Influence of Temperature and Acid Etching Time on the Superficial Characteristics of Ti

Chrcanovic, Bruno Ramos; Wennerberg, Ann; Martins, Maximiliano Delany

doi:10.1590/1516-1439.014115

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Articles • Mater. Res. 18 (5) • Sep-Oct 2015 • https://doi.org/10.1590/1516-1439.014115 copy

Influence of Temperature and Acid Etching Time on the Superficial Characteristics of Ti

Authorship SCIMAGO INSTITUTIONS RANKINGS

Abstract

We evaluated the influence of the etching time and temperature of an acid solution (HCl/H₂SO₄) on the chemical and topographical superficial characteristics of cpTi grade IV. Samples were analyzed by electron microscopy, interferometry, and grazing incidence XRD. The surfaces kept the irregularity aspect when submitted to the same etching temperature. On the other hand, the irregularities increased in size and depth with increasing etching time. The etching treatments that produced higher values for roughness parameters showed a combination of high temperature for a longer etching time. Some treatments produced very large irregularities, with a brittle surface in some regions. According to statistical correlation, the temperature made the strongest contribution in the variance of the mean values of the surface roughness parameters when compared to the etching time. Titanium and oxygen were the only elements on the surface in all groups. All test group samples showed the presence of titanium hydride.

Keywords:
titanium; surface modification; acid-etching; temperature; surface characterization

Group	S_a (µm)	S_dr (%)	S_ds (µm^–2)
Control	0.275 ± 0.034	6.3 ± 1.5	128938 ± 9184
	Temperature 60 °C
AT1 (5 min)	0.518 ± 0.282 a	34.9 ± 20.9 a	221262 ± 24576 a,b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
AT2 (15 min)	1.067 ± 0.551 a	63.2 ± 28.8 a	208891 ± 14510 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
AT3 (30 min)	1.510 ± 0.306 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	87.6 ± 24.1 a	207126 ± 17793 b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
p-value	<0.001	<0.001	0.011
	Temperature 90 °C
AT4 (5 min)	0.832 ± 0.307 a,b	49.1 ± 17.7 a	194404 ± 19415 ^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
AT5 (15 min)	2.017 ± 0.915 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	99.0 ± 38.0 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	188516 ± 32480 ^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
AT6 (30 min)	2.381 ± 0.663 b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	138.3 ± 36.3 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	201927 ± 23019 ^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
p-value	<0.001	<0.001	0.132
	Temperature 120 °C
AT7 (5 min)	2.547 ± 1.273 a,b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	142.4 ± 92.3 a,b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	186831 ± 16759 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
AT8 (15 min)	5.836 ± 2.454 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	376.5 ± 198.8 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	159629 ± 23477 a,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
AT9 (30 min)	6.247 ± 2.690 b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	462.1 ± 266.5 b,^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).	172987 ± 26681 ^c c Indicates statistically significant difference when compared to the control group. Observation: In the case of difference between the groups of the same etching time (5, 15, and 30 minutes), the following groups denoted with the same superscripted letter (a, b) indicate statistically significant difference in surface roughness (P < 0.05), according to the Tukey's HSD test: 5 minutes: Sa (AT1a, AT4b, AT7a,b), Sdr (AT1a, AT4b, AT7a,b), Sds (AT1a,b, AT4a, AT7b); 15 minutes: Sa (AT2a, AT5a, AT8a), Sdr (AT2a, AT5b, AT8a,b), Sds (AT2a, AT5a, AT8a); 30 minutes: Sa (AT3a, AT6b, AT9a,b), Sdr (AT3a, AT6b, AT9a,b), Sds (AT3a, AT6b, AT9a,b).
p-value	<0.001	<0.001	<0.001

Roughness parameter	Temperature			Correlation (Pearson)	Equation	Standard Error
Roughness parameter	R	R²	p-value	Correlation (Pearson)	Equation	Standard Error
S_a	0.657	0.432	<0.001	Strong	y = –3.217 + 0.064x	1.806
S_dr	0.588	0.346	<0.001	Moderate	y = –236.2 + 4.4x	149.5
S_ds	–0.560	0.313	<0.001	Moderate	y = 252424 - 654x	23825

Roughness parameter	Etching time			Correlation (Pearson)	Equation	Standard Error
Roughness parameter	R	R²	p-value	Correlation (Pearson)	Equation	Standard Error
S_a	0.339	0.115	<0.001	Weak	y = 1.238 + 0.079x	2.255
S_dr	0.331	0.109	<0.001	Weak	y = 62.6 + 5.9x	174.4
S_ds	–0.074	0.006	0.223	Very Weak	y = 196964 - 207x	28672

Roughness parameter	Temperature + Etching time			Equation	Standard Error	Collinearity
Roughness parameter	R	R²	p-value	Equation	Standard Error	Tolerance	VIF
S_a	0.740	0.547	<0.001	y = -4.530 + 0.064x₁ + 0.079x₂	1.616	1.000^a	1.000^a
S_dr	0.675	0.455	<0.001	y = -335.0 + 4.4x₁ + 5.9x₂	136.7	1.000^a	1.000^a
S_ds	0.565	0.319	<0.001	y = 255880 - 654x₁ - 207x₂	23773	1.000^a	1.000^a

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