ISIJ International,

ISIJ International, Vol. 59 (2019), No. 1 Vol. 59 (2019), No. 1, pp. 104–112

Nitriding Behavior of Titanium Sponge Studied using Nitrogen Gas

and Dissolution Behavior of a Titanium Nitride Sponge in Titanium
Alloy Melt

Hideo MIZUKAMI,1)* Tomoyuki KITAURA2) and Yoshihisa SHIRAI3)

1) Steel Research Laboratories, Research & Development Bureau, Nippon Steel & Sumitomo Metal Corporation, 2-12-1
Minato, Joetsu, Nigata, 942-8510 Japan.
2) Naoetsu Works, Nippon Steel & Sumitomo Metal Corporation, 2-12-1 Minato, Joetsu, Nigata, 942-8510 Japan.
3) Steel Research Laboratories, Research & Development Bureau, Nippon Steel & Sumitomo Metal Corporation, 20-1
Shintomi, Futtu, Chiba, 293-8511 Japan.
(Received on July 30, 2018; accepted on September 6, 2018)

The nitriding behavior of titanium sponges with nitrogen gas and the dissolution behavior of titanium
nitride titanium sponges in titanium alloy melt were examined.
A titanium nitride sponge was produced using nitrogen gas. A high nitriding temperature corresponded
to a longer nitriding time, and thus to a higher nitrogen concentration in the sponge. Both the titanium
sponge and titanium nitride sponge featured a porous structure. Porous structures at both the surface
layer and inside were formed at intervals of about 5.0 × 10 − 5 m. When the titanium nitride sponge was
immersed into a titanium alloy melt, the melt permeated into the pores. The nominal dissolution rate of
the titanium nitride sponge in the titanium alloy melt depends on the temperature of the melt. Higher melt
temperatures corresponded to higher nominal dissolution rates. However, the concentration of nitrogen in
the titanium nitride sponge had no influence on the nominal dissolution rate. Nitriding models of the tita-
nium sponge with nitrogen gas, and the dissolution model of the titanium nitride sponge into the titanium
alloy melt were proposed. These models considered the structure of the sponge; thus, the behavior of
both the nitriding and dissolution sponges was predicted and confirmed.

KEY WORDS: titanium; sponge; nitride; inclusion; dissolution.

not yet been conducted.

1. Introduction
The demand for high-quality titanium alloy ingots for the
aerospace industry is growing. Therefore, it is important to
remove the inclusions from the melt before casting.
There are two kinds of inclusions in titanium alloys:
high-density and low-density inclusions. High-density inclu-
sions are bits of tools and machine components, which
contaminate the raw material before the ingots are cast;
therefore, such inclusions can be avoided in an environ-
ment with controlled conditions for handling raw materials.
However, contamination due to low-density inclusions is
more difficult because they are caused by a reactions, which
originates in the raw materials. To prevent contamination
due to with low-density in the ingot, these inclusions need
to be dissolved in the titanium alloy melt before cast-
ing. Therefore, many studies1–9) on the dissolution rate of
low-density inclusions in titanium alloy melt have been
conducted. It is necessary to understand the nitriding and
dissolution behaviors of the titanium sponge. However,
systematic experimental studies for these phenomena have
* Corresponding author: E-mail: mizukami.4m7.hideo@jp.nssmc.com
DOI: https://doi.org/10.2355/isijinternational.ISIJINT-2018-474
Titanium nitride sponges with different nitrogen concen-
trations were prepared from titanium sponges as the raw
material, and the nitriding behavior was studied. Moreover,
the dissolution behavior of the titanium nitride sponge in
the titanium alloy melt was examined using a small electron
beam furnace.
2. Experimental Procedures
2.1. Nitriding of Titanium Sponge
In this study, the nitride formation in a titanium sponge
was examined as a simulated low-density inclusion forma-
tion. For this purpose, it was necessary to prepare a titanium
nitride sponge with a known concentration of nitrogen.
There are many studies10–17) on the nitriding behavior
for titanium alloy plates. However, only a single study16)
focused on the nitriding behavior of titanium sponges sub-
jected to heat treatment under an Ar-5 vol% N2 mixture gas
atmosphere. To ensure uniformity in the concentration of
nitrogen in the titanium nitride sponge, a lower nitriding
temperature to decrease the temperature gradient and longer
nitriding time were used, as compared to the previous study.
Figure 1 shows a schematic diagram of the experimental

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 ISIJ International, Vol. 59 (2019), No. 1
apparatus for the heat treatment used in this study. The
sponges were passed through sieves of sizes 5.6 × 10 − 3 m
and 6.7 × 10 − 3 m, and thus separated according to their size.
These titanium sponges were then placed in a molybdenum
container, which was set in the heat-treating furnace. The
atmosphere in the vessel was replaced by an Ar-5 vol% N2
mixed gas after evacuation with a diffusion pump to 1.0 ×
10 − 1 Pa before the experiment. Then, two valves of the
vessel were opened, and the mixed gas was fed from one
valve side at a flow rate of 9.5 L·min − 1. The concentration
of nitrogen for the titanium nitride sponge was varied with
the heat treatment temperature over 3 h. The concentration
of nitrogen in the sponge was controlled by the thermal
conductivity technique.
2.2. Dissolution of Titanium Nitride Sponge
Figure 2 shows a schematic diagram of the experimental
apparatus with the small electron beam furnace. The tita-
nium alloy ingot, which was cast previously, was set in a
water-cooled copper crucible in a vacuum vessel. This ingot
had an upper diameter of 1.8 × 10 − 1 m, lower diameter of
1.2 × 10 − 1 m, and height of 9.0 × 10 − 2 m, and its composi-
tion was Ti-6.4 mass% Al-4.2 mass% V. The power of the
electron beam was set to 30 kW and the current was varied
from 0.8 A to 1.0 A. A molten pool was formed in the upper
part of the ingot by irradiating its top surface with an elec-
Fig. 1. Schematic diagram of heat treatment furnace for titanium
sponges with nitrogen gas.
Fig. 2. Schematic diagram of electron beam furnace for dissolu-
tion of titanium nitride sponge in titanium alloy melt.
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tron beam. To avoid direct irradiation of the center region
of the top surface of the ingot, the electron beam shape was
set to a circular ring. After about 1 h, the temperature of
the melt was adjusted to the prescribed temperature. The
titanium nitride sponge, which was located above the melt,
was immersed into the melt about 1.5 × 10 − 2 m below the
surface melt. At this position, the titanium nitride sponge
was completely immersed. After 20 to 120 s, the titanium
nitride sponge was removed out of the melt. In this study,
the titanium nitride sponge, with sizes in the range of 1.1 ×
10 − 2 m to 1.3 × 10 − 2 m, as determined by sieving, was
used. The concentration of the titanium nitride sponge was
chosen in the range of 5 to 15 mass% by heat treatment
with the mixed gas. A hole of 3.5 × 10 − 3 m in diameter
was made at the center of this titanium nitride sponge, and
then a tungsten rod of 3.0 × 10 − 3 m in diameter, with an
L-type-shaped front edge, was inserted in this hole. The tita-
nium nitride sponge was then moved to the central area of
the circular ring of the electron beam. This was done so that
that area would not be irradiated directly; thus, the direct
dissolution of the titanium nitride sponge was prevented by
electron beam irradiation before immersion into the melt.
The temperature of the alloy melt was measured with
a two-color pyrometer from outside the vacuum vessel
through the window. To calibrate the values of a two-color
optical pyrometer, the temperature of the alloy melt was
measured using a thermocouple of W-5 mass% Re/W-26
mass% Re with 5.0 × 10 − 3 m in diameter.
3. Results and Discussion
3.1. Nitriding Behavior of the Titanium Sponge
There are many studies on the nitriding behavior for a
titanium alloy plate. In this study, a titanium sponge, which
featured a porous structure, was used as feed material of
nitride, the validity of this experimental procedure was
examined.
Figure 3 shows the relationship between the concentra-
tion of nitrogen in the titanium nitride sponge and the time
for the 1 323 K heat treatment. The concentration of nitro-
gen increased with time until 12 h, after which it exhibited
a constant value.
Figure 4 shows the relationship between the concentra-
tion of nitrogen in the titanium nitride sponge and the tem-
Fig. 3. Relationship between concentration of nitrogen in tita-
nium nitride sponge and time.
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perature at a time of 3 h after the experiment was started.
The concentration of nitrogen increased with the tem-
perature until 1 273 K, following which the rate of increase
declined. By changing the heat treatment temperature, the
desired concentration of nitrogen for the titanium nitride
sponge can be achieved.
It is thought that the nitriding behavior of the titanium
sponge depends on its structure. Therefore, the structure of
the titanium sponge was examined.
Figure 5 shows the structure of the titanium sponge.
Figure 5(b) is a secondary electron image of the surface
Fig. 4. Change in concentration of nitrogen titanium nitride
sponge with temperature for a duration of 3 h.
Fig. 5. (a) External view, (b) surface, and (c) center of titanium
sponge before nitriding, respectively. (Online version in
color.)
© 2019 ISIJ
of sponge. The image shows that surface structure features
porosity with an interval of about 5.0 × 10 − 5 m. Figure 5(c)
shows the microstructure in the center region of the titanium
sponge observed by using an optical microscope. A porous
structure was also formed in the center region of the sponge
with an interval of about 5.0 × 10 − 5 m, in addition to on
the surface. It was found that the titanium sponge formed
a completely porous structure. Therefore, the nitrogen gas
permeated into the sponge easily, and the nitriding reaction
progressed from both sides of the solid to a distance of about
5.0 × 10 − 5 m in the thickness direction.
Figure 6 shows the microstructure of the titanium nitride
sponge. Figure 6(b) is the secondary electron image of the
surface of the sponge and Fig. 6(c) is the optical microscope
image in the center region of the sponge. It was found that
the titanium nitride sponge formed as a porous structure
with an interval of about 5.0 × 10 − 5 m, in addition to that
observed for the titanium sponge.
Figure 7(a) shows the optical microscopy image of the
microstructure of the cross-section of the center of the
titanium nitride sponge when the concentration of nitro-
gen was 8 mass%. The outer white region of the titanium
nitride sponge was perfused with in an embedded resin.
Figure 7(b) shows the concentration distribution for nitro-
gen and titanium in the titanium nitride sponge obtained via
energy-dispersive X-ray spectrometry (EDS). From these
results, it was confirmed that both the surface and the cen-
ter of the sponge were uniformly nitrided. It is thought that
the nitriding reaction in both the surface and center of the
Fig. 6. (a) External view, (b) surface and (c) center of titanium
nitride sponge, respectively. (Online version in color.)
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Fig. 7. EDS analysis of N and Ti at surface and center of titanium nitride sponge. (Online version in color.)
titanium sponge progressed because the nitrogen-mixed gas
permeated into the center region. These results necessitated
an examination of the reaction in the sponge to examine the
nitriding behavior of the titanium sponge.
The type of the reaction product formed by the reaction
between titanium and nitrogen gas was hypothesized to
change depending on the concentration of nitrogen. The
phases in the titanium nitride sponge varied with the con-
centration of nitrogen, and were identified and characterized
by X-ray diffraction.
Figure 8 shows the XRD patterns of the titanium sponge
and titanium nitride sponge. Both were composed of TiN
and Ti2N.
Figure 9 shows the relationship between the fraction of
nitriding and the concentration of nitrogen in the titanium
sponge and titanium nitride sponge. TiN and Ti2N were
formed, and the fraction of these nitrides depended on the
concentration of nitrogen.
However, these nitrides are reaction products, which are
obtained from the reactions with 1 mol of nitrogen; more-
over, these reactions are limited by the diffusion of nitrogen.
Therefore, the difference between the generation of TiN
and Ti2N is thought to be small. Therefore, in the following
analysis, it was assumed that the only titanium nitride is
TiN, in the following analysis.
107
Figure 10 shows the analytical model of the nitriding
reaction for the titanium sponge. A two-dimensional simple
analytical model was constructed, because the entire tita-
nium sponge consisted of porous structures, and elemental
titanium that was part of the structure was surrounded by
the nitrogen-mixed gas.
According to the kinetic theory of gases,18) the molecule
flux of nitrogen JN2, at the surface of titanium, can be pre-
dicted using the following equation.
p N2
J N2  ............................ (1)
2 mk B T
where, m: molar weight of nitrogen gas ( = 28.014), kB:
Boltzmann constant ( = 1.3806 × 10 − 23 JK − 1), T: temperature
(K), pN2: partial pressure of nitrogen gas (atm). The value of
pN2 was obtained from a previous study.19)
The diffusion of nitrogen in titanium is predicted by the
following equation. In this study, a generalized software20)
was used for this calculation.
dC
J Ti   ................................. (2)
dx
Mass balance between the nitrogen on the titanium side
and nitrogen on the gas side at the interface was assumed.
J N2 = J Ti ................................... (3)
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Figure 11 shows the concentration change of nitrogen in

titanium within the analytical element at a distance away
from the interface when the time is 0.25 h, 0.5 h, and 3 h,
respectively. The calculation temperature was 1 073, 1 173,
and 1 323 K. A longer heat treatment time corresponded to
a higher concentration of nitrogen. However, the concentra-
tion gradient of nitrogen was small, because the diffusion
length was small as well, i.e., 2.5 × 10 − 5 m.
The change in the calculated concentration of nitrogen
with the temperature is also shown in Fig. 4 for a heat treat-
ment time of 3 h. The calculated data agree with the experi-
mental data, thus confirming the validity of this analysis.

Fig. 8. Phases of titanium nitride in titanium nitride sponge deter-

mined by X-ray diffraction analysis. Concentration of
nitrogen: (a) 0 mass%, (b) 3, (c) 8 and (d) 15.

Fig. 9. Relationship between fraction of titanium nitride phase

and concentration of nitrogen determine by X-ray diffrac-
tion analysis.

Fig. 11. Relationship between concentration of nitrogen in tita-

Fig. 10. Schematic diagram of model for nitriding titanium nium sponge and distance. (a) 1 073 K, (b) 1 173 K and
sponge using nitrogen gas. (c) 1 323 K.

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3.2. Dissolution of Titanium Nitride Sponge
To calibrate the measured value of the two-color pyrom-
eter, this value was compared with the measurement result
of the titanium alloy melt by using a thermocouple. An
example of the measurement result is shown in Fig. 12.
After holding and preheating the thermocouple above the
alloy melt, it was immersed. The end position of the ther-
mocouple corresponded to the center of the titanium nitride
sponge. Thus, it was confirmed that the temperature of the
alloy melt could be maintained for about 200 s at 1 173 K.
The temperature of the alloy melt varied according to the
power of the current of the electron beam. The temperature
of the alloy melt was measured with a thermocouple while
changing the power current of the electron beam repeatedly,
in order to calibrate the output of the two-color pyrometer.
Figure 13 shows the shape of the pool for the alloy melt
where the titanium nitride sponge was immersed. After
the upper part of the ingot had been remelted, that melt
was solidified again. The longitudinal cross-section of the
solidification microstructure at the center of the ingot was
revealed by nitric-5 vol% hydrofluoric acid, and the bound-
ary in the molten pool was evaluated. As the depth of the
molten pool was about 4.0 × 10 − 2 m, a titanium nitride
sponge could be immersed completely in the molten pool.
Figure 14 shows photographs of the titanium nitride
Fig. 12. Measurement result of melt temperature by thermocouple
made with W-5%Re/W-26%Re.
Fig. 13. Molten pool depth near top surface of titanium alloy
ingot. Dashed line shows interface between melt and
solid. (Online version in color.)
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sponge before and after immersion in the molten pool. The
concentration of nitrogen of the titanium nitride sponge was
8 mass% in this sample. The diameter of the titanium nitride
sponge after immersion reduced as result of immersion. It
was confirmed that it dissolved almost evenly without any
localized dissolution. It is thought that the titanium nitride
sponge was held in the uniform temperature region of the
molten pool. The nominal dissolution rate was calculated
from the diameter difference of the titanium nitride sponge
before and after immersion, and immersion time.
Figure 15 shows the relationship between the nominal
dissolution rate obtained by the experiment and the recipro-
cal temperature when the concentration of nitrogen was 5,
8, 10, and 15 mass%. When the temperature of the alloy
melt was high, the nominal dissolution rate was high in all
cases. However, the experimental values deviated slightly;
thus, the influence of the concentration of nitrogen on the
Fig. 14. Titanium nitride sponge (a) before and (b) after immer-
sion into titanium alloy melt. (Online version in color.)
Fig. 15. Change in nominal dissolution rate of titanium nitride
sponges with temperature of titanium alloy melt.
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nominal dissolution rate was not observed. It is thought which the solid phase of the titanium nitride was staggered
that the influence of the concentration of nitrogen was not in the alloy melt as liquid at 5.0 × 10 − 5 m intervals, as
evident because the nominal dissolution rate of the titanium shown in Fig. 17(a). By considering structural symmetry,
nitride sponge, which was formed with a porous structure of an analyzed element was cut, as shown in Fig. 17(b). The
about 5.0 × 10 − 5 m in thickness of porous part, was high as nominal dissolution rate was evaluated using that element.
a result of the permeation of the alloy melt into the porous The nitrogen diffused from the titanium nitride sponge as
structure. In this figure, the relationship between the nomi- a solid to the alloy melt as a liquid. Conversely, aluminum
nal dissolution rate and the reciprocal of the temperature, and vanadium both diffused from the melt to the sponge.
which were obtained from previous studies, are also shown. As local equilibrium is gradually established at the inter-
These values are close to the lower limit obtained for this face between the titanium nitride sponge and alloy melt,
study. For this reason, it is thought that a simulated inclu- the interface shifts with time. As the thermal conductivity
sion, which was added to the top surface of the melt, went of the titanium nitride sponge is low, there is a temperature
to the bottom of the molten pool, where the temperature was gradient between the surface and the core when the sponge
lower, and cooled. is immersed in the alloy melt. Therefore, it is thought that
To predict the nominal dissolution rate of the titanium
nitride sponge, a simple dissolution model was prepared,
and the validity of the predicted values was examined by
comparing them with the experimental results. In a previous
study,4) a dissolution model assumed that the α phase and
β phase, which were part of simulated inclusions, were
arranged in a concentric pattern and that the outer of these
phases was surrounded by the alloy melt. Then, the dif-
fusion of nitrogen was calculated between the phases. By
using the relationship between the concentration of nitrogen
and temperature in the phase diagram, it was examined
whether a simulated inclusion would melt or not at a given
temperature.
Figure 16 shows the photograph of the cross section of
the titanium nitride sponge that was immersed into the melt,
held for 60 s, and pulled out to be inspected with an optical
microscope. It was found that the alloy melt filled the pores
of the titanium nitride sponge at the center in addition to the
surface. Therefore, it is necessary to prepare a dissolution
model of the titanium nitride sponge, which has a porous
structure. Subsequently, a structural model was assumed in

Fig. 17. Analytical model for dissolution of titanium nitride

sponge immersed in titanium alloy melt. (a) Entire tita-
nium nitride sponge, (b) ordered configuration of sponge
Fig. 16. Titanium nitride sponge after immersion into titanium and melt and (c) interface movement by diffusion in the
alloy melt. volume element.

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 ISIJ International, Vol. 59 (2019), No. 1
the outermost nth layer, in which the temperature is the
highest in the sponge, begins to dissolve in series. If the
dissolution time of the nth layer is evaluated, the nominal
dissolution rate can be calculated from the length of the
analyzed element.
Figure 18 shows the change in the concentration of nitro-
gen with time when the initial concentration of nitrogen in
the titanium nitride sponge is 8 mass% and the initial con-
centration of aluminum and vanadium in the alloy melt are
6 mass% and 4 mass%, respectively. The nitrogen diffused
Fig. 18. Calculated relationship between concentration of (a)
nitrogen, (b) aluminum and (c) vanadium and distance.
111
into the alloy melt and its concentration decreased. Further,
both aluminum and vanadium diffused into the titanium
nitride sponge and their concentrations decreased.
Figure 19 shows the relationship between a fraction
of the liquid in the analyzed element and the time when
the temperature was 2 023, 2 073, and 2 123 K. When the
fraction of liquid reaches 1.0, the titanium nitride sponge
in an analyzed element will dissolve completely. At any
temperature, the fraction of liquid increased with to time
and reached 1.0 finally. The shorter the time taken by the
Fig. 19. Calculated relationship between fraction of liquid and
time at (a) 2 023 K, (b) 2 073 K and (c) 2 123 K.
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 ISIJ International, Vol. 59 (2019), No. 1
fraction of the liquid to reach 1.0, the higher the temperature
of the element.
The relationship between the calculated nominal dissolu-
tion rate of the titanium nitride sponge and temperature is
also shown in Fig. 15. It was confirmed that the nominal
dissolution rate of the titanium nitride sponge could be pre-
dicted by using this analytical model because the calculated
value was in the range of experimental results.
4. Conclusions
The demand for high-quality titanium alloy ingots for
the aerospace industry is growing. Therefore, it is impor-
tant to remove the inclusions from the melt before casting,
even when the inclusions caused by the raw materials are
mixed. However, it is difficult to prevent the contamination
by nitrides, because it involves the generation of a reaction
product in the raw material. Therefore, it is necessary to
dissolve the nitride in the alloy melt before casting.
In this study, the nitriding and dissolution behavior of a
titanium sponge as the raw material was examined system-
atically. From these results, the following conclusions were
obtained.
(1) The titanium sponge and titanium nitride sponge
were formed with a porous structures. The porosity interval
was about 5.0 × 10 − 5 m at both the surface and center of
the sponge. When the nitride sponge was immersed in the
titanium alloy melt, this melt permeated into the pores of
the sponge.
(2) The titanium nitride sponge could be produced with
a titanium sponge as the raw material by heat treatment with
nitrogen gas. A high concentration of the titanium nitride
sponge corresponds to a higher nitriding temperature, and
thus a longer nitriding time.
(3) The nominal dissolution rate of the titanium nitride
sponge in the titanium alloy melt changed with the tempera-
© 2019 ISIJ
ture of the melt. The nominal dissolution rate of the sponge
increased with increasing temperature. The influence of the
concentration of the titanium nitride sponge on the nominal
dissolution rate was small.
(4) An analytical model was constructed to nitride
titanium sponge with nitrogen gas. In addition, an analyti-
cal model for the dissolution of the titanium nitride sponge
in the titanium alloy melt was constructed. By using these
models, both, the nitriding and dissolution behaviors of the
sponge could be predicted.
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