CN104371550A - Chemical mechanical polishing liquid for polishing silicon material - Google Patents
Chemical mechanical polishing liquid for polishing silicon material Download PDFInfo
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- CN104371550A CN104371550A CN201310354651.6A CN201310354651A CN104371550A CN 104371550 A CN104371550 A CN 104371550A CN 201310354651 A CN201310354651 A CN 201310354651A CN 104371550 A CN104371550 A CN 104371550A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Abstract
The present invention provides a silane coupling agent-containing chemical mechanical polishing liquid for polishing a silicon layer. According to the present invention, with the chemical mechanical polishing liquid, the high concentration and the colloid stability of the chemical mechanical polishing liquid can be achieved, and the polishing rate of the silicon material can be improved.
Description
Technical field
The present invention relates to a kind of containing silicon-containing organic compound, for the chemical mechanical polishing liquid of polished silicon material.
Background technology
Along with the development of semiconductor technology, and the continuous increase of large-scale integrated circuit interconnection layer, the planarization of conductive layer and insulating medium layer becomes particularly crucial.Twentieth century eighties, the chemically machinery polished initiated by IBM Corporation (CMP) technology is considered to the most effective means of current global planarizartion.
Chemically machinery polished (CMP) is combined into by chemical action, mechanical effect and this two kinds of effects.It is usually by a grinding stage with polishing pad, and one for carrying the grinding head composition of chip.Wherein grinding head fixes chip, is then pressed on polishing pad in the front of chip.When carrying out chemically machinery polished, grinding head moves at polishing pad Linear or rotates along the direction of motion the same with grinding stage.Meanwhile, the slurries containing abrasive grains are dripped on polishing pad, and are laid on polishing pad because of centrifugation.Chip surface realizes global planarizartion under machinery and chemical dual function.
At present, chemical mechanical polishing liquid (CMP) abrasive grains used adopts silicon-dioxide usually, comprises silicon sol (colloidal silica) and aerosil (fumed silica).They itself are solids, but in aqueous can be dispersed, and not sedimentation even can keep the permanent stability of 1 to 3 year.
The stability (not sedimentation) of abrasive grains in aqueous phase can explain with double electrode layer theory-because each particle surface is with identical electric charge, and they repel mutually, can not produce cohesion.
According to Stern model, colloid ion, when moving, the face of cutting can produce Zeta electric potential.Zeta electric potential is an important indicator of colloidal stability, because the stable of colloid is closely-related with interparticle electrostatic repulsion forces.The reduction of Zeta electric potential can make electrostatic repulsion forces reduce, and causes interparticle van der Waals magnetism to be dominant, thus causes gathering and the sedimentation of colloid.The height of ionic strength is the important factor affecting Zeta electric potential.
The stability of colloid, except the impact by zeta electromotive force, is also permitted multifactorial impact by other.Such as, by the impact of temperature, at relatively high temperatures, the random thermal motion aggravation of particle, the probability of collision mutually increases, and can accelerate cohesion; Such as, affect by pH value, than indifferent equilibrium under strong basicity, strong acidic condition, its neutral and alkali is the most stable, and pH value 4-7 interval is least stable; Such as, by the impact of kinds of surfactants, some surfactivity can play the effect of dispersion agent, improve stability, and some tensio-active agent can reduce nanoparticle surface charge, reduces Coulomb repulsion, Accelerated subsidence.In tensio-active agent, usual aniorfic surfactant is conducive to the stability of nano particle, and cationic surfactant easily reduces stability; Again such as, relevant with the molecular weight of additive, oversize polymkeric substance long-chain is wound around nano particle sometimes, increases the viscosity of dispersion liquid, accelerates particle aggregation.Therefore, the stability of silicon sol is subject to the impact of many factors.
United States Patent (USP) 60142706 and United States Patent (USP) 09609882 disclose polishing fluid containing silane coupling agent and finishing method.
The finishing method of United States Patent (USP) 60142706 is that such as, the pH value of 2,3 is all 2.3, for the polishing of tungsten for polishing, embodiment 1 under acid and partial neutral condition; The pH value of embodiment 4 is all 7.7, for the polishing on the blocking layers such as copper tantalum.Under this pH value condition, the polishing velocity of silicon can be very low.United States Patent (USP) 60142706 silicon-dioxide quality per-cent used is less than 15%, because the dioxide-containing silica of high density can cause system unstable, therefore can not make the polishing fluid of high enrichment, can not put for a long time.
In United States Patent (USP) 09609882, silane coupling agent is for improving surfaceness.
Chinese patent application 200880108217.7 discloses polishing fluid containing silane coupling agent for the method for polishing silicon oxide and silicon nitride.
Above patent does not all find: when high ionic strength (>0.1mol/Kg), and silane coupling agent can play effect, the stable nanoparticles of antagonism high ionic strength.Because usually when containing very high ionic strength (such as containing being greater than >0.2mol/Kg potassium ion), the electrostatic double layer of silica sol granule can significantly be compressed, electrostatic repulsion forces reduces, and forms rapidly gel, precipitation.And above patent does not all find: silane coupling agent can improve the polishing velocity of silicon (silicon single crystal and polysilicon), more do not find: have significant synergy between silane coupling agent and other silicon polishing promotor, the polishing velocity of silicon is existed to the effect of 1+1>2.
Chinese patent application 200880108217.7 discloses and utilizes through the abrasive particles polishing silicon dioxide of aminosilane-treated and the method for silicon nitride.Because " silicon " and " silicon-dioxide ", " silicon nitride " are diverse materials, carry out polishing by method disclosed in this patent to simple substance " silicon ", speed is very low.
Chinese patent application 200980103153.6 discloses the method improving the polishing velocity of silicon with azole and guanidine, the problem of the method is, under high ionic strength, such as add a large amount of potassium ion (>0.1mol/Kg), the median size of abrasive grains can increase gradually, and polishing fluid is unstable.
Summary of the invention
Technical problem to be solved by this invention is how under high ionic strength, extends stability and the dispersity of abrasive grains in silicon dioxide layer materials chemistry machine polishing liquor, and improves the polishing speed of silicon.
The present invention discloses a kind of method, adopts siliceous organic compound, when polyelectrolyte ionic strength, can stablize abrasive grains, meanwhile, there is significant synergy, significantly improve the polishing velocity of silicon between this silicon-containing compound and other silicon polishing promotor.
This siliceous organic compound can represent with following general formula:
Herein, R is unhydrolyzable substituting group, is generally alkyl, containing 1-50 carbon atom, is good with 1-20 carbon atom, and wherein 2-10 carbon atom is best; Carbon atom on this Long carbon chain can also continue to be continued to replace by other atoms such as oxygen, nitrogen, sulphur, phosphine, halogen, silicon.D is the organo-functional group be connected on R, can be amino, urea groups, sulfydryl, epoxy group(ing), acrylic etc.A, B are identical or different hydrolyzable substituting group or hydroxyl; C can be hydrolysable group or hydroxyl, also can be the alkyl substituent of non-hydrolysable; A, B and C be chloro, methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group, hydroxyl etc. normally, generates silanol (Si (OH) 3), and is combined with inorganic substance, form siloxanes during the hydrolysis of these groups.D is vinyl, amino, epoxy group(ing), acryloxy, sulfydryl or urea groups.These reactive groups can react with organic substance and combine.
Representational siliceous organic compound is silane coupling agent, such as following structure:
APTES (trade(brand)name KH-550)
γ-(2,3-glycidoxy) propyl trimethoxy silicane (trade(brand)name KH-560)
γ-(methacryloxypropyl) propyl trimethoxy silicane (trade(brand)name KH-570)
Gamma-mercaptopropyltriethoxysilane (trade(brand)name KH-580)
γ-mercaptopropyl trimethoxysilane (trade(brand)name KH-590)
N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane (trade(brand)name KH-602)
γ-aminoethylaminopropyl Trimethoxy silane (trade(brand)name KH-792)
This siliceous organic compound can be added in polishing fluid through number of ways, 1: abrasive grains is first and silicon-containing compound bonding (the particle surface modification be commonly called as, surface treatment) before preparing polishing fluid, is then joined in polishing fluid by the abrasive grains after surface modification.2: this siliceous organic compound when producing polishing fluid and abrasive grains and other components mix simultaneously.3: this siliceous organic compound can first complete hydrolysis or partial hydrolysis, generate Si-OH group, and then add in polishing fluid, Si-OH group and the particle surface complete bonding of Si-OH or moiety in polishing fluid.The variforms such as free, bonding, partial hydrolysis, complete hydrolysis may be there is in the siliceous organic compound that therefore the present invention adopts when polishing.
Based on above-mentioned discovery, another aspect of the present invention is to provide a kind of chemical mechanical polishing liquid for polished silicon material, containing Silica abrasive particle, one or more silicon polishing accelerators, the electrolyte ion being more than or equal to the ionic strength of 0.1mol/Kg and siliceous organic compound, wherein said siliceous organic compound for be freely dispersed in aqueous phase, or and between abrasive grains is connected by chemical bond.
Wherein, siliceous organic compound has following molecular structure:
Wherein, R is unhydrolyzable substituting group; D is the organo-functional group be connected on R; A, B are identical or different hydrolyzable substituting group or hydroxyl; C is hydrolysable group or hydroxyl, or the alkyl substituent of non-hydrolysable; D is amino, sulfydryl, epoxy group(ing), acrylic, vinyl, acryloxy or urea groups, preferably, in siliceous organic compound, R is alkyl, and the carbon atom on described alkyl carbon chain is continued to replace by other atoms such as oxygen, nitrogen, sulphur, phosphine, halogen, silicon; A, B and C are respectively chloro, methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group or hydroxyl.
Wherein, the siliceous organic compound of siliceous organic compound is silane coupling agent, preferably, siliceous organic compound is APTES (trade(brand)name KH-550), γ-(2, 3-glycidoxy) propyl trimethoxy silicane (trade(brand)name KH-560), γ-(methacryloxypropyl) propyl trimethoxy silicane (trade(brand)name KH-570), gamma-mercaptopropyltriethoxysilane (trade(brand)name KH-580), γ-mercaptopropyl trimethoxysilane (trade(brand)name KH-590), N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane (trade(brand)name KH-602), one or more in γ-aminoethylaminopropyl Trimethoxy silane (trade(brand)name KH-792).Wherein, for economical and practical consideration, preferred γ-(2,3-glycidoxy) propyl trimethoxy silicane (trade(brand)name KH-560).
Wherein, the concentration of siliceous organic compound is mass percent 0.01% ~ 3%.
Wherein, the concentration of Silica abrasive particle is mass percent 0.1% ~ 40%, is preferably 16% ~ 40%.
Wherein, the electrolyte ion being more than or equal to the ionic strength of 0.1mol/Kg is metal ion and nonmetallic ion, is preferably, potassium ion and/or tetramethyl-ammonium (quaternary amine) ion.
Wherein, the pH value of chemical mechanical polishing liquid is 10 to 12.
Wherein, one or more silicon polishing accelerators are: concrete triazole can be: 1-hydrogen-1,2,4-triazole (TAZ) or derivatives thereof, amino acid can be conventional glycine, Methionin, the common amino acids such as Histidine and derivative thereof, organic phospho acid can be: Amino Trimethylene Phosphonic Acid (ATMP), Triethylene-tetramine Hexmethanephonic Acid (DEDTMP), ethylene diamine tetra methylene phosphonic acid (EDTMP), diethylene triamine pentamethylene phosphonic (DTPMPA), 2-phosphonobutane-1, 2, 4 tricarboxylic acid, 2-phosphonic acids butyric acid, 2-phosphonic acids acetic acid, 2-phosphonic acids propionic acid, 2-HPAA, 1-hydroxyl-2-pyridine-1, 1-di 2 ethylhexyl phosphonic acid ethane, di 2 ethylhexyl phosphonic acid methylene dichloride, hydroxy methylene di 2 ethylhexyl phosphonic acid, methylenediphosphonate (MDP), 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid, 3-amino-1-hydroxy propane-1, 1-di 2 ethylhexyl phosphonic acid and 4-amino-1-hydroxy propane-1, 1-di 2 ethylhexyl phosphonic acid etc.Guanidine and biguanides can be Guanidinium carbonate, Guanidinium hydrochloride, biguanides alkali, phenformin, Moroxydine and other guanidine derivatives.
Wherein, the concentration of silicon polishing accelerator is mass percent 0.1% ~ 2%.
Positive progressive effect of the present invention is:
1: by achieving the stably dispersing sex chromosome mosaicism of the chemical mechanical polishing liquid under high ionic strength at silane coupling agent.
2: by the synergy of silane coupling agent and complexing agent, significantly improve the polishing velocity of silicon further.
3: the chemical mechanical polishing liquid that high enrichment can be prepared by this method.
4: can significantly reduce the costs such as product starting material, packaging, transport, storage, management, manpower by high enrichment.
5: by improving ion and triazole, amino acid, the speed rising agents such as guanidine class material, can improve the removal speed of silicon.
Embodiment
Set forth advantage of the present invention further below by specific embodiment, but protection scope of the present invention is not only confined to following embodiment.
According to composition and the proportions polishing fluid thereof of embodiment each in table 1 and comparative example, mix, supply mass percent to 100% with water.With KOH or HNO
3be adjusted to required pH value.Wherein polishing condition is: polishing machine platform is Logitech(Britain) 1PM52 type, politex polishing pad, 4cm*4cm square polysilicon Wafer, grinding pressure 3psi, grinding stage rotating speed 70 revs/min, grinding head rotation rotating speed 150 revs/min, polishing fluid rate of addition 100ml/min.
Table 1 specific embodiment of the invention and comparative example formula
Comparative example 1 and comparative example 5 show: improve the removal speed that ionic strength can improve silicon slightly, known from comparative example 1 and comparative example 2, add triazole further, greatly can improve the removal speed of silicon, but polishing fluid are unstable, rapid delaminating deposition.Embodiment 1 and comparative example 1 contrast and show: under very high ionic strength, add silane coupling agent, and the removal speed of silicon adds 220A/min, and polishing fluid is very stable, and abrasive grains median size does not increase.Comparative example 2 shows: add triazole, the polishing velocity of silicon can be made to increase 1000A/min, but polishing fluid is unstable, rapid delaminating deposition.Embodiment 2 and comparative example 2 contrast and show: under TAZ exists, add silane coupling agent, the removal speed ratio of silicon does not add TAZ and does not add silane coupling agent, add 2200A/min, this increasing amount is greater than silane coupling agent (220A/min) and both contribution sums of TAZ (1000A/min), show: there is synergy between silane coupling agent and TAZ and other complexing agents, significantly can improve the polishing velocity of silicon.Comparative example 3,4 and embodiment 3,4 contrast, and can see obvious synergy.Comparative example 1 ~ 4 does not all add silane coupling agent, and polishing fluid is unstable.Embodiment 1 ~ 4, has silane coupling agent, and polishing fluid is stablized, and the removal speed of silicon significantly promotes.
Embodiment 1 ~ 13, all shows, silane coupling agent has " effect of anti-high ionic strength ", and polishing fluid is highly stable.
Should be understood that, % of the present invention all refers to mass percentage.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (16)
1. the chemical mechanical polishing liquid for polished silicon material, it is characterized in that, containing Silica abrasive particle, one or more silicon polishing accelerators, the electrolyte ion being more than or equal to the ionic strength of 0.1mol/Kg and siliceous organic compound, wherein said siliceous organic compound for be freely dispersed in aqueous phase, or and between abrasive grains is connected by chemical bond.
2. chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, described siliceous organic compound has following molecular structure:
Wherein, R is unhydrolyzable substituting group; D is the organo-functional group be connected on R; A, B are identical or different hydrolyzable substituting group or hydroxyl; C is hydrolysable group or hydroxyl, or the alkyl substituent of non-hydrolysable; D is amino, sulfydryl, epoxy group(ing), acrylic, vinyl, acryloxy or urea groups.
3. chemical mechanical polishing liquid as claimed in claim 2, it is characterized in that, in described siliceous organic compound, R is alkyl, and the carbon atom on described alkyl carbon chain is continued to replace by other atoms such as oxygen, nitrogen, sulphur, phosphine, halogen, silicon; A, B and C are respectively chloro, methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group or hydroxyl.
4. chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, described siliceous organic compound is silane coupling agent.
5. chemical mechanical polishing liquid as claimed in claim 4, it is characterized in that, described siliceous organic compound is APTES (trade(brand)name KH-550), γ-(2, 3-glycidoxy) propyl trimethoxy silicane (trade(brand)name KH-560), γ-(methacryloxypropyl) propyl trimethoxy silicane (trade(brand)name KH-570), gamma-mercaptopropyltriethoxysilane (trade(brand)name KH-580), γ-mercaptopropyl trimethoxysilane (trade(brand)name KH-590), N-(β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane (trade(brand)name KH-602), one or more in γ-aminoethylaminopropyl Trimethoxy silane (trade(brand)name KH-792).
6. chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, the concentration of described siliceous organic compound is mass percent 0.01% ~ 3%.
7. chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, described siliceous organic compound is γ-(2,3-glycidoxy) propyl trimethoxy silicane (trade(brand)name KH-560).
8. chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, the concentration of described Silica abrasive particle is mass percent 0.1% ~ 40%.
9. chemical mechanical polishing liquid as claimed in claim 1, it is characterized in that, the concentration of described Silica abrasive particle is mass percent 16% ~ 40%.
10. chemical mechanical polishing liquid as claimed in claim 1, is characterized in that, described in be more than or equal to the ionic strength of 0.1mol/Kg electrolyte ion be metal ion and nonmetallic ion.
11. chemical mechanical polishing liquids as claimed in claim 10, is characterized in that, described electrolyte ion is potassium ion and/or tetramethyl-ammonium (quaternary amine) ion.
12. chemical mechanical polishing liquids as claimed in claim 1, is characterized in that, the pH value of described chemical mechanical polishing liquid is 10 to 12.
13. chemical mechanical polishing liquids as claimed in claim 1, is characterized in that, one or more silicon polishing accelerators described are triazole, amino acid, carboxylic acid, guanidine, biguanides and its derivative.
14. chemical mechanical polishing liquids as claimed in claim 13, is characterized in that, one or more silicon polishing accelerators described are selected from 1-hydrogen-1,2,4-triazole (TAZ) or derivatives thereof; Glycine, Methionin, Histidine and derivative thereof; Guanidinium carbonate, Guanidinium hydrochloride, biguanides alkali, phenformin, Moroxydine and other guanidine derivatives.
15. chemical mechanical polishing liquids as claimed in claim 1, is characterized in that, the concentration of described silicon polishing accelerator is mass percent 0.1% ~ 2%.
16. 1 kinds of chemical mechanical polishing liquids as described in any one of claim 1-15 are improving the application in Si polishing speed.
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| CN110922897A (en) * | 2019-11-18 | 2020-03-27 | 宁波日晟新材料有限公司 | Low-haze nondestructive polishing solution for silicon compound and preparation method thereof |
| CN112920717A (en) * | 2021-02-23 | 2021-06-08 | 中山荣拓智能装备有限公司 | Silicon carbide single crystal polishing solution and using method thereof |
| CN114341287A (en) * | 2019-09-04 | 2022-04-12 | Cmc材料股份有限公司 | Compositions and methods for chemical mechanical polishing of polysilicon |
| CN115651543A (en) * | 2022-09-06 | 2023-01-31 | 苏州博来纳润电子材料有限公司 | Silicon wafer rough polishing solution composition and application thereof |
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| TWI815035B (en) * | 2019-09-04 | 2023-09-11 | 美商Ｃｍｃ材料股份有限公司 | Composition and method for polysilicon cmp |
| CN114341287B (en) * | 2019-09-04 | 2024-03-15 | Cmc材料有限责任公司 | Composition and method for polysilicon chemical mechanical polishing |
| CN110922897A (en) * | 2019-11-18 | 2020-03-27 | 宁波日晟新材料有限公司 | Low-haze nondestructive polishing solution for silicon compound and preparation method thereof |
| CN110922897B (en) * | 2019-11-18 | 2024-03-08 | 宁波日晟新材料有限公司 | Low-haze nondestructive polishing solution for silicon compound and preparation method thereof |
| CN112920717A (en) * | 2021-02-23 | 2021-06-08 | 中山荣拓智能装备有限公司 | Silicon carbide single crystal polishing solution and using method thereof |
| CN115651543A (en) * | 2022-09-06 | 2023-01-31 | 苏州博来纳润电子材料有限公司 | Silicon wafer rough polishing solution composition and application thereof |
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