CN102585706A - Acidic chemical and mechanical polishing composition - Google Patents
Acidic chemical and mechanical polishing composition Download PDFInfo
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- CN102585706A CN102585706A CN2012100048016A CN201210004801A CN102585706A CN 102585706 A CN102585706 A CN 102585706A CN 2012100048016 A CN2012100048016 A CN 2012100048016A CN 201210004801 A CN201210004801 A CN 201210004801A CN 102585706 A CN102585706 A CN 102585706A
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Abstract
The invention provides an acidic chemical and mechanical polishing composition. The pH value of the acidic chemical and mechanical polishing composition is 2-7, and the acidic chemical and mechanical polishing composition comprises 1-20% by weight of abrasive material, 0.5-10% by weight of oxidant, 0.1-10% by weight of complexing agent, 0.001-1% by weight of corrosion inhibitor, 0.001-5% by weight of organic film-forming auxiliaries and the balance of pH regulator and deionized or distilled water, wherein the abrasive material is of colloidal silica sol after modification in the special step, and the average particle size is of 10-200nm. According to the chemical and mechanical polishing composition provided by the invention, the abrasive material is refined and modified; by using the method, the stability of the abrasive material in polishing slurry can be effectively upgraded, and polishing removal rate and surface roughness degree are respectively optimized to a certain extent; and the unique adding effect of the organic film-forming auxiliaries can well balance the strength of chemical corrosion action and the strength of mechanical grinding action, and achieve the effects of improving polishing removal efficiency and performing global planarization.
Description
Technical field
The present invention relates to the chemical-mechanical polishing compositions field, especially relate to the acidic chemical mechanical polishing composition.
Background technology
IC chip by on silicon substrate or millions of activation elements that form in the silicon substrate constitute, the method interconnection of these activation elements disconnected from each other through metal line forms functional circuit and parts.Because Cu has low resistivity and high electromigration resisting property, make it become a kind of ideal intraconnections material and replace the aluminium wiring of conventional.Cu is a metal behind the hydrogen, is difficult for being etched, and therefore generally adopts inlay to connect up at present in the world, removes unnecessary copper and the diffusion impervious layer in upper strata through chemical Mechanical Polishing Technique.Along with the development of microelectronics, characteristic dimension has got into nano level, and nearly hundred procedures that this requires in the microelectronic technique must carry out leveling.Traditional planarization technique can only provide part planization, and smooth effect is extremely limited.Chemically machinery polished (CMP) technology has brought ic manufacturing technology to change greatly for planarization.
CMP is the polishing technology that the particulate mechanical effect combines with the chemical action of etching reagent; Its principle is that workpiece rotates with respect to polishing pad in the presence of pressure and polishing composition (containing abrasive particle, etching reagent etc.), thereby utilizes abrasive particle grinding and chemical composition corrosive nature to realize the removal of workpiece surface material is reached the effect of planarization.The performance of CMP is by the operational condition of CMP device, the type of polishing composition and factors such as the type decision of polishing pad.
Polishing composition is a kind of significant effects factor in the CMP step.Can regulate polishing composition according to the oxygenant of choosing, abrasive material and other additive that is fit to,, simultaneously surface imperfection, corrosion reduced to minimumly, and obtain best complanation effect effective polishing to be provided by required polishing speed.In recent years, more existing patent reports employed polishing composition, for example CN101240147A, CN1256765C, CN100491072C, CN101333419A, CN101368068A in the integrated circuit multilayer copper wiring CMP process.
Along with integrated circuit technique enters into deep-submicron, the interconnection performance of being brought by continuous down feature sizes reduces more and more obvious.Adopting medium with low dielectric constant material (being the low k dielectric material) then is one of effective way that improves the interconnection performance.But when k＜2.2, the physical strength of low k dielectric layer descends, and is prone to low k film delamination, so must exploitation low pressure polissoir and polishing composition.
Generally, reducing overdraft can have a negative impact to the CMP overall performance that comprises polishing speed, has a strong impact on throughput.There have been some patents to propose the low downforce pressure polishing compsn, for example CN201110065350.2, US6,620,037, CN1644644A, but research in this respect still need be strengthened.The development of semicon industry is to can still existing demand by the improvement polishing waterborne compositions of copper on polishing of semiconductor wafers under 0.5Psi (3.45kPa) and the above polish pressure condition; Particularly below the 2.0Psi; Like effective polishing copper interconnection layer under the 0.5Psi pressure, thereby adapt to dielectric introducing of low-k and development.
Summary of the invention
The present invention is intended to solve at least one of technical problem that exists in the prior art.
The invention provides a kind of acidic chemical mechanical polishing composition, its pH value is 2-7, and its composition comprises abrasive material 1-20wt%; Oxygenant 0.5-10wt%, complexing agent 0.1-10wt%, inhibiter 0.001-1wt%; Organic film coalescence aid 0.001-5wt%, pH regulator agent and deionized water or zero(ppm) water.Wherein abrasive material is the colloidal silica sol of modification; Mean particle size is the 10-200 nanometer; Its preparation method is following: (1) deionization: the good strong acid type styrene type cation exchange resin post of will regenerating uses deionized water to be washed till outflow water pH value with strong base styrene series anion exchange resin post to be neutrality; Again raw silicon colloidal sol is flow through through good cation exchange resin column and the anion-exchange resin column of regenerating successively, flow rate control 1-10 rice/hour, promptly obtain the silicon dioxide gel of deionization; Adopt organic bases to regulate the pH value to 9.0-10.0, to prolong its stable storage period; (2) modification is handled: after said deionization silicon dioxide gel is heated to 50-60 ℃, under agitation slowly splash into organosilicon liquid, insulated and stirred after 6 hours thin up to effective solid content be 30% water silica sol solution.
Chemical-mechanical polishing compositions provided by the invention, its abrasive material have carried out refining and modification is handled, and this method can effectively promote the stability of abrasive material in the polishing slurries.
One of according to the embodiment of the present invention, organic bases is thanomin (MEA), TMAH (TMAH), trolamine in the above-mentioned deionization step.
According to another embodiment of the present invention, organosilicon liquid is selected from the group that comprises methyltrimethoxy silane, dimethyldimethoxysil,ne, octyl group Trimethoxy silane, isobutyl-Trimethoxy silane, dodecyl Trimethoxy silane, gamma-methyl allyl acyloxypropyl trimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane and the compsn of their arbitrary proportions in the above-mentioned modification treatment step.
Preferably, organosilicon liquid is gamma-methyl allyl acyloxypropyl trimethoxysilane, and its add-on is 0.01-10wt%.More preferably, the add-on of gamma-methyl allyl acyloxypropyl trimethoxysilane is 0.1-1wt%.
One of according to the embodiment of the present invention, the content of colloidal silica sol described in the chemical-mechanical polishing compositions is 3-5wt%, mean particle size is the 50-80 nanometer.
One of according to the embodiment of the present invention; Oxygenant described in the chemical-mechanical polishing compositions is inorganic or the organic peroxy compound; Be contain in the molecule at least one peroxy-radical (compound O-O-) with contain the compound of the element that is in high oxidation state, include but not limited to hydrogen peroxide, Urea Peroxide, two persulphates, Peracetic Acid, Lucidol, di-t-butyl peroxide, sodiumperoxide etc.; The high oxidation state compound comprises Periodic acid 99, periodate, hyperbromic acid, hyperbromic acid salt, perchloric acid, perchlorate, periodic acid, periodates, peroxyboric acid, perborate, iodate, bromate, oxymuriate, hypochlorite, nitrite, chromic salt, molysite and permanganate.Preferably, oxygenant is a hydrogen peroxide, and its content is 0.9-3wt%.
In the acidic chemical mechanical polishing composition provided by the invention, complexing agent refers to and can promote polishing composition to metal, copper for example, oxygenizement, increase the Ammonia or the carboxylic class organic acids and base of polishing speed.One of according to the embodiment of the present invention, complexing agent described in the chemical-mechanical polishing compositions is selected from the group that comprises Padil, L-Ala, L-glutamic acid, proline(Pro), hydroxyglutamic acid, HEDP, ATMP, 2-HPAA, acetate, oxalic acid, Hydrocerol A, oxamide and the compsn of their arbitrary proportions.Preferably, complexing agent is a Padil, and its content is 0.5-3wt%.
In the acidic chemical mechanical polishing composition provided by the invention, inhibiter refers to any compound or its mixture that helps to form on the surface of special metal layer such as Cu dense oxide passivation layer and dissolving inhibition layer.One of according to the embodiment of the present invention, inhibiter described in the chemical-mechanical polishing compositions is selected from the group that comprises benzotriazole, benzoglyoxaline, imidazoles, benzothiazole, urea, thiocarbamide, ethylene thiourea and the compsn of their arbitrary proportions.Preferably, inhibiter preferably contains the heterocyclic organic compounds of one or more 5 or 6 yuan of heterocycles as active function groups, and like benzotriazole or benzoglyoxaline or their mixture, content is 0.001-0.05wt%.
In the acidic chemical mechanical polishing composition provided by the invention, organic film coalescence aid refers to the polymer organic polymer that can possess outstanding oilness and wettability in the surperficial formation advantage absorption of metal level (like the Cu layer), institute's film forming.One of according to the embodiment of the present invention, organic film coalescence aid described in the chemical-mechanical polishing compositions is selected from the group that comprises Z 150PH, polyoxyethylene glycol, polyalkylene glycol, ROHM, SEPIGEL 305, AEO, polyoxyethylenated alcohol sodium sulfate and the compsn of their arbitrary proportions.Preferably, organic film coalescence aid is a polyalkylene glycol, and its content is 0.01-1wt%.The organic film coalescence aid of polymer that the present invention adopts can effectively promote the polish removal rate of material.
In the chemical-mechanical polishing compositions provided by the invention; The pH regulator agent can be a kind of or compsn of any known acid, alkali or amine and salt thereof, includes but not limited to the mixture of a kind of or its arbitrary proportion in sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, Mono Chloro Acetic Acid, propanedioic acid, sodium hydroxide, Pottasium Hydroxide, ammoniacal liquor, thanomin, diethylolamine, trolamine, Yi Bingchunan, aminopropanol, HSDB 338, quadrol, tetramethylphosphonihydroxide hydroxide base amine, hydroxide tetraethyl-amine, hydroxide tetrapropyl amine, choline, piperidines, piperazine, polyethylene imines, yellow soda ash, salt of wormwood, sodium phosphate, potassiumphosphate, Sodium phosphate, dibasic, the ammonium hydrogen phosphate etc.One of according to the embodiment of the present invention, the pH regulator agent is inorganic or organic acids and base, and preferably, the pH regulator agent is selected from the group that comprises sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, Pottasium Hydroxide, ammoniacal liquor, thanomin, trolamine and the compsn of their arbitrary proportions.
One of according to the embodiment of the present invention, acidic chemical mechanical polishing composition provided by the invention, its pH value is preferably 3-5.
The polishing mechanism and the advantage of the inventive method are following:
1, it is refining and surface silicon is siloxane modified that polish abrasive colloid silica used in the present invention has carried out deionization before use; This measure can effectively promote the stability of abrasive particle in the polishing slurries; Make the total composition liquid of polishing slurries after placing 7 days, still keep excellent polishing effect, polish removal rate and surfaceness all have optimization to a certain degree.
2. this polishing composition is acid partial neutral, and the pH value when keeping nanometer silicon dioxide particle stability with dispersiveness, has also been given guarantee to the stability of oxidants hydrogen peroxide between 3-5, and less to corrosion on Equipment property.
3. preferred organic film coalescence aid polyalkylene glycol used in the present invention (PAG) can form the self assembly molecule rete with oilness and wettability in the metallic surface of oxidation.Under the situation of low downforce pressure polishing, residing polishing environment common mechanical action intensity far is weaker than chemical action intensity, and the molecule rete on this MOX top layer can effectively be protected polished depression in the surface zone, and the highly selective of pattern is provided; And when polish pressure increased, the polymer molecule rete was not enough to resist the mechanical grinding effect of increase, and the disengaging of rete drives the disengaging of MOX rete, can effectively increase polish removal rate.Can think, more than the exclusive good balance of additive effect of organic film coalescence aid polyalkylene glycol chemical corrosion action intensity and mechanical grinding action intensity, improve the effect that efficient and overall planarization are removed in polishing thereby reach.
4. be low to moderate under the overdraft situation of 0.5～7.0Psi; The polish removal rate of optimum combination composition formula reaches as high as 1738.0nm/min under the experiment condition, and surfaceness is minimum can be to 0.599nm, and polish removal rate is high; Surface finish is good, and the shelf-stability of total composition liquid is good.Can be used for the polishing of multilayer copper wire in large scale integrated circuit copper.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously with easily understanding becoming the description of embodiment below in conjunction with accompanying drawing, wherein:
Fig. 1 is the polishing clearance of the embodiment of the invention 1～6 and the rule synoptic diagram of pressure dependence;
Fig. 2 is the surfaceness of the embodiment of the invention 1～6 and the rule synoptic diagram of pressure dependence;
Fig. 3 is the surface of polished pattern observation figure of the embodiment of the invention 9.
Embodiment
Describe embodiments of the invention below in detail, the example of said embodiment is shown in the drawings.Be exemplary through the embodiment that is described with reference to the drawings below, only be used to explain the present invention, and can not be interpreted as limitation of the present invention.
Experiment all uses CETR CP4 to be the polishing experiments machine among the embodiment; Use the Rodel IC1000/SUBA IV of company microvoid polyurethane polishing pad; The polishing speed of relative movement is fixed as 1m/s, the polishing fluid flow is 100mL/min, and polished is 2 cun electroplating surface copper sheets.It is the precise electronic balance check weighing calculating of 0.01mg that polish removal rate (MRR) adopts precision, uses the three-dimensional white light interference surface topographic apparatus fo of the Veeco microXAM of company to observe surface topography and gauging surface roughness (Sa).
Embodiment 1
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 0.5Psi overdraft immediately copper polish, polish removal rate MRR is 421.0nm/min, surfaceness Sa is 4.01nm.
Embodiment 2
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 1.0Psi overdraft immediately copper polish, polish removal rate MRR is 569.4nm/min, surfaceness Sa is 3.02nm.
Embodiment 3
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 2.0Psi overdraft immediately copper polish, polish removal rate MRR is 692.5nm/min, surfaceness Sa is 1.39nm.
Embodiment 4
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 3.0Psi overdraft immediately copper polish, polish removal rate MRR is 857.4nm/min, surfaceness Sa is 1.14nm.
Embodiment 5
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 4.0Psi overdraft immediately copper polish, polish removal rate MRR is 897.0nm/min, surfaceness Sa is 0.965nm.
Embodiment 6
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 5.0Psi overdraft immediately copper polish, polish removal rate MRR is 991.6nm/min, surfaceness Sa is 0.833nm.
Embodiment 7
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 7.0Psi overdraft immediately copper polish, polish removal rate MRR is 1597.6nm/min, surfaceness Sa is 0.835nm.
Embodiment 8
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0 adds water at last and supplies 1000 and restrain and stir.Place the copper polishing of carrying out the 7.0Psi overdraft after 3 days, polish removal rate MRR is 1643.9nm/min, and surfaceness Sa is 0.668nm.
Embodiment 9
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram Padils, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0 adds water at last and supplies 1000 and restrain and stir.Place the copper polishing of carrying out the 7.0Psi overdraft after 7 days, polish removal rate MRR is 1738.0nm/min, and surfaceness Sa is 0.599nm.
Comparative experimental example 1 silicon-dioxide is made with extra care and the influence of modification to polishing effect
1. divide into groups and treatment process:
Experimental group 1-3 adopts the chemical-mechanical polishing compositions of embodiment 7-9 respectively.
Comparative group 1-3 adopts following method to prepare chemical-mechanical polishing compositions and polished finish respectively.
Comparative group 1
10 gram glycocoll, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively; Stirring and dissolving, evenly after; Slowly stir the not refining 50nm silica hydrosol of handling with modification that adds 100 grams 30%; Add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 7.0Psi overdraft immediately copper polish.
Comparative group 2
10 gram glycocoll, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively; Stirring and dissolving, evenly after; Slowly stir the not refining 50nm silica hydrosol of handling with modification that adds 100 grams 30%; Add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0 adds water at last and supplies 1000 and restrain and stir.Place the copper polishing of carrying out the 7.0Psi overdraft after 3 days.
Comparative group 3
10 gram glycocoll, 0.1 gram benzotriazole and 0.1 gram polyalkylene glycol are added in the 800 gram deionized waters successively; Stirring and dissolving, evenly after; Slowly stir the not refining 50nm silica hydrosol of handling with modification that adds 100 grams 30%; Add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0 adds water at last and supplies 1000 and restrain and stir.Place the copper polishing of carrying out the 7.0Psi overdraft after 7 days.
2. result and analysis:
Detailed results is seen table 1.
Table 1 abrasive particle is made with extra care and the influence of modification front and back to the polishing slurries shelf-stability
| Test | The abrasive particle disposition | Storage period (my god) | Overdraft (Psi) | MRR(nm/min) | Sa(nm) |
| Comparative group 1 | Be untreated | 0 | 7.0 | 1457.7 | 1.12 |
| Comparative group 2 | Be untreated | 3 | 7.0 | 1171.8 | 2.10 |
| Comparative group 3 | Be untreated | 7 | 7.0 | 1066.0 | 3.29 |
| Experimental group 1 | Make with extra care and modification | 0 | 7.0 | 1597.6 | 0.835 |
| Experimental group 2 | Make with extra care and modification | 3 | 7.0 | 1643.9 | 0.668 |
| Experimental group 3 | Make with extra care and modification | 7 | 7.0 | 1738.0 | 0.599 |
As shown in table 1, abrasive particle is without the increase with storage period of the polishing slurries of refining and modification, and MRR continues to descend, and the glazed surface quality also worsens significantly.And use through abrasive particle refining and the modification processing; Increase with storage period; The polishing performance of polishing slurries has optimization to a certain degree on the contrary; Can find out that from the surface of polished pattern synoptic diagram of Fig. 3 with the copper sheet that the polishing slurries of placing 7 days polishes out, surface roughness has been low to moderate 0.599nm.
Can find out that from above embodiment the polishing composition that process is optimized provides beyond thought optimization effect to the polishing speed and the glazed surface quality of copper-connection, has also effectively promoted the shelf-stability of polishing slurries.
The interpolation of comparative experimental example 2 organic membrane-forming agents is to the influence of polishing effect
1. divide into groups and treatment process:
Experimental group 1-6 adopts the chemical-mechanical polishing compositions of embodiment 1-6 respectively.
Comparative group 1-2 adopts following method to prepare chemical-mechanical polishing compositions and polished finish respectively.
Comparative group 1:
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram glycocoll and 0.1 gram benzotriazole are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 0.5Psi overdraft immediately copper polish.
Comparative group 2
With raw silicon colloidal sol successively with flow velocity 1-10 rice/hour flow through through good cation exchange resin column and the anion-exchange resin column of regenerating; Obtain the silicon dioxide gel of deionization; After adopting TMAH to regulate pH value to 10.0; Be heated to 50-60 ℃, under agitation slowly splash into the gamma-methyl allyl acyloxypropyl trimethoxysilane of 0.6wt%, insulated and stirred after 6 hours thin up to effective solid content be 30% 50nm silica hydrosol.
10 gram glycocoll and 0.1 gram benzotriazole are added in the 800 gram deionized waters successively, stirring and dissolving, evenly after, slowly stir and add 100 grams through the refining silica hydrosol of handling with modification.
Before polishing is carried out, add the oxidants hydrogen peroxide solution of 100 grams 30%, use H
2SO
4Calibration pH value to 4.0, add at last water supply 1000 grams and stir after carry out the 5.0Psi overdraft immediately copper polish.
2. result and analysis:
Detailed results is seen table 2.
The adding of table 2 polyalkylene glycol (PAG) is to the influence of polishing effect
| Test | The abrasive particle disposition | PAG(％) | Overdraft (Psi) | MRR(nm/min) | Sa(nm) |
| Comparative group 1 | Make with extra care and modification | 0 | 0.5 | 390.6 | 4.33 |
| Comparative group 2 | Make with extra care and modification | 0 | 5.0 | 842.7 | 1.26 |
| Experimental group 1 | Make with extra care and modification | 0.01 | 0.5 | 421.0 | 4.01 |
| Experimental group 2 | Make with extra care and modification | 0.01 | 1.0 | 569.4 | 3.02 |
| Experimental group 3 | Make with extra care and modification | 0.01 | 2.0 | 692.5 | 1.39 |
| Experimental group 4 | Make with extra care and modification | 0.01 | 3.0 | 857.4 | 1.14 |
| Experimental group 5 | Make with extra care and modification | 0.01 | 4.0 | 897.0 | 0.965 |
| Experimental group 6 | Make with extra care and modification | 0.01 | 5.0 | 991.6 | 0.833 |
As shown in table 2, no matter be under low pressure or the highly compressed situation, the interpolation of organic film coalescence aid polyalkylene glycol (PAG) can improve the polish removal rate and optimization surface quality of copper.Can find out that from Fig. 1-2 under PAG content fixed situation, with the increase of polish pressure, MRR presents power exponent and increases progressively, just break through 600nm/min behind the polish pressure 1.0Psi rapidly; Sa then presents power exponent with the increase of polish pressure and successively decreases, and behind 4.0Psi, begins to be lower than 1.0nm.
Can find out from above-mentioned contrast experiment; Acidic chemical mechanical polishing composition of the present invention and preparation method thereof utilizes the refining and modification of raw silicon colloidal sol; And adding can promote organic film coalescence aid of polishing effect; Can in the pressure range of broad, effectively promote the polishing speed and the surface quality of the polishing of wafer copper-connection, avoid the generation of polishing defect to greatest extent.Specifically, under the polishing experiments condition of embodiment, in the overdraft scope of 0.5～7.0Psi, the polish removal rate of optimum combination composition formula reaches as high as 1738.0nm/min, and surfaceness can reach 0.599nm.
Although illustrated and described embodiments of the invention; For those of ordinary skill in the art; Be appreciated that under the situation that does not break away from principle of the present invention and spirit and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited accompanying claims and equivalent thereof.
Claims (10)
1. acidic chemical mechanical polishing composition, its pH value is 2-7, its composition comprises
Abrasive material 1-20wt%, oxygenant 0.5-10wt%, complexing agent 0.1-10wt%, inhibiter 0.001-1wt%, organic film coalescence aid 0.001-5wt%, pH regulator agent and deionized water or zero(ppm) water, wherein
Said abrasive material is the colloidal silica sol of modification, and mean particle size is the 10-200 nanometer, and its preparation method is following:
(1) deionization: the good strong acid type styrene type cation exchange resin post of will regenerating uses deionized water to be washed till outflow water pH value with strong base styrene series anion exchange resin post to be neutrality; Again raw silicon colloidal sol is flow through through good cation exchange resin column and the anion-exchange resin column of regenerating successively; Flow rate control 1-10 rice/hour; Promptly obtain the silicon dioxide gel of deionization, adopt organic bases to regulate the pH value to 9.0-10.0;
(2) modification is handled: after said deionization silicon dioxide gel is heated to 50-60 ℃, under agitation slowly splash into organosilicon liquid, insulated and stirred after 6 hours thin up to effective solid content be 30% water silica sol solution.
2. chemical-mechanical polishing compositions as claimed in claim 1, wherein said organic bases are thanomin, TMAH, trolamine.
3. chemical-mechanical polishing compositions as claimed in claim 1, wherein said organosilicon liquid are selected from the group that comprises methyltrimethoxy silane, dimethyldimethoxysil,ne, octyl group Trimethoxy silane, isobutyl-Trimethoxy silane, dodecyl Trimethoxy silane, gamma-methyl allyl acyloxypropyl trimethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane and the compsn of their arbitrary proportions; Said organosilicon liquid is preferably gamma-methyl allyl acyloxypropyl trimethoxysilane, and its add-on is 0.01-10wt%, and being preferably add-on is 0.1-1wt%.
4. chemical-mechanical polishing compositions as claimed in claim 1, the content of wherein said colloidal silica sol are 3-5wt%, and mean particle size is the 50-80 nanometer.
5. chemical-mechanical polishing compositions as claimed in claim 1, wherein said oxygenant are inorganic or the organic peroxy compound; Its content is 0.9-3wt%.
6. chemical-mechanical polishing compositions as claimed in claim 1, wherein said complexing agent are selected from the group that comprises Padil, L-Ala, L-glutamic acid, proline(Pro), hydroxyglutamic acid, HEDP, ATMP, 2-HPAA, acetate, oxalic acid, Hydrocerol A, oxamide and the compsn of their arbitrary proportions; Said complexing agent is preferably Padil, and its content is 0.5-3wt%.
7. chemical-mechanical polishing compositions as claimed in claim 1, wherein said inhibiter are selected from the group that comprises benzotriazole, benzoglyoxaline, imidazoles, benzothiazole, urea, thiocarbamide, ethylene thiourea and the compsn of their arbitrary proportions; Said inhibiter is preferably benzotriazole or benzoglyoxaline or their mixture, and content is 0.001-0.05wt%.
8. chemical-mechanical polishing compositions as claimed in claim 1, wherein said organic film coalescence aid are selected from the group that comprises Z 150PH, polyoxyethylene glycol, polyalkylene glycol, ROHM, SEPIGEL 305, AEO, polyoxyethylenated alcohol sodium sulfate and the compsn of their arbitrary proportions; Said organic film coalescence aid is preferably polyalkylene glycol, and its content is 0.01-1wt%.
9. chemical-mechanical polishing compositions as claimed in claim 1; Wherein said pH regulator agent is inorganic or organic acids and base, is selected from the group that comprises sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, Pottasium Hydroxide, ammoniacal liquor, thanomin, trolamine and the compsn of their arbitrary proportions.
10. chemical-mechanical polishing compositions as claimed in claim 1, its pH value is 3-5.
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