Abstract

Very thin films deposited using atomic layer deposition (ALD) on aluminum mirrors showed extraordinary resistance toward concentrated alkali solutions, various chemical etchants, and solvents. Aluminum mirrors with no surface protection dissolved immediately in 24% aqueous KOH. Mirrors protected with 30nm electron-beam deposited silica film were fully removed in 30min. Mirrors with 10, 30, and 120nm films grown by ALD required, respectively, 10, 15, and 60 h of exposure to the alkali for the mirror to be fully removed. Likewise, large-scale hydrogen bubbling was observed immediately upon immersing mirrors coated with electron-beam deposited silica in aqueous KOH, whereas no visible hydrogen bubbling was detected for the mirror protected by ALD silica. For mirrors protected by 120nm ALD silica, a 2 h soak in various acid and solvent media produced no discernible change.

© 2009 Optical Society of America

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References

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  1. “Harsh-environment optics growing--market intelligence,” Fiber Optics Weekly Update, http://findarticles.com/p/articles/mi_m0NVN/is_4_24/ai_112985420/.
  2. “Fiber optics for harsh environment,” http://www.timbercon.com/Fiber-Optics-for-Harsh-Environment/.
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    [CrossRef]
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    [CrossRef] [PubMed]
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    [CrossRef]
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    [CrossRef]
  8. T. Suntola, “Atomic layer epitaxy,” Thin Solid Films 216, 84-89 (1992).
    [CrossRef]
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    [CrossRef]
  11. P. F. Carria, M. D. Groner, and S. M. George, “Ca test of Al2O3 gas diffusion barriers grown by atomic layer deposition on polymers,” Appl. Phys. Lett. 89, 031915 (2006).
    [CrossRef]
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    [CrossRef] [PubMed]
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    [CrossRef]
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    [CrossRef]
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    [CrossRef]
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    [CrossRef] [PubMed]
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  22. B. C. Wilson, “Optical coating applications on automotive polymers and displays,” presented at the New Technologies in Decorating and Assembly Meeting, Dearborn, Michigan, 10-11 June 2008.

2008 (4)

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

R. Cooper, T. K. Minton, X. Du, and S. M. George, “Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings,” Thin Solid Films 516, 4036-4039 (2008).
[CrossRef]

B. B. Burton, M. P. Boleslawski, A. T. Desombre, and S. M. George, “Rapid SiO2 atomic layer deposition using tris(tert-pentoxy) silanol,” Chem. Mater. 20, 7031-7043 (2008).
[CrossRef]

S. V. Mutilin and T. Khasanov, “The refractive index of homogeneous SiO2 thin films,” Opt. Spectrosc. 105, 461-465 (2008).
[CrossRef]

2006 (4)

M. D. Groner, S. M. George, and R. S. Mclean, “Gas diffusion barriers on polymers using Al2O3 atomic layer deposition,” Appl. Phys. Lett. 88, 051907 (2006).
[CrossRef]

P. F. Carria, M. D. Groner, and S. M. George, “Ca test of Al2O3 gas diffusion barriers grown by atomic layer deposition on polymers,” Appl. Phys. Lett. 89, 031915 (2006).
[CrossRef]

C. Chu, P. D. Fuqua, and J. D. Barrie, “Corrosion characterization of durable silver coatings by electrochemical impedance spectroscopy and accelerated environmental testing,” Appl. Opt. 45, 1583-1593 (2006).
[CrossRef] [PubMed]

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

2005 (1)

2002 (1)

D. Hausmann, J. Becker, S. Wang, and R. G. Gorden, “Rapid vapor deposition of highly conformal silica nanolaminates,” Science 298, 402-406 (2002).
[CrossRef] [PubMed]

1996 (2)

K. J. Hebert, S. Zafar, and E. A. Irene, “Measurement of the refractive index of thin SiO2 films using tunneling current oscillations and ellipsometry,” Appl. Phys. Lett. 68, 266-268 (1996).
[CrossRef]

S. M. George, A. W. Ott, and J. W. Klaus, “Surface chemistry for atomic layer growth,” J. Phys. Chem. 100, 13121-13131 (1996).
[CrossRef]

1992 (1)

T. Suntola, “Atomic layer epitaxy,” Thin Solid Films 216, 84-89 (1992).
[CrossRef]

Barrie, J. D.

Bates, S. C.

M. Pollack and S. C. Bates, “Taking optical probes into harsh environments,” http://archives.sensorsmag.com/articles/0600/76/.

Becker, J.

D. Hausmann, J. Becker, S. Wang, and R. G. Gorden, “Rapid vapor deposition of highly conformal silica nanolaminates,” Science 298, 402-406 (2002).
[CrossRef] [PubMed]

Boleslawski, M. P.

B. B. Burton, M. P. Boleslawski, A. T. Desombre, and S. M. George, “Rapid SiO2 atomic layer deposition using tris(tert-pentoxy) silanol,” Chem. Mater. 20, 7031-7043 (2008).
[CrossRef]

Burton, B. B.

B. B. Burton, M. P. Boleslawski, A. T. Desombre, and S. M. George, “Rapid SiO2 atomic layer deposition using tris(tert-pentoxy) silanol,” Chem. Mater. 20, 7031-7043 (2008).
[CrossRef]

Carria, P. F.

P. F. Carria, M. D. Groner, and S. M. George, “Ca test of Al2O3 gas diffusion barriers grown by atomic layer deposition on polymers,” Appl. Phys. Lett. 89, 031915 (2006).
[CrossRef]

Chu, C.

Cooper, R.

R. Cooper, T. K. Minton, X. Du, and S. M. George, “Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings,” Thin Solid Films 516, 4036-4039 (2008).
[CrossRef]

Desombre, A. T.

B. B. Burton, M. P. Boleslawski, A. T. Desombre, and S. M. George, “Rapid SiO2 atomic layer deposition using tris(tert-pentoxy) silanol,” Chem. Mater. 20, 7031-7043 (2008).
[CrossRef]

Du, X.

R. Cooper, T. K. Minton, X. Du, and S. M. George, “Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings,” Thin Solid Films 516, 4036-4039 (2008).
[CrossRef]

Fan, Z.

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

Fuqua, P. D.

George, S. M.

R. Cooper, T. K. Minton, X. Du, and S. M. George, “Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings,” Thin Solid Films 516, 4036-4039 (2008).
[CrossRef]

B. B. Burton, M. P. Boleslawski, A. T. Desombre, and S. M. George, “Rapid SiO2 atomic layer deposition using tris(tert-pentoxy) silanol,” Chem. Mater. 20, 7031-7043 (2008).
[CrossRef]

M. D. Groner, S. M. George, and R. S. Mclean, “Gas diffusion barriers on polymers using Al2O3 atomic layer deposition,” Appl. Phys. Lett. 88, 051907 (2006).
[CrossRef]

P. F. Carria, M. D. Groner, and S. M. George, “Ca test of Al2O3 gas diffusion barriers grown by atomic layer deposition on polymers,” Appl. Phys. Lett. 89, 031915 (2006).
[CrossRef]

S. M. George, A. W. Ott, and J. W. Klaus, “Surface chemistry for atomic layer growth,” J. Phys. Chem. 100, 13121-13131 (1996).
[CrossRef]

Gorden, R. G.

D. Hausmann, J. Becker, S. Wang, and R. G. Gorden, “Rapid vapor deposition of highly conformal silica nanolaminates,” Science 298, 402-406 (2002).
[CrossRef] [PubMed]

Groner, M. D.

P. F. Carria, M. D. Groner, and S. M. George, “Ca test of Al2O3 gas diffusion barriers grown by atomic layer deposition on polymers,” Appl. Phys. Lett. 89, 031915 (2006).
[CrossRef]

M. D. Groner, S. M. George, and R. S. Mclean, “Gas diffusion barriers on polymers using Al2O3 atomic layer deposition,” Appl. Phys. Lett. 88, 051907 (2006).
[CrossRef]

Hausmann, D.

D. Hausmann, J. Becker, S. Wang, and R. G. Gorden, “Rapid vapor deposition of highly conformal silica nanolaminates,” Science 298, 402-406 (2002).
[CrossRef] [PubMed]

Hebert, K. J.

K. J. Hebert, S. Zafar, and E. A. Irene, “Measurement of the refractive index of thin SiO2 films using tunneling current oscillations and ellipsometry,” Appl. Phys. Lett. 68, 266-268 (1996).
[CrossRef]

Hong, R.

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

Irene, E. A.

K. J. Hebert, S. Zafar, and E. A. Irene, “Measurement of the refractive index of thin SiO2 films using tunneling current oscillations and ellipsometry,” Appl. Phys. Lett. 68, 266-268 (1996).
[CrossRef]

Jerman, M.

Khasanov, T.

S. V. Mutilin and T. Khasanov, “The refractive index of homogeneous SiO2 thin films,” Opt. Spectrosc. 105, 461-465 (2008).
[CrossRef]

Klaus, J. W.

S. M. George, A. W. Ott, and J. W. Klaus, “Surface chemistry for atomic layer growth,” J. Phys. Chem. 100, 13121-13131 (1996).
[CrossRef]

LaRocca, F.

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

Leskela, M.

M. Ritala and M. Leskela, “Atomic layer deposition,” in Handbook of Thin Film Materials, H. S. Nalwa, ed. (Academic, 2001), pp. 103-161.

MacMurphy, S.

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

Makela, M.

M. Makela, P. Soininen, and S. Sneck, “Protective coating of silver,” U.S. patent application, IPC8 Class AC23C1640FI, USPC Class 42725519.

Mclean, R. S.

M. D. Groner, S. M. George, and R. S. Mclean, “Gas diffusion barriers on polymers using Al2O3 atomic layer deposition,” Appl. Phys. Lett. 88, 051907 (2006).
[CrossRef]

Mergel, D.

Minton, T. K.

R. Cooper, T. K. Minton, X. Du, and S. M. George, “Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings,” Thin Solid Films 516, 4036-4039 (2008).
[CrossRef]

Mutilin, S. V.

S. V. Mutilin and T. Khasanov, “The refractive index of homogeneous SiO2 thin films,” Opt. Spectrosc. 105, 461-465 (2008).
[CrossRef]

Nguyen, N. V.

N. V. Nguyen and C. A. Richer, “Thickness determination of ultra-thin SiO2 films on Si by spectroscopic ellipsometry,” in Silicon Nitride and Silicon Dioxide Insulating Thin Films, M. J. Deen, W. D. Brown, K. B. Sundaram, and S. I. Raider, eds. (Academic, 1997), pp. 183-193.

Ott, A. W.

S. M. George, A. W. Ott, and J. W. Klaus, “Surface chemistry for atomic layer growth,” J. Phys. Chem. 100, 13121-13131 (1996).
[CrossRef]

Ott, M. N.

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

Pollack, M.

M. Pollack and S. C. Bates, “Taking optical probes into harsh environments,” http://archives.sensorsmag.com/articles/0600/76/.

Qi, H.

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

Qiao, Z.

Raider, S. I.

N. V. Nguyen and C. A. Richer, “Thickness determination of ultra-thin SiO2 films on Si by spectroscopic ellipsometry,” in Silicon Nitride and Silicon Dioxide Insulating Thin Films, M. J. Deen, W. D. Brown, K. B. Sundaram, and S. I. Raider, eds. (Academic, 1997), pp. 183-193.

Richer, C. A.

N. V. Nguyen and C. A. Richer, “Thickness determination of ultra-thin SiO2 films on Si by spectroscopic ellipsometry,” in Silicon Nitride and Silicon Dioxide Insulating Thin Films, M. J. Deen, W. D. Brown, K. B. Sundaram, and S. I. Raider, eds. (Academic, 1997), pp. 183-193.

Ritala, M.

M. Ritala and M. Leskela, “Atomic layer deposition,” in Handbook of Thin Film Materials, H. S. Nalwa, ed. (Academic, 2001), pp. 103-161.

Shao, J.

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

Sneck, S.

M. Makela, P. Soininen, and S. Sneck, “Protective coating of silver,” U.S. patent application, IPC8 Class AC23C1640FI, USPC Class 42725519.

Soininen, P.

M. Makela, P. Soininen, and S. Sneck, “Protective coating of silver,” U.S. patent application, IPC8 Class AC23C1640FI, USPC Class 42725519.

Sun, X.

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

Suntola, T.

T. Suntola, “Atomic layer epitaxy,” Thin Solid Films 216, 84-89 (1992).
[CrossRef]

Switzer, R.

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

Thomes, W. J.

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

Wang, S.

D. Hausmann, J. Becker, S. Wang, and R. G. Gorden, “Rapid vapor deposition of highly conformal silica nanolaminates,” Science 298, 402-406 (2002).
[CrossRef] [PubMed]

Wilson, B. C.

B. C. Wilson, “Optical coating applications on automotive polymers and displays,” presented at the New Technologies in Decorating and Assembly Meeting, Dearborn, Michigan, 10-11 June 2008.

Zafar, S.

K. J. Hebert, S. Zafar, and E. A. Irene, “Measurement of the refractive index of thin SiO2 films using tunneling current oscillations and ellipsometry,” Appl. Phys. Lett. 68, 266-268 (1996).
[CrossRef]

Acta Phys. Sin. (1)

X. Sun, R. Hong, H. Qi, Z. Fan, and J. Shao, “Microstructure and optical constants of sputtered Ag films of different thickness,” Acta Phys. Sin. 55, 4923-4927 (2006).

Appl. Opt. (2)

Appl. Phys. Lett. (3)

M. D. Groner, S. M. George, and R. S. Mclean, “Gas diffusion barriers on polymers using Al2O3 atomic layer deposition,” Appl. Phys. Lett. 88, 051907 (2006).
[CrossRef]

P. F. Carria, M. D. Groner, and S. M. George, “Ca test of Al2O3 gas diffusion barriers grown by atomic layer deposition on polymers,” Appl. Phys. Lett. 89, 031915 (2006).
[CrossRef]

K. J. Hebert, S. Zafar, and E. A. Irene, “Measurement of the refractive index of thin SiO2 films using tunneling current oscillations and ellipsometry,” Appl. Phys. Lett. 68, 266-268 (1996).
[CrossRef]

Chem. Mater. (1)

B. B. Burton, M. P. Boleslawski, A. T. Desombre, and S. M. George, “Rapid SiO2 atomic layer deposition using tris(tert-pentoxy) silanol,” Chem. Mater. 20, 7031-7043 (2008).
[CrossRef]

J. Phys. Chem. (1)

S. M. George, A. W. Ott, and J. W. Klaus, “Surface chemistry for atomic layer growth,” J. Phys. Chem. 100, 13121-13131 (1996).
[CrossRef]

Opt. Spectrosc. (1)

S. V. Mutilin and T. Khasanov, “The refractive index of homogeneous SiO2 thin films,” Opt. Spectrosc. 105, 461-465 (2008).
[CrossRef]

Proc. SPIE (1)

M. N. Ott, F. LaRocca, W. J. Thomes, R. Switzer, and S. MacMurphy, “Optical fiber assemblies in harsh environments, the journey past, present, and future,” Proc. SPIE 7070, 707009 (2008).
[CrossRef]

Science (1)

D. Hausmann, J. Becker, S. Wang, and R. G. Gorden, “Rapid vapor deposition of highly conformal silica nanolaminates,” Science 298, 402-406 (2002).
[CrossRef] [PubMed]

Thin Solid Films (2)

R. Cooper, T. K. Minton, X. Du, and S. M. George, “Protection of polymer from atomic-oxygen erosion using Al2O3 atomic layer deposition coatings,” Thin Solid Films 516, 4036-4039 (2008).
[CrossRef]

T. Suntola, “Atomic layer epitaxy,” Thin Solid Films 216, 84-89 (1992).
[CrossRef]

Other (9)

M. Ritala and M. Leskela, “Atomic layer deposition,” in Handbook of Thin Film Materials, H. S. Nalwa, ed. (Academic, 2001), pp. 103-161.

M. Pollack and S. C. Bates, “Taking optical probes into harsh environments,” http://archives.sensorsmag.com/articles/0600/76/.

“Harsh-environment optics growing--market intelligence,” Fiber Optics Weekly Update, http://findarticles.com/p/articles/mi_m0NVN/is_4_24/ai_112985420/.

“Fiber optics for harsh environment,” http://www.timbercon.com/Fiber-Optics-for-Harsh-Environment/.

N. V. Nguyen and C. A. Richer, “Thickness determination of ultra-thin SiO2 films on Si by spectroscopic ellipsometry,” in Silicon Nitride and Silicon Dioxide Insulating Thin Films, M. J. Deen, W. D. Brown, K. B. Sundaram, and S. I. Raider, eds. (Academic, 1997), pp. 183-193.

“nSILVER--Invisible protection against silver tarnishing,” http://www.beneq.com/nsilver.php.

“Surfaces becoming 'nano' clean,” http://www.finnfacts.com/english/newsletter/news/beneq_0409.html.

M. Makela, P. Soininen, and S. Sneck, “Protective coating of silver,” U.S. patent application, IPC8 Class AC23C1640FI, USPC Class 42725519.

B. C. Wilson, “Optical coating applications on automotive polymers and displays,” presented at the New Technologies in Decorating and Assembly Meeting, Dearborn, Michigan, 10-11 June 2008.

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Figures (5)

Fig. 1
Fig. 1

Measured film thickness and refractive index of Si O 2 films deposited by ALD as a function of the number of ALD cycles used. The result of linear regression connecting the film thickness to the number of ALD cycles is also indicated.

Fig. 2
Fig. 2

(a) 2D and (b) 3D AFM images of a 120 nm thick Si O 2 film grown at 300 ° C by TBS/TMA ALD on a silica-covered Si(100) substrate, indicating the high uniformity of the film and its small rms roughness.

Fig. 3
Fig. 3

Visual comparison of the effect of immersion in 24% KOH solution on three of the aluminum mirror samples tested as indicated by the rate of H 2 bubbling. The photo was taken 10 min after the mirrors were immersed in the alkali solution. The two samples coated with ALD-formed films show almost no H 2 bubbling in contrast with the film covered by 30 nm of silica deposited by e-beam evaporation.

Fig. 4
Fig. 4

Photos of an aluminum mirror (left) coated with a 30 nm ALD Si O 2 film, and (right) obtained from Thorlab and reported to be coated with 100 nm of SiO, after both were soaked in 24% KOH solution for 1 h.

Fig. 5
Fig. 5

Reflectance spectra of aluminum mirrors coated by 120 nm ALD silica measured after immersion for 2 h in the solvents and other chemical media indicated. A reflectance measurement taken before immersion (blank) is also included. The reflectance properties of the samples are essentially unaffected by exposure to the chemicals indicated.

Tables (1)

Tables Icon

Table 1 Time to Start of H 2 Bubbling (First Number), and for Total Removal of Metal from the Mirror by Soaking in 24% Aqueous KOH

Equations (1)

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2 Al ( s ) + 6 H 2 O ( aq. ) + 2 K OH ( aq. ) 2 K [ Al ( OH ) 4 ] ( aq. ) + 3 H 2 ( g ) .

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