CN103865402A - Chemically mechanical polishing liquid - Google Patents
Chemically mechanical polishing liquid Download PDFInfo
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- CN103865402A CN103865402A CN201210546342.4A CN201210546342A CN103865402A CN 103865402 A CN103865402 A CN 103865402A CN 201210546342 A CN201210546342 A CN 201210546342A CN 103865402 A CN103865402 A CN 103865402A
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Abstract
The invention discloses a chemically mechanical polishing liquid. The chemically mechanical polishing liquid comprises nano cerium oxide abrasive polishing solution, an oxidizing agent, a complexing agent, a corrosion inhibitor, and a chemical additive. Under the synergistic effects of cerium oxide, the oxidizing agent, the complexing agent, and the corrosion inhibitor, the chemically mechanical polishing liquid is capable of reaching a certain copper polishing removing rate, and avoiding or reducing generation of polishing defects on copper surfaces after polishing.
Description
Technical field
The present invention relates to a kind of chemical mechanical polishing liquid.
Background technology
Along with unicircuit is towards the development of the integrated direction of height, copper has replaced aluminium gradually as interconnecting material, and this is mainly because copper has relatively low resistivity, high deelectric transferred energy rate and short RC time of lag, can effectively improve the yield rate of chip, reduce the number of plies of wiring, shorten process period.
Copper is in the time of the interconnection line for the manufacture of unicircuit, and accurate polishing need to be carried out in its surface, to reach overall planarization, realizes multilayer interconnection.At present, about the existing more report of polishing fluid of copper polishing, but the document of reporting, patent mainly take silicon oxide or aluminum oxide as abrasive, research contents is mainly paid close attention to chemical reagent choosing and using as oxygenant, complexing agent or corrosion inhibitor, as people (Thin Solid Films such as Li Ying, 2006v497, p321) study and compared different abrasives as silicon oxide, aluminum oxide polishing effect and the mechanism to copper.To be that US6616717, US6821897 and CN100491072C more pay close attention to choosing and using of chemical reagent to the patent No., and ignored the research about cerium oxide abrasive particles in abrasive grains.
Cerium oxide is wide concerned a kind of chemically machinery polished abrasive material in recent years, and this is mainly due to its highly selective polishability ability to silicon-dioxide, and can reach high polishing effect under lower solid content.Therefore, the chemical mechanical polishing liquid take cerium oxide as abrasive material still has larger application prospect and the market advantage than traditional silicon oxide or alumina material in performance and cost.But because cerium oxide crystal pellet density is larger, in the aqueous solution, easily cause and reunite and sedimentation, in addition cerium oxide particle surface is often with sharp corners, easily cause producing various defects at polished dielectric surface in polishing process, be particularly very easy to cause the appearance of scuffing at relative softer copper surface.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of chemical mechanical polishing liquid take cerium oxide as abrasive material, add suitable chemical additive by selection, under the synergy of oxygenant, complexing agent and corrosion inhibitor, can realize copper is had to higher polish removal rate, reduce simultaneously or avoid the appearance of copper surface imperfection after polishing, polishing fluid has satisfactory stability.
In order to solve the problems of the technologies described above, the invention provides a kind of chemical mechanical polishing liquid, it contains chemical additive, polishing particles, oxygenant, complexing agent and corrosion inhibitor.
Wherein, chemical additive be in polycarboxylic acid compound, organic phospho acid compounds or polyvinylpyrrolidone (PVP) compounds one or more, concentration is 0.1-1.5wt%(mass percent).
Wherein, polycarboxylic acid compound can comprise poly carboxylic acid and salt compounds thereof, as poly-epoxy succinic acid is received (PESA), polyacrylic acid (PAA), maleic acid-acrylic acid copolymer (MA-AA), sodium polyacrylate (PAAS), hydrolytic polymaleic anhydride (HPMA) etc.; Organic phospho acid compounds includes machine phosphonic acid and salt compounds thereof, as Amino Trimethylene Phosphonic Acid (ATMP), 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (HEDP), ethylene diamine tetra methylene phosphonic acid (EDTMPA), diethylene triamine pentamethylene phosphonic (DTPMPA), ethylene diamine tetra methylene phosphonic acid sodium (EDTMPS) 2-HPAA (HPAA) etc.; Polyvinylpyrrolidone (PVP) compounds can be that relative molecular weight is one or more polymkeric substance within the scope of 1000-10000000, as PVP-K15, PVP-K17, PVP-K25, PVP-K30, PVP-K90 etc.Wherein, PVP is divided into level Four by its molecular-weight average size, and traditionally often with K value representation, different K values represents respectively corresponding PVP average molecular weight range.K value is actually the eigenwert relevant with the relative viscosity of the PVP aqueous solution, and viscosity is the physical quantity relevant with molecular weight of high polymer, therefore can characterize by K value the molecular-weight average of PVP.Conventionally K value is larger, and its viscosity is larger, and cementability is stronger.
Wherein, polishing particles is cerium oxide, and the median size of cerium oxide abrasive particle is 80-300 nanometer, preferably 120-280 nanometer.
Wherein, the concentration of cerium oxide abrasive is 0.25-2.5wt%, preferably 0.5-1.5wt%;
Wherein, oxygenant is without particular requirement, can be various commercially available oxygenants, be preferably hydrogen peroxide, Potassium Iodate, ammonium persulphate, Potassium Persulphate or ammonium nitrate, initiator system of ammonium persulfate or Potassium Iodate, the concentration of this oxygenant, without particular requirement, is generally 0.01-0.5wt%, and preferred concentration is 0.05-0.1wt%.
Wherein, complexing agent can be one or more in L-arginine, Padil, citric acid, quadrol, acetic acid, preferably acetic acid, quadrol and/or Padil, and the concentration of complexing agent is without particular requirement, be generally 0.01-1wt%, preferable range is 0.1-0.25wt%.
Wherein, the preferred benzotriazole compounds of corrosion inhibitor, is preferably benzotriazole and/or 3-amino-1,2,4-triazole, and the concentration of corrosion inhibitor, without particular requirement, is generally 0.01-0.1wt%, and preferable range is 0.05-0.1wt%.
Wherein, the pH value of polishing fluid disclosed in this invention is without particular restriction, and preferably pH value scope is 6.0-11.0, in polishing fluid disclosed in this invention, can add pH value conditioning agent, and described pH adjusting agent can be KOH or H
2sO
4;
Positive progressive effect of the present invention is: polishing fluid of the present invention selects cerium oxide as abrasive grains, and the synergy of combined oxidant, complexing agent and corrosion inhibitor has copper polishing speed and glazed surface feature relatively preferably.
Embodiment
Further set forth advantage of the present invention below by specific embodiment, but protection scope of the present invention is not only confined to following embodiment.
According to the composition of each embodiment and comparative example in table 1 and ratio preparation polishing fluid thereof, mix.It should be noted that in addition, the cerium oxide particle using in polishing fluid is the aqueous dispersions of original concentration 10wt% to 20wt%, and the particle diameter of particle is on average amounting to diameter, and its median size is measured by the Nano-ZS90 laser particle size analyzer of Malvern company; The grain fineness number of the cerium oxide particle using in polishing fluid is by the test of XRD-6100 Shimadzu X-ray diffractometer.
In table 1, the concrete dispensing mode of polishing fluid is: by the component except abrasive grains according to table in listed content, in deionized water, mix, be adjusted to required pH value with KOH, then add dispersion of abrasive particles, if declining, pH is adjusted to required pH value with KOH, and supply percentage composition to 100wt% with deionized water, can make chemical mechanical polishing liquid.
The formula of table 1 embodiment of the present invention and comparative example
Effect embodiment 1
In order further to investigate the polishing situation of such polishing fluid, the present invention has adopted following technique means: with the chemical mechanical polishing slurry of polishing fluid 1-5 in above-described embodiment and contrast 1-4, blank Cu wafer is carried out to polishing respectively, polishing condition is identical, burnishing parameters is as follows: Logitech polishing pad, downward pressure 3psi, rotary speed/rubbing head rotating speed=60/80rpm, polishing time 60s, chemical machinery is thrown flow rate of slurry 100mL/min.Polishing Cu wafer coupons used for example, forms by commercially available (U.S. SVTC company produces) 8 inches of plated film wafer coupons.The RT-7O/RG-7B tester that in polishing Cu wafer coupons used, Cu layer thickness is produced by NAPSON company records, and consumes the time obtain Cu and remove speed by the thickness difference recording before and after polishing divided by polishing.Polishing time is 1 minute.
The experimental technique of unreceipted actual conditions in embodiment, conventionally according to normal condition, or the condition of advising according to manufacturer.
As for scratch, after polishing, washing dry Cu wafer detect by an unaided eye subsequently and exist or do not have scratch spot under the pointolite in darkroom, and judgement criteria is as follows:
● detect by an unaided eye less than scratch spot
Zero detects by an unaided eye less than obvious scratch spot
× observe with the naked eye some scratch spots, but they are also unlikely to reach the amount that causes quality problems
△ observes with the naked eye obvious scratch spot, and reaches the amount that causes quality problems
Concrete outcome is as shown in table 2:
The polishing effect of table 2 embodiment 1-5 and comparative example 1-4
As can be seen from Table 2, in embodiment 1-5, by cerium oxide abrasives and specific oxygenant, complexing agent and corrosion inhibitor composite, compares with comparative example 1-4, has copper polishing speed and glazed surface feature relatively preferably.
Should be understood that, wt% of the present invention all refers to quality percentage composition.
Above specific embodiments of the invention be have been described in detail, 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 alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (29)
1. a chemical mechanical polishing liquid, is characterized in that, comprises chemical additive, polishing particles, oxygenant, complexing agent and corrosion inhibitor.
2. polishing fluid as claimed in claim 1, is characterized in that, selected chemical additive is selected from polycarboxylic acid compound, organic phospho acid compounds or polyvinylpyrrolidone (PVP) compounds one or more.
3. polishing fluid as claimed in claim 2, is characterized in that, described polycarboxylic acid compound is poly carboxylic acid and salt compounds thereof.
4. polishing fluid as claimed in claim 3, it is characterized in that, described polycarboxylic acid compound is selected from poly-epoxy succinic acid and receives (PESA), polyacrylic acid (PAA), maleic acid-acrylic acid copolymer (MA-AA), sodium polyacrylate (PAAS), one or more in hydrolytic polymaleic anhydride (HPMA).
5. polishing fluid as claimed in claim 2, is characterized in that, described organic phospho acid compounds is organic phospho acid and salt compounds thereof.
6. polishing fluid as claimed in claim 5; it is characterized in that, described organic phospho acid compounds is selected from one or more in Amino Trimethylene Phosphonic Acid (ATMP), 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid (HEDP), ethylene diamine tetra methylene phosphonic acid (EDTMPA), diethylene triamine pentamethylene phosphonic (DTPMPA), ethylene diamine tetra methylene phosphonic acid sodium (EDTMPS) 2-HPAA (HPAA).
7. polishing fluid as claimed in claim 2, is characterized in that, described polyvinylpyrrolidone (PVP) compounds is that relative molecular weight is one or more polymkeric substance within the scope of 1000-10000000.
8. polishing fluid as claimed in claim 7, is characterized in that, the K value of described polyvinylpyrrolidone (PVP) compounds is 15,17,25,30 and/or 90.
9. polishing fluid as claimed in claim 1, is characterized in that, described polishing particles is cerium oxide abrasive particles.
10. polishing fluid as claimed in claim 1, is characterized in that, the median size of described polishing particles is 80-300 nanometer.
11. polishing fluids as claimed in claim 10, is characterized in that, the median size of described polishing particles is 120-280 nanometer.
12. polishing fluids as claimed in claim 1, is characterized in that, the concentration of described polishing particles is 0.25-2.5wt%.
13. polishing fluids as claimed in claim 12, is characterized in that, the concentration of described polishing particles is 0.5-1.5wt%.
14. polishing fluids as claimed in claim 1, is characterized in that, described oxygenant is selected from one or more in hydrogen peroxide, Potassium Iodate, ammonium persulphate, Potassium Persulphate or ammonium nitrate.
15. polishing fluids as claimed in claim 14, is characterized in that, described oxygenant is selected from ammonium persulphate or Potassium Iodate.
16. polishing fluids as claimed in claim 1, is characterized in that, described oxidant concentration is 0.01-0.5wt%.
17. polishing fluids as claimed in claim 16, is characterized in that, described oxidant concentration is 0.05-0.1wt%.
18. polishing fluids as claimed in claim 1, is characterized in that, described complexing agent is selected from one or more in L-arginine, Padil, citric acid, quadrol, acetic acid.
19. polishing fluids as claimed in claim 18, is characterized in that, described complexing agent is selected from acetic acid, quadrol and/or Padil.
20. polishing fluids as claimed in claim 1, is characterized in that, the concentration of described complexing agent is 0.01-1wt%.
21. polishing fluids as claimed in claim 20, is characterized in that, the concentration of described complexing agent is 0.1-0.25wt%.
22. polishing fluids as claimed in claim 1, is characterized in that, described corrosion inhibitor is selected from benzotriazole compounds.
23. polishing fluids as claimed in claim 22, is characterized in that, described corrosion inhibitor is benzotriazole and/or 3-amino-1,2,4-triazole.
24. polishing fluids as claimed in claim 1, is characterized in that, the concentration of described corrosion inhibitor is 0.01-0.1wt%.
25. polishing fluids as claimed in claim 24, is characterized in that, the concentration of described corrosion inhibitor is 0.05-0.1wt%.
26. polishing fluids as claimed in claim 1, is characterized in that, the concentration of described chemical additive is 0.1-1.5wt%.
27. polishing fluids as described in claim 1-26 any one, is characterized in that, the pH value scope of described polishing fluid is 6.0-11.0.
28. polishing fluids as described in claim 1-26 any one, is characterized in that, described polishing fluid further comprises pH value conditioning agent.
The application in the medium surface finish including copper of 29. 1 kinds of polishing fluids as described in claim 1-26 any one.
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| CN201210546342.4A CN103865402A (en) | 2012-12-17 | 2012-12-17 | Chemically mechanical polishing liquid |
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| CN201210546342.4A CN103865402A (en) | 2012-12-17 | 2012-12-17 | Chemically mechanical polishing liquid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104592896A (en) * | 2014-12-31 | 2015-05-06 | 上海新安纳电子科技有限公司 | Chemical mechanical polishing solution |
| WO2016101332A1 (en) * | 2014-12-23 | 2016-06-30 | 尹先升 | Chemical mechanical polishing slurry |
| WO2018120807A1 (en) * | 2016-12-28 | 2018-07-05 | 安集微电子科技（上海）股份有限公司 | Chemical mechanical polishing liquid and applications thereof |
| CN110052898A (en) * | 2019-04-12 | 2019-07-26 | 东莞市嘉逸光电有限公司 | A kind of preparation method of ultra-thin glass |
| CN111378972A (en) * | 2018-12-29 | 2020-07-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN114790367A (en) * | 2022-04-28 | 2022-07-26 | 广东粤港澳大湾区黄埔材料研究院 | Nano spheroidal cerium oxide polishing solution for monocrystalline silicon and polycrystalline silicon and application |
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Cited By (7)
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| CN111378972A (en) * | 2018-12-29 | 2020-07-07 | 安集微电子（上海）有限公司 | Chemical mechanical polishing solution |
| CN110052898A (en) * | 2019-04-12 | 2019-07-26 | 东莞市嘉逸光电有限公司 | A kind of preparation method of ultra-thin glass |
| CN114790367A (en) * | 2022-04-28 | 2022-07-26 | 广东粤港澳大湾区黄埔材料研究院 | Nano spheroidal cerium oxide polishing solution for monocrystalline silicon and polycrystalline silicon and application |
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