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Chinese Journal of Materials Research  2014, Vol. 28 Issue (3): 233-240    DOI: 10.11901/1005.3093.2013.832
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Optimization of Preparation Technology of Micro-arc Oxidation Coatings on Pure Titanium
Yuhai LI1,**(),Shisong LU1,Hui ZHAO1,Yan ZHAO2
1. College of Materials Science and Engineering, Shenyang Ligong University, Shenyang 110159
2. School of Mechanical Engineering, Liaoning Shihua University, Fushun 113001
Cite this article: 

Yuhai LI,Shisong LU,Hui ZHAO,Yan ZHAO. Optimization of Preparation Technology of Micro-arc Oxidation Coatings on Pure Titanium. Chinese Journal of Materials Research, 2014, 28(3): 233-240.

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Abstract  

The preparation parameters were systematically optimized in order to produce an appropriate micro-arc oxidation (MAO) coating on pure titanium. Then the optimized MAO ceramic coating was subjected to alkali treatment. The bioactivity of the alkalized coating was evaluated by immersion test in a simulated body fluid (SBF) for certain times. The porosity, pore density and pore diameter of the MAO coatings were examined by formula scoring method. The results show that the best MAO may be produced with the following electrical parameters: positive voltage 400 V, duty ratio 60%, frequency 550 Hz, and oxidation time 25 min. The results of examination by XRD, SEM and EDS show that a uniform porous anatase TiO2 coating grew on titanium with porosity 12%, pore density 0.70×108, and a mean pore diameter 3 μm. The alkalized coating treated by alkali method was completely covered by bone-like apatite when it was cultured in SBF for 14 days. The calcium deficiency like apatite with a composition similar to that of human bone grew on the coating exhibits excellent bioactivity. But the apatite could dissolve with the extension of the culturing time.
Key words:  inorganic non-metallic materials      pure titanium      micro-arc oxidation      formula scoring method      electrical parameter     
Received:  07 November 2013     
Fund: *Supported by Science & Technology Project in Shenyang No.F12-268-4-00
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Yuhai LI
Shisong LU
Hui ZHAO
Yan ZHAO

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https://www.cjmr.org/EN/10.11901/1005.3093.2013.832     OR     https://www.cjmr.org/EN/Y2014/V28/I3/233

Element C Fe Si N H Ti
0.20 0.03 0.15 0.05 0.15 Margin
Table 1  Chemical compositions of TA2 (mass fraction, %)
Level Factor A Factor B Factor C Factor D
Positive voltage ∕ V Frequency ∕ Hz Duty ratio ∕ % Oxidation time ∕ min
1 350 500 50 10
2 400 550 55 15
3 450 600 60 20
4 500 650 65 25
Table 2  Factors and levels in orthogonal design
Order Reagent Amount
1 NaCl 7.996 g
2 NaHCO3 0.350 g
3 KCl 0.224 g
4 K2HPO43H2O 0.228 g
5 MgCl26H2O 0.305 g
6 1 mol/L HCl 40 mL
7 CaCl2 0.278 g
8 Na2SO4 0.071 g
9 (CH2OH)3CNH2 6.057 g
Table 3  Reagents for preparation of SBF(1 L, pH=7.25)
No. Factors∕Levels Experimental targets
A B C D Error Diameter/μm PPI/（×108） ε/%
1 1 1 1 1 1 1.5 0.63 9.9
2 1 2 2 2 2 1.5 0.61 11.0
3 1 3 3 3 3 1.6 0.62 11.3
4 1 4 4 4 4 2.0 0.51 10.6
5 2 1 2 3 4 2.5 0.41 11.1
6 2 2 1 4 3 3.0 0.72 12.1
7 2 3 4 1 2 2.8 0.65 12.8
8 2 4 3 2 1 4.0 0.44 11.7
9 3 1 3 4 2 4.0 0.33 11.7
10 3 2 4 3 1 4.0 0.37 10.9
11 3 3 1 2 4 4.0 0.33 10.6
12 3 4 2 1 3 4.0 0.29 9.9
13 4 1 4 2 3 5.0 0.23 12.1
14 4 2 3 1 4 5.0 0.38 12.0
15 4 3 2 4 1 — — —
16 4 4 1 3 2 — — —
Table 4  Design and result of the orthogonal test
Fig.1  Photograph of seriously ablated coatings
No. Score of experimental target
Diameter PPI ε Comprehensive Score
1 0 0.82 0 1.64
2 0.03 0.78 0.38 2.73
3 0.03 0.80 0.48 3.07
4 0.14 0.57 0.24 2.00
5 0.29 0.37 0.41 2.26
6 0.43 1.00 0.76 4.71
7 0.37 0.86 1.00 5.09
8 0.71 0.43 0.62 3.43
9 0.71 0.20 0.62 2.97
10 0.71 0.29 0.34 2.31
11 0.71 0.20 0.24 1.83
12 0.71 0.12 0 0.95
13 1.00 0 0.76 3.28
14 1.00 0.31 0.72 3.78
15 — — — —
16 — — — —
Table 5  Results of the formula scoring method
Factor Comprehensive score
A B C D E
K1 9.44 10.15 8.18 11.46 7.38 ∑＝40.05
K2 15.49 13.53 5.94 11.27 10.79
K3 8.06 9.99 13.25 7.64 12.01
K4 7.06 6.38 12.68 9.68 9.87
k1 2.36 2.54 2.73 2.87 2.46
k2 3.87 3.38 1.98 2.82 3.60
k3 2.02 3.33 3.31 2.55 3.00
k4 3.53 2.13 3.17 3.23 2.47
Range 1.85 1.25 1.33 0.68 1.14
Secondary factors A C B D
Excellent scheme A2C3B2D4
Table 6  Statistical results of the formula scoring method
Fig.2  SEM images of coatings’ surface after process optimization, Fig.b is partial enlarged image of Fig.2a
Fig.3  SEM photograph on cross sections of coating after process optimization
Element Atomic fraction ∕ %
O 67.52
P 8.66
Ti 23.82
Table 7  Elemental composition of the surfaces of coatings
Fig.4  XRD pattern of coating surface after process optimization
Fig.5  SEM images of the surfaces of NaOH treated Ti coatings cultured in SBF for14 d (a) and 21 d (b)
Element Composition
14 d 21 d
Ti 0 17.85
O 69.17 78.26
P 14.19 1.94
Ca 16.64 1.96
Ca ∕ P 1.17 1.01
Table 8  Elemental composition of the surfaces of NaOH treated Ti coatings after cultured in SBF for different days (atomic fraction, %)
Fig.6  XRD patterns of the precipitation on the surfaces of NaOH treated Ti coatings after cultured in SBF for different days
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