CN101870851B - Chemico-mechanical polishing liquid and polishing method - Google Patents
Chemico-mechanical polishing liquid and polishing method Download PDFInfo
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- CN101870851B CN101870851B CN 201010189611 CN201010189611A CN101870851B CN 101870851 B CN101870851 B CN 101870851B CN 201010189611 CN201010189611 CN 201010189611 CN 201010189611 A CN201010189611 A CN 201010189611A CN 101870851 B CN101870851 B CN 101870851B
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Abstract
The invention discloses a chemico-mechanical polishing liquid, comprising a liquid. Composite abrasive particles are distributed in the liquid and are formed by attaching small particle diameter abrasive particles to the outside of big magnetic polymer particles, wherein the magnetic polymer particles are formed by polymer materials coating the magnetic materials. The invention also discloses a chemico-mechanical polishing method. By adopting the chemico-mechanical polishing liquid , the composite abrasive particles are kept on a soft polishing pad or the surface of a hard polisher by using an auxiliary magnetic field, and the polished surface of the polishing material is polished. When the chemico-mechanical polishing is carried out on materials, such as semiconductor substrates, oxides, metal, and the like, and a Cu/low-k medium during the processing of the semiconductor parts, the technical scheme can improve the polishing rate, control and reduce the collapsing edge of the polishing surface and improve the metal surface quality of a polishing workpiece.
Description
Technical field
The invention belongs to the chemical Mechanical Polishing Technique field, relate to the chemically machinery polished processing of materials such as being applied to semiconductor material (such as monocrystalline silicon piece), oxide compound (such as glass) and metal (such as copper, tungsten, tantalum) and the chemically machinery polished processing technology of semiconductor device manufacturing process (such as shallow trench isolation, the planarization of Cu/ low k dielectric etc.), relate in particular to a kind of chemical mechanical polishing liquid, adopt the preparation method of finishing method and this polishing fluid of this polishing fluid.
Background technology
Chemically machinery polished (Chemical Mechanical Polishing, be called for short CMP), claim again chemical-mechanical planarization (Chemical Mechanical Planarization), it is the combination technique of mechanical mill and chemical corrosion, it is by the chemical corrosion effect of grinding and the polishing fluid (slurry) of ultramicron, in the alternation procedure of chemical membrane and mechanical striping, get on except as thin as a wafer layer of material from polished dielectric surface, realize the processing of ultraprecise flat surfaces.Chemically machinery polished is widely used in the processing of the materials such as semi-conductor (such as monocrystalline silicon piece), oxide compound (such as glass) and metal (such as copper, tungsten, tantalum) and the manufacturing process of semiconductor device (such as shallow trench isolation (Shallow Trench Isolation, STI), the planarization of Cu/ low k dielectric etc.).
Typical CMP comprises the solid-liquid two-phase with polishing fluid, and liquid phase mainly is comprised of chemical compositions such as deionized water and oxygenant, tensio-active agent, buffer reagent, corrosion inhibitors; Solid phase mainly is comprised of abrasive particle, comprises the inorganic oxides such as aluminum oxide, silicon oxide, cerium oxide, and grit size is generally 20～50nm.In CMP (Chemical Mechanical Polishing) process, wafer surface and pad interface are in contact with one another, and the nano level abrasive particle is partially submerged in polishing pad, and part is pressed into the polished section surface, and the disome wearing and tearing occur.If abrasive particle is reunited, stay cut at workpiece surface easily in the course of processing.In the minimum gap of workpiece and polishing pad, the polishing product also scratches the polished section surface easily; The polishing product also may embed in the polishing pad, constantly scratches the polished section surface.
For the problems referred to above, the researchist of Japanese Toshiba semiconductor company of group and JSR group precise electronic research laboratory, reference [1] proposes to utilize inorganic abrasive particle (Al in calendar year 2001
2O
3The composite abrasive grain polishing solution that)/organic filler (resin) forms carries out chemically machinery polished to aluminium, niobium and low-k materials, namely based on the chemical Mechanical Polishing Technique of utilizing composite abrasive grain polishing solution under the soft polishing pad of tradition.As shown in Figure 1, so-called inorganic abrasive particle/molecular Compostie abrasive particles of organic resin grain refers to also add resin particle except conventional abrasive particle in polishing fluid, these two kinds of particles in polishing fluid with surface potential different, effect by electrostatic force, they attract each other together, forming kernel is the macrobead resin, the Compostie abrasive particles of shell parcel small particle size abrasive particle.
The principle of utilizing inorganic/organic composite abrasive grain polishing solution to carry out CMP processing is: during single abrasive grain polishing solution CMP, because the particle diameter of abrasive particle is little, and soft pad interface is more coarse, causes only having a small amount of abrasive particle to contact with wafer; Resin particle is softer, and test shows the removal that can't realize wafer material; When the two formed Compostie abrasive particles, the particle diameter of Compostie abrasive particles was much bigger than alumina abrasive, and the wear particle concentration that is wrapped in the resin particle surface is high, and the chance that contacts with workpiece increases, and material removal effect strengthens.Simultaneously, resin particle has preferably elasticity, plays the effect of miniature polishing pad between polishing pad and workpiece, can avoid abrasive particle, polishing resultant or the foreign matter of conglomerate to the scuffing of wafer, has improved surface quality.Compare with single abradant polishing solution, the polishing speed that this method obtains is higher, and the defective of wafer surface still less.
In patent documentation [a], disclose the grinding Liquid composition that in water-medium, contains silicon dioxide granule, polymer particle and cationic compound, be used for the leveling that precise part is used wafer.Also disclose the chemically machinery polished aqueous dispersions that contains " the compound abrasive particle of organic-inorganic " in the polishing fluid in the patent documentation [b], be used for the polishing of copper film and insulating film.
Increased polymer particle in the polishing fluid of above-mentioned research or patent record, to improve material removing rate and the surface quality of polishing.But these polymer particles do not have magnetic, can't apply magnetic force to it by auxiliary magnetic field and control.
In the traditional C MP technique, the soft polishing pad of being made by polyurethane material is indispensable integral part, and it plays a part to carry polishing fluid and abrasive material to polishing material.In polishing process, because workpiece, abrasive material and polishing pad interact, polishing pad bears periodic shear-stress, constantly weares and teares, and is blocked by abrasive dust.The damage of polishing pad will cause polishing stable variation, Efficiency Decreasing.The polishing pad wear surface can increase production cost but revise technique regularly with a diamond abrasive dish finishing, has reduced simultaneously the work-ing life of polishing pad.On the other hand, because polishing pad is serious in the recoverable deformation of workpiece periphery, cause the workpiece edge stress to concentrate, workpiece is very easy to produce the limit phenomenon of collapsing.It is very difficult to eliminate the workpiece limit defective of collapsing under soft polishing pad environment.
For this reason, Tokyo Univ Japan's production technology research has proposed a kind of chemical Mechanical Polishing Technique based on utilizing composite abrasive grain polishing solution under the hard polisher, reference [2], as shown in Figure 2, this technology has been removed the flexibel polyurethane polishing pad among the traditional C MP, in polishing process, the Compostie abrasive particles that is formed by polymer particle and abrasive particle is held in the microcosmic groove that forms by grinding on hard polisher (the being generally glass material) surface by handle, they play a part numerous miniature polishing pad between workpiece and polisher, workpiece does not directly contact with polisher, thus the various shortcoming of having avoided traditional polishing to be caused by polishing pad.
The hard polisher that Tokyo Univ Japan's production technology research proposes can be made with mechanically resistant materials such as imporous glass or cast irons, the disclosed difference that essence is arranged by the hexagonal boron nitride polishing disk in this and the patent documentation [c].What patent documentation [c] proposed is that porosity is the hexagonal boron nitride stupalith of 20-70%, Young's modulus is 20GPa (concrete experimental example all less than 10GPa), and is all more much smaller than the Young's modulus (about 155GPa) of the Young's modulus (about 55GPa) of glass or cast iron.In other words, low Young's modulus and suitable porosity have just consisted of the suitability of the polishing disk of patent documentation [c] proposition.Up to the present, based on imporosity glass or cast iron quality polishing disk, utilize single SiO
2, Al
2O
3The polishing example of abrasive grain polishing solution yet there are no report.
Under based on the hard polisher, utilize in the CMP (Chemical Mechanical Polishing) process of composite abrasive grain polishing solution, only have those Compostie abrasive particles of " being controlled " by hard polisher microscopic pockets to play scratching removal effect to wafer.Compostie abrasive particles size relatively " pit " is too little, then workpiece may with the direct scratching in polisher surface; Compostie abrasive particles size relatively " pit " is too large, then can't be controlled.Therefore, adapt based on the glossing requirement polisher microscopic appearance (or surface roughness value) of hard polisher and the diameter dimension of Compostie abrasive particles, the polisher surface needs obtain by precise finiss processing.But in the reality polishing, Compostie abrasive particles also weares and teares to the surface generation of hard polisher except the friction workpiece simultaneously.Through the polishing of certain hour, the surface of hard polisher is also more and more smooth smooth, and surface roughness value is more and more less, and polisher reduces gradually to " hold " of Compostie abrasive particles, causes polishing efficiency to reduce.Test shows that generally through about 5 hours polishing, hard polisher surface roughness value will reduce one-level (as changing to Ra1.6 μ m from Ra3.2 μ m), needs again cutting down.Reference [3], Zhou Wenjun etc. is added to metal saponification particle in polishing fluid, attempt to reduce Compostie abrasive particles to the wearing and tearing of polisher, but this method can only mitigate wear speed, can not thoroughly eradicate the problem of existence.
In addition, document shows the auxiliary polishing technology in existing multiple magnetic field:
Y.Tani and K.Kawati[4] proposed the earliest to utilize magnetic liquid to carry out precision machined technology.This technology will fill non magnetic mill abrasive particle (silicon carbide, diameter 4 μ m, volume content 40%) and magnetic liquid, and (diameter is
Fe
3O
4Magnetic particle is blended in the eicosyl naphthyl liquid equably) evenly the bulge of mixed solution be placed in the auxiliary magnetic field.Field gradient floats abrasive particle and contacts with workpiece in being immersed in magnetic liquid.In order to obtain larger polish pressure, Umehara[5] etc. the people in magnetic liquid, put one " buoyancy aid ", under the effect in magnetic field, magnetic liquid supplying " buoyancy aid " is with the effect of power, it is contacted with workpiece, polish by the abrasive particle between " buoyancy aid " and workpiece.Therefore, the characteristics of this finishing method be during without the action of a magnetic field abrasive particle and magnetic particle physical mixed together, abrasive particle then separates with magnetic particle during the action of a magnetic field, the upper strata abrasive particle relies on workpiece one side, lower floor's magnetic particle relies on magnetic field one side.
Kurobe[6] etc. the auxiliary precise polished technology in another kind of magnetic field then proposed.Flexible rubber pad is with the magnetic fluid sealing of copper polishing disk trench bottom, and polishing fluid is placed on the top of rubber pad, separates with magnetic liquid, and workpiece then is dipped in the polishing fluid.Under the effect in magnetic field, magnetic liquid is stressed and be applied on the rubber pad polishing disk, and flexible rubber pad polishing disk stress deformation makes that its shape and workpiece face shape kissing are incompatible to be polished workpiece.Therefore, the characteristics of this finishing method are that abrasive particle is to separate with magnetic particle.
T.Shinmura[7] the magnetic force polishing rule that proposes is that workpiece to be machined is contacted with a lot of magnetic abrasive grains, under the effect of outside magnetic field, the magnetic abrasive grain formation " magnetic brush " that flocks together.When workpiece and " magnetic brush " when relative movement is arranged, phase mutual friction between them, thereby realization is to the polishing of workpiece.Magnetic abrasive grain is the granular solid that a kind of median size is about 150 μ m, the solid particulate that is mixed by a certain percentage by the strong aluminum oxide powder of the large iron powder of susceptibility and grinding capacity or carborundum powder etc.
MRF (magnetorheological finishing, the MRF) technology that W.I.Kordonski etc. [8] proposition utilizes the rheological of Magnetorheologicai polishing liquid in magnetic field to polish.Magnetic flow liquid is that a kind of micron-sized magnetic particle is scattered in the insulation carrier fluid and the non-soliquid that forms, and magnetic particle commonly used generally has carbonyl iron or ferrite particle.Magnetorheologicai polishing liquid then obtains through stirring by add a certain amount of abrasive particle in magnetic flow liquid.The MRF principle: Magnetorheologicai polishing liquid is with the flow through gap of workpiece and dish of moving wall; When applying gradient magnetic, the magnetic particle in the polishing fluid is to the large side shifting of gradient magnetic, and the structure of formation column or cluster-shaped, the Magnetorheologicai polishing liquid hardening, and abrasive particle then floats on the surface of polishing fluid; When very little space that workpiece and moving wall form, the polishing fluid of hardening produces very large shearing force to the zone that workpiece surface contacts with it, thereby the workpiece surface material is removed.
As from the foregoing, the polishing fluid that the auxiliary polishing technology in existing magnetic field adopts comprises pure magnetic particle (carbonyl iron etc.) and two kinds of particles of abrasive particle, magnetic particle and abrasive particle are dispersed in the polishing fluid independently of one another, magnetic particle in the polishing fluid so just causes material removing rate and surface quality restive owing to existed by the effect of gradient magnetic and abrasive particle layering.And in the magnetic force polishing, the iron powder in the magnetic abrasive and abrasive particle are one to react on workpiece surface, like this so that surface quality be a greater impact.
Reference:
[1]Hiroyuki?Yano，Yukiteru?Matsui，Gaku?Minamihaba，Nobuo?Kawahashi，Masayuki?Hattori，High-performance?CMP?Slurry?with?Inorganic/Resin?Abrasivefor?Al/Low?k?Damascene，Mat.Res.Soc.Symp.Proc.2001，671：M2.4.1-M2.4.6
[2]Y.Lu，Y.Tani，K.Kawata，Proposal?of?New?Polishing?Technology?without?Usinga?Polishing?Pad，CIRP?Annals-Manufacturing?Technology，2002，51(1)：255-258
[3]Zhou?Wenjun，Tani?Yasuhiro?and?Kawata?Kenji，Proposal?of?5-Body?FinishingTechnology?for?Long?Tool?Life，7th?International?Conference?on?Progress?ofMachining?Technology，275-280
[4]Y.Tani?and?K.Kawata，Development?of?High-Efficiency?Fine?Finishing?ProcessUsing?Magnetic?Fluid，CIRP?Annals-Manufacturing?Technology，1984，33(1)：217-220
[5]Umehara?N.，Kato.K?and?I.Kanagawa，Magnetic?Fluid?Grinding?of?Ceramic?FlatSurfaces，Electromagnetic?Forces?and?Applications，Elsevier?Science?Publishers，1992，143-146
[6]T.Kurobe?and?O.Imanaka，Magnetic?Field-Assisted?Fine?Finishing，PrecisionEngineering，1984，6(3)，119-124，
[7]T.Shinmura，K.Takazawa，E.Hatano，M.Matsunaga，T.Matsuo，Study?onMagnetic?Abrasive?Finishing，CIRP?Annals-Manufacturing?Technology，1990，39(1)：325-328
[8]I.V.Prokhorov，W.I.Kordonski，L.K.Gleb，G.R.Gorodkin?and?M.L.Levin，NewHigh-precision?Magnetorheological?Instrument-Based?Method?of?PolishingOptics，OSA?OF&T?Workshop?Digest?24，1992，134-136
Patent documentation [a]: grinding Liquid composition, publication number: CN 1517424A;
Patent documentation [b]: the cmp method of semiconductor substrate and chemically machinery polished aqueous dispersions, publication number: CN 1434491A;
Patent documentation [c]: a kind of polishing disk and manufacture method thereof for chemically machinery polished, publication number: CN1174869A;
Summary of the invention
In order to solve above-mentioned technical problem, the purpose of this invention is to provide a kind of chemical mechanical polishing liquid and use the finishing method of this polishing fluid, when Cu/ low k dielectric etc. carries out chemically machinery polished in to the materials such as semiconductor chip, oxide compound and metal and semiconductor device processing procedure, can improve polishing speed, control and reduce collapse limit or improve the metal interconnecting layer flatness of polished surface.
To achieve the above object, the present invention has adopted following technical scheme:
A kind of chemical mechanical polishing liquid comprises liquid, is distributed with Compostie abrasive particles in the liquid, and described Compostie abrasive particles depends on the small particle size abrasive material by macrobead magnetic polymer particles outside and consists of, and described magnetic polymer particles is made of polymer materials coated magnetic material.Wherein, liquid is mainly deionized water, can comprise that also the chemical compositions such as pH adjusting agent, oxygenant, tensio-active agent, buffer reagent, corrosion inhibitor form, and described abrasive material and magnetic polymer particles shared ratio in polishing fluid is 1～20 % by weight.In order to guarantee polishing effect, the particle diameter ratio of magnetic polymer particles and abrasive material is preferably 10～1000: 1, in the polishing fluid mass ratio of magnetic polymer particles and abrasive material be preferably 1: 0.5～1.
A kind of cmp method adopts aforesaid chemical mechanical polishing liquid, utilize auxiliary magnetic field with Compostie abrasive particles being held in soft polishing pad or hard polisher surface, the polished surface of polishing material is polished.
With respect to prior art, the difference of essence is arranged aspect the mechanism of action of the present invention program's Compostie abrasive particles during at the composition of polishing fluid and in polishing.Magnetic particle and polymer materials are combined into magnetic polymer microsphere, and make magnetic polymer microsphere and abrasive particle mutually adsorb the magnetic coupling abrasive particle that forms abrasive particle (shell)/magnetic polymer (nuclear) structure; Like this, magnetic coupling abrasive particle in the polishing fluid is held in the polishing area by handle by magnetic force under the effect of auxiliary magnetic field, namely quilt is being held between soft polishing pad or hard polisher and the workpiece, play the effect of miniature polishing pad, be adsorbed on the abrasive particle on magnetic polymer particles surface by under the polish pressure effect workpiece surface being produced mechanical scratching, remove the corrosion layer of workpiece surface, thereby reach higher polishing velocity and the purpose of better planarization.During the utilizing soft polishing pad, the magnetic coupling abrasive particle quantity that participates in polishing obtains increasing, and material is removed efficient and improved; When using the hard polisher, the magnetic coupling abrasive particle reduces the surface topography dependency of hard polisher, and material is removed efficient and significantly improved.
The below is elaborated to the present invention program:
For abrasive material and magnetic polymer particles
Above-mentioned abrasive material can be enumerated silicon-dioxide (SiO
2), aluminum oxide (Al
2O
3), cerium dioxide (CeO
2), zirconium dioxide (ZrO
2), titanium dioxide (TiO
2) and Manganse Dioxide (MnO
2) etc. inorganic particulate.Preferred silicon-dioxide wherein.Can enumerate colloidal silica particles, pyrogenic silica particle etc. as this silicon-dioxide.And preferred colloidal silica particles wherein.The colloidal silica particles shape can long-term stability be dispersed in water-medium near spherical, is conducive to reduce the scratch to polished surface.Colloidal silica particles can be synthetic by the sol-gel method of the silicate base metal-salt hydrolytic condensations such as water glass; The pyrogenic silica particle can carry out the gas phase hydrolysis method preparation at oxy-hydrogen burner by volatile silicon compound such as silicon tetrachlorides.In order both can to have obtained half sliding surface in when polishing, can keep higher material removing rate again, the median size of silicon dioxide granule is preferably 1～1000nm, more preferably 5～200nm, 20～100nm more preferably.
Above-mentioned magnetic polymer particles is to be that magneticsubstance, shell are the core-shell type magnetic polymer particles of polymer materials by nuclear, as shown in Figure 3; Perhaps ectonexine is that polymer materials, middle layer (nuclear) are the shell of magneticsubstance-core-shell type magnetic polymer particles, as shown in Figure 4.
Wherein polymer materials can be enumerated the carbon chain polymers such as (1) polyethylene, polypropylene, polystyrene, polyhutadiene, (2) heterogeneous chain polymers such as polyethers, polyester, polymeric amide, urethane and polysulfones, the elemento-organic polymers such as (3) silicone resin etc.In these polymer materialss, concrete preferred polystyrene and styrene copolymer, polymethylmethacrylate etc. (methyl) acrylic resin and (methyl) acrylic copolymer, and the multipolymer with these crosslinking structures.
Wherein the magneticsubstance particle can be enumerated the metal series magnetic particle of the metal nanoparticle such as (1) Ni, Co, Fe and alloy (such as Ni-Fe, Co-Fe) thereof, (2) Fe
3O
4, γ-Fe
3O
4, MeFe
2O
4The series such as (Me=Mn, Co, Ni) wustite magnetic particle, (3) nitrided iron series magnetic particle, (4) organic magnetic particle.These magnetic particles can be used mechanical milling method, chemical coprecipitation, thermal decomposition method, two phase process and the adsorption from aqueous solution-methods such as organic phase dispersion method preparation.In these magnetic particles, concrete preferable shape is the Fe of spherical (or needle-like), particle diameter (or major diameter) 5～200nm
3O
4Magnetic particle, when the preparation magnetic compound particles, the magnetic particle of particle diameter is wrapped in polymer particle inside easily like this, avoids magnetic particle to scratch glazed surface.
Above-mentioned magnetic polymer particles can adopt the single stage method that obtains required magnetic polymer particles when preparing magnetic particle, perhaps prepares first the two-step approach that magnetic particle uses appropriate means to be combined with polymkeric substance again.Preferred two-step approach wherein.One of above-mentioned magnetic polymer particles, namely nuclear can adopt the method preparations such as Transfer Radical Polymerization, swelling method, emulsion polymerization, dispersion copolymerization method, suspension polymerization and entrapping method for magnetic particle, shell are the particle magnetic polymer particles of polymkeric substance.One of above-mentioned magnetic polymer particles, be that ectonexine is that polymkeric substance, middle layer are the magnetic polymer particles of magnetic particle, can adopt the two-stage polymerization method: the first step prepares first the polymer particle with functional group of single dispersion, good stability, adopts chemical reduction method or interphase precipitate method that inorganic particle is connected on the polymer beads sub-surface again; Second step is in the polymer beads sub-surface trigger monomer polymerization that is coated with magnetic particle and to wrap up seed and make ectonexine be that polymkeric substance, middle layer are the magnetic polymer particles of magnetic particle.
In order the time both to have obtained more level and smooth surface in polishing, can keep higher material removing rate again, the median size of above-mentioned magnetic polymer particles is preferably 500～20000nm, more preferably 1000～15000nm, 3000～10000nm more preferably.
The saturation magnetization of above-mentioned magnetic polymer particles is preferably 5～100emu/g, more preferably 10～50emu/g, 20～30emu/g more preferably.
For Compostie abrasive particles
The abrasive material that contains in the above-mentioned polishing fluid and magnetic polymer particles, Compostie abrasive particles form with shell (abrasive material)/nuclear (magnetic polymer particles) type structure exists, as shown in Figure 5, namely abrasive material and magnetic polymer particles form particle not segregative, that be combined in one in polishing fluid.
Above-mentioned Compostie abrasive particles can be in the water system of certain pH scope, because abrasive material is larger with the absolute value gap that magnetic polymer particles has the different Zeta potentials of symbol or Zeta potential, abrasive material is adsorbed on the magnetic polymer particles surface by electrostatic force and realizes.In addition, Zeta potential jack per line when abrasive material and magnetic polymer particles, when perhaps the absolute value of Zeta potential is more or less the same, can use aniorfic surfactant or cationic surfactant, change the Zeta potential value of abrasive material or magnetic polymer particles, preferably adopt promoting agent to change the method for magnetic polymer particles Zeta potential.
Above-mentioned cationic surfactant can be enumerated amine salt type, quaternary ammonium salt cationic type tensio-active agent.Preferred quaternary ammonium salt cationic type tensio-active agent, more preferably polymer quaternary ammonium salt, particularly preferably Poly Dimethyl Diallyl Ammonium Chloride.Above-mentioned aniorfic surfactant can be enumerated sulfonate type, sulfuric ester and phosphate type aniorfic surfactant.Preferred sulfonate type cationic surfactant, more preferably polymer sulfonate, particularly preferably sodium polystyrene sulfonate.
For so that the Zeta potential of the magnetic polymer particles after the modification enough guarantee by electrostatic force absorption abrasive material, thereby form the Compostie abrasive particles of shell/caryogram structure, the consumption of above-mentioned tensio-active agent, amount according to magnetic polymer particles is determined, reaching capacity on the magnetic polymer particles surface with tensio-active agent is adsorbed as principle, in the amount of magnetic polymer particles under 100 % by weight bases, below preferred 10 % by weight, more preferably 5～0.01 % by weight, particularly preferably 2～0.05 % by weight.
Preparation for polishing fluid
Polishing fluid of the present invention, different according to the polishing object, can select different pH values.The pH value of acid polishing slurry is preferably 1～6, and more preferably 2～5, be particularly preferably 3～4.The pH value of alkalescence polishing liquid is preferably 7～13, and more preferably 8～12, be particularly preferably 9～11.The pH value of above-mentioned polishing fluid can be used pH adjusting agent.As pH adjusting agent, can enumerate the mineral acids such as nitric acid, hydrochloric acid, sulfuric acid, the organic acids such as acetic acid, oxalic acid, oxysuccinic acid, phenylformic acid, Whitfield's ointment, the alkali metal hydroxides such as sodium hydroxide, potassium hydroxide, and ammoniacal liquor, water-soluble organic amine etc.
Polishing fluid of the present invention can add various additives as required.Can enumerate oxygenant, dispersion agent etc.As oxygenant, can enumerate hydrogen peroxide and derivative thereof, urea peroxide, peroxyformic acid, Peracetic Acid, persulphate, Periodic acid and salt thereof etc.As dispersion agent, can enumerate the tensio-active agents such as aniorfic surfactant, cationic surfactant, nonionic surface active agent.Wherein preferred nonionic surface active agent can be enumerated as polyvinyl alcohol, fatty alcohol-polyoxyethylene ether, polyvinyl alcohol and polystyrene block copolymer, polyoxyethylene glycol, polypropylene glycol, polyoxyethylene alkyl amine etc.
The compound method of polishing fluid of the present invention, preferred method has: first other components of the polishing fluid except magnetic polymer particles are mixed in proportion and through ultrasonic stirring, add again magnetic polymer particles or adding through surfactant-modified magnetic polymer particles, make finally by ultrasonic stirring.
Polishing fluid of the present invention also can adopt magnetic polymer particles and commercially available chemical mechanical polishing liquid to be mixed to get.Can enumerate alkaline silicon dioxide (SiO
2) polishing fluid is mixed to get acidic alumina (Al with the magnetic polymer particles with positive Zeta potential
2O
3) abrasive grain polishing solution is mixed to get with the magnetic polymer particles with negative Zeta potential.
For auxiliary magnetic field
Finishing method of the present invention is provided with auxiliary magnetic field.Magnetic compound particles in the polishing fluid being held on polishing pad or the polisher, promotes the material removing rate of polishing at quilt under the effect of magnetic force, improves surface quality.
Above-mentioned auxiliary magnetic field can be produced by permanent magnet, is perhaps produced by electromagnetic generator.Above-mentioned permanent magnet can list natural magnetite and artificial magnet steel, preferably selects artificial magnet steel.Artificial magnet steel can list ndfeb magnet, SmCo magnet, alnico magnet, ferrite magnet etc., preferably selects ndfeb magnet.The cross-sectional shape of permanent magnet can list circle, annular, square, rectangle etc., and the molectron of different cross section shape.Above-mentioned electromagnetic generator can be enumerated single stem stem or multicore post direct current, alternating electromagnetic generating unit.The cross-sectional shape of generating unit can list circle, annular, square, rectangle etc.
The auxiliary magnetic field device is arranged on below, top and other positions that needs of polishing disk, is guarantee effect effect and convenient layout, and preferred arrangements is below polishing disk.The zone of action of above-mentioned auxiliary magnetic field can be enumerated around polishing area, the polishing area and other zones that need, and is guarantee effect effect and convenient the layout, and the preferred zone of action is polishing area.
For burnishing device
Finishing method of the present invention, the equipment that uses, such as Fig. 6, shown in Figure 7, comprise sample tray, the sample tray of fixing and the polished workpiece of clamping pressurizing device, be affixed with the polishing disk of soft polishing pad or be fixed with the polishing disk, auxiliary magnetic field device, polishing fluid feedway etc. of hard polisher.
Above-mentioned soft polishing pad can be enumerated have felt mattress, porous synthetic leather pad, polyurethane foam solidify pad, without the weavy grain urethane pad.Above-mentioned hard polisher material can be enumerated glass, pottery, cast iron, iron alloy, non-ferrous metal etc., the hard polisher of preferred glass, ceramic material.The glass material of above-mentioned polisher can be enumerated soda-lime glass, magnalium glass, potassic glass, lead glass, borosilicate glass and silica glass etc., preferred soda-lime glass, silica glass, more preferably soda-lime glass.The ceramic material of above-mentioned polisher can be enumerated aluminum oxide, zirconium white, silicon nitride, silicon carbide, boron nitride etc., preferential oxidation aluminium, zirconia ceramics, more preferably alumina-ceramic.Above-mentioned auxiliary magnetic field device can be enumerated magnetic field of permanent magnet generating unit, electromagnetic field generator.
For glossing
Object as the auxiliary chemically machinery polished in magnetic field of the present invention, the material of the polished thing take the precise part substrate as representative, can enumerate semi-metal or the metals such as silicon, aluminium, copper, tungsten, tantalum, the oxide compounds such as silicon-dioxide, aluminum oxide, silicon nitride, the semiconductor compound such as gallium arsenide, gan, the advanced low-k materials such as the silicon oxide that fluorine mixes, polyamide-based resin.
Method as the auxiliary chemically machinery polished in magnetic field of the present invention, preferably, polished thing take the precise part substrate as representative is pasted or is clamped on the sample tray, sample tray is pressed to soft polishing pad or hard polisher under the effect of polish pressure, sample tray and polishing disk rotate respectively, it is identical that the rotating speed of sample tray and polishing disk is preferably big or small direction, the polishing fluid feedway then is fed to soft polishing pad with magnetic coupling abrasive grain polishing solution of the present invention or has on the hard polisher, magnetic coupling abrasive particle in the polishing fluid is subjected to the magneticaction of auxiliary magnetic field, quilt is being held in polishing area, promote the mechanical scratching effect in the chemically machinery polished, promote material removing rate, improve the surface quality of polished thing.
The method of the chemically machinery polished that magnetic field of the present invention is auxiliary, the rotating speed of sample tray and polishing disk is 20～200rpm, preferred 40～100rpm.And fixedly precise part is 0.5kPa～100.0kPa with the sample tray of substrate to the pressure of polishing disk, preferred 10.0kPa～50.0kPa, more preferably 15.0kPa～30.0kPa.
The method of the chemically machinery polished that magnetic field of the present invention is auxiliary, the polishing fluid feedway is preferably 20～500ml/min, more preferably 100～300ml/min to the feed rate of polishing disk supply magnetic coupling abrasive grain polishing solution.
In addition, the method for the chemically machinery polished that magnetic field of the present invention is auxiliary, the magneticstrength on polishing pad or polisher surface is 5～1000mT, is preferably 10～500mT, more is preferably 30～100mT.
The present invention is owing to adopted above technical scheme, when Cu/ low k dielectric etc. carries out chemically machinery polished in to the materials such as semiconductor chip, oxide compound and metal and semiconductor device processing procedure, can improve polishing speed, control also reduces the polished surface limit of collapsing, and improves the metallic surface quality of polishing workpiece; Especially when adopting the hard polisher to carry out chemically machinery polished, not only can avoid the polished surface limit of collapsing, also can significantly improve material removing rate; Simultaneously, can also greatly reduce the surface topography dependency to polishing pad or polisher, the work-ing life of improving polishing pad or polisher.
Description of drawings
Fig. 1 is the formation synoptic diagram of Compostie abrasive particles in the prior art;
Wherein, 1 is the Al of positively charged
2O
3Abrasive particle, 2 is electronegative organic resin microballoon, 3 is Compostie abrasive particles.Fig. 2 is based on the CMP synoptic diagram that utilizes composite abrasive grain polishing solution under the hard polisher in the prior art;
Wherein, 1 is sample tray, and 2 is polish pressure, and 3 is workpiece, and 4 is polymer microballoon, and 5 is free abrasive, and 6 is the glass polishing device.
Fig. 3 is one of structural representation of magnetic polymer particles of the present invention;
Fig. 4 be magnetic polymer particles of the present invention structural representation two;
Wherein, 1 is magneticsubstance, and 2 is polymer materials.
Fig. 5 is Compostie abrasive particles structural representation of the present invention.
Wherein, 1 is magneticsubstance, and 2 is polymer materials, and 3 is abrasive particle.
Fig. 6 is the CMP synoptic diagram that the present invention is based on the hard polisher;
Fig. 7 is the CMP synoptic diagram that the present invention is based on soft polishing pad;
Wherein, 3 is abrasive particle, and 11 is magnetic polymer particles, and 12 is permanent magnet, and 13 is sample tray, and 14 is cere, and 15 is workpiece, and 16 is the hard polisher, and 17 is polishing disk, and 18 is soft polishing pad.
Embodiment
The following specific embodiments of the present invention is to make a detailed explanation.
A kind of chemical mechanical polishing liquid comprises liquid, is distributed with Compostie abrasive particles in the liquid, and described Compostie abrasive particles depends on the small particle size abrasive material by macrobead magnetic polymer particles outside and consists of, and described magnetic polymer particles is made of polymer materials coated magnetic material.Concrete preparation and the polishing experiments of polishing fluid are compared as follows:
1. the preparation of magnetic particle and magnetic polymer particles
1-1, Fe
3O
4The preparation of nanoparticle
FeCl with 0.196 mole
36H
2O and 0.098 mole of FeSO
46H
2O places the three-necked flask of 5000mL, add again deionized water dissolving, the mechanical stirring of 2000mL and pass into high-purity argon gas except the oxygen in anhydrating, argon gas atmosphere is warming up to 80 ℃, adding 40mL massfraction is 25% ammoniacal liquor, splash at last 20mL oleic acid, continue to be warming up to 96 ℃ of reactions after 0.5 hour, separation, washing, drying obtain oleic acid parcel, median size is about the black Fe of 8nm
3O
4Nanoparticle.
The preparation of 1-2, magnetic polystyrene particle (magnetic PS)
With 8 gram magnetic Fe
3O
4Nanoparticle is dissolved in 200mL vinylbenzene, 4mL vinylformic acid and the 1.0mL p-divinyl benzene, adds 1.0 gram Diisopropyl azodicarboxylates behind the ultrasonic mixing, stirs and makes its dissolving, gets the brownish black mixed solution; 8 gram polyvinylpyrrolidones and 2000mL dehydrated alcohol are added in the three-necked flask; be warming up to 70 ℃ after dissolving, mechanical stirring, the high-purity argon gas deoxygenation; and the brownish black mixed solution joined in the three-necked flask; reaction is 48 hours under constant temperature, the argon shield, and centrifugation, washing, drying obtain the Magnetic Polystyrene Microsphere that median size is about 5 μ m.
The preparation of 1-3, magnetic polymethyl methacrylate particle (magnetic PMMA)
The 1000mL aqueous solution that adds 15 gram polyvinyl alcohol in polymerization reaction kettle is 80 ℃ of lower constantly stirrings; With 10 gram Fe
3O
4Nanoparticle is scattered in the organic carrier fluid of 30mL methyl methacrylate, obtains oiliness Fe
3O
4Magnetic fluid; In the oil phase container for storing liquid, add 25 gram oiliness Fe
3O
4The oil-phase solution that magnetic fluid, 70mL methyl methacrylate, 5mL divinylbenzene and 4 gram benzoyl peroxides form stirs and forms homodisperse oil phase fluid; Keeping the pressure of oil phase container for storing liquid is 0.1Mpa, and the oil phase fluid enters by the jet nozzle jet flow that aqueous phase forms uniform drop in the polymerization reaction kettle; 80 ℃ of reactions of constant temperature 1 hour cool to 60 ℃ of slakings 2 hours again, through cooling, magnetic resolution, washing, obtain the magnetic polymethyl methacrylate particle that median size is about 10 μ m.
2. the modification of magnetic polymer particles
2-1, magnetic polystyrene particle (magnetic PS) modification
The Zeta potential that utilizes Zeta-Meter System 3.0+ potentiometer to detect to obtain the magnetic polystyrene particle that makes by the 1-2 method is-35mV.
Getting the particle diameter that makes by the 1-2 method is the polystyrene magnetic particle 30g of 5 μ m, places the beaker of 1000mL, adds the 500mL deionized water, fully stirs.In polystyrene magnetic particle solution, add the 0.3g Poly Dimethyl Diallyl Ammonium Chloride, ultrasonic stirring again.Will be through ultrasonic agitation, the solution centrifugation 10min under 4000rpm after reaching adsorption equilibrium, remove supernatant liquor, obtain the polystyrene magnetic particle through the modification of cats product Poly Dimethyl Diallyl Ammonium Chloride, its Zeta potential is+31mV.2-2, magnetic polymethyl methacrylate particle (magnetic PMMA) modification
The Zeta potential that utilizes Zeta-Meter System 3.0+ potentiometer to detect to obtain the magnetic polymethyl methacrylate particle that makes by the 1-3 method is-28mV.
Getting the particle diameter that makes by the 1-3 method is the magnetic polymethyl methacrylate particle 40g of 10 μ m, places the beaker of 1000mL, adds the 500mL deionized water, fully stirs.In the polymethylmethacrylate particle solution, add the 0.4g Poly Dimethyl Diallyl Ammonium Chloride, ultrasonic stirring again.Will be through ultrasonic agitation, the solution centrifugation 10min under 4000rpm after reaching adsorption equilibrium, remove supernatant liquor, obtain the polymethylmethacrylate particle through the modification of cats product Poly Dimethyl Diallyl Ammonium Chloride, its Zeta potential is+29mV.
3. the preparation of single abrasive grain polishing solution or selection
3-1, single SiO
2Abrasive grain polishing solution (model is called for short S1)
The silicon-dioxide powdery of getting 20 gram particles and directly be 30～40nm is abrasive material, and adding 2 gram polyvinyl alcohol is surface dispersant, under the stirring of 1500rpm, adds deionized water 78 grams, makes the single SiO of 100 grams
2Abrasive grain polishing solution.Regulate polishing fluid pH value to 10.5 with KOH.
3-2, commercially available silicon substrate polishing fluid
The silicon substrate polishing fluid of selecting Tianjin Jingling Electronic Material Technology Co., Ltd to produce, model FA/OS8010, SiO
2Particle diameter 30～40nm, pH value 10.0～12.0, SiO
2Content＞35%.
3-3, commercially available multilayer wiring copper polishing fluid
The multilayer wiring copper polishing fluid of selecting Tianjin Jingling Electronic Material Technology Co., Ltd to produce, model FA/OC6201, SiO
2Particle diameter 15～20nm, pH value 10.0～12.0, SiO
2Content＞40%.
4. the chemically machinery polished preparation of magnetic coupling abrasive grain polishing solution (polishing fluid of the present invention)
With single SiO
2Abrasive grain polishing solution or FA/O S8010 silicon substrate polishing fluid, modification magnetic polymer particles join in the flask that volume is 1000mL by different ratios, fully stir.Add again a certain amount of deionized water, and regulate the pH value with the KOH aqueous solution, guarantee that at last the polishing fluid of allotment is settled to 1000mL, obtain magnetic coupling abrasive grain polishing solution [1]～[4] that polished silicon slice is used.The proportioning of various polishing fluids is shown in Table 1.
Table 1
FA/O C6201 multilayer wiring copper polishing fluid, modification magnetic polymer particles are joined in the flask that volume is 1000mL by different ratios, fully stir.Add again a certain amount of oxygenant, deionized water, and regulate the pH value with the KOH aqueous solution, guarantee that at last the polishing fluid of allotment is settled to 1000mL, obtain magnetic coupling abrasive grain polishing solution [5]～[6] of copper wiring usefulness.The proportioning of various polishing fluids is shown in Table 2.
Table 2
5. polishing experiments is routine
Silicon substrate or copper sheet are fixed on polishing machine (Shenyang Kejing Equipment Manufacture Co., Ltd. with paraffin, the UNIPOL-1260 type) on the sample tray, use polyurethane foam to solidify the soda-lime glass polishing disk of polishing pad or surface roughness Ra 1.6, adopt table 3,4 listed processing parameter polished silicon substrate or copper sheets, polishing time all unification is 60 minutes, and synoptic diagram such as Fig. 6, shown in Figure 7 are arranged in concrete processing.
The performance of various polishings (material removing rate and surfaceness) is with seeing Table 3,4.
Wherein, polishing speed obtains by the thickness difference of measuring before and after the polishing of silicon chip or copper sheet, and surface roughness Ra records by the three-dimensional white light interference scanning profile of Zygo NewView600s type instrument, and the limit of collapsing, surface is then determined according to the edge contour pattern that records.
Wherein, experimental example 5～12 and experimental example 16～19 are cmp method of the present invention, its utilize auxiliary magnetic field with Compostie abrasive particles being held in soft polishing pad or hard polisher surface, the polished surface of polishing material is polished.
Table 3
Table 4
Show according to table 3,4 polish results:
1. utilize the S1 polishing fluid of autogamy or the commercially available single abrasive material silicon slice polishing liquid of FA/O S8010, polished silicon slice under polyurethane flexible polishing pad environment can obtain higher material removing rate, but the limit maximum of collapsing (experimental example 1～2) of silicon chip edge.Embodiment shows: autogamy and commercially available polishing fluid have preferably polishing performance, but soft polishing pad causes the workpiece edge error that collapses easily.
2. do not apply auxiliary magnetic field when utilizing magnetic coupling abrasive grain polishing solution [1] and polishing, material removing rate is improved under the polyurethane flexible polishing pad environment, but the limit of collapsing reduces not obvious (comparative experiments example 3 and experimental example 1); Material removing rate reduces to some extent under the hard polisher environment, but the limit of collapsing reduces obviously (comparative experiments example 4 and experimental example 1).Experimental example shows: under polyurethane flexible polishing pad environment, utilize composite abrasive grain polishing solution can improve the polishing material clearance, but that the limit of collapsing reduces is not obvious; Under hard polisher environment, utilize composite abrasive grain polishing solution polishing material clearance to decrease, the limit of collapsing reduces obviously.This be since the ability that polisher surface microscopic groove is controlled Compostie abrasive particles a little less than, Compostie abrasive particles weakens the mechanical scratching effect of material, material removing rate descends.The Compostie abrasive particles that plays miniature polishing pad effect separates silicon chip and polisher, and finished edge is stressed to be reduced, and the limit of collapsing is obviously descended.
3. utilize magnetic coupling abrasive grain polishing solution [1] and when polishing to apply auxiliary magnetic field, the material removing rate under the soft polishing pad environment increase (comparative experiments example 5 and experimental example 3); Material removing rate increase rate under the hard polisher environment large (comparative experiments example 6 and experimental example 4).Experimental example shows: applying auxiliary magnetic field can increase controlling property to the magnetic coupling abrasive particle, particularly under hard polisher condition, the magnetic coupling abrasive particle is effectively controlled by magnetic force at smooth surface, the abrasive particle that is adsorbed on the magnetic microsphere surface is strengthened the mechanical scratching effect of material, and material removing rate improves.
4. by PMMA magnetic microsphere and SiO
2The polishing fluid [2] that abrasive particle preparation obtains with by PS magnetic microsphere and SiO
2The polishing performance of the polishing fluid that abrasive particle obtains [1] similar (comparative experiments example 7,8 and experimental example 5,6), but the material removing rate that polishing fluid [2] obtains is slightly less than polishing fluid [1], and this is main more relevant with PMMA magnetic microsphere particle diameter.
5. basically identical with the polishing performance of the polishing fluid [3] of the single abrasive material silicon slice polishing liquid of commercially available FA/O S8010 and PS, the preparation of PMMA magnetic microsphere, [4] and polishing fluid [1], [2], material removing rate is height (comparative experiments example 9,10,11,12 and experimental example 5,6,7,8) slightly.
6. do not apply auxiliary magnetic field when polishing, under polyurethane flexible polishing pad environment, the material removing rate of the single abrasive material copper of commercially available FA/O C6201 polishing fluid is lower than magnetic coupling abrasive grain polishing solution [5], the copper sheet edge error basically identical and large (comparative experiments example 13 and experimental example 14) that collapses.Experimental example shows: under soft polishing pad environment, utilize composite abrasive grain polishing solution can improve the material removing rate of copper, but that the limit of collapsing reduces is not obvious.
7. do not apply auxiliary magnetic field when polishing, the copper removal rate of polishing fluid [5] is starkly lower than the material removing rate under the soft polishing pad environment under the hard polisher environment, but the limit of collapsing of copper bound edge obviously reduces (comparative experiments example 15 and experimental example 14).Experimental example shows: the ability that polisher surface microscopic groove is controlled Compostie abrasive particles a little less than, Compostie abrasive particles weakens the mechanical scratching effect of material, material removing rate descends.The Compostie abrasive particles that plays miniature polishing pad effect separates silicon chip and polisher, and finished edge is stressed to be reduced, and the limit of collapsing is obviously descended.
8. under the effect of auxiliary magnetic field, no matter under soft polishing pad or hard polisher environment, the copper product clearance of magnetic coupling abrasive grain polishing solution [5], [6] all increases (comparative experiments example 16,17,18,19 and experimental example 14,15).This is that material removing rate improves because after the magnetic coupling abrasive particle was subjected to magneticaction, being held in polishing pad or polisher surface, Compostie abrasive particles increased the mechanical scratching effect of material by effectively.
In sum, utilize chemical mechanical polishing liquid of the present invention and magnetic field auxiliary chemical mechanical polishing method, under soft polishing pad condition, can improve the polishing speed of silicon substrate and copper sheet; Under hard polisher condition, in the polishing speed that can improve silicon substrate and copper sheet, also can suppress the limit phenomenon of collapsing of silicon substrate and copper sheet.
Claims (9)
1. chemical mechanical polishing liquid, comprise liquid, be distributed with Compostie abrasive particles in the liquid, it is characterized in that, described Compostie abrasive particles depends on the small particle size abrasive material by macrobead magnetic polymer particles outside and consists of, and described magnetic polymer particles is made of polymer materials coated magnetic material; Wherein, described abrasive material and magnetic polymer particles shared ratio in polishing fluid is 1～20 weight ﹪, and the particle diameter ratio of magnetic polymer particles and abrasive material is 10～1000:1, and the mass ratio of magnetic polymer particles and abrasive material is 1:0.5～1 in the polishing fluid; The median size of described magnetic polymer particles is 500～20000nm, and the saturation magnetization of magnetic polymer particles is 5～100emu/g.
2. a kind of chemical mechanical polishing liquid according to claim 1, it is characterized in that, described magnetic polymer particles be nuclear for magneticsubstance, shell be that magnetic polymer particles or the ectonexine of polymer materials is that polymer materials, middle layer are the magnetic polymer particles of magneticsubstance.
3. a kind of chemical mechanical polishing liquid according to claim 1 is characterized in that, described abrasive material is colloidal silica particles.
4. a kind of chemical mechanical polishing liquid according to claim 1 is characterized in that, described polymer materials is polystyrene, styrene copolymer, methacrylic resin or methacrylic copolymer.
5. a kind of chemical mechanical polishing liquid according to claim 1 is characterized in that, described magneticsubstance is the Fe that is shaped as sphere, particle diameter 5～200nm
3O
4Magnetic particle.
6. a kind of chemical mechanical polishing liquid according to claim 1 is characterized in that, described Compostie abrasive particles is to be adsorbed mutually by electrostatic force in liquid by abrasive material and magnetic polymer particles to form.
7. cmp method, it is characterized in that, adopt such as each described chemical mechanical polishing liquid in the claim 1 to 6, utilize auxiliary magnetic field that Compostie abrasive particles is surperficial being held in soft polishing pad or hard polisher, the polished surface of polishing material is polished.
8. a kind of cmp method according to claim 7 is characterized in that, the rotating speed of described soft polishing pad or hard polisher is 20～200rpm, and described polishing material is applied in the polish pressure of 0.5～100kPa.
9. a kind of cmp method according to claim 8 is characterized in that, described auxiliary magnetic field is arranged on polishing area, and magnetic field is produced by permanent magnet or produced by electromagnetic generator.
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