SEMICONDUCTOR TECHNOLOGY

Removal of residual CuO particles on the post CMP wafer surface of multi-layered copper

Yan Li, Ming Sun, Xinhuan Niu, Yuling Liu, Yangang He, Hailong Li, Aochen Wang and Hongbo Li

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 Corresponding author: Liu Yuling, Email:lyl@hebut.edu.cn

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Abstract: This article introduces the removal technology of CuO particles on the post CMP wafer surface of multi-layered copper. According to the Cu film corrosion curve with different concentrations of H2O2 and the effect curve of time on the growth rate of CuO film, CuO film with the thickness of 220 nm grown on Cu a surface was successfully prepared without the interference of CuCl2· 2H2O. Using the static corrosion experiment the type of chelating agent (FA/O Ⅱ type chelating agent) and the concentration range (10-100 ppm) for CuO removal was determined, and the Cu removal rate was close to zero. The effect of surfactant on the cleaning solution properties was studied, and results indicated that the surfactant has the effect of reducing the surface tension and viscosity of the cleaning solution, and making the cleaning agent more stable. The influence of different concentrations of FA/O Ⅰ type surfactant and the mixing of FA/O Ⅱ type chelating agent and FA/O Ⅰ type surfactant on the CuO removal effect and the film surface state was analyzed. The experimental results indicated that when the concentration of FA/O Ⅰ type surfactant was 50 ppm, CuO particles were quickly removed, and the surface state was obviously improved. The best removal effect of CuO on the copper wiring film surface was achieved with the cleaning agent ratio of FA/O Ⅱ type chelating agent 75 ppm and FA/O Ⅰ type surfactant 50 ppm. Finally, the organic residue on the copper pattern film after cleaning with that cleaning agent was detected, and the results showed that the cleaning used agent did not generate organic residues on the film surface, and effectively removes the organic residue on the wafer.

Key words: electrochemical curvesCuO particleschelating agentthe step value of corrosion pointalkaline cleaning solutionsurface roughnessorganic residues



[1]
Hu Yi, Liu Yuling, Liu Xiaoyan. Effect of copper slurry on polishing characteristics. Journal of Semiconductors, 2011, 32(11):116001 doi: 10.1088/1674-4926/32/11/116001
[2]
Hu Yi, Liu Yuling, Liu Xiaoyan. Effect of alkaline slurry on the electric character of the pattern Cu wafer. Journal of Semiconductors, 2011, 32(7):076002 doi: 10.1088/1674-4926/32/7/076002
[3]
Gao Baohong, Liu Yuling, Wang Chenwei. A new cleaning process for the metallic contaminants on a post-CMP wafer's surface. Journal of Semiconductors, 2010, 31(10):106004 doi: 10.1088/1674-4926/31/10/106004
[4]
Sulyma C M, Roy D. Electrochemical characterization of surface complexes formed on Cu and Ta in succinic acid based solutions used for chemical mechanical planarization. Appl Surf Sci, 2010, 256:2583 doi: 10.1016/j.apsusc.2009.10.108
[5]
Oh S, Seok J. An integrated material removal model for silicon dioxide layers in chemical mechanical polishing processes. Wear, 2009, 266(7/8):839 http://www.sciencedirect.com/science/article/pii/S0043164808004328
[6]
Tsai T C, Tsao W C, Lin W, et al. CMP process development for the via-middle 3D TSV applications at 28 nm technology node. Microelectron Eng, 2012, 92(3):29 http://dl.acm.org/citation.cfm?id=2169899
[7]
Pandija S, Roy D, Babu S V. Achievement of high planarization efficiency in CMP of copper at a reduced down pressure. Microelectron Eng, 2009, 86:367 doi: 10.1016/j.mee.2008.11.047
[8]
Zhang W, Lu X C, Liu Y H, et al. Inhibitors for organic phosphonic acid system abrasive free polishing of Cu. Appl Surf Sci, 2009, 255:4114 doi: 10.1016/j.apsusc.2008.10.096
[9]
Weng T, Mishra A, Guo Y. Regulation of lung surfactant secretion by microRNA-150. Biochemical and Biophysical Research Communications, 2012, 422:586 doi: 10.1016/j.bbrc.2012.05.030
[10]
Peterson E R, Shearer M. Simulation of spreading surfactant on a thin liquid film. Applied Mathematics and Computation, 2012, 218:5157 doi: 10.1016/j.amc.2011.11.002
[11]
Ochedzan-Siodlak W, Dziubek K, Siodlak D. Densities and viscosities of imidazolium and pyridinium chloroaluminate ionic liquids. Journal of Molecular Liquids, 2013, 177:85 doi: 10.1016/j.molliq.2012.10.001
[12]
Gharagheizi F, Ilani-Kashkouli P, Mohammadi A H, et al. Development of a group contribution method for determination of viscosity of ionic liquids at atmospheric pressure. Chem Eng Sci, 2012, 80:326 doi: 10.1016/j.ces.2012.06.045
[13]
Murata J, Sadakuni S, Okamoto T. Structural and chemical characteristics of atomically smooth GaN surfaces prepared by abrasive-free polishing with Pt catalyst. J Crystal Growth, 2012, 349:83 doi: 10.1016/j.jcrysgro.2012.04.007
[14]
Shattuck K G, Lin J Y, Cojocaru P. Characterization of phosphate electrolytes for use in Cu electrochemical mechanical planarization. Electrochemical Acta, 2008, 53:8211 doi: 10.1016/j.electacta.2008.05.077
[15]
Yang J C, Oh D W, Lee G W, et al. Step height removal mechanism of chemical mechanical planarization (CMP) for sub-nano-surface finish. Wear, 2010, 268(3/4):505 http://www.sciencedirect.com/science/article/pii/S0043164809005353
[16]
Ng D, Kulkarni M, Johnson J. Oxidation and removal mechanisms during chemical-mechanical planarization. Wear, 2007, 263:1477 doi: 10.1016/j.wear.2006.11.023
[17]
Zheng J P, Roy D. Electrochemical examination of surface films formed during chemical mechanical planarization of copper in acetic acid and dodecyl sulfate solutions. Thin Solid Films, 2009, 517(16):4587 doi: 10.1016/j.tsf.2009.03.063
Fig. 1.  Structure schematic of the Cu blanket film.

Fig. 2.  Structure schematic of the copper wiring film.

Fig. 3.  The electrochemical curves of different concentrations of H$_{2}$O$_{2}$.

Fig. 4.  Effect of time on the thickness of CuO film.

Fig. 5.  Step test chart of CuO corrosion point.

Fig. 6.  Topography of CuO corrosion transition zone before cleaning.

Fig. 7.  Step test chart of CuO corrosion point after cleaning using DIW.

Fig. 8.  Step test chart of CuO corrosion point before and after cleaning using DIW.

Fig. 9.  Effect of concentration of chelating agent of Cu and CuO.

Fig. 10.  The effect of concentration of surfactant on the corrosion rate viscosity and surface tension.

Fig. 11.  The effect of time on the viscosity of cleaning solution.

Fig. 12.  The surface roughness of the center and middle before and after cleaning.

Fig. 13.  The surface morphology of center and middle before and after cleaning.

Fig. 14.  The surface roughness of different areas before and after cleaning.

Fig. 15.  The surface morphology of different area before and after cleaning.

Fig. 16.  The infrared spectra of the copper wiring film before cleaning.

Fig. 17.  The infrared spectra of the copper wiring film after cleaning.

Fig. 18.  The infrared spectra of the copper wiring film before and after cleaning.

[1]
Hu Yi, Liu Yuling, Liu Xiaoyan. Effect of copper slurry on polishing characteristics. Journal of Semiconductors, 2011, 32(11):116001 doi: 10.1088/1674-4926/32/11/116001
[2]
Hu Yi, Liu Yuling, Liu Xiaoyan. Effect of alkaline slurry on the electric character of the pattern Cu wafer. Journal of Semiconductors, 2011, 32(7):076002 doi: 10.1088/1674-4926/32/7/076002
[3]
Gao Baohong, Liu Yuling, Wang Chenwei. A new cleaning process for the metallic contaminants on a post-CMP wafer's surface. Journal of Semiconductors, 2010, 31(10):106004 doi: 10.1088/1674-4926/31/10/106004
[4]
Sulyma C M, Roy D. Electrochemical characterization of surface complexes formed on Cu and Ta in succinic acid based solutions used for chemical mechanical planarization. Appl Surf Sci, 2010, 256:2583 doi: 10.1016/j.apsusc.2009.10.108
[5]
Oh S, Seok J. An integrated material removal model for silicon dioxide layers in chemical mechanical polishing processes. Wear, 2009, 266(7/8):839 http://www.sciencedirect.com/science/article/pii/S0043164808004328
[6]
Tsai T C, Tsao W C, Lin W, et al. CMP process development for the via-middle 3D TSV applications at 28 nm technology node. Microelectron Eng, 2012, 92(3):29 http://dl.acm.org/citation.cfm?id=2169899
[7]
Pandija S, Roy D, Babu S V. Achievement of high planarization efficiency in CMP of copper at a reduced down pressure. Microelectron Eng, 2009, 86:367 doi: 10.1016/j.mee.2008.11.047
[8]
Zhang W, Lu X C, Liu Y H, et al. Inhibitors for organic phosphonic acid system abrasive free polishing of Cu. Appl Surf Sci, 2009, 255:4114 doi: 10.1016/j.apsusc.2008.10.096
[9]
Weng T, Mishra A, Guo Y. Regulation of lung surfactant secretion by microRNA-150. Biochemical and Biophysical Research Communications, 2012, 422:586 doi: 10.1016/j.bbrc.2012.05.030
[10]
Peterson E R, Shearer M. Simulation of spreading surfactant on a thin liquid film. Applied Mathematics and Computation, 2012, 218:5157 doi: 10.1016/j.amc.2011.11.002
[11]
Ochedzan-Siodlak W, Dziubek K, Siodlak D. Densities and viscosities of imidazolium and pyridinium chloroaluminate ionic liquids. Journal of Molecular Liquids, 2013, 177:85 doi: 10.1016/j.molliq.2012.10.001
[12]
Gharagheizi F, Ilani-Kashkouli P, Mohammadi A H, et al. Development of a group contribution method for determination of viscosity of ionic liquids at atmospheric pressure. Chem Eng Sci, 2012, 80:326 doi: 10.1016/j.ces.2012.06.045
[13]
Murata J, Sadakuni S, Okamoto T. Structural and chemical characteristics of atomically smooth GaN surfaces prepared by abrasive-free polishing with Pt catalyst. J Crystal Growth, 2012, 349:83 doi: 10.1016/j.jcrysgro.2012.04.007
[14]
Shattuck K G, Lin J Y, Cojocaru P. Characterization of phosphate electrolytes for use in Cu electrochemical mechanical planarization. Electrochemical Acta, 2008, 53:8211 doi: 10.1016/j.electacta.2008.05.077
[15]
Yang J C, Oh D W, Lee G W, et al. Step height removal mechanism of chemical mechanical planarization (CMP) for sub-nano-surface finish. Wear, 2010, 268(3/4):505 http://www.sciencedirect.com/science/article/pii/S0043164809005353
[16]
Ng D, Kulkarni M, Johnson J. Oxidation and removal mechanisms during chemical-mechanical planarization. Wear, 2007, 263:1477 doi: 10.1016/j.wear.2006.11.023
[17]
Zheng J P, Roy D. Electrochemical examination of surface films formed during chemical mechanical planarization of copper in acetic acid and dodecyl sulfate solutions. Thin Solid Films, 2009, 517(16):4587 doi: 10.1016/j.tsf.2009.03.063
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    Received: 19 September 2013 Revised: Online: Published: 01 April 2014

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      Yan Li, Ming Sun, Xinhuan Niu, Yuling Liu, Yangang He, Hailong Li, Aochen Wang, Hongbo Li. Removal of residual CuO particles on the post CMP wafer surface of multi-layered copper[J]. Journal of Semiconductors, 2014, 35(4): 046001. doi: 10.1088/1674-4926/35/4/046001 Y Li, M Sun, X H Niu, Y L Liu, Y G He, H L Li, A C Wang, H B Li. Removal of residual CuO particles on the post CMP wafer surface of multi-layered copper[J]. J. Semicond., 2014, 35(4): 046001. doi: 10.1088/1674-4926/35/4/046001.Export: BibTex EndNote
      Citation:
      Yan Li, Ming Sun, Xinhuan Niu, Yuling Liu, Yangang He, Hailong Li, Aochen Wang, Hongbo Li. Removal of residual CuO particles on the post CMP wafer surface of multi-layered copper[J]. Journal of Semiconductors, 2014, 35(4): 046001. doi: 10.1088/1674-4926/35/4/046001

      Y Li, M Sun, X H Niu, Y L Liu, Y G He, H L Li, A C Wang, H B Li. Removal of residual CuO particles on the post CMP wafer surface of multi-layered copper[J]. J. Semicond., 2014, 35(4): 046001. doi: 10.1088/1674-4926/35/4/046001.
      Export: BibTex EndNote

      Removal of residual CuO particles on the post CMP wafer surface of multi-layered copper

      doi: 10.1088/1674-4926/35/4/046001
      Funds:

      the National Natural Science Foundation of Hebei Province, China E2013202247

      the Fund Project of Hebei Provincial Department of Education, China 2011128

      Project supported by the Major National Science and Technology Special Projects (No. 2009ZX02308), the National Natural Science Foundation of Hebei Province, China (No. E2013202247), and the Fund Project of Hebei Provincial Department of Education, China (No. 2011128)

      the Major National Science and Technology Special Projects 2009ZX02308

      More Information
      • Corresponding author: Liu Yuling, Email:lyl@hebut.edu.cn
      • Received Date: 2013-09-19
      • Published Date: 2014-04-01

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