicon-dioxide are applied in the CMP polishing fluid, often need lot of energy to come the dispersed silicon dioxide particle.Compare with preceding two kinds of silicon-dioxide, silicon dioxide gel have be uniformly dispersed, particle diameter is controlled, surface functional group is more advantage, become the topmost abrasive material of CMP polishing fluid in recent years gradually.
The particle diameter of most of silicon dioxide gel particle is 5-150nm, and its dispersion medium is water, ethanol or other organic solvents.Silica particle surface is rich in oh group, and number of hydroxyl groups reaches 3-8#/nm
2, so silicon dioxide granule has stronger wetting ability and polarity, can stable dispersion in water.The oh group of silica particle surface has stronger activity, can produce ionization under higher pH, also can with some chemical reaction.
Utilize the oh group reaction of some chemical substances and silica particle surface, thereby change the surface chemistry of silicon dioxide granule, this processing mode is called the chemical modification of silicon-dioxide.Silane coupling agent is the most commonly used silicon dioxide particle modified dose, and its modified-reaction is active greatly, reaction conditions is gentle.Have siloxane groups in the silane coupling agent, can with the oh group generation hydrolysis condensation reaction of silica particle surface, thereby make the organic segment on the silane coupling agent be grafted on silica particle surface, change the polarity of silica particle surface.
Abrasive material to polishing fluid carries out special processing, obtains special polishing performance with expectation, and existing partial monopoly has disclosed the research of this respect.The component of a kind of silane coupling agent as polishing fluid disclosed as patent documentation US6646348, forming oligopolymer after this silane coupling agent hydrolysis mixes mutually with abrasive material and other chemical reagent in the polishing fluid, can obtain lower TEOS and the polishing speed of Ta, and obtain glazed surface preferably.Patent documentation US6656241 discloses a kind of silica aggregate of dichlorodimethylsilane modification, and be applied to the Cu polishing fluid, silica aggregate is handled and can be dispersed in the polishing fluid well through modification, and the polishing speed of Cu and Ta with select than the influence that is subjected to the modification processing.Patent US6582623 discloses a kind of polishing fluid of modified abrasive, and silane coupling agent is directly mixed mutually with the abrasive material dispersion, is configured to polishing fluid then, can be applied to polish various crystal column surfaces such as W, Cu.
Summary of the invention
The objective of the invention is to disclose and a kind ofly can produce modification two silicon dioxide gels of remarkably influenced the polishing performance of polishing fluid.
In the modified silicon dioxide sol of the present invention, the surface bond of silicon-dioxide contain the silane coupling agent of cycloalkyl groups.The described silane coupling agent that contains cycloalkyl groups can be selected from γ-glycidoxypropyltrimewasxysilane, γ-glycidoxypropyl dimethoxy silane, γ-glycidoxypropyl triethoxyl silane, γ-glycidoxypropyl diethoxy silane or γ-glycidoxypropyl chlorinated silane etc., and preferable is γ-glycidoxypropyltrimewasxysilane.
Among the present invention, that the particle diameter of described modified silicon dioxide sol is preferable is 10~500nm, and that better is 10~150nm.
Another purpose of the present invention is the preparation method who discloses a kind of modified silicon dioxide sol of the present invention, and it comprises the steps: silicon dioxide gel, tensio-active agent and after containing the silane coupling agent mixing of cycloalkyl groups, carries out modified-reaction and get final product.
In the method for the present invention, the described silane coupling agent that contains cycloalkyl groups can be selected from γ-glycidoxypropyltrimewasxysilane, γ-glycidoxypropyl dimethoxy silane, γ-glycidoxypropyl triethoxyl silane, γ-glycidoxypropyl diethoxy silane or γ-glycidoxypropyl chlorinated silane etc., and preferable is γ-glycidoxypropyltrimewasxysilane.The described dosage of silane coupling agent that contains epoxide group is preferable is the mass percent 0.02~1% of silicon dioxide gel, and better is 0.2~0.5%.
In the method for the present invention, in reactant, also add tensio-active agent, its objective is improve properties-correcting agent in water dispersed and with the consistency of silicon dioxide gel particle.Described tensio-active agent can be selected from anion surfactant, cats product, nonionogenic tenside and zwitterionics.Wherein, preferable is polyacrylic acid, polyoxyethylene glycol, trimethyl-glycine or dodecyl bromination ammonium.What the consumption of described tensio-active agent was preferable is the mass percent 0.01~1% of reaction-ure mixture, and better is mass percent 0.01~0.1%.
In the method for the present invention, modification temperature generally can be 20 ℃ to 100 ℃, and preferable is 20~70 ℃; Modification time generally can be 1 hour to 24 hours, even the longer time so that the reaction fully carry out, preferable is 2~24 hours, better is 2~7 hours; The pH environment of reaction generally can be 1~14, and preferable is 2~12, and better is 7~12, is more conducive to solve the problem of the easy gel of silicon-dioxide under the alkaline condition.The general pH value that adopts regulator solutions such as hydrochloric acid, nitric acid, sulfuric acid, sodium hydroxide, potassium hydroxide, ammoniacal liquor, organic amine in the modifying process.In the preparation process, can add less water.
Further purpose of the present invention is the polishing fluid that openly contains modified silicon dioxide sol of the present invention.Employing contains the silane modifier of epoxide group, after as stated above silica particle surface being carried out modification and handled, can change the wetting ability of silica particle surface.And, behind the silica particle surface grafting epoxide group, can change the interaction between silicon dioxide granule and wafer, the pad interface, thereby can influence the final performance of polishing fluid.This polishing fluid can contain other this area conventional additives.
Agents useful for same of the present invention and raw material are all commercially available to be got.
Positive progressive effect of the present invention is: in the modified silicon dioxide sol of the present invention, the silica particle surface grafting epoxide group, change the wetting ability of silicon dioxide granule on the one hand, changed the interaction of silicon dioxide granule and wafer, pad interface on the other hand.Based on above two kinds of improvement in performance, adopt the CMP polishing fluid of the described improved silica preparation of this patent can have higher TEOS and BD polishing speed, little to Ta, Cu polishing influence simultaneously.
Description of drawings
Fig. 1 is polishing fluid 1~3 that contains the different-grain diameter improved silica among the embodiment 1 and the polishing speed that contrasts polishing fluid 1~3 couple of BD, TEOS, Ta and Cu.
Fig. 2 is a polishing fluid 4~5 and the polishing speed that contrasts polishing fluid 4~5 couples of BD, TEOS, Ta and Cu among the embodiment 2.
Fig. 3 is for containing the polishing speed of the polishing fluid 6~9 couples of BD, TEOS, Ta and the Cu that adopt the improved silica that the modification of different amounts silane modifier makes among the embodiment 3.
Fig. 4 is for containing the polishing speed of polishing fluid 10~12 couples of BD, TEOS, Ta and the Cu of prepared improved silica under the differing temps among the embodiment 4.
Fig. 5 is for containing the polishing speed through polishing fluid 13~15 couples of BD, TEOS, Ta and the Cu of prepared improved silica of differential responses time among the embodiment 5.
Fig. 6 is for containing the polishing speed of polishing fluid 16~18 couples of BD, TEOS, Ta and the Cu of prepared improved silica under the different pH among the embodiment 6.
Fig. 7 is for containing polishing fluid 19~23 that adds the prepared improved silica of different surfaces promoting agent and the polishing speed that contrasts polishing fluid 6~10 couples of BD, TEOS, Ta and Cu among the embodiment 7.
Fig. 8 is for containing the polishing speed of polishing fluid 24~27 couples of BD, TEOS, Ta and the Cu of the prepared improved silica of tensio-active agent that adopts different amounts among the embodiment 8.
Embodiment
Mode below by embodiment further specifies the present invention, but does not therefore limit the present invention among the described scope of embodiments.
In following examples, percentage composition all refers to mass percent except that specifying.
Method embodiment 1
Silicon dioxide gel (30% solid content, particle diameter 10nm) 94.7%, γ-glycidoxypropyltrimewasxysilane (consumption be silicon dioxide gel 0.1%), beet alkali ampholytic surface active agent (consumption be reaction-ure mixture 0.05%), surplus is a water.After said mixture regulated pH=12 with 50%KOH solution,, can obtain modified silicon dioxide sol (10nm) 20 ℃ of following stirring reactions 24 hours.
Silicon dioxide gel (30% solid content, particle diameter 50nm) 94.7%, γ-glycidoxypropyltrimewasxysilane (consumption be silicon dioxide gel 0.2%), beet alkali ampholytic surface active agent (consumption be reaction-ure mixture 0.5%), surplus is a water.After said mixture regulated pH=10 with 50%KOH solution,, can obtain modified silicon dioxide sol (50nm) 40 ℃ of following stirring reactions 6 hours.
Method embodiment 3
Silicon dioxide gel (30% solid content, particle diameter 100nm) 94.7%, γ-glycidoxypropyltrimewasxysilane (consumption be silicon dioxide gel 0.02%), polyacrylic acid tensio-active agent (consumption be reaction-ure mixture 1%), surplus is a water.After said mixture regulated pH=2 with 50%KOH solution,, can obtain modified silicon dioxide sol (100nm) 50 ℃ of following stirring reactions 7 hours.
Method embodiment 4
Silicon dioxide gel (30% solid content, particle diameter 150nm) 94.7%, γ-glycidoxypropyltrimewasxysilane (consumption be silicon dioxide gel 1%), polyglycol surfactants (consumption be reaction-ure mixture 0.1%), surplus is a water.After said mixture regulated pH=7 with 50%KOH solution,, can obtain modified silicon dioxide sol (150nm) 70 ℃ of following stirring reactions 2 hours.
Method embodiment 5
Silicon dioxide gel (30% solid content, particle diameter 500nm) 94.7%, γ-glycidoxypropyltrimewasxysilane (consumption be silicon dioxide gel 0.5%), dodecyl bromination ammonium surfactant (consumption be reaction-ure mixture 0.01%), surplus is a water.After said mixture regulated pH=9,, can obtain modified silicon dioxide sol (500nm) 30 ℃ of following stirring reactions 10 hours.
In following examples, A187 is γ-glycidoxypropyltrimewasxysilane, and CAB-30 is a beet alkali ampholytic surface active agent.
Effect embodiment 1
Contrast polishing fluid 1: silicon-dioxide (10nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Contrast polishing fluid 2: silicon-dioxide (90nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing fluid 1:A187 improved silica (10nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing fluid 2:A187 improved silica (90nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of contrast polishing fluid 1~2 and polishing fluid 1~2 as shown in Figure 1, as we can see from the figure, the polishing fluid that contains the improved silica particle has higher TEOS and BD polishing speed.Especially work as silicon dioxide granule hour (10nm), through after the surface modification treatment, the polishing speed of TEOS and BD is significantly improved.
Polishing fluid 3:A187 improved silica (20nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Contrast polishing fluid 3: silicon-dioxide (20nm) sol particles 7.0%, A187 and CAB-30 reaction mixture 2.46%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, the preparation method of pH=3.0.A187 and CAB-30 reaction mixture is: 2%A187,1%CAB-20, surplus is a water, this solution stirring reaction under 40 ℃, pH=10 got final product in 6 hours.
Polishing fluid 4:A187 improved silica (20nm) colloidal sol type 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Contrast polishing fluid 4: silicon-dioxide (20nm) sol particles 7.0%, A187 reactant 2.46%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, the preparation method of pH=3.0.A187 reactant is: 2%A187, and surplus is a water, this solution stirring reaction under 40 ℃, pH=10 got final product in 6 hours.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of contrast polishing fluid 3,4 and polishing fluid 3,4 as shown in Figure 2.As we can see from the figure, the polishing fluid that contains the silicon dioxide gel after the silane modifier A187 modification has higher BD and the polishing speed of TEOS.
Effect embodiment 3
Silicon-dioxide (20nm) sol particles 7.0% of polishing fluid 5:0.02%A187 modification, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Silicon-dioxide (20nm) sol particles 7.0% of polishing fluid 6:0.2%A187 modification, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Silicon-dioxide (20nm) sol particles 7.0% of polishing fluid 7:0.5%A187 modification, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of polishing fluid 5~7 as shown in Figure 3.As we can see from the figure, among the preparation method, use the consumption of different properties-correcting agent, 0.2%~0.5% consumption especially, the improved silica that obtains all makes polishing fluid have higher TEOS and BD polishing speed.
Effect embodiment 4
Silicon-dioxide (20nm) sol particles 7.0% of polishing fluid 8:20 ℃ of following A187 modification, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Silicon-dioxide (20nm) sol particles 7.0% of polishing fluid 9:40 ℃ of following A187 modification, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Silicon-dioxide (20nm) sol particles 7.0% of polishing fluid 10:70 ℃ of following A187 modification, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of polishing fluid 8~10 as shown in Figure 4.As we can see from the figure, the polishing fluid that contains the silicon-dioxide of modification under the differential responses temperature all has higher TEOS and BD polishing speed.
Effect embodiment 5
Polishing fluid 11: silicon-dioxide (20nm) sol particles 7.0% of reaction following modification in 2 hours, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing fluid 12: silicon-dioxide (20nm) sol particles 7.0% of reaction following modification in 4 hours, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing fluid 13: silicon-dioxide (20nm) sol particles 7.0% of reaction following modification in 7 hours, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of polishing fluid 11~13 as shown in Figure 5.As we can see from the figure, contain the improved silica polishing fluid that the differential responses time makes and all have higher TEOS and BD polishing speed.
Effect embodiment 6
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 14:pH=2, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 15:pH=7, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 16:pH=11, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of polishing fluid 14~16 as shown in Figure 6.As we can see from the figure, different pH values down, especially the improved silica that makes of the above modified-reaction of pH7 makes polishing fluid have higher TEOS and BD polishing speed.
Polishing fluid 17: tensio-active agent is silicon-dioxide (20nm) sol particles 7.0% of modification under the beet alkali ampholytic surface active agent CAB-30, and BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Contrast polishing fluid 5: silicon-dioxide (20nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, CAB-30240ppm, water are surplus, pH=3.0.
Polishing fluid 18: tensio-active agent is silicon-dioxide (20nm) sol particles 7.0% of modification under the aniorfic surfactant polyacrylic acid, and BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Contrast polishing fluid 6: silicon-dioxide (20nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.074%, water is surplus, pH=3.0.
Polishing fluid 19: tensio-active agent is silicon-dioxide (20nm) sol particles 7.0% of modification under the anion surfactant Witco 1298 Soft Acid, and BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.074%, water is surplus, pH=3.0.
Contrast polishing fluid 7: silicon-dioxide (20nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, Phenylsulfonic acid 240ppm, water are surplus, pH=3.0.
Polishing fluid 20: tensio-active agent is silicon-dioxide (20nm) sol particles 7.0% of modification under the nonionic surfactant polyoxyethylene glycol (PEG200), and BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.074%, water is surplus, pH=3.0.
Contrast polishing fluid 8: silicon-dioxide (20nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, PEG200240ppm, water are surplus, pH=3.0.
Polishing fluid 21: tensio-active agent is silicon-dioxide (20nm) sol particles 7.0% of modification under the cationic surfactant dodecyl bromination ammonium (CTAB), and BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.074%, water is surplus, pH=3.0.
Contrast polishing fluid 9: silicon-dioxide (20nm) sol particles 7.0%, BTA 0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, CTAB 240ppm, water are surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of polishing fluid 17~21 and contrast polishing fluid 6~10 as shown in Figure 7.As we can see from the figure, adopt different tensio-active agents in the modifying process, the polishing performance surface of its improved silica is different.But compare with the silicon-dioxide that does not carry out the modification processing, the polishing fluid that contains improved silica always shows as higher TEOS and BD polishing speed.
Effect embodiment 8
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 22:0.01%CAB-30, BTA0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 23:0.10%CAB-30, BTA0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 24:0.30%CAB-30, BTA0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
The silicon-dioxide of modification (20nm) sol particles 7.0% under the polishing fluid 25:0.50%CAB-30, BTA0.1%, H
2O
20.03%, tartrate 0.2%, polyacrylic acid anion surfactant (Bi Ke chemical company) 0.05%, water is surplus, pH=3.0.
Polishing condition: polish pressure 2.0psi, polishing disk rotating speed 70rpm, polishing fluid flow velocity 100ml/min, polishing pad Politex, Logitech PM5 Polisher.
The polishing performance of polishing fluid 22~25 as shown in Figure 8.As we can see from the figure, adopt different amounts in the modifying process, the tensio-active agent of 0.01-0.1% consumption especially, the improved silica that makes can make polishing fluid have higher BD and TEOS polishing speed.
Claims (18)
1. modified silicon dioxide sol is characterized in that: the silica sphere bonding contain the silane coupling agent of cycloalkyl groups.
2. modified silicon dioxide sol as claimed in claim 1 is characterized in that: the described silane coupling agent that contains cycloalkyl groups is γ-glycidoxypropyltrimewasxysilane.
3. modified silicon dioxide sol as claimed in claim 1 is characterized in that: the particle diameter of described modified silicon dioxide sol is 10~500nm.
4. modified silicon dioxide sol as claimed in claim 3 is characterized in that: the particle diameter of described modified silicon dioxide sol is 10~150nm.
5. the preparation method of modified silicon dioxide sol as claimed in claim 1 is characterized in that: with silicon dioxide gel, tensio-active agent and after containing the silane coupling agent mixing of cycloalkyl groups, carry out modified-reaction and get final product.
6. method as claimed in claim 5 is characterized in that: the described silane coupling agent that contains cycloalkyl groups is γ-glycidoxypropyltrimewasxysilane.
7. method as claimed in claim 5 is characterized in that: the described dosage of silane coupling agent that contains epoxide group is 0.02~1% of a silicon dioxide gel quality.
8. method as claimed in claim 7 is characterized in that: the described dosage of silane coupling agent that contains epoxide group is 0.2~0.5% of a silicon dioxide gel quality.
9. method as claimed in claim 5 is characterized in that: described tensio-active agent is anion surfactant, cats product, nonionogenic tenside and zwitterionics.
10. method as claimed in claim 9 is characterized in that: described tensio-active agent is polyacrylic acid, polyoxyethylene glycol, trimethyl-glycine or dodecyl bromination ammonium.
11. method as claimed in claim 5 is characterized in that: the consumption of described tensio-active agent is the mass percent 0.01~1% of reaction-ure mixture.
12. method as claimed in claim 11 is characterized in that: the consumption of described tensio-active agent is the mass percent 0.01~0.1% of reaction-ure mixture.
13. method as claimed in claim 5 is characterized in that: the temperature of described modified-reaction is 20~70 ℃.
14. method as claimed in claim 5 is characterized in that: the time of described modified-reaction is 2~24 hours.
15. method as claimed in claim 14 is characterized in that: the time of described modified-reaction is 2~7 hours.
16. method as claimed in claim 5 is characterized in that: described modified-reaction is to carry out under 2~12 the environment at pH.
17. method as claimed in claim 16 is characterized in that: the pH of described modified-reaction carries out under 7~12 the environment.
18. contain the polishing fluid of modified silicon dioxide sol as claimed in claim 1.
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PCT/CN2008/001259 WO2009006784A1 (en) | 2007-07-06 | 2008-07-01 | A modified silicon dioxide sol, the manufacturing method and use of the same |
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CN101754929A (en) | 2010-06-23 |
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