CN104745083A - Chemical mechanical polishing liquid and polishing method - Google Patents
Chemical mechanical polishing liquid and polishing method Download PDFInfo
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- CN104745083A CN104745083A CN201310726698.0A CN201310726698A CN104745083A CN 104745083 A CN104745083 A CN 104745083A CN 201310726698 A CN201310726698 A CN 201310726698A CN 104745083 A CN104745083 A CN 104745083A
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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
Abstract
The invention relates to application of a chemical mechanical polishing liquid in increasing polishing rate of silicon dioxide. The chemical mechanical polishing liquid contains abrasive particles, an organic compound containing silicon, electrolyte ions with ionic strength greater than or equal to 0.1mol / Kg, and acid. The organic compound containing silicon has the following formula, wherein R is a non-hydrolyzable substituent, D is an organic functional group connected to R, and can react with organic substances for combination, A and B are same or different hydrolyzable substituents or hydroxyl, and C is a hydrolyzable group or hydroxyl, or a non-hydrolyzable alkyl substituent.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid and finishing method.
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.Wherein silane coupling agent plays the polishing velocity changing multiple material and the effect improving surfaceness.These two sections of patents do not 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 United States Patent (USP) 60142706 and United States Patent (USP) 09609882 do not find that silane coupling agent can improve the polishing velocity of silicon-dioxide, more do not find: between silane coupling agent and other additives, have significant synergy, the polishing velocity of silicon-dioxide is existed to the effect of 1+1>2.
Summary of the invention
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-dioxide between this silicon-containing compound and other additives.
The present invention relates to a kind of chemical mechanical polishing liquid and improving the application in silicon-dioxide polishing speed, chemical mechanical polishing liquid comprises abrasive grains, siliceous organic compound, is more than or equal to the electrolyte ion of the ionic strength of 0.1mol/Kg, and acid.
This siliceous organic compound can represent with following general formula:
General formula:
In above formula, R is unhydrolyzable substituting group, and D is the organo-functional group be connected on R, and these reactive groups can react with organic substance and combine.A, B are identical or different hydrolyzable substituting group or hydroxyl, and C can be hydrolysable group or hydroxyl, also can be the alkyl substituents of non-hydrolysable.Say further, R is alkyl normally, such as the alkyl of 1-50 carbon atom, more preferably, is the alkyl of 1-20 carbon atom, best, is the alkyl of 2-10 carbon atom.And it will be appreciated by persons skilled in the art that the carbon atom in R substituent can also continue to be continued to replace by other atoms such as oxygen, nitrogen, sulphur, phosphine, halogen, silicon.D can be amino, urea groups, sulfydryl, epoxy group(ing), acrylic, vinyl, acryloxy etc.A, B and C be chloro, methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group, hydroxyl etc. normally, generates silanol (Si (OH) during the hydrolysis of these groups
3), and be combined with inorganic substance, form siloxanes.
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)
γ-aminopropyltriethoxy diethoxy silane (trade(brand)name KH-902)
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.
The present invention's acid used can be organic acid and/or mineral acid.Organic acid is preferably polycarboxylic acid and/or hydroxycarboxylic acid, is preferably one or more in phenylformic acid, glycine, acetic acid, citric acid, toxilic acid, propanedioic acid, propionic acid, tartrate, oxalic acid and aspartic acid; Described organic acid content is preferably mass percent 0.01 ~ 1.5%, and better is 0.05 ~ 0.5%.The present invention's mineral acid used be preferably in boric acid and phosphoric acid one or more; The content of described mineral acid is preferably mass percent 0.01 ~ 1.5%, and better is 0.05 ~ 0.5%.
Described polishing composition can work under acid ph value or alkaline ph values.Preferably, the pH value of polishing composition is at 1-7.Within the scope of this, its pH value should be more than or equal to 2, and less than or equal to 6, most preferably pH value is 3-5.
Affiliated polishing composition also can comprise inorganic or organic pH value regulator, so that the pH value of polishing composition is down to acid ph value, or pH value is increased to alkaline ph values.Suitable inorganic pH value reduces agent and comprises such as nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid or comprise the combination that the above-mentioned inorganic pH value of at least one reduces agent.Suitable pH value growth promoter comprises following one: metal hydroxides, ammonium hydroxide or nitrogenous organic base or above-mentioned pH value increase the combination of agent.
In this polishing fluid, the concentration of siliceous organic compound is mass percent 0.001% ~ 1%, is preferably 0.01% ~ 0.5%.
In this polishing fluid, the concentration of Silica abrasive particle is mass percent 1% ~ 50%, is preferably 2% ~ 10%.Particle diameter is 20 ~ 200nm, is preferably 20 ~ 120nm.
In this polishing fluid, the electrolyte ion being more than or equal to the ionic strength of 0.1mol/Kg is metal ion and nonmetallic ion.For example, can be potassium ion, sodium ion, calcium ion, one or more in ammonium ion and TBuA ion.Preferably, electrolyte ion is potassium ion.
Positive progressive effect of the present invention is:
1: the present invention is 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 organic/inorganic acid, significantly improve the polishing velocity of silicon-dioxide 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.
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, HNO
3or pH adjusting agent is adjusted to required pH value.Wherein polishing condition is: polishing machine platform is Mirra board, Fujibo polishing pad, 200mm Wafer, overdraft 3psi, polishing fluid rate of addition 150ml/ minute.
Comparative example 1 shows: under very high ionic strength, and the removal speed of silicon-dioxide only has 350A/min, and polishing fluid is unstable, rapid delaminating deposition.Comparative example 3 and comparative example 1 contrast and show: under very high ionic strength, add silane coupling agent, and the removal speed of silicon-dioxide adds 120A/min, and polishing fluid is very stable, and abrasive grains median size (particle mean size) does not increase.Comparative example 2 shows: add aspartic acid, the polishing velocity of silicon-dioxide can be made to increase 517A/min, but polishing fluid is unstable, rapid delaminating deposition.Embodiment 1 and comparative example 2 contrast and show: under aspartic acid exists, add silane coupling agent, the removal speed ratio of silicon-dioxide does not add aspartic acid and does not add silane coupling agent, add 1082A/min, this increasing amount is greater than silane coupling agent (120A/min) and both contribution sums of aspartic acid (517A/min), show: there is synergy between silane coupling agent and aspartic acid and other organic/inorganic acids, significantly can improve the polishing velocity of silicon-dioxide.Comparative example 1 ~ 2 does not all add silane coupling agent, and polishing fluid is unstable.Embodiment 1 ~ 14, has silane coupling agent, and polishing fluid is more stable, and the removal speed of silicon-dioxide significantly promotes.
Embodiment 1 ~ 14, all shows, silane coupling agent has " effect of anti-high ionic strength ", and polishing fluid is highly stable.
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 (20)
1. a chemical mechanical polishing liquid is improving the application in silicon-dioxide polishing speed, it is characterized in that, described chemical mechanical polishing liquid comprises abrasive grains, siliceous organic compound, be more than or equal to the electrolyte ion of the ionic strength of 0.1mol/Kg, and acid, and described siliceous organic compound is following general formula
Wherein, R is unhydrolyzable substituting group, and D is the organo-functional group be connected on R, and it can react with organic substance and combine, A, and B is identical or different hydrolyzable substituting group or hydroxyl, and C is hydrolysable group or hydroxyl, or the alkyl substituent of non-hydrolysable.
2. apply as claimed in claim 1, it is characterized in that, described abrasive grains is Silica abrasive particle.
3. apply as claimed in claim 1, it is characterized in that, the concentration of described abrasive grains is mass percent 1% ~ 50%.
4. apply as claimed in claim 3, it is characterized in that, the concentration of described abrasive grains is mass percent 2% ~ 10%.
5. apply as claimed in claim 1, it is characterized in that, the particle diameter of described abrasive grains is 20 ~ 200nm.
6. apply as claimed in claim 5, it is characterized in that, the particle diameter of described abrasive grains is 20 ~ 120nm.
7. apply as claimed in claim 1, it is characterized in that, wherein R is alkyl, and the carbon atom on described alkyl carbon chain is continued to replace by oxygen, nitrogen, sulphur, phosphine, halogen, Siliciumatom; A, B and C are respectively chloro, methoxyl group, oxyethyl group, methoxy ethoxy, acetoxyl group or hydroxyl; D is amino, urea groups, sulfydryl, epoxy group(ing), acrylic, vinyl or acryloxy.
8. apply as claimed in claim 1, it is characterized in that, described siliceous organic compound is silane coupling agent.
9. apply as claimed in claim 8, 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), γ-aminoethylaminopropyl Trimethoxy silane (trade(brand)name KH-792), one or more in γ-aminopropyltriethoxy diethoxy silane (trade(brand)name KH-902).
10. apply as claimed in claim 1, it 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. apply as claimed in claim 10, it is characterized in that, described in be more than or equal to the ionic strength of 0.1mol/Kg electrolyte ion be potassium ion, sodium ion, calcium ion, one or more in ammonium ion and TBuA ion.
12. apply as claimed in claim 1, it is characterized in that, described in be more than or equal to the electrolyte ion of the ionic strength of 0.1mol/Kg concentration be 0.1mol/Kg-1mol/Kg.
13. apply as claimed in claim 1, it is characterized in that, described acid is organic acid and/or mineral acid, and wherein, organic acid is polycarboxylic acid and/or hydroxycarboxylic acid.
14. apply as claimed in claim 13, it is characterized in that, preferred organic acid is one or more in phenylformic acid, glycine, acetic acid, citric acid, toxilic acid, propanedioic acid, propionic acid, tartrate, oxalic acid and aspartic acid; Described mineral acid be preferably in boric acid and phosphoric acid one or more.
15. apply as claimed in claim 13, it is characterized in that, described organic acid content is mass percent 0.01 ~ 1.5%, and the content of mineral acid is mass percent 0.01 ~ 1.5%.
16. apply as claimed in claim 15, it is characterized in that, described organic acid content is mass percent 0.05 ~ 0.5%, and the content of mineral acid is mass percent 0.05 ~ 0.5%.
17. apply as claimed in claim 1, it is characterized in that, the concentration of described siliceous organic compound is mass percent 0.001% ~ 1%.
18. apply as claimed in claim 17, it is characterized in that, the concentration of described siliceous organic compound is mass percent 0.01% ~ 0.5%.
19. apply as claimed in claim 1, it is characterized in that, the pH of described chemical mechanical polishing liquid is 1-7.
20. apply as claimed in claim 1, it is characterized in that, the pH of described chemical mechanical polishing liquid is 3-5.
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