International Journal of Heat and Mass Transfer 101 (2016) 699–706

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International Journal of Heat and Mass Transfer

journal homepage: www.elsevier.com/locate/ijhmt

Study of Ti–6Al–4V alloy spectral emissivity characteristics during

thermal oxidation process
Longfei Li, Kun Yu ⇑, Kaihua Zhang, Yufang Liu ⇑
Infrared Optoelectronic Science and Technology Key Laboratory of Henan Province, College of Physics and Electronic Engineering, Henan Normal University, Xinxiang, Henan 453007,
PR China

a r t i c l e i n f o a b s t r a c t

Article history: The infrared normal spectral emissivity of an oxidized Ti–6Al–4V alloy has been measured during a ther-
Received 29 September 2015 mal oxidation process. It gradually increased with oxidation time below 873 K, and strong oscillation was
Received in revised form 14 April 2016 observed above 923 K. To explore the possible reasons for emissivity variation under different tempera-
Accepted 13 May 2016
tures and oxidation time, the changes of surface composition and roughness were investigated before and
Available online 7 June 2016
after oxidation by X-ray diffraction (XRD) and roughness tester. The surface oxide film thickness has been
estimated by using the theory of radiative effects of films and the actual value of thickness has been mea-
Keywords:
sured utilizing spectroscopic ellipsometry (SE) and scanning electron microscopy (SEM), respectively. The
Spectral emissivity
Ti–6Al–4V alloy
measurement results were in good agreement with the estimated values. It is found that the interference
Thermal oxidation effect of oxide film could be responsible for the oscillatory behavior in spectral emissivity. The thickness
Oscillation values indicate that the oxide film growth follows parabolic law and that the growth rate increases
Film thickness rapidly above 923 K.
Ó 2016 Elsevier Ltd. All rights reserved.

1. Introduction speed and non-contact measurement. The accuracy of this method

The Ti–6Al–4V alloy is widely used in aerospace and
shipbuilding industries, energy and power fields, and biomedical
engineering due to its attractive properties such as super specific
strength, low elastic modulus, nonmagnetic behavior, enhanced
corrosion resistance and excellent biocompatibility [1–5]. Never-
theless, the low wear resistance limits its use in wear-related
fields, like graft biomaterial application and manufacturing
engineering [6]. A large number of works have been conducted
to promote its hardness and to decrease its wear rate by changing
the surface microstructure and mechanics properties with differ-
ent methods, such as glow-discharge nitriding treatment, chemical
treatment, physical vapor deposition, thermal spray and oxidation,
etc. Among these methods, thermal oxidation is most concise and
effective [7–11].
The accurate measurement of temperature is important in a
thermal oxidation process. Excessively high temperature would
lead to an oxide de-bonding and an oxide film produced at exces-
sively low temperature would be too thin to improve the ware per-
formance effectively. The radiation thermometry is widely used in
many industrial applications due to its advantage of high response
⇑ Corresponding authors. Tel.: +86 0373 3329297.
E-mail addresses: yukun@htu.edu.cn (K. Yu), yf-liu@htu.edu.cn (Y. Liu).
mainly relies on the knowledge of emissivity, and variation of this
quantity with temperature, wavelength and oxidation could cause
a big error in monitoring the temperature [12–14]. As the emissiv-
ity changes acutely with oxidation time in the thermal oxidation
process, establishing an emissivity model with temperature and
oxidation time is necessary for the promotion of the accurate
non-contact temperature measurement of Ti–6Al–4V alloy. Thus,
emissivity of the oxidized sample should be measured during the
thermal oxidation process, and the effect of oxidation degree on
the emissivity needs to be systematically discussed.
Several studies have reported some emissivity data of both solid
and liquid phases of the Ti–6Al–4V alloy at high temperatures. For
instance, the normal spectral emissivity at 665 nm of this alloy
shows a linear dependence on the temperature between 1200
and 1700 K in the literature reported by Betz et al. [15]. Deduced
from their results, the emissivity value at the melting point
(1943 K) would be 0.369, which is approximately in accordance
with the data presented in Ref. [16]. Normal spectral emissivity
at 684.5 nm from melting temperature to 2920 K has been mea-
sured using a fast laser polarimeter [17]. Recently, the hemispher-
ical emissivity from 780 to 1670 K and the normal spectral
emissivity at 900 nm between 1300 and 1730 K have been
presented in Ref. [18]. Pérez-Sáez et al. reported the normal spec-
tral emissivity at the wavelength between 2.5 and 22 lm over the

http://dx.doi.org/10.1016/j.ijheatmasstransfer.2016.05.069
0017-9310/Ó 2016 Elsevier Ltd. All rights reserved.
700 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706
temperature range from 500 to 1150 K, and illustrated the influ-
ence of surface stress on the normal emissivity [19]. However,
the emissivity data of thermally oxidized Ti–6Al–4V alloy is scar-
cely reported and the effect of oxidation scale on the emissivity
is still uncertain.
In the present research, the infrared normal spectral emissivity
of the thermally oxidized Ti–6Al–4V alloy is measured in the wave-
length range of 1500–2200 nm and between 823 and 973 K. The
aim of this research is to obtain the available emissivity data of
the oxidized alloy and to consider the reasons for emissivity vari-
ation with oxidation.
2. Experiment
2.1. Method and apparatus
Defined as the ratio of sample radiation to blackbody radiation,
the normal spectral emissivity of Ti–6Al–4V alloy is calculated by
the direct measurement method [20]. In the actual measurement,
the influence of background radiation is taken into consideration.
The emissivity is obtained after subtracting the background
radiation:
M s ðT s ; kÞ  M am ðT am ; kÞ
eðk; T s Þ ¼
M b ðT s ; kÞ  Mam ðT am ; kÞ
where, Ms (Ts, k) and Mb (Ts, k) are the radiation intensities of the
sample at temperature Ts and the blackbody at the same tempera-
ture, respectively, while Mam (Tam, k) is the background radiation
intensity at temperature Tam calculated from the Planck’s law.
Ms (Ts, k) and Mb (Ts, k) are measured by a home-made device
(Fig. 1), which is composed of five parts: the heating and
temperature controlling system, the blackbody (ISOTECH R970),
the optical system, the detection system and the data processing
system. The sample is heated in the atmosphere-controlled cham-
ber, which is protected by a water-cooling system. The surface
temperature of the sample is measured utilizing a type K thermo-
couple which is welded on the edge of the measurement area. The
optical system includes one motorized rotation stage and two off-
axis parabolic gold-coated mirrors (controlled by the motorized
rotation system). The detection system consists of a grating
Fig. 1. Experimental apparatus for measuring the normal spectral emissivity under atmosphere-controlled condition.
monochromator (omni-k5007) and an InGaAs detector. The best
spectrum response range of this detection system is 1500–
2200 nm. The data processing system is comprised of an optical
chopper (SR540), an amplifier (SR830) and a computer. The radia-
tion from the sample and the blackbody are firstly modulated
using the chopper and then translated into electrical single
through the detection system. Finally, the received AC detector
output signal is amplified by the lock-in amplifier and the spectral
emissivity is calculated according to Eq. (1).
2.2. Samples and measurements
Nine commercial Ti–6Al–4V alloy samples (disk-shape, 13 mm
diameter and 2 mm thickness) were prepared. All the samples
were polished with SiC abrasive paper up to 1000 grit. The polished
surfaces were washed by acetone and absolute alcohol succes-
sively. Then the samples were cleaned up in the distilled water
using an ultrasonic cleaner. The chemical composition of the alloy
tested by an X-ray fluorescence spectrometer (Rigaku: ZSX Primus
II) is shown in Table 1. To decrease the surface stress, all samples
were heated to 1000 K and then cooled to room temperature in
argon environment [19]. The roughness value (tested by a rough-
ness tester: Time TR220) of the treated sample can be described
ð1Þ by four parameters: Ra = 0.201 ± 0.014 lm, Rq = 0.275 ± 0.036 lm,
Rz = 1.553 ± 0.181 lm, Rt = 2.157 ± 0.349 lm, where Ra is the aver-
age roughness, Rq is the root-mean-square deviation of the profile,
Rz is the maximum height in one sampling length, and Rt is the
total maximum height of the profile.
At the beginning of the experiment, four samples (randomly
selected from the nine samples) were respectively heated to
823 K, 873 K, 923 K and 973 K in argon environment. The normal
spectral emissivities were measured when the four samples reach
thermal equilibriums. During the oxidation process, air was
steadily pumped into the chamber, keeping the barometric
pressure and the oxygen concentration approximately constant.
The emissivities of these samples were measured every 10 min in
the first two hours, 20 min in 2–4 h, 30 min in 4–7 h and 90 min
in 7–10 h, respectively. After the oxidation, the samples were
cooled to room temperature in argon atmosphere to prevent fur-
ther oxidation. The other five samples were oxidized at 973 K for
 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706
Table 1
Composition of the Ti–6Al–4V alloy.
Element Al V Ti
Composition (mass%) 5.2405 2.8692 91.8902
30 min, 90 min, 150 min, 240 min and 600 min, where the five oxi-
dation periods were chosen based on the above results.
To study the change of the surface composition, the X-ray
diffraction analyses (Cu Ka radiation, DX2000) were performed in
the diffraction angle range from 20° to 80° before and after oxida-
tion. After the XRD measurements, the roughness of the oxidized
samples was measured again. Based on the theory of radiative
effects of films [21–24], the oxide film thickness was estimated
to explore the relation between the oxidation and the emissivity
in Ti–6Al–4V alloy. The actual values of the oxide films were
obtained by both the indirect and the direct methods. The indirect
method employs a spectroscopic ellipsometer (Ellitop ESS03 UI),
which could estimate the thickness of thin film by using the exper-
imental data of ellipsometric parameters. The direct method uti-
lizes a scanning electron microscopy (Zeiss SUPPA 40), which
measures the film thickness by observing the cross-section of the
oxidized samples.
3. Results and discussion
3.1. Unoxidized alloy
In Fig. 2, the normal spectral emissivity of the alloy shows
different levels of increase with temperature before the oxidation.
A slight peak is found at about 2000 nm in each curve, and it was
possibly caused by the absorption of H2O molecule since the
radiation was exposed to air when the transmission in the optical
system took place. In order to precisely discuss the effect of tem-
perature, a more detailed analysis of emissivity is conducted in
Fig. 3. It is worth noting that, the emissivity at the given wave-
length in 1500–2200 nm approximately follows a linear rule as a
function of temperature (Table 2).
3.2. Oxidized alloy
Previous research shows that surface oxidation has a remark-
able influence on the normal spectral emissivity [25]. In order to
Fig. 2. Normal spectral emissivity of the Ti–6Al–4V alloy at 823 K, 873 K, 923 K and
973 K.
701
C, N, O, H, etc
60.0001
Fig. 3. Spectral emissivity of the unoxidized Ti–6Al–4V alloy as a function of
temperature.
Table 2
Emissivity functions of temperature at different wavelengths.
Wavelength Linear fit Wavelength Linear fit
(nm) (nm)
1500 1.1  103 T0.634 1900 1.53  103 T-0.991
1600 1.14  103 T0.658 2000 1.69  103 T1.780
1700 1.26  103 T0.744 2100 1.56  103 T0.975
1800 1.35  103 T0.832 2200 1.56  103 T0.970
systematically investigate this influence, the normal spectral
emissivity was measured at different time points in the oxidation
process. As shown in Fig. 4, the curve became smoother when
the sample was oxidized at an elevated temperature. This was
because the signal–noise ratio increased gradually with the rise
of temperature. Emissivity values at 823 and 873 K (plotted in
Fig. 4) both increased with oxidation time, and strong oscillation
in emissivity was observed at 923 and 973 K. The amplitude of
the oscillation attenuated seriously and the period of oscillation
increased gradually with the oxidation time. The similar phe-
nomenon was scarcely reported in the literature relating to the
Ti–6Al–4V alloy [26,27]. The possible reasons for the changes in
emissivity were generally considered to be variation of composi-
tion, change in surface morphology and the interference effect of
oxide film growth.
3.2.1. Variation of surface composition
The X-ray diffraction measurements of both the unoxidized and
the oxidized samples showed that the anatase, the rutile and the
complicated hybrid oxides (TiO, Ti2O3, etc.) appeared in the ther-
mal oxidation process (Fig. 5). The peak intensities of anatase at
823 and 973 K were lower than the quantities at 873 and 923 K.
However, both the peaks of the rutile and the hybrid oxide
increased with the oxidation temperature, and the former (rutile)
increased rapidly and the latter (hybrid oxide) rose slowly. The
data in Fig. 5 indicates that the oxide film is mainly made up of
the anatase and the hybrid oxides at the temperature below
923 K, and that the rutile grows rapidly at higher temperature.
The analysis above shows that the growth of rutile is likely to be
the cause of the oscillation in emissivity.
A further discussion of the rutile growth was performed by
measuring the samples oxidized at 973 K for different periods of
time. Fig. 6 showed that the rutile grew gradually with the
702 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706

Fig. 4. Normal spectral emissivity of the samples oxidized at 823 K, 873 K, 923 K and 973 K.

oxidation time, and that the peak values of the anatase and the
hybrid oxides remained practically constant. The results (Figs. 5
and 6) demonstrate that the rutile growth has a remarkable influ-
ence on spectral emissivity, but this cannot clearly explain the
oscillation in emissivity.
3.2.2. Change in surface morphology
The morphology of the oxidized Ti–6Al–4V alloy can be charac-
terized by surface roughness. The measurements of roughness
were carried out in both horizontal and vertical directions. The
average value (Table 3) between the two directions showed that

Fig. 5. X-ray diffraction pattern of the unoxidized sample (A) and the oxidized one for 10 h at (B) 823 K, (C) 873 K, (D) 923 K and (E) 973 K.
 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706 703

Fig. 6. X-ray diffraction pattern of the unoxidized sample (a) and the oxidized one at 973 K for (b) 30 min, (c) 90 min, (d) 150 min, (e) 240 min and (f) 600 min.

Table 3
Roughness of the samples oxidized at different conditions.

Roughness Ra Rq Rz Rt
823 K for 10 h 0.221 0.269 1.280 1.748
873 K for 10 h 0.236 0.322 1.804 3.349
923 K for 10 h 0.312 0.459 2.808 4.873
973 K for 30 min 0.713 0.885 4.039 5.273
973 K for 90 min 0.564 0.703 3.213 4.287
973 K for 150 min 0.428 0.550 2.978 3.502
973 K for 240 min 0.455 0.581 2.749 3.632
973 K for 10 h 0.230 0.295 1.347 2.011

Fig. 8. Normal spectral emissivity at 1600, 1900 and 2200 nm of the sample
oxidized at 973 K for 10 h.

3.2.3. Interference effect of oxide film

Fig. 7. Radiations emitted from substrate (Ti–6Al–4V and oxygen-diffusion zone)
and transmitted through the oxidation film (TiO2).
the roughness at 973 K increased sharply in the first 30 min and
then decreased slowly with the oxidation time. This was possibly
because the particles, which were yielded on the thermal oxidized
surface, grew rapidly with the increasing temperature and then
increased the surface roughness. When the sample was oxidized
at an elevated temperature for a long time, the particles would
gather together, leading to a decrease in roughness. The trend of
this decrease conformed to the attenuation trendency of the oscil-
lation amplitude in emissivity at 923 and 973 K. However, the phe-
nomenon still cannot account for the oscillatory behavior.
The analysis (Sections 3.2.1 and 3.2.2) demonstrates that both
the variation of composition and the change in surface morphology
cannot explain the oscillation. Thus, we suppose that the key rea-
son for the phenomenon is the interference effect and that the
amplitude attenuation might be caused by the proportion changes
of the radiations from the film and the substrate [22]. To discuss
the oscillatory behavior, the oxide film thickness was estimated
by using a model composed of substrate and oxide film (Fig. 7).
The substrate (including the Ti–6Al–4V alloy and the adjacent
oxygen-diffusion zone) is considered to be opaque and the film
(well adhered to the substrate) is mainly composed of TiO2.
According to the literature reported by Won et al. the refraction
index of TiO2 film can be estimated to be 2.3 at 973 K, 2.2 at
923 K, 2.1 at 873 K and 2.05 at 823 K [28]. The refraction index
of the air was assumed to be approximately 1, which corresponds
to the vacuum value. The subsequent arguments were discussed in
the normal direction (h = 0) in correspondence with the experi-
ments. As shown in Fig. 7, part of the thermal radiation (I) from
the substrate transmitted through the film directly, and the other
704 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706

Fig. 9. Comparation of the estimated thickness and the values measured by the Fig. 11. Estimation of the film thickness of the samples oxidized for 10 h.
ellipsometer. Dotted line is the best fitted curve of the estimated data as a function
of oxidation time.

Dd ¼ 2n2 Dh ¼ k ð3Þ
part (II) passed through the film for three times because of the
reflections at the air/film interface and the substrate. The film thickness at different oxidation time can be estimated
Based on the theory of interference (n3 > n2), the optical path by the number of peaks and valleys [21,23]. For instance, the thick-
difference between the two parts of the emergent ray is ness of the sample oxidized at 973 K for 10 h was calculated using
three emissivity curves at the chosen wavelengths shown in Fig. 8.
k The calculated values were 1391, 1445 and 1435 nm, respectively
d ¼ 2hn2  ð2Þ
2 with the statistically obtained relative standard deviation of 2.2%.
When the film grows with oxidation time, the optical path dif- In order to simplify the calculation process, the following esti-
ference between the adjacent two peaks of the oscillatory curve mations were made only at 1900 nm, where the detector showed
(923 K and 973 K at Fig. 4) is the best response. As shown in Fig. 9, the measured film thickness

Fig. 10. Scanning electron micrographs of the cross-sections of the samples oxidized at 973 K for (a) 30 min, (b) 90 min, (c) 150 min, (d) 240 min, (e) 600 min and (f) at 923 K
for 600 min.
 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706
Table 4
Uncertainty estimation in emissivity measurement.
Parameter
Sample temperature
Blackbody temperature
Background temperature
Wavelength precision
Blackbody effective emissivity
Combined uncertainty (%)
Expanded uncertainty (coverage factor k = 2) (%)
data of the samples, which were oxidized at 973 K for 30 min,
90 min, 150 min, 240 min and 600 min, were in good agreement
with the estimated results. Moreover, the thickness of oxide film
can be fitted with a parabolic function of oxidation time (dotted
line)
h ¼ 3:27  103 t 2 þ 3:87t þ 302:55
To further demonstrate the validity of this estimation method,
the thickness of oxidized film was characterized by observing the
cross-section of the treated samples with a scanning electron
microscopy. The estimated results showed good agreement with
the film thicknesses observed through the micrographs of the
cross-sections (Fig. 10). In addition, the change trend of the film
morphology could be obtained, and the result was well in accor-
dance with the measured roughness.
The results measured by ellipsometer and scanning electron
microscopy indicate that the thickness estimation method is valid.
This in turn illustrates that the oscillatory behavior in emissivity is
mainly caused by the interference effect. In this research, the avail-
able normal spectral emissivity data at different oxidation time
were obtained, which could contribute to establishing the emissiv-
ity model needed in the radiation thermometry. In addition, as it is
usually difficult to measure the thickness and roughness at high
temperature, this estimation method may provide the values of
the film thickness, the roughness and even the rate of oxidation
through the radiation signal curve without contaminating the sam-
ple surface in the thermal oxidation process. For instance, the film
thicknesses of the samples oxidized at the four temperature points
for 10 h were approximatively calculated using the emissivity
curves and the thickness was fitted as a function of temperature
as shown in Fig. 11. It was found that the alloy was oxidized slowly
at the temperature below 923 K and the oxidation speed increased
rapidly above 923 K.
3.3. Measurement uncertainties
According to the ISO Guide to the Expression of uncertainty in
Measurement (GUM) [29], the measurement uncertainty of the
experiment can be calculated as

2
2
2
@e @e @e
u2e ¼ uT þ uT þ uT
@T s s @T B B @T am am
þ u2B
where uT S , uT B and uT am is the combined temperature uncertainty of
the sample, the blackbody and the background, respectively, uk is
the wavelength uncertainty of the monochromator, and uB is the
emissivity uncertainty of the blackbody. The combined sample tem-
perature uncertainty uT S was calculated according to Ref. [30].
qffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
uTs ¼ u2t þ u2s þ u2K þ u2d
where the surface temperature uncertainty ut, caused by the emis-
sivity variation in the oxidation process, was calculated to be 0.75 K
705
Standard uncertainty Contribution
T = 823 K, k ¼ 2200nm e ¼ 0:417762 T = 973 K, k ¼ 1500nm e ¼ 0:438175
3.48 K at 823 K 0.014037 0.021576
4.86 K at 973 K
0.2 K 0.00081 0.00089
2.2 K 0.000231 8.4437E8
0.1155 nm 0.000018 0.000026
0.0025 0.0025 0.0025
1.4283 2.1748
2.8566 4.3496
at 823 K and 3.08 K at 973 K by the equation of heat conduction. The
temperature difference between the temperature readings of the
thermocouple and the calculated surface temperature values was
mainly caused by the thermocouple installation method and the
heat transfer loss of the thermocouple lead wires. Taken as a known
systematic error, this temperature difference was calculated to be
ð4Þ 5.96 K with an uncertainty us = 2.21 K at 823 K and 10.35 K with
an uncertainty us = 2.73 K at 973 K. The uncertainty of the thermo-
couple uK was specified by the manufacturer (Omega: type K, diam-
eter: 0.2 mm) to 2.2 K below 1000 K. The surface temperature
difference between the center of the sample and the measurement
points (3.5 mm from the center) was determined by repeated mea-
surements using five thermocouples of same type and this quantity
was revealed to be 5.2 K with an uncertainty ud = 1.35 K. Thus, the
uT S was calculated to be 3.48 K at 823 K and 4.86 K at 973 K.
The contribution of each parameter is listed in Table 4. The sam-
ple temperature gives the main contribution to the measurement
uncertainty and the combined uncertainty is determined mainly
at short wavelength according to Ref. [31]. In this work, the com-
bined uncertainty (presented in Table 4) was not more than
2.1748%, and the expanded uncertainty (with a coverage factor of
k = 2 for the 95.45% level of confidence) was less than 4.35%.
4. Conclusion
This research measured the normal spectral emissivity of the
oxidized Ti–6Al–4V alloy and explored the possible reasons for
the oscillatory behavior in emissivity during the thermal oxidation
process. Before oxidation, the emissivity shows an approximately
linear increase between 823 and 973 K. The emissivity increases
gradually with the oxidation time when the sample is oxidized in
air below 873 K and strong oscillations in emissivity are observed
in transient oxidation period above 923 K.
The measurement results of surface composition, roughness
and the film thickness indicate that variation in surface roughness
is one of the factors influencing the amplitude of oscillation, and
that the interference effect of the oxide film growth is the primary
reason for the oscillatory behavior. The oxide film thickness, the
roughness and the rate of oxidation can be estimated by using

2 the theory of radiative effects of films. The oxide film growth fol-
@e
þ uk lows the parabolic rule when the Ti–6Al–4V alloy is oxidized in
@k air environment, and the oxidation rate increases rapidly above
ð5Þ 923 K.
Conflict of interest
None declared.
Acknowledgments
ð6Þ
This work was supported by the National Natural Science Foun-
dation of China (Grant Nos. 61127012, 61307122 and 61475043),
University key scientific research project of Education Department
706 L. Li et al. / International Journal of Heat and Mass Transfer 101 (2016) 699–706
of Henan Province (Grant No. 14B140001), and Basic and Advanced
Technology Research Program of Henan Province (Grant No.
142102210450).
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