CN102533121A - Chemically mechanical polishing solution for polishing tungsten - Google Patents
Chemically mechanical polishing solution for polishing tungsten Download PDFInfo
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- CN102533121A CN102533121A CN2010106069549A CN201010606954A CN102533121A CN 102533121 A CN102533121 A CN 102533121A CN 2010106069549 A CN2010106069549 A CN 2010106069549A CN 201010606954 A CN201010606954 A CN 201010606954A CN 102533121 A CN102533121 A CN 102533121A
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- Prior art keywords
- mechanical polishing
- chemical mechanical
- polishing liquid
- polishing
- liquid according
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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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
-
- 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
Abstract
The invention discloses chemically mechanical polishing solution which comprises water, gas phase method silicon dioxide, silver ions, sulfate ions and peroxides. The polishing solution has extremely great tungsten polishing speed, and meanwhile, the polishing selection ratio of tungsten and carbon dioxide are obviously improved.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid, relate in particular to a kind of chemical mechanical polishing liquid that is used for the polish tungsten material.
Background technology
Continuous development along with semiconductor technology; And the continuous increase of large-scale integrated circuit interconnection layer; It is particularly crucial that the planarization of conductive layer and insulating medium layer becomes; Wherein, by IBM Corporation twentieth century eighties initiative chemically machinery polished (CMP) technology be considered to the effective means of present overall planarization.Chemically machinery polished (CMP) is a kind ofly to be combined by chemical action, mechanical effect and this two kinds of effects and realize the technology of planarization; It is usually by a grinding stage that has polishing pad, and a grinding head that is used for carries chips is formed.Wherein grinding head is fixed chip, and the front with chip is pressed on the polishing pad then, and when carrying out chemically machinery polished, grinding head linearity on polishing pad moves or rotates along the heading the same with grinding stage; Meanwhile, the slurries that contain abrasive are dripped on the polishing pad, and are tiled on the polishing pad because of centrifugation.Chip surface is realized overall planarization under machinery and chemical dual effect.
Main mechanism to metal level chemically machinery polished (CMP) is considered to: oxygenant is first with the oxidation on metal surface film forming, is that the abrasive of representative is removed this layer sull machinery with silicon-dioxide and aluminum oxide, produces new metallic surface; The new metallic surface that produces is continued oxidized, these two kinds collaborative the carrying out of effect.
As the tungsten of one of chemically machinery polished (CMP) object, under HCD, anti-electronic migration ability is strong, and can form good ohmic contact with silicon, so can be used as the filler metal and the diffusion impervious layer of contact hole and interlayer hole.
The chemically machinery polished (CMP) of tungsten at present; Several different methods is arranged; As: the Tripotassium iron hexacyanide of reports such as F. B. Kaufman is used for method (" Chemical Mechanical Polishing for Fabricating Patterned W Metal Features as Chip Interconnects ", Journal of the Electro chemical Society, the Vol.138 of tungsten chemically machinery polished; No.11; In November, 1991), U.S. Pat 5340370 disclosed a kind of formula of size that are used for tungsten chemically machinery polished (CMP), wherein contain the Tripotassium iron hexacyanide and silica abrasive, contain acetate simultaneously as the pH buffer reagent.Because the Tripotassium iron hexacyanide is under UV-light or sun exposure, and in acidic medium, can decomposite the prussic acid of severe toxicity, thereby limit it and be widely used.
U.S. Pat 5527423 disclosed metal level chemical mechanical polishing liquids, the disclosed method of polishing semiconductor wafer of U.S. Pat 006008119A and U.S. Pat 6284151 disclosed tungsten chemical mechanical polishing slurries etc. all adopt Fe (NO
3)
3/ alumina system is used for tungsten mechanical polishing (CMP).This polishing body ties up to static etch rate (static etch rate) aspect and has advantage, but owing to adopt aluminum oxide as abrasive, product defects (defect) aspect exists significantly not enough.The iron nitrate of high density makes the pH value of polishing fluid be strongly-acid simultaneously, and severe corrosion equipment simultaneously, generates iron rust, pollutes polishing pad.In addition, the conduct of the iron ion of high density is metals ion movably, has seriously reduced the safety of semiconductor components and devices.
USP 5225034 discloses hydrogen peroxide and the common finishing method that carries out metal (copper) as oxygenant that uses of Silver Nitrate with USP 5354490.But in the type method, the Silver Nitrate consumption is big (greater than 2%) very, causes the polishing fluid cost too high, unstable, the easy deposition of abrasive, problems such as the quick decomposition of ydrogen peroxide 50.
U.S. Pat 5958288 disclosed metal CMP polishing compositions adopt iron nitrate to be used as catalyzer; Hydrogen peroxide is used as oxygenant, carries out the tungsten chemically machinery polished, it should be noted that; In this patent; Mentioned multiple transition metal, significantly effectively had only ferro element by experiment confirm, actual implementation result and the scope that therefore should invent are very limited.Though this method has reduced the consumption of iron nitrate significantly, because iron ion still exists, and the Fenton reaction takes place between the ydrogen peroxide 50, ydrogen peroxide 50 can be rapidly and decomposition failure tempestuously, so there is the problem of poor stability in this polishing fluid.
U.S. Pat 5980775 open metal CMP polishing slurries and U.S. Pat 6068787 disclosed polishing slurries are on U.S. Pat 5958288 bases; Add organic acid and make stablizer; Improved the rate of decomposition of hydrogen peroxide, but hydrogen peroxide decomposition speed is still higher, hydrogen peroxide concentration can reduce more than 10% in common two weeks; Cause polishing velocity to descend, polishing fluid is decomposition failure gradually.
Because the static corrosion speed of tungsten is very fast in the system of iron and ydrogen peroxide 50, directly have influence on the yield of production, need further to add the static corrosion suppressor factor of tungsten for this reason.Like disclosed polishing composition and the disclosed polishing composition that comprises inhibitor of tungsten etching of CN1966594A that comprises inhibitor of tungsten etching of Chinese patent CN1326199C; The erosion inhibitor that all in the system of ydrogen peroxide 50 and iron catalyst, has added tungsten suppresses the corrosion of tungsten.
Above patent has also improved the polishing velocity of silicon-dioxide in the speed that improves tungsten, but has but reduced the polishing selection ratio of tungsten and silicon-dioxide.
Therefore, need a kind of chemical mechanical polishing liquid polishing selection ratio, polish tungsten that promptly can have very high tungsten polishing velocity, can improve tungsten and silicon-dioxide simultaneously again now.
Summary of the invention
The invention provides a kind of chemical mechanical polishing liquid that is used for tungsten, adopt fumed silica, to obtain a kind of polishing fluid that tungsten and silicon-dioxide polish fast selection ratio that improves as abrasive and silver ions and sulfate ion, superoxide combination.The technical problem that the present invention solves is in the polishing velocity that guarantees very high tungsten, has reduced the polishing velocity of silicon-dioxide, thereby has improved the polishing selection ratio of tungsten and silicon-dioxide.
Technical scheme of the present invention is following:
Invent a kind of chemical mechanical polishing liquid, comprise water, fumed silica abrasive, can produce the compound of silver ions, the compound that can produce sulfate ion, superoxide.
Wherein, the quality percentage composition of said fumed silica abrasive is 0.1 ~ 10%, and is preferably 0.5 ~ 6%; Said fumed silica abrasive median size is 100 ~ 200 nanometers (light scattering methods).
Wherein, In the soluble silver salt that the said compound that can produce silver ions can be Sulfuric acid disilver salt, Silver Nitrate, tachyol and/or silver perchlorate one or more; The mass percent of said soluble silver salt is preferably 0.05% ~ 0.3%, and best mass percent is 0.1 ~ 0.25%.
Wherein, the said compound that can produce sulfate ion can be a vitriol, preferablely is chosen as in the nonmetallic vitriol one or more; Wherein, said nonmetal vitriol is preferably ammonium sulfate.Said vitriol mass percent is preferably 0.005% ~ 1.%, and further is preferably 0.1% ~ 0.5%.
Wherein, said superoxide is preferably hydrogen peroxide, and its content is preferably mass percent 0.1 ~ 5%, and optimum content is a mass percent 1 ~ 2%.
Polishing fluid of the present invention can also further contain the pH regulator agent; Preferably, polishing fluid pH value of the present invention is 0.5 ~ 5.
Positive progressive effect of the present invention is:
The present invention provides a kind of polishing fluid, and this polishing fluid has very high tungsten polishing velocity, has improved the polishing selection ratio of tungsten and silicon-dioxide simultaneously.
Embodiment
The invention provides a kind of chemical mechanical polishing liquid that is used for polish tungsten, comprise water, fumed silica abrasive, can produce the compound of silver ions, the compound that can produce sulfate ion, superoxide.
Wherein, one or more in the soluble silver salt that the said compound that can produce silver ions can be Sulfuric acid disilver salt, Silver Nitrate, tachyol and/or silver perchlorate, the mass percent of silver salt is preferably 0.05% ~ 0.3%, and best mass percent is 0.1 ~ 0.25%.
Wherein, the said compound that can produce sulfate ion can be a vitriol, preferable comes from the nonmetallic vitriol one or more; Said vitriol mass percent is preferably 0.005% ~ 1%, and further is preferably 0.1% ~ 0.5%.
The above-mentioned compound that can produce silver ions and sulfate ion can be with a kind of compound, like Sulfuric acid disilver salt.
Wherein, said fumed silica abrasive quality percentage composition is preferably 0.1 ~ 10%, further is preferably 0.5 ~ 6%.Said fumed silica abrasive median size is preferably 100 ~ 200 nanometers (light scattering method).
Wherein, chemical mechanical polishing liquid of the present invention can also comprise the pH regulator agent, and the pH value of said polishing fluid is adjusted to 0.5 ~ 5.
Be described in detail through the chemical mechanical polishing liquid of specific embodiment below polish tungsten of the present invention, so that better understand the present invention, but following embodiment does not limit the scope of the invention.
Embodiment 1
The chemical mechanical polishing liquid of polish tungsten of the present invention comprises Silver Nitrate (silver ions is provided), ammonium sulfate (sulfate ion is provided), ydrogen peroxide 50 (hydrogen peroxide) and vapor phase process silica abrasive.The quality percentage composition and the pH value of each main ingredient are seen table 1.
Each component mixes in deionized water, and the pH value of using the pH regulator agent to regulate polishing fluid is 2.5.
Embodiment 2 ~ 5 and 11
With reference to embodiment 1, the embodiment of the invention 2 ~ 5 and 11 chemical mechanical polishing liquid main ingredient mass content are seen table 1.
Embodiment 6 and 10
With reference to embodiment 1, the embodiment of the invention 6 and 10 chemical mechanical polishing liquids adopt vitriolate of tartar that sulfate ion is provided, and each main ingredient mass percent is seen table 1.
Embodiment 7
With reference to embodiment 1, the embodiment of the invention 7 chemical mechanical polishing liquids adopt manganous sulfate that sulfate ion is provided, and each main ingredient mass percent is seen table 1.
Embodiment 8 ~ 9
The embodiment of the invention 8 and 9 adopts Sulfuric acid disilver salt that silver ions and sulfate ion are provided simultaneously, and abrasive adopts fumed silica, and ydrogen peroxide 50 is an oxygenant.Each component mixes in deionized water, adds the pH regulator agent and regulates the pH value.
Each main ingredient mass content and polishing fluid pH value are seen table 1.
Comparative Examples 1 ~ 7
With the silicon sol is abrasive, and ydrogen peroxide 50 is an oxygenant, the chemical mechanical polishing liquid of preparation Comparative Examples 1 ~ 7.
Wherein, Comparative Examples 1 does not add silver ions and sulfate ion; Comparative Examples 2 adds Silver Nitrate on the basis of Comparative Examples 1 provide silver ions; Comparative Examples 3 ~ 7 adds ammonium sulfate on the basis of Comparative Examples 2 provide sulfate ion.
Each component mixes in deionized water, adds pH value regulator and regulates the pH value, prepares the contrast polishing fluid.
Comparative Examples main ingredient mass percent and polishing fluid pH value are seen table 2.
In
table 1, the fumed silica median size records by light scattering method.
carries out the chemically machinery polished of tungsten respectively with the polishing fluid of preparing in the foregoing description and the Comparative Examples, and polishing effect is compared.Table 3 is seen in concrete contrast.
Polishing condition: polishing machine platform is Logitech (Britain) 1PM52 type, polytex polishing pad, 4cm * 4cm square wafer (Wafer); Grinding pressure 4psi; 70 rev/mins of grinding stage rotating speeds, 150 rev/mins of grinding head rotation rotating speeds, polishing fluid rate of addition 100 ml/ minutes.
Comparative Examples 2 shows: under abrasive, ydrogen peroxide 50 and Silver Nitrate combination, the polishing velocity of tungsten is very low, and the silicon-dioxide polishing speed is higher, and the polishing selection ratio of tungsten and silicon-dioxide is also very low.
Comparative Examples 3 ~ 7 shows: under the combination of silver ions, sulfate radical and ydrogen peroxide 50, use the abrasive of silicon sol, though can significantly improve the polishing velocity of tungsten, the silicon-dioxide polishing speed obviously improves, and the polishing selection ratio of tungsten and silicon-dioxide is very low.
Embodiment 1 ~ 5 shows: under the combination of silver ions, sulfate radical and ydrogen peroxide 50; Use the abrasive of fumed silica; When significantly improving the polishing velocity of tungsten, reduced the polishing velocity of silicon-dioxide, thereby improved the polishing selection ratio of tungsten and silicon-dioxide.
More than specific embodiment of the present invention is described in detail, but it is just as example, the present invention is not restricted to the specific embodiment of above description.To those skilled in the art, any equivalent modifications that the present invention is carried out with substitute also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of being done under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (17)
1. the chemical mechanical polishing liquid of a polish tungsten is characterized in that, comprising: water, fumed silica abrasive, the compound that can produce silver ions, the compound that can produce sulfate ion, superoxide.
2. chemical mechanical polishing liquid according to claim 1 is characterized in that, said fumed silica abrasive mass percent is 0.1 ~ 10%.
3. chemical mechanical polishing liquid according to claim 2 is characterized in that, said fumed silica abrasive mass percent is 0.5 ~ 6%.
4. according to claim 1,2 or 3 described chemical mechanical polishing liquids, it is characterized in that said fumed silica abrasive median size is 100 ~ 200 nanometers.
5. chemical mechanical polishing liquid according to claim 1 is characterized in that, the said compound that can produce silver ions is the soluble silver salt of Sulfuric acid disilver salt, Silver Nitrate, tachyol and/or silver perchlorate.
6. chemical mechanical polishing liquid according to claim 5 is characterized in that, the mass percent of said soluble silver salt is 0.05% ~ 0.3%.
7. chemical mechanical polishing liquid according to claim 6 is characterized in that, the mass percent of said soluble silver salt is 0.1% ~ 0.25%.
8. chemical mechanical polishing liquid according to claim 1 is characterized in that, the said compound that can produce sulfate ion is a vitriol.
9. chemical mechanical polishing liquid according to claim 8 is characterized in that, said vitriol is nonmetal vitriol.
10. chemical mechanical polishing liquid according to claim 9 is characterized in that, said nonmetal vitriol is ammonium sulfate.
11. chemical mechanical polishing liquid according to claim 8 is characterized in that, said vitriol mass percent is 0.005% ~ 1%.
12. chemical mechanical polishing liquid according to claim 11, wherein, said vitriol mass percent is 0.1% ~ 0.5%.
13. chemical mechanical polishing liquid according to claim 1 is characterized in that, said superoxide is a hydrogen peroxide.
14. chemical mechanical polishing liquid according to claim 13 is characterized in that, said hydrogen peroxide mass percent is 0.1 ~ 5%.
15. chemical mechanical polishing liquid according to claim 14 is characterized in that, said superoxide mass percent is 1 ~ 2%.
16. chemical mechanical polishing liquid according to claim 1 is characterized in that, described chemical mechanical polishing liquid also comprises the pH regulator agent.
17. chemical mechanical polishing liquid according to claim 16 is characterized in that, the pH value of described chemical mechanical polishing liquid is 0.5 ~ 5.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010606954.9A CN102533121B (en) | 2010-12-27 | 2010-12-27 | A kind of chemical mechanical polishing liquid of polish tungsten |
| PCT/CN2011/002134 WO2012088756A1 (en) | 2010-12-27 | 2011-12-19 | Chemical mechanical polishing slurry for polishing tungsten |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010606954.9A CN102533121B (en) | 2010-12-27 | 2010-12-27 | A kind of chemical mechanical polishing liquid of polish tungsten |
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| CN102533121A true CN102533121A (en) | 2012-07-04 |
| CN102533121B CN102533121B (en) | 2016-01-27 |
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| WO (1) | WO2012088756A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103774150A (en) * | 2012-10-25 | 2014-05-07 | 安集微电子（上海）有限公司 | CMP (Chemical Mechanical Polishing) solution |
| CN109269867A (en) * | 2018-09-11 | 2019-01-25 | 大连理工大学 | Tungsten nickel iron alloy polishing fluid and alloy surface polishing, metallographic preparation method |
| US10655035B2 (en) | 2017-05-25 | 2020-05-19 | Saint-Gobain Ceramics & Plastics, Inc. | Oxidizing fluid for the chemical-mechanical polishing of ceramic materials |
| CN111378373A (en) * | 2018-12-28 | 2020-07-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution for polishing tungsten |
| CN111378374A (en) * | 2018-12-28 | 2020-07-07 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10655035B2 (en) | 2017-05-25 | 2020-05-19 | Saint-Gobain Ceramics & Plastics, Inc. | Oxidizing fluid for the chemical-mechanical polishing of ceramic materials |
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| CN109269867A (en) * | 2018-09-11 | 2019-01-25 | 大连理工大学 | Tungsten nickel iron alloy polishing fluid and alloy surface polishing, metallographic preparation method |
| CN109269867B (en) * | 2018-09-11 | 2020-12-11 | 大连理工大学 | Tungsten-nickel-iron alloy polishing solution and alloy surface polishing and metallographic phase preparation method |
| CN111378373A (en) * | 2018-12-28 | 2020-07-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution for polishing tungsten |
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| CN111378374B (en) * | 2018-12-28 | 2022-05-13 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing solution |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2012088756A1 (en) | 2012-07-05 |
| CN102533121B (en) | 2016-01-27 |
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