CN107075309A - Paste compound, rinse composition, substrate polishing method and rinse method - Google Patents

Paste compound, rinse composition, substrate polishing method and rinse method Download PDF

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Publication number
CN107075309A
CN107075309A CN201580047704.7A CN201580047704A CN107075309A CN 107075309 A CN107075309 A CN 107075309A CN 201580047704 A CN201580047704 A CN 201580047704A CN 107075309 A CN107075309 A CN 107075309A
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water
soluble polymer
paste compound
polishing
polymer
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CN107075309B (en
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增田刚
北村启
松村义之
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CMC Materials LLC
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Nihon Cabot Microelectronics KK
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • 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
    • C09G1/04—Aqueous dispersions
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/37—Polymers
    • C11D3/3746—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C11D3/3753—Polyvinylalcohol; Ethers or esters thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Materials Engineering (AREA)
  • Cleaning Or Drying Semiconductors (AREA)

Abstract

Paste compound for chemically mechanical polishing, rinse composition, substrate polishing method and rinse method are provided.The paste compound of the present invention is the paste compound for chemically mechanical polishing, and it contains：Water；Abrasive particles；And one or more water-soluble polymers, the water-soluble polymer includes polyvinyl alcohol structures unit.In the case of there is a kind of water-soluble polymer in the paste compound, the polyoxy alkylidene oxide structure unit and polyvinyl alcohol structures unit of the water-soluble polymer can form the main chain or side chain of the water-soluble polymer.The paste compound of the present invention can be included：PH value regulator；Water-soluble polymer selected from the polymer based on cellulose and the polymer based on polyalkylene oxides；And mist degree modifier.The water-soluble polymer can be present in the paste compound with 1ppm~5000ppm.

Description

Paste compound, rinse composition, substrate polishing method and rinse method
Technical field
Thrown the present invention relates to the technology being polished to semiconductor substrate, and more specifically to for chemical machinery Paste compound, rinsing (rinse) composition, substrate polishing method and the rinse method of light (CMP) etc..
Background technology
The semiconductor substrate of the wafer form used in the production of semiconductor devices is used to undergo various types of Semiconductor devices is provided after photoetching, deposition processes, polishing etc..Many process steps are applied to silicon wafer to manufacture half Conductor device, also, due to that must also improve the yield of semiconductor devices, therefore, the surface quality of silicon wafer is by strict It is required that.Routinely, surface quality is ensured by mirror finish silicon wafer using chemically mechanical polishing (CMP).
When using CMP to polish silicon wafer, typically, silicon wafer is maintained at the carrier for fixing silicon wafer, Then, silicon wafer is put between upper surface panel and lower face plate to (plate has abrasive cloth attached thereto, the grinding Cloth is comprising synthetic resin foaming body or micro suede artificial leather etc.), and then, silicon wafer is being pressed and is being rotated and while carries For including silica (silica, silica), aluminum oxide (alumina, alumina), cerium oxide (ceria, ceria), zirconium oxide (zirconium oxygen Soil, zirconia) or other colloidal particles (particle, grain) dispersion waterborne compositions (hereinafter referred to as slurry compositions Thing) while, polish silicon wafer.
When on silicon carry out CMP when, due in recent years for productivity ratio and surface quality improvement it is increasingly urgent Requirement and along with increase demand, higher performance of semiconductor device level and higher integration density, tasted Examination improves polishing velocity, surface roughness, mist degree (external haze), flatness and (including roll-offs that (roll-off) (end face hangs low (end face sagging)), SFQR and ESFQR) and scratch reduction.
The technology of the surface nature for improving semiconductor substrate has been proposed in the past, for example, Japanese Unexamined Patent is public Open No.2014-38906 (PTL 1) and describe a kind of polishing composition, it includes the polyvinyl alcohol for backbone structure, is used for Suppress particle and be attached to polishing object to be polished on surface.In addition, Japanese Unexamined Patent Publication No.H11-140427 (PTL 2) describe containing the polymer based on straight-chain hydrocarbons with the long chain backbone of carbon and in its side chain with group hydroxyl-lower alkylene Polishing fluid and using the polishing fluid polishing method.
Although these technologies are known, along with the demand for higher semiconductor devices integrated horizontal, need The size of device is even further reduced, so as to need further to improve the surface state of semiconductor substrate, to improve collection Into the yield and other parameters of circuit products.
Citation list
Patent document
PTL 1：Japanese Unexamined Patent Publication No.2014-38906
PTL 2：Japanese Unexamined Patent Publication No.H11-140427
The content of the invention
Technical problem
In view of above-mentioned situation, it is an object of the invention to provide paste compound, rinse composition, substrate polishing method and Rinse method, it is possible to improve the surface state of semiconductor substrate.
The technical scheme solved the problems, such as
According to the present invention there is provided the paste compound for chemically mechanical polishing, it is included：
Water,
Abrasive particles, and
One or more include the water-soluble polymer of polyvinyl alcohol structures unit.
In the present invention, foregoing water-soluble polymer can be one or more respectively comprising poly (oxyalkylene) base oxide The water-soluble polymeric of (polyoxygenated epoxyalkane, polyoxyalkylene oxide) construction unit or polyvinyl alcohol structures unit Thing.In the case of there is a kind of foregoing water-soluble polymer in afore-mentioned slurry composition, the poly (oxyalkylene) of water-soluble polymer Base oxide construction unit or polyvinyl alcohol structures unit can form the main chain or side chain of water-soluble polymer.In addition, water-soluble Property polymer preferably comprises pH value regulator.In addition, the present invention can contain selected from the polymer based on cellulose and based on poly- The water-soluble polymer of the polymer of alkylene oxide (polyalkylene oxide, polyalkylene oxide).The present invention may be used also To contain mist degree modifier.In the present invention, it is preferred to, water-soluble polymer is included with 1ppm~5000ppm.
In addition, according to the second of the present invention the configuration there is provided the rinse composition for polishing substrate, it is included：
Water, and
One or more include the water-soluble polymer of polyvinyl alcohol structures unit.
In the present invention, foregoing water-soluble polymer can be one or more respectively comprising polyalkylene oxides structure The water-soluble polymer of unit or polyvinyl alcohol structures unit.In addition, containing a kind of water-soluble poly in afore-mentioned slurry composition In the case of compound, the foregoing polyalkylene oxides construction unit and polyvinyl alcohol structures unit of water-soluble polymer can be with shapes Into the main chain or side chain of water-soluble polymer.In addition, the present invention can contain selected from the polymer based on cellulose and based on poly- The water-soluble polymer of the polymer of alkylene oxide.The present invention can further contain mist degree modifier.Moreover it is preferred that Water-soluble polymer is included with 1ppm~5000ppm.
In addition, there is provided the polishing method of substrate in the 3rd configuration of the present invention, it includes：
Make the step of afore-mentioned slurry composition is attached to polishing substrate, and
Using the paste compound, the step of being polished with polishing pad to the polishing substrate.
In addition, according to the 4th of the present invention the configuration there is provided the method rinsed to polishing substrate, it is including the use of foregoing The step of rinse composition is rinsed to polishing substrate.
The beneficial effect of invention
According to the present invention, there is provided paste compound, rinse composition, substrate polishing method and rinse method so that has It may improve and be referred to as such as light point defects (LPD), mist degree, mist degree scratch (haze scratch) or mist degree line (haze ) etc. line microcosmic surface scrambling (or, in other words, nanoscale polishing defect).
Embodiment
Although providing the explanation of the present invention following by embodiments of the present invention, the present invention is not It is limited to hereafter described embodiment.In addition, in the present embodiment, nanoscale polishing defect is referred to as a nanometer scratch.This The paste compound or rinse composition of invention include polyalkylene oxides construction unit and poly- respectively comprising one or more The water-soluble polymer of vinyl alcohol construction unit., can be in each group in the first aspect of the water-soluble polymer of present embodiment The water-soluble polymer for being included in compound and forming two kinds of different poly (oxyalkylene) base oxides and polyvinyl alcohol.The present invention's In second aspect, polyalkylene construction unit or polyvinyl alcohol structures unit can be to constitute the graft polymers of main chain or side chain Form be present in each composition.Polyvinyl alcohol structures unit in the present invention is present in the situation in main chain or side chain Under, a part of hydroxyl can be replaced by acyloxy.For acyloxy, preferably using the acyl with two or more carbon atoms Epoxide, and particularly preferably (CH3COO-) group.
Poly (oxyalkylene) base oxide in polyalkylene oxides (polyalkylene oxide) construction unit (polyoxyalkylene oxide) can be that PEO, PPOX or (epoxy ethane-epoxy propane) are total to Polymers, also, the copolymer can be random copolymer or block copolymer.The alkylene oxide of polyalkylene oxides Repetition chain a length of 1~1000, more preferably 2~300 and even more preferably about 3~200.
Constituted respectively in the way of polyalkylene oxides or polyvinyl alcohol solely in the water-soluble polymer of present embodiment In the case of vertical water-soluble polymer, its abundance ratio (abundance ratio) is preferably 5 in terms of mole %:95~40: 60, moreover, from the perspective of nanoscale polishing defect is improved, the abundance ratio can be 10:90 to 30:70 scope It is interior.In addition, the molecular weight of polyalkylene oxides and polyvinyl alcohol can be in the range of 1,000 to 10,000,000.
In addition, in the present embodiment, in the case of polyalkylene oxides and polyvinyl alcohol formation graft polymers, The molecular weight of the graft polymers can cause weight average molecular weight to be 5,000~500,000, and in view of solution (for example Pulp solution) the rheological equationm of state, weight average molecular weight preferably in the range of 10,000~300,000 and more preferably 10, In the range of 000~200,000.
The abundance ratio of polyalkylene oxides main chain and polyvinyl alcohol backbones in the graft polymers of present embodiment with Mole % meter is preferably 5:95~40:60, moreover, from the perspective of nanoscale polishing defect is improved, preferably 10:90 to 30:In the range of 70.
Alkylene oxide (alkylene oxide) main chain of present embodiment can be oxirane (ethylene Oxide), expoxy propane (propylene oxide), or, chain can be formed by its atactic polymerization or block polymerization.Its In, the alkylene oxide is most preferably oxirane.
Add with graft polymers form foregoing water-soluble polymer in the case of, water-soluble polymer it is specific Example can be the water-soluble polymer with formula (1) as shown below.
[chemical formula 1]
In aforementioned formula (1) and (1') in, R represents hydroxyl or the acyloxy with two or more carbon atoms, and a is represented 1~10000 integer, moreover, M1, M2, N1 and N2 represent 0 or bigger real number (grafting rate (grating rate)).Logical In formula (1), R1Represent hydrogen atom or acyl group.In addition, R2And R3Can for it is identical or different and represent have two or more carbon The straight or branched alkyl of atom, and b represents 2~10,000 integer.In addition, aforementioned formula (1) and (1') in R can have Wherein there is hydroxyl and the mixed structure both acyloxy, i.e. wherein acyloxy has been saponified into the structure of hydroxyl.
The instantiation of preferred water-soluble polymer in present embodiment includes having structure as shown below formula (2) (3) water-soluble polymer.In addition, the part or terminal hydroxyl of the hydroxyl of below general formula (2) and (3) can be by acyloxy Substitution.
[chemical formula 2]
[chemical formula 3]
In the present embodiment, amount of the foregoing water-soluble polymer in paste compound can be in 1ppm (0.001 Weight %) in the range of 5000ppm (0.5 weight %).In addition, the polishing speed in order to remain able to assign actual production yield Degree, the addition of water-soluble polymer is preferably in the range of 10ppm~1000ppm.
The paste compound of present embodiment may be embodied in its backbone structure the polymer with tertiary amine structure, and it is used Make the mist degree modifier of the LPD and mist degree on improvement semiconductor substrate surface.
Aforementioned polymer used can be by producing as follows in the present invention：Alkylidene oxidation at least containing oxirane Thing is with having two or more primary amino radicals and/or secondary amino group and the polyamines chemical combination in the molecule thereof containing 4~100 N atoms The addition polymerization of the reactive hydrogen of thing.The weight average molecular weight of the polymer can be in the range of 5,000~100,000.In addition, From water-soluble is provided to be applied to from the perspective of CMP, contained N atomicities are excellent in the polymer of present embodiment Elect 2~10,000 or lower as, moreover, from the perspective of appropriate CMP compatibility and simultaneously improvement mist degree are provided, N Atomicity is preferably 2~1000.In the explanation explained below of present embodiment, the polymer is referred to as alkylidene-poly- alkylene Base oxide amine polymer (alkylene-polyalkylene oxide amine polymer, APOA).
In the present embodiment, assigning the example of the polyamine compounds of backbone structure can include：Polyethylene polyamine, example Such as, trien, tetren, penten or the amine of six ethylidene seven；And, polyalkylene imines, example Such as, the polyethylene imines obtained by the polymerization of aziridine.Aforesaid compound can be used alone, or, can be two kinds Or more plant be applied in combination, so as to form the polyamines backbone structure of present embodiment.
The example for the alkylene oxide being added in aforementioned backbone structure includes oxirane, expoxy propane and epoxy fourth Alkane (butylene oxide), moreover, these alkylene oxides can be used alone or as a variety of mixture therein Use.
The alkylene oxide main chain that can be used in present embodiment is preferably selected from oxirane main chain and/or polypropylene (polypropylene) main chain.The ratio for the oxirane being added in the alkylene oxide in the polymer of present embodiment Rate is 5% or higher and preferably 10% or higher, moreover, by making the ratio be 50%~90%, can assign preferred CMP Process compatibility.In addition, in the case of containing expoxy propane main chain in the present embodiment, from widening process margin (margin) From the perspective of, similarly, comprising amount preferably in the range of 10~20%.
The polymer of present embodiment can easily be manufactured by conventional method.For example, the polymer of present embodiment It can be manufactured by the following：At 100 DEG C~180 DEG C of temperature and 1atm~10atm atmospheric pressure, in base catalyst In the presence of, alkylene oxide is carried out addition polymerization with the initial substance with foregoing polyamine compounds form, (grafting is poly- Close).
It is not particularly limited for alkylene oxide to the addition pattern of the backbone structure with polyamine compounds form, Moreover, in the case of adding the patterns of two or more alkylene oxides wherein, addition pattern can add with block Into or random addition form.The weight average molecular weight of the polymer of present embodiment can be 5000 or higher and be preferably 10000 or higher, furthermore, it is possible to as in 100,000 or lower and 80,000 or lower scope.In weight average molecular weight mistake In the case of low, mist degree can not fully be improved, and in the case where weight average molecular weight is too high, every kind of property is for addition The dependence increase of amount, so that process margin narrows and causes this departing from expectation.
In this manual, backbone structure refers to such structure, and it contains comprising two or more and causes poly- alkylene The constitutional repeating unit of the tertiary amine of the graft polymerization of base oxide group (polyalkylene oxide group).In addition, structure Tertiary amine into the backbone structure of present embodiment preferably comprises N- alkylidenes.The number of C atoms for constituting N- alkylidenes does not have There is special limitation, and the alkylidene of the straight or branched with 2~10 C atomicities can be selected.
The instantiation of the polymer of present embodiment can be illustrated as the polymer represented by below general formula (4), and it passes through The addition polymerization of alkylene oxide and polyethylene polyamine (polyethylene polyamine, polyethylene polyamine) and shape Into, also, in its backbone structure, at least contain tertiary amine structure.
[chemical formula 4]
In aforementioned formula (4), x and y represent positive integer and R4Represent alkylidene.R3And R4Represent that there are two or more The alkylidene of the straight or branched of individual carbon atom, moreover, from the perspective of productivity ratio, cost performance and mist degree is improved, most preferably Ethylidene.In the present embodiment, x can be 2 to 1, and in the range of 000 and preferably in the range of 2 to 20, and y can be 2 In the range of to 10,000 and preferably in the range of 2 to 500.If R4The chain length of O chains is long, then for surface nature Improvement is reduced, and if y is 10,000 or higher, then every kind of property increases for the dependence of addition, so that, for Process margin has harmful effect.R4O can use two or more alkylene oxides to be formed, moreover, in this implementation In the case of mode, different alkylene oxide groups can have block form or random pattern.
In the present invention, the solubility parameters of those compounds gone out given in preceding formulae (1)~(4) be preferably 9~ In the range of 16.In addition, in this manual, solubility parameters (SP) refers to the SP of the water-soluble polymer of the SP values based on monomer Value, it is according to Ueda etc. (" Research on Coatings ", the 152nd phase, in October, 2010, the 41-46 pages) Fedors methods are determined.
In addition, in the present invention it is possible in combination using other water-soluble polymers.The reality of such water-soluble polymer Example may include the homopolymer or copolymer formed by the polymerization of vinyl monomer.The example of such vinyl monomer includes： Water-soluble polymer or copolymer, its be styrene, chlorostyrene, α-methylstyrene, the homopolymer of divinylbenzene and Any combination of their copolymer；Vinyl carboxylates, for example, vinyl acetate, propionate, vinyl butyrate, octanoic acid Vinyl acetate, caprate, vinyl laurate, myristic acid ethene ester, stearic acid vinyl ester, hexanedioic acid vinyl ester, (first Base) vinyl acrylate, Vinyl crotonate, sorbic vinyl ester, vinyl benzoate or vinyl cinnamate；Acrylonitrile, Limonene, cyclohexene；N- vinyl compounds, for example, 2- vinylpyridines, 3- vinylpyridines, 4-vinylpridine, N- second Vinyl pyrrolidone, N- vinyl acetamides or N- vinyl methylacetamides；Cyclic ether vinyl compound, for example, ethene Base furans or 2- vinyl oxo oxinanes；Mono vinyl ether, for example, methyl vinyl ether, ethyl vinyl ether, propyl group second Alkene ether, butyl vinyl ether, amyl group vinyl ethers, 2- ethylhexyl vinyl ethers, octyl vinyl ether, nonyl vinyl Ether, dodecyl vinyl, cetyl vinylether, octadecyl vinyl ether, butoxyethyl group vinyl ethers, spermaceti Base vinyl ethers, Phenoxyethyl vinyl ethers, allyl vinyl ether, Methallyl vinyl ether, glycidyl second Alkene ether, 2- chloroethyl vinyl ethers or cyclohexyl vinyl ether, ethylene glycol monovinyl ether, polyethylene glycol mono vinyl ether, Propane diols mono vinyl ether, polypropylene glycol mono vinyl ether, 1,3- butylene glycols mono vinyl ether, tetramethylene glycol list ethene Base ether, hexamethylene glycol mono vinyl ether, neopentyl glycol mono vinyl ether, trimethylolpropane mono vinyl ether, glycerine list Vinyl ethers, pentaerythrite mono vinyl ether or 1,4-CHDM mono vinyl ether, also, its saponification degree can be appropriate Ground adjusts to improve water solubility.
In addition to foregoing acrylic resin, cellulose derivative can be used in the present invention, for example, Methyl cellulose Element, hydroxyethyl cellulose, hydroxypropyl cellulose or hydroxypropyl methyl cellulose.It is 50,000~2 that mean molecule quantity, which can be used, 000,000 cellulose derivative.
The instantiation for the water-soluble polymer that can be applied in combination can include poly-N-vinyl pyrrolidones, poly- N- PEG/PEO, PLURONIC F-127, alkylene that vinyl acetamide, polyglycereol, molecular weight are 1,000 to 1,000,000 Base oxide ethylenediamine adduct (EO weight ratio：35%, PPG molecular weight：4400, reversal (reverse type)), it is poly- (2- ethylsOxazoline) (mean molecule quantity：500,000), polyvinyl alcohol (mean molecule quantity：200,000), polyacrylic acid is (average Molecular weight：25,000) with polyacrylate (mean molecule quantity：5,000).
In the case of there is alkylidene-polyalkylene oxides amine polymer in the paste compound of the present invention, it adds Dosage can be in the range of 1ppm (0.001 weight %)~5000ppm (0.5 weight %).In addition, in order to remain able to assign The silicon wafer polishing speed of actual production yield, addition is preferably in the range of 5ppm~1000ppm, moreover, from without slurry From the perspective of other regulations of feed composition, more preferably in the range of 5ppm~500ppm.
In addition to foregoing water-soluble polymer, paste compound of the invention can be comprising polishing component, for example, grinding Agent particle, acid or alkali, buffer, catalyst or various types of salt.For abrasive particles used in the present invention, it can be used It is typically used in the abrasive particles of polishing.The example of abrasive particles may include metal, metallic (metallic) or half gold Carbide, nitride, oxide, boride and the diamond of category.
The abrasive particles that can be used in the present invention are preferably capable of polishing substrate surface without introducing on the surface of the substrate The metal oxide of harmful scratch (vestige) or other defects.The preferred embodiment of metal oxide abrasive particle may include oxidation Aluminium, silica, titanium oxide, cerium oxide, zirconium oxide, magnesia, the product formed altogether by them, their mixture and it Chemical mixture.Abrasive particles are typically chosen from aluminum oxide, cerium oxide, silica, zirconium oxide and their group Close.The silica and cerium oxide of silica and particularly colloidal state are preferred abrasive particles, and cabosil is more preferably 's.
The grinding agent of the paste compound of the present invention can be by the way that abrasive particles be dispersed in preferred liquid-carrier And add various types of additives (such as water-soluble polymer) to be formed in the form of dispersion or suspension.In many In the case of, in order to reduce cost of transportation, paste compound is prepared with the concentration higher than concentration for polishing.In following description In, be described the place of the concentration of paste compound each mean it is dense after it is diluted as the polishing fluid for polishing Degree.It is preferred that the example of liquid-carrier can include polar solvent, and preferably water or aqueous solvent, also, wrap in the slurry In the case of abrasive particles, it is the weight of 0.1 weight % or higher and more preferably 0.1 weight %~50 that slurry, which preferably comprises concentration, % abrasive particles (in polishing) are measured, and even further preferably, can be by the abrasive particles of cabosil form with 0.1 The weight % of weight %~10 concentration is added in paste compound.
In view of polishing velocity, the pH of the paste compound of the present invention can suitably be adjusted.In the present invention, In the case where being processed by shot blasting to silicon wafer, the pH of paste compound is preferably in the range of 5~12 and more preferably 7 In the range of~12.
From the perspective of polishing velocity is improved, the primary granule average grain diameter of abrasive particles (particle, grain) is preferred For 0.01 μm~3 μm, more preferably 0.01 μm~0.8 μm and particularly preferably 0.02 μm~0.5 μm.In addition, in primary granule In the case that aggregation is to form secondary granule, from improvement polishing velocity and the similar angle of the surface roughness of reduction polishing object From the point of view of, the average grain diameter of secondary granule is preferably 0.02 μm~3 μm, is more preferably 0.05 μm~1 μm and is particularly preferably 0.03 μm~0.15 μm.In addition, the primary granule average grain diameter of abrasive particles can be by being identified below：Use scanning electron Microscope or transmission electron microscope are observed, the image obtained by analysis and the diameter for measuring particle.In addition, secondary granule Average grain diameter the equal grain diameter measurement of body can be used as using laser scattering method.
In the present invention, the various other additives corresponding to polishing substrate can be used.It may be present in polishing system The preferred embodiment of additive may include amine, ammonium salt, alkali metal ion, film forming agent, complexing agent, surfactant, rheology control Agent, the stabilizer of polymer-type or dispersion, and/or halide ion.Additive can be present in throwing with any preferred concentration In body of light system.
Furthermore, it is possible to amines is added in paste compound, also, the amines can be selected from aliphatic series Amine, cyclammonium, heterocyclic amine, aromatic amine, polyamines and combinations thereof.In a preferred embodiment, the amines can contain There are at least one oxygen atom and at least one polar portion, such as amino acid or amino alcohol, moreover, its instantiation may include two Methyl-prop hydramine (also referred to as 2- dimethylaminos -2- methyl isophthalic acids-propyl alcohol or DMAMP), 2-amino-2-methyl-1-propanol (AMP), 2- (2- aminoethylaminos) ethanol, 2- (isopropylamino) ethanol, 2- (methylamino) ethanol, 2- (diethyl aminos Base) ethanol, 2- (2- (dimethylamino) ethyoxyl) ethanol, 1,1'- [[3- (dimethylamino) propyl group] imino group]-bis- -2- Propyl alcohol, 2- (butylamino) ethanol, 2- (tert-butylamino) ethanol, 2- (diisopropylaminoethyl) ethanol, N- (3- aminopropyls) Morpholine and their mixture.
In the present invention, in addition to amines, ammonium salt can also be added, and it is, for example, possible to use through hydroxylated Amine (such as tetramethyl ammonium hydroxide (TMAH)) and quaternary ammonium compound.
In addition, alkali metal ion can be present in paste compound in the form of the counter ion counterionsl gegenions of various types of salt. The preferred embodiment of alkali metal (alkaline metal) ion can include the monovalence alkali metal (base for belonging to the race of periodic table the 1st metal).The instantiation for the alkali metal ion that can be used can include sodium ion, potassium ion, rubidium ion and cesium ion.It is excellent Select potassium ion and cesium ion, more preferably potassium ion.
In addition, in the present invention, corrosion inhibitor can be used together with polishing system, moreover, the example of corrosion inhibitor can be wrapped Include alkylamine, alkanolamine, azanol, phosphate, lauryl sodium sulfate, aliphatic acid, polyacrylate (salt), polymethylacrylic acid Ester (salt), PVPA ester (salt), polymalic acid ester (salt), poly styrene sulfonate (ester), polyvinylsulfonic acid salt (ester), BTA, triazole, benzimidazole and their mixture.
In addition, in the present invention it is possible to chelating agent and the like is arbitrarily added into paste compound.Chelating agent Example may include：Carbonyls, for example, acetylacetonate；Carboxylate (ester), for example, acetate (ester) or aryl carboxylic acid Salt (ester)；Carboxylate (ester) containing at least one hydroxyl, for example, glycol hydrochlorate (ester), lactate (ester), gluconate (ester) Or gallic acid and its salt；Dicarboxylate (ester), tricarboxylate (ester) and multi-carboxylate's (ester), for example, oxalates (ester), adjacent benzene Diformate (ester), citrate (ester), succinate (ester), tartrate (ester), malate (ester), ethylenediamine tetra-acetic acid Salt (edetate) such as EDETATE SODIUM and their mixture.The preferred embodiment of chelating agent may include dihydric alcohol, trihydroxylic alcohol or The compound of polyalcohol such as ethylene glycol, catechol, 1,2,3,-thrihydroxy-benzene or tannic acid and phosphate-containing (ester).
In the present invention, surfactant, viscosity modifier or flocculating agent arbitrarily can be used together with polishing system.It is viscous The preferred embodiment of degree conditioning agent may include that acrylate (salt) and carbamate containing at least one acrylic units gather Compound.The instantiation of viscosity modifier may include the carboxylate (ester) of low molecule amount and the polyacrylamide amine compounds of HMW Thing, and the preferred embodiment of surfactant may include cationic surface active agent, anionic surfactant, anionic Polyelectrolyte, nonionic surface active agent, amphoteric surfactant, fluorinated surfactant and their mixture.
It can use and be equipped with the polishing system of suitable polishing pad to polish substrate.For polishing pad, for example, can be with excellent Choosing uses braiding or non-woven polishing pad.The instantiation for the preferred polishing pad that can be used can be synthetic resin polishing Pad, moreover, the preferred embodiment of used polymer can include, for example, the fluorination of polyvinyl chloride, polyvinyl fluoride, nylon, carbon is closed Thing, makrolon, polyester, polyacrylate, polyethers, polyethylene, polyamide, polyurethane, polystyrene, polypropylene and it Form product and mixture altogether.
In addition, the paste compound and substrate polishing method of the present invention can be applied not only to silicon substrate, and it can answer Substrate for polishing can be applied, for example, with the polysilicon film, SiO that are formed thereon2Film or metal wiring film TSV substrates, silicon substrate, sapphire substrate, SiC substrate, GaAs substrates or GaN substrate.In addition, the present invention can not only be applied In wherein previously prepared paste compound then by prepared paste compound be supplied to polishing substrate while polishing Pad the method that is polished, and apply also for wherein implementing on so-called platform (on-platen) prepare and prepare (including Diluent and not diluted slurry are supplied on polishing pad and are used for the slurry of substrate polishing in the neighbouring preparation of polishing pad Feed composition) polishing method.
In addition, in the present invention it is possible to use the aqueous molten of the water-soluble polymer represented containing water and by formula (1) Liquid is used as the rinsing solution for the rinsing polishing substrate after polishing.In addition water and the water solubility by formula (1) expression Polymer and various types of additives in addition to abrasive particles are (for example, the polymer based on cellulose, poly- alkylene Oxide polymer, other water-soluble polymers or pH value regulator (such as acid or alkali)) after, the rinsing of present embodiment Composition can be used.
Explanation of the present invention is provided underneath with specific embodiment, although description above is by this hair Bright embodiment is to the invention provides detailed explanation.In addition, for the ease of understanding the present invention, showing following reality Example is applied, moreover, following examples are not intended to limit the present invention in any way.
Embodiment
The paste compound of the present invention is manufactured by the way that the additive with following structural formula is added in pulp solution, Then, its LPD and external haze (DWO mist degrees) are measured.The preparation of paste compound and the polishing of silicon wafer has been illustrated below Condition.
1. the preparation of paste compound (polishing liquid concentrate)
Paste compound with the composition shown in table 1 below is prepared by adding following material respectively：With poly- second The exemplary compounds (80 of the structural formula (2) of enol-PEO graft copolymer form:20 moles of %, Mw=93, 600, degree of gelation：98.5%, main chain：Polyvinyl alcohol, side chain：PEO)；With PEO-polyvinyl alcohol graft copolymerized The exemplary compounds (25 of the structural formula (3) of copolymer form:75 moles of %, Mw=45,000, degree of gelation：92%~99%, Main chain：PEO, side chain：Polyvinyl alcohol)；And/or, with alkylidene-polyalkylene oxides polyamines polymer form Structural formula (4) exemplary compounds (EO:PO=8:2, average nitrogen-atoms numbers：5, Mw=46,000).In addition, embodiment 1 ~3 be embodiments of the invention, and embodiment 4 is comparative example.
Table 1
HEC is hydroxyethyl cellulose.
2. polishing condition
By rinsing 2 minutes at 23 DEG C with hydrogen fluoride (0.5%) come after removing natural oxide film, using foregoing The paste compound prepared in 1, also, the paste compound concentrate is used after being diluted with water 20 times as polishing fluid, Under the conditions of following, to 0.1 Ω cm~100 Ω cm resistivity and<100>Crystal orientation 12 inches of p-type silicon crystalline substances Piece applies polishing.
(1) burnishing device：12 inches of single side polishing machine (SPP800S types, by Okamoto Machine Tool Works Ltd. manufacture)
(2) wafer head：Template way (Template type)
(3) polishing pad：SPM3100 (is manufactured) by Dow Corp.
(4) surface plate rotary speed：31rpm
(5) polishing pad rotary speed：33rpm
(6) polish pressure：3psi=210g/cm2=20.7kPa
(7) slurry feed speed：500mL/ minutes (free-flowing)
After a polish, using SC-1, (containing ratio is 1:1:(29 weight %'s is water-soluble for the ammonia (ammonia) of 4 (volume ratios) Liquid), the solution of hydrogen peroxide (the 31 weight % aqueous solution) and pure water) batch (-type) rinses (batch-rinse) 20 at 23 DEG C Minute, then, further, using SC-200S type Brush Scrubber (by Shibaura Mechatronics Corp. Manufacture), using SC-1, (containing ratio is 1:4:Ammonia (the 29 weight % aqueous solution), hydrogen peroxide (31 weights of 20 (volume ratios) Measure the % aqueous solution) and pure water solution) cleaned at 23 DEG C with PVA brushes, also, rinsed using pure water.
3. measuring method
The surface roughness (mist degree) of the silicon wafer surface after polishing, the DWO haze values are evaluated using DWO haze values It is with scotopia field width raceway groove (DWO) mould with oblique incidence using Surfscan SP2 (being manufactured by KLA-Tencor Ltd.) Formula measurement.Similarly, using Surfscan SP2 (being manufactured by KLA-Tencor Ltd.) with the dark field with oblique incidence Wide raceway groove (DCO) pattern determines used LPD values.The polishing defect of nanoscale is defined as its intensity less than LPD signals The quantity of the signal of intensity, also, in this regard, the scattering strength from surface is partly better than baseline intensity.More specifically, exist In the present embodiment, counted to carry out by the quantity of those signals to observing in setting regions (set region) Evaluate.For identical additive, each measured value is measured at least twice under the same conditions, also, is entered using its average value Row outstanding (A), good (B), the relative evaluation of general (C) or poor (E).
4. result
Evaluation result is shown in table 2 below.
Table 2
Embodiment LPD DWO mist degrees Nanometer scratch
1 C A A
2 C A A
3 C A
4 C B
Note：A：Outstanding, B：Well, C：Typically, D：Difference
In addition, in rinse composition of the manufacture without abrasive particles, moreover, by using the drift after foregoing polishing Cleaning composition is brushed to rinse the polishing substrate of Examples 1 and 2, and simultaneously similarly to LPD, mist degree (DWO) and nanometer When yardstick polishing defect is evaluated, favourable result is obtained.
As described above, according to the present invention it is possible to provide can be while improve mist degree, LPD and nanoscale polishing defect Paste compound and substrate polishing method.
Although description above provides explanation of the present invention using embodiments of the present invention, The invention is not restricted to current embodiment, it can in those of ordinary skill in the art it is conceivable that in the range of (for example with The form of other embodiment) it is changed, augment, replace or omits, moreover, any aspect in those aspects is included in In the scope of the present invention, as long as they demonstrate operation and the effect of the present invention.

Claims (15)

1. for the paste compound chemically-mechanicapolish polished, contain：
Water；
Abrasive particles；And
One or more include the water-soluble polymer of polyvinyl alcohol structures unit.
2. the paste compound of claim 1, wherein, the water-soluble polymer includes poly (oxyalkylene) respectively to be one or more The water-soluble polymer of base oxide construction unit or polyvinyl alcohol structures unit.
3. the paste compound of claim 1 or 2, wherein, there is a kind of water-soluble polymeric in the paste compound In the case of thing, the polyoxy alkylidene oxide structure unit or polyvinyl alcohol structures unit shape of the water-soluble polymer Into the main chain or side chain of the water-soluble polymer.
4. any one of claim 1-3 paste compound, further comprising pH value regulator.
5. any one of claim 1-4 paste compound, containing selected from the polymer based on cellulose and based on poly- alkylene The water-soluble polymer of the polymer of base oxide.
6. any one of claim 1-5 paste compound, further containing mist degree modifier.
7. any one of claim 1-6 paste compound, the water-soluble polymer containing 1~5000ppm.
8. the rinse composition for polishing substrate, contains：
Water；And
One or more polyvinyl alcohol structures units.
9. the rinse composition of claim 8, wherein, the water-soluble polymer includes poly (oxyalkylene) respectively to be one or more The water-soluble polymer of base oxide construction unit or polyvinyl alcohol structures unit.
10. the rinse composition of claim 8 or 9, wherein, there is a kind of water-soluble polymeric in the rinse composition In the case of thing, the polyoxy alkylidene oxide structure unit or polyvinyl alcohol structures unit shape of the water-soluble polymer Into the main chain or side chain of the water-soluble polymer.
11. any one of claim 8-10 rinse composition, containing selected from the polymer based on cellulose and based on poly- Asia The water-soluble polymer of the polymer of trialkylphosphine oxide.
12. any one of claim 8-11 rinse composition, further containing mist degree modifier.
13. any one of claim 8-12 rinse composition, the water-soluble polymer containing 1~5000ppm.
14. the polishing method of substrate, including：
Make the step of any one of claim 1-7 paste compound is attached to polishing substrate；And
Using the paste compound, the step of being polished with polishing pad to the polishing substrate.
15. the method that pair polishing substrate is rinsed, including：
Usage right requires any one of 8-13 rinse composition, the step of being rinsed to polishing substrate.
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