CN107686703A - A kind of chemical mechanical polishing liquid - Google Patents
A kind of chemical mechanical polishing liquid Download PDFInfo
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- CN107686703A CN107686703A CN201610633767.7A CN201610633767A CN107686703A CN 107686703 A CN107686703 A CN 107686703A CN 201610633767 A CN201610633767 A CN 201610633767A CN 107686703 A CN107686703 A CN 107686703A
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- Prior art keywords
- chemical mechanical
- mechanical polishing
- polishing liquid
- organic compound
- daiamid
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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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- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The present invention discloses a kind of chemical mechanical polishing liquid, wherein containing abrasive grains, siliceous organic compound, electrolyte ion and complexing agent.The present invention utilizes the existing significant polishing velocity for acting synergistically, can greatly improving silica between siliceous organic compound and daiamid dissaving polymer PAMAM and its end group functional derivative.Meanwhile under polyelectrolyte ionic strength, abrasive grains can be stablized, improve polishing fluid pH stability.In addition, polishing fluid can be prepared as highly concentrated liquid in the present invention, the costs such as product raw material, packaging, transport, storage, management, manpower can be greatly reduced, possess excellent application prospect.
Description
Technical field
It is more particularly to a kind of to be applied in integrated circuit the present invention relates to a kind of chemical mechanical polishing liquid, possess excellent
Scattered and pH stabilities chemical mechanical polishing liquid.
Background technology
With the continuous development of semiconductor technology, and large scale integrated circuit interconnection layer is continuously increased, semiconductor core
Development of the planarization problem of piece conductive layer and insulating medium layer for integrated circuit becomes particularly critical.Twentieth century 80 years
Generation, the chemically mechanical polishing initiated by IBM Corporation (CMP) technology are considered as the most efficient method of current global planarizartion.
Chemically mechanical polishing (CMP) is combined into by chemical action, mechanism and both effects.It is generally by one
The individual grinding table with polishing pad, and a grinding head composition for being used to carry chip.Wherein grinding head fixes chip, then
The front of chip is pressed on polishing pad.When being chemically-mechanicapolish polished, grinding head linear movement or edge on polishing pad
The direction of motion rotation as grinding table.At the same time, the slurries containing abrasive grains are dripped on polishing pad, and because from
Heart effect is laid on polishing pad.Chip surface realizes global planarizartion under double action mechanically and chemically.
At present, the abrasive grains generally use silica used in chemical mechanical polishing liquid (CMP), including Ludox
(colloidal silica) and aerosil (fumed silica).Themselves it is solid, but in aqueous
It can not settled with dispersed, it might even be possible to keep the long-time stability of 1 to 3 year.
Stability (do not settle) of the abrasive grains in aqueous phase can be explained with double electrode layer theory-due to each particle
Surface carries identical electric charge, and they are mutually exclusive, will not produce cohesion.According to Stern models, colloid ion in motion,
Zeta electric potential can be produced on the face of cutting.Zeta electric potential is an important indicator of colloidal stability, because the stabilization of colloid is
It is closely related with interparticle electrostatic repulsion forces.The reduction of Zeta electric potential can reduce electrostatic repulsion forces, cause interparticle
Van Der Waals attractions are dominant, so as to cause the aggregation of colloid and sedimentation.The height of ionic strength is to influence Zeta electric potential
An important factor for.
The stability of colloid is also influenceed except being influenceed by Zeta electric potential by other many factors.For example, by temperature
Influence, at relatively high temperatures, the random warm-up movement aggravation of particle, the probability increase mutually collided, can accelerate to condense；For example, by
PH value influences, and than indifferent equilibrium under strong basicity, strong acidic condition, its neutral and alkali is most stable, and pH value 4-7 sections are least stable；
For example, being influenceed by kinds of surfactants, some surface-actives can play a part of dispersant, improve stability, and have
A little surfactants can reduce nanoparticle surface charge, reduce Coulomb repulsion, Accelerated subsidence.In surfactant, generally
Anionic surfactant is advantageous to the stability of nano particle, and cationic surface active agent is easily reduced stability；
For another example relevant with the molecular weight of additive, too long of polymer long-chain winds nano particle sometimes, increases the viscous of dispersion liquid
Degree, accelerate particle aggregation.Therefore, the stability of Ludox is influenceed by many factors.
United States Patent (USP) 60142706 and United States Patent (USP) 09609882 disclose the polishing fluid containing silane coupler and polishing
Method.Wherein silane coupler plays a part of changing the polishing velocity of multiple material and improves surface roughness.This two
Patent is not found：High ionic strength (>When 0.1mol/Kg), silane coupler can play confrontation high ionic strength
Effect, stable nanoparticles.Because generally when containing very high ionic strength (such as containing more than>0.2mol/Kg potassium from
Son), the electric double layer of silica sol granule can significantly be compressed, and electrostatic repulsion forces reduce, and quickly form gel, precipitation.And the U.S.
Patent 60142706 and United States Patent (USP) 09609882, which are not found silane coupler, can improve the polishing velocity of silica,
More do not find：There is significant synergy between silane coupler and other complexing agents, the polishing velocity of silica is deposited
In 1+1>2 effect.
Dissaving polymer is the tree form modification of highly branched three-D space structure, contains the end that can be largely modified
Base, there is intermolecular less entanglement, dissolubility is good, viscosity is low, easy film forming and reactivity are high.Superbrnaching end-hydroxy gathers
The one kind of compound as dissaving polymer, not only all properties with dissaving polymer, simultaneously as mechanism outer end contains
There is substantial amounts of hydroxyl, reactivity is high, easily according to the different hyperbranched polies for needing progress chemical modification, synthesizing various performances
Compound, meet the various performance requirements in modern various fields.Due to all having inside dendrimers and hyperbranched polymer molecule
Have cavity, molecular surface has high functional group densities because can effectively complex ion, adsorb small molecule.
Daiamid PAMAM is to study most extensive, most deep dendrimers, its height cladodification, high degree of symmetry at present
It is one of the dendrimer of three kinds of commercializations and a large amount of functional groups are contained on surface, its compound with regular structure, molecular structure essence
Really, relative molecular mass is controllable, has high density surface functional group, the geometrical symmetry of height, and global molecular squeezes interior pine outside, point
Cavity in son be present and can adjust.The researchs such as Diallo find PAMAM (daiamid) dendrimers and Cu2+Complexing very
By force.Thick ability of Xu etc. has studied in detail PAMAM dendrimers and Cu2+Complexing diversified forms.According to two kinds of macromolecular knots
The similitude of structure understands that dissaving polymer equally has complex performance, therefore can be applied to the stabilization of hydrogen peroxide.1992
Year, the Kim and Webster of E.I.Du Pont Company have synthesized the first highly branched polymer, and are named as dissaving polymer.
It has substantial amounts of chain end functional group, therefore has higher end group reactivity, can carry out reaction kinetic, prepares feature
Material.Dissaving polymer preparation process is simple, and without fine separating-purifying, strict rate-determining steps are not needed in building-up process,
It can be advantageous to mass produce with one-step synthesis.
Hydrocarbon chain in daiamid PAMAM dendrimers is oil loving group, and carboxyl and amido are hydrophilic
Group, acted on so daiamid PAMAM dendrimers have possessed by the surfactant such as solubilising, demulsification, stable.But
Daiamid PAMAM dendrimers as surfactant be in structure with traditional surfactant it is different, with
Algebraically increases, and it is close to spherical, and traditional surfactant is mostly linear.Thus, daiamid PAMAM dendrimers
The characteristics of having its own again as surfactant.
Nano material it is small-sized, surface energy is very big, is easy to reunite in preparation process, thus prepare nanometer material
Select suitable dispersant and stabilizer critically important during material.Daiamid PAMAM dendrimers not only have internal cavities, and
With abundant surface functional group, so daiamid PAMAM dendrimers are the good templates for preparing nano material.Li Guoping
Deng using Amino End Group daiamid pamam dendrimer molecule as template, hydrazine hydrate is reducing agent, has obtained good dispersion in atmosphere,
Grain size is evenly distributed, the Cu cluster of structure and stable performance.
The present invention discloses a kind of method, hyperbranched using siliceous organic compound, the silicon-containing compound and daiamid
Significant synergy between polymer P AMAM and its end group functional derivative be present, greatly improve the polishing of silica
Speed.Meanwhile in polyelectrolyte ionic strength, abrasive grains can be stablized, improve polishing fluid pH stability.
The content of the invention
The present invention discloses a kind of chemical mechanical polishing liquid, and it contains siliceous organic compound, is organised using siliceous
Existing significantly synergy between compound and other complexing agents, the polishing velocity of silica can be greatly improved.Meanwhile in height
Under electrolyte ion intensity, abrasive grains can be stablized, improve polishing fluid pH stability.
Specifically, the present invention a kind of chemical mechanical polishing liquid is disclosed, include abrasive grains, siliceous organic compound,
Electrolyte ion and complexing agent.
Wherein, the abrasive grains are silica, and its particle diameter is 20-120nm, and content is preferably 1-7wt%.
Wherein, the siliceous organic compound can be represented with following formulas：
Wherein, R is unhydrolyzable substituent；A, B are identical or different hydrolyzable substituent or hydroxyl；C is can
Hydrolysising group or hydroxyl, or the alkyl substituent for non-hydrolysable；D is the organo-functional group being connected on R.
Preferably, the R in the formula is alkyl, wherein containing 1-10 carbon atom；A, B and C be chloro, methoxyl group,
Ethyoxyl, methoxy ethoxy, acetoxyl group, hydroxyl etc., silanol (Si (OH) is generated when these groups hydrolyze3), so that with
Inorganic substances combine, and form siloxanes；D is selected from vinyl, amino, urea groups, sulfydryl, epoxy radicals, acrylic or acryloyl-oxy
Base, such reactive group can be reacted with organic substance so as to be combined.
More preferably, the alkyl contains 3-7 carbon atom, and the carbon atom on the alkyl carbon chain can by oxygen, nitrogen, sulphur,
Phosphine, halogen or silicon atom substitution.
More preferably, the siliceous organic compound is silane coupler, selected from APTES (business
Name of an article KH-550), γ-(2,3- glycidoxies) propyl trimethoxy silicane (trade name KH-560), γ-(methacryl
Oxygen) propyl trimethoxy silicane (trade name KH-570), gamma-mercaptopropyltriethoxysilane (trade name KH-580), N- (β-ammonia
Ethyl)-γ-aminopropyltriethoxy dimethoxysilane (trade name KH-602), γ-aminoethylaminopropyl trimethoxy silane (business
Name of an article KH-792) and/or γ-aminopropyltriethoxy diethoxy silane (trade name KH-902) in one or more.Its structure
Formula can enumerate as follows：
Wherein, the content of the siliceous organic compound is preferably 0.001~1wt%；More preferably 0.01~
0.5wt%.
Wherein, the complexing agent is daiamid dissaving polymer.
Preferably, the daiamid dissaving polymer is selected from the daiamid dissaving polymer of amino end group
And/or the daiamid dissaving polymer of carboxyl end groups, its structural formula can enumerate as follows：
Wherein, the molecular weight of the daiamid dissaving polymer is preferably 6000~100000；More preferably 9000~
50000。
Wherein, the content of the complexing agent is preferably 0.001~1.0wt%, more preferably 0.01~0.5wt%.
Wherein, the electrolyte ion is selected from metal ion and/or nonmetallic ion, and its concentration is 0.1~1mol/Kg.
Preferably, the electrolyte ion is potassium ion.
Wherein, the pH of the chemical mechanical polishing liquid is preferably 1-7, more preferably 4-5.
The polishing composition can also include inorganic or organic pH value regulator, and the pH value of polishing composition is down to
Acid ph value, or pH value is increased into proper pH value.Suitable inorganic pH value, which reduces agent, includes such as nitric acid, sulfuric acid, hydrochloric acid, phosphorus
Acid or the combination for reducing agent comprising at least one above-mentioned inorganic pH value.Suitable pH value height increasing agent includes following one kind：Metal
Hydroxide, ammonium hydroxide or nitrogenous organic base or the combination of above-mentioned pH value increase agent.
Wherein, the siliceous organic compound can be added in polishing fluid by following any approach：
A. abrasive grains before polishing fluid is prepared first and silicon-containing compound bonding (the particle surfaces that are commonly called as are modified,
Surface treatment), then the modified abrasive grains in surface are added in polishing fluid；
B. when producing polishing fluid, by the siliceous organic compound and the abrasive grains, the electrolyte ion
And the complexing agent mixes simultaneously；And/or
C. the siliceous organic compound complete hydrolysis or partial hydrolysis are first generated into Si-OH groups, then added again
Enter in polishing fluid, Si-OH groups and particle surfaces Si-OH bondings completely or part bonding in polishing fluid.
Therefore the siliceous organic compound that uses of the present invention there may be free, bonding, partial hydrolysis, complete in polishing
The variforms such as all-hydrolytic.
The polishing composition can also include inorganic or organic pH value regulator, and the pH value of polishing composition is down to
Acid ph value, or pH value is increased into required pH value.Suitable inorganic pH value, which reduces agent, includes such as nitric acid, sulfuric acid, hydrochloric acid, phosphorus
One or more combinations in acid.Suitable pH value height increasing agent includes such as metal hydroxides, ammonium hydroxide or nitrogenous had
One or more combinations in machine alkali.
The positive effect of the present invention is：
1：The present invention is by realizing the scattered steady of the chemical mechanical polishing liquid under high ionic strength in silane coupler
Qualitative and pH stability problems.
2：By silane coupler and the synergy of daiamid dissaving polymer and its end group functional derivative,
The polishing velocity of silica further greatly improved；
3：Highly concentrated chemical mechanical polishing liquid can be prepared by this method.
4：The costs such as product raw material, packaging, transport, storage, management, manpower can be greatly reduced by highly concentrated.
Embodiment
Advantages of the present invention is expanded on further below in conjunction with specific embodiment, but is not limited the present invention to this described
Scope of embodiments among.
Polishing fluid is prepared according to the composition of each embodiment and comparative example in table 1 and its ratio, is well mixed, uses water
Mass percent is supplied to 100%.With KOH, HNO3Or required pH value is arrived in the regulation of other pH adjusting agents.Wherein polishing condition
For：Polishing machine platform is Mirra boards, Fujibo polishing pads, 200mm Wafer, lower pressure 1.5psi, polishing fluid rate of addition
150ml/ minutes.
The specific embodiment of the invention of table 1 and comparative example formula
Comparative example 1 shows：Under very high ionic strength, the removal rate of silica only has 250A/min, and throws
Light liquid is unstable, and pH value was increased to 6.6 in 30 days from 4.0, rapid delaminating deposition.Comparative example 3 and comparative example 1 contrast table
It is bright：Under very high ionic strength, silane coupler is added, the removal rate of silica adds 420A/min, also, throws
Light liquid is very stable, and abrasive grains average grain diameter (particle mean size) does not increase, but the pH value of polishing fluid raises from 4.0
To 6.8.Comparative example 2 shows：Daiamid dissaving polymer is added, although the polishing velocity of silica can not be made increase,
And polishing fluid is unstable simultaneously, rapid delaminating deposition, but the pH value of polishing fluid is very stable, only increases 0.1 within 30 days.Embodiment
1 and comparative example 2 contrast and show：In the presence of daiamid dissaving polymer, silane coupler is added, silica is gone
Removal rates ratio is not added with daiamid dissaving polymer and is not added with silane coupler, adds 642A/min, this increments
Sum is contributed more than both silane coupler (420A/min) and daiamid dissaving polymer (17A/min), is shown：Silane
Between coupling agent and daiamid dissaving polymer and other daiamid dissaving polymers and its end group derivative
In the presence of synergy, the polishing velocity of silica can be greatly improved.Comparative example 1~2 does not all add silane coupler, polishing fluid
It is unstable.Embodiment 1~14, there are silane coupler and daiamid dissaving polymer and its end group derivative, polishing fluid
More stable, pH value is also more stable, and the removal speed of silica is obviously improved.
Embodiment 1~14, all shows, silane coupler has the function that " anti-high ionic strength " so that polishing fluid is very
It is stable, meanwhile, daiamid dissaving polymer and its end group derivative have the function that to stablize polishing fluid pH value.
It should be appreciated that wt% of the present invention refers to weight/mass percentage composition.
It should be noted that embodiments of the invention have preferable implementation, and not the present invention is made any type of
Limitation, any one skilled in the art change or are modified to possibly also with the technology contents of the disclosure above equivalent effective
Embodiment, as long as without departing from the content of technical solution of the present invention, above example is made according to technical spirit of the invention
Any modification or equivalent variations and modification, in the range of still falling within technical solution of the present invention.
Claims (21)
1. a kind of chemical mechanical polishing liquid, include abrasive grains, siliceous organic compound, electrolyte ion and complexing agent.
2. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the abrasive grains are silica.
3. chemical mechanical polishing liquid as claimed in claim 2, it is characterised in that the particle diameter of the abrasive grains is 20-
120nm。
4. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the content of the abrasive grains is 1-7wt%.
5. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the formula of the silicon-containing organic compound is：
Wherein, R is unhydrolyzable substituent；A, B are identical or different hydrolyzable substituent or hydroxyl；C is hydrolyzable
Group or hydroxyl, or the alkyl substituent for non-hydrolysable；D is the organo-functional group being connected on R, selected from vinyl, amino,
Urea groups, sulfydryl, epoxy radicals, acrylic or acryloxy.
6. chemical mechanical polishing liquid as claimed in claim 5, it is characterised in that the R in the formula is alkyl, wherein containing
1-10 carbon atom, A, B and C in the formula are respectively selected from chloro, methoxyl group, ethyoxyl, methoxy ethoxy, acetyl oxygen
Base or hydroxyl.
7. chemical mechanical polishing liquid as claimed in claim 6, it is characterised in that the alkyl contains 3-7 carbon atom, and institute
Stating the carbon atom on alkyl carbon chain can be substituted by oxygen, nitrogen, sulphur, phosphine, halogen or silicon atom.
8. chemical mechanical polishing liquid as claimed in claim 7, it is characterised in that the silicon-containing organic compound is selected from 3- amino
Propyl-triethoxysilicane (trade name KH-550), γ-(2,3- glycidoxies) propyl trimethoxy silicane (trade name KH-
560), γ-(methacryloxypropyl) propyl trimethoxy silicane (trade name KH-570), gamma-mercaptopropyltriethoxysilane (business
Name of an article KH-580), N- (β-aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane (trade name KH-602), γ-aminoethyl ammonia
In propyl trimethoxy silicane (trade name KH-792) and/or γ-aminopropyltriethoxy diethoxy silane (trade name KH-902)
One or more.
9. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the content of the siliceous organic compound is
0.001~1wt%.
10. chemical mechanical polishing liquid as claimed in claim 9, it is characterised in that the content of the siliceous organic compound
For 0.01~0.5wt%.
11. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the complexing agent is that daiamid is hyperbranched
Polymer.
12. chemical mechanical polishing liquid as claimed in claim 11, it is characterised in that the daiamid dissaving polymer choosing
From the daiamid dissaving polymer of amino end group and/or the daiamid dissaving polymer of carboxyl end groups.
13. chemical mechanical polishing liquid as claimed in claim 11, it is characterised in that the daiamid dissaving polymer
Molecular weight is 6000~100000.
14. chemical mechanical polishing liquid as claimed in claim 13, it is characterised in that the daiamid dissaving polymer
Molecular weight is 9000~50000.
15. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the content of the complexing agent be 0.01~
1.5wt%.
16. chemical mechanical polishing liquid as claimed in claim 15, it is characterised in that the content of the complexing agent be 0.01~
0.5wt%.
17. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the electrolyte ion is selected from metal ion
And/or nonmetallic ion, its concentration are 0.1~1mol/Kg.
18. chemical mechanical polishing liquid as claimed in claim 17, it is characterised in that the electrolyte ion is potassium ion.
19. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the pH of the chemical mechanical polishing liquid is 1-
7。
20. chemical mechanical polishing liquid as claimed in claim 19, it is characterised in that the pH of the chemical mechanical polishing liquid is 4-
5。
21. chemical mechanical polishing liquid as claimed in claim 1, it is characterised in that the siliceous organic compound by with
Under type is added in the chemical mechanical polishing liquid：
A. abrasive grains are first bonded before polishing fluid is prepared with silicon-containing compound, then add the modified abrasive grains in surface
Enter into chemical mechanical polishing liquid；
B. when producing chemical mechanical polishing liquid, by the siliceous organic compound and the abrasive grains, the electrolyte
Ion and the complexing agent mix simultaneously；And/or
C. the siliceous organic compound complete hydrolysis or partial hydrolysis are first generated into Si-OH groups, then adding
Learn in machine polishing liquor.
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|---|---|---|---|
| CN201610633767.7A CN107686703A (en) | 2016-08-04 | 2016-08-04 | A kind of chemical mechanical polishing liquid |
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| CN201610633767.7A CN107686703A (en) | 2016-08-04 | 2016-08-04 | A kind of chemical mechanical polishing liquid |
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| CN107686703A true CN107686703A (en) | 2018-02-13 |
Family
ID=61151444
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115109519A (en) * | 2021-03-18 | 2022-09-27 | 三星Sdi株式会社 | Chemical mechanical polishing slurry composition and method for polishing tungsten pattern wafer |
| CN115305010A (en) * | 2021-03-18 | 2022-11-08 | 三星Sdi株式会社 | Chemical mechanical polishing slurry composition and method for polishing tungsten pattern wafer |
| CN115710463A (en) * | 2021-08-23 | 2023-02-24 | 三星Sdi株式会社 | CMP slurry composition for patterning tungsten wafer and tungsten polishing method |
-
2016
- 2016-08-04 CN CN201610633767.7A patent/CN107686703A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115109519A (en) * | 2021-03-18 | 2022-09-27 | 三星Sdi株式会社 | Chemical mechanical polishing slurry composition and method for polishing tungsten pattern wafer |
| CN115305010A (en) * | 2021-03-18 | 2022-11-08 | 三星Sdi株式会社 | Chemical mechanical polishing slurry composition and method for polishing tungsten pattern wafer |
| CN115305010B (en) * | 2021-03-18 | 2024-04-26 | 三星Sdi株式会社 | Chemical mechanical polishing slurry composition and method for polishing tungsten pattern wafer |
| CN115710463A (en) * | 2021-08-23 | 2023-02-24 | 三星Sdi株式会社 | CMP slurry composition for patterning tungsten wafer and tungsten polishing method |
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