Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave
A novel method of the synthesis of titanium silicide nanoparticles via solid-state route in an autoclave at 700 °C is reported. The reaction of titanium silicide could be described briefly as: 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD pattern indicated that the product was hexagonal Ti₅Si₃. The Ti₅S...
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| Опубліковано в: : | Сверхтвердые материалы |
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Інститут надтвердих матеріалів ім. В.М. Бакуля НАН України
2017
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| Цитувати: | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave / W. Mao, K. Bao, F. Cao, L. Ye, H. Xie, B. Li, W. Wang // Сверхтвердые материалы. — 2017. — № 2. — С. 56-61. — Бібліогр.: 21 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860228438226370560 |
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| author | Mao, W. Bao, K. Cao, F. Ye, L. Xie, H. Li, B. Wang, W. |
| author_facet | Mao, W. Bao, K. Cao, F. Ye, L. Xie, H. Li, B. Wang, W. |
| citation_txt | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave / W. Mao, K. Bao, F. Cao, L. Ye, H. Xie, B. Li, W. Wang // Сверхтвердые материалы. — 2017. — № 2. — С. 56-61. — Бібліогр.: 21 назв. — англ. |
| collection | DSpace DC |
| container_title | Сверхтвердые материалы |
| description | A novel method of the synthesis of titanium silicide nanoparticles via solid-state route in an autoclave at 700 °C is reported. The reaction of titanium silicide could be described briefly as: 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD pattern indicated that the product was hexagonal Ti₅Si₃. The Ti₅Si₃ particle size (about 20–40 nm) is confirmed by the TEM images. Furthermore, the thermal stability and oxidation resistance of the titanium silicide nanoparticles were also investigated.
Повідомлено про новий метод синтезу наночастинок силіциду титану твердотільним шляхом в автоклаві при температурі 700 °С. Реакція силіциду титану може бути коротко записана як 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD-зображення показало, що продукт є гексагональним Ti₅Si₃. Розмір частинок Ti₅Si₃ (∼ 20–40 нм) підтверджено ПЕМ-зображенням. Також досліджено термостабільність і опір окисленню частинок силіциду титану.
Сообщается о новом методе синтеза наночастиц силицида титана твердотельным путем в автоклаве при температуре 700 °С. Реакция силицида титана может быть кратко записана как 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD-изображение показало, что продукт является гексагональным Ti₅Si₃. Размер частиц Ti₅Si₃ (∼ 20–40 нм) подтвержден ПЭМ-изображением. Также исследованы термостабильность и сопротивление окислению частиц силицида титана.
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| first_indexed | 2025-12-07T18:20:59Z |
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www.ism.kiev.ua/stm 56
UDC 66.091.1:669.295:543.442.3
W. Mao, K. Bao*, F. Cao, L. Ye, H. Xie, B. Li, W. Wang
College of Chemistry and Pharmacy Engineering,
Nanyang Normal University, Henan, P. R. China
**baokeyan@126.com
Facile and scalable synthesis of Ti5Si3
nanoparticles via solid-state route
in an autoclave
A novel method of the synthesis of titanium silicide nanoparticles via
solid-state route in an autoclave at 700 °C is reported. The reaction of titanium silicide
could be described briefly as: 5TiO2 + 3Si + 20Li = Ti5Si3 + 10Li2O. XRD pattern
indicated that the product was hexagonal Ti5Si3. The Ti5Si3 particle size (about 20–
40 nm) is confirmed by the TEM images. Furthermore, the thermal stability and
oxidation resistance of the titanium silicide nanoparticles were also investigated.
Keywords: titanium alloys, nanocrystalline materials, X-ray
diffraction (XRD).
INTRODUCTION
In recent years, alloys systems have attracted widespread attention
from researchers home and abroad, because of their excellent physical and
chemical properties [1–3]. Metal silicides are a broad family of refractory
intermetallic compounds between transition metals and silicon. Titanium silicide
(Ti5Si3) has attracted considerable attention due to its outstanding properties in-
cluding high melting temperature (2122 °C), low density (4.32 g/cm3) and high
hardness, as well as excellent strength at elevated temperature and high oxidation
resistance, which consequently promote Ti5Si3 as a promising material for high-
temperature structural applications [4–7].
Simple and scalable synthesis of Ti5Si3 nanomaterials will be vital for their
technological applications [8, 9]. Generally, titanium-silicon alloy is prepared
through conventional methods, such as combustion synthesis [10, 11], self-
propagating high temperature synthesis (SHS) [12], ball-milling method [13],
molten salt rod [14], reaction hot pressing [15], chloride-generated route [16],
mechanical alloying (MA) [17], chemical vapour deposition [18, 19], electro-
pressure sintering [20]. It is difficult now to obtain the Ti5Si3 nanomaterials. So far,
Ti5Si3 nanopaticles have only been prepared in molten salts system at 700 °C [21].
In this work, a solid-state route in an autoclave for preparation of Ti5Si3
nanomaterials at low temperature was reported for the first time, with process
being described by the following equation: 5TiO2 + 3Si + 20Li → Ti5Si3 + 10Li2O.
The approach to synthesize Ti5Si3 nanoparticles in an autoclave is favorable and
could be exploited for practical industrial Ti5Si3 nanomaterials production.
EXPERIMENTAL
Preparation of Ti5Si3 nanomaterials
All the chemical reagents were purchased from Sinopharm Chemical Reagent Co.,
Ltd. and used without further purification. The synthesis was carried out in a stainless
steel autoclave (20 mL), in which 0.8 g of titanium dioxide, 0.168 g of silicon powders
© W. MAO, K. BAO, F. CAO, L. YE, H. XIE, B. LI, W. WANG, 2017
ISSN 0203-3119. Сверхтвердые материалы, 2017, № 2 57
and 1.5 g of Lithium powders were added. The temperature of the stove was raised
from room temperature to 700 °C with a heating ramp rate of 5 °C/min and maintained
at the target temperature for 10 h, and then it was cooled to room temperature naturally.
The precipitates in the autoclave were collected and washed with absolute ethanol,
dilute hydrochloric acid, and distilled water several times to remove the impurity. The
final products were dried in vacuum at 60 °C for 6 h.
Characterization
The XRD measurements were carried out with a Philips X-ray diffractometer.
TEM images, high-resolution transmission electron microscopy (HRTEM) images,
and the corresponding selected-area electron diffraction (SAED) patterns were
taken on a JEOL-2000 transmission electron microscope with an accelerating
voltage of 200 kV. Thermogravimetric analysis (TGA) profile was collected with a
Shimadzu-50 thermoanalyzer apparatus under flowing of air.
RESULTS AND DISCUSSION
The Powder X-ray diffraction (XRD) pattern of the sample prepared at 600 °C
is shown in Fig. 1, a. The diffraction peaks (200), (111), (002), (210), (211), (300),
(112), (221), (311), (400), (222), (410), (213), (402) and (322) in the figure are
completely consistent with the standard card of hexagonal Ti5Si3 (JCPDS PDF
No. 29-1362; space group P63/mcm, a = 7.444 Å, c = 5.143 Å.). The EDS
spectrum (see Fig. 1, b) reveals the presence of Ti and Si elements at a Ti/Si atomic
ratio of 1.67:1, indicating the formation of Ti5Si3 (the signals of Cu came from the
copper grid used for the EDS observation). Both XRD pattern and EDS spectrum
confirm that the sample is Ti5Si3.
20 30 40 50 60 70
40
0 31
1
22
1
21
0
00
2 21
3
40
2 22
2
41
0
32
2
30
0
11
2
21
1
10
2
11
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te
n
si
ty
, a
rb
. u
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it
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b
Fig. 1. XRD pattern (a) and EDS spectrum (b) of Ti5Si3 nanoparticles.
www.ism.kiev.ua/stm 58
Representative Ti5Si3 nanocrystals are compiled in Fig. 2. Scanning electron
microscopy (SEM) images of the Ti5Si3 nanoparticles reveal that the as-prepared
NPs are homogeneous, with particle size clearly at the nanoscale (see Fig. 2, a).
Transmission electron microscopy (TEM) images revealed an average particle size
of 20–40 nm (see Fig. 2, b). The corresponding SAED pattern (see Fig. 2, b, inset)
indicates that the sample is polycrystalline, confirming the particle size is relatively
small. The high magnification TEM image recorded three Ti5Si3 nanocrystals about
20 nm of size shown in Fig. 2, c. The average distance between the neighboring
fringes (shown in Fig. 2, d) is about 0.245 nm, corresponding to the (210) plane of
hexagonal Ti5Si3.
a b
c d
Fig. 2. SEM image (a), TEM image and SAED pattern (right corner) (b), higher magnification
TEM image (c), HRTEM image (d) of the as-prepared Ti5Si3 nanoparticles.
The thermal stability of the as-prepared Ti5Si3 nanoparticles was examined by
TGA-DTA under flowing air. The TGA-DTA curves of Ti5Si3 nanoparticles
oxidation tests (air flow) are shown in Figs. 3, a and b. From the TGA curve (see
Fig. 3, a) it is found that the weight of the product does not change significantly
below 300 °C. From 300 °C to 1000 °C, the weight of the powder increases
gradually by about 70 %. As shown in the DTA curve (see Fig. 3, b), there is only
one big exothermic peak, which starts at 500 °C and ends at 570 °C. Combining
the results of the two curves, we can reach the following conclusions: the sample
has basically been not oxidized from the room temperature to 300 °C. From 300 to
1000 °C, the sample suffered gradual oxidation. The oxidation process becomes
intensified as the temperature rises to 540 °C, concluded from the DTA curve (see
Fig. 3, a) and DrTGA curve (Fig. 4).
ISSN 0203-3119. Сверхтвердые материалы, 2017, № 2 59
0 100 200 300 400 500 600 700 800 900 1000 1100
1.0
1.1
1.2
1.3
1.4
1.5
TGA, %
Temperature, °C
–50
–40
–30
–20
–10
0
10
W
ei
gh
t g
ai
n
DTA, uv/mg
Fig. 3. TGA-DTA curves of the Ti5Si3 nanoparticles under flowing air.
0 200 400 600 800 1000
–0.0005
0
0.0005
0.0010
0.0015
0.0020
0.0025
0.0030 DrTGA, mg/min
W
ei
gh
t g
ai
n
Temperature, °C
Fig. 4. DrTGA spectrum of the Ti5Si3 nanoparticles under flowing air.
CONCLUSIONS
It is challenging to synthesize nanostructured refractory silicides, such as Ti5Si3
and other metal-rich silicides (M5Si3). In this work, titanium dioxide, silicon
powders and lithium powders placed in an autoclave at 700 °C results in the
formation of Ti5Si3 nanoparticles with an average particle size of 30 nm. The XRD
pattern indicated that the product is hexagonal Ti5Si3. The structure and
morphology of the obtained product were derived from SEM, TEM, EDS, and
DTA-TGA. The approach to synthesize Ti5Si3 nanoparticles in an autoclave could
be exploited for industrial Ti5Si3 nanomaterials production and may provide new
insights into the synthesis of other alloys.
This work is supported by the National Natural Science Foundation of China
(No. U1404505), The Program for Innovative Talent in the University of Henan
Province (16HASTIT010) and Henan Province Project Education Fund
(14A150047).
www.ism.kiev.ua/stm 60
Повідомлено про новий метод синтезу наночастинок силіциду титану
твердотільним шляхом в автоклаві при температурі 700 °С. Реакція силіциду титану
може бути коротко записана як 5TiO2 + 3Si + 20Li = Ti5Si3 + 10Li2O. XRD-зображення
показало, що продукт є гексагональним Ti5Si3. Розмір частинок Ti5Si3 (∼ 20–40 нм) під-
тверджено ПЕМ-зображенням. Також досліджено термостабільність і опір окисленню
частинок силіциду титану.
Ключові слова: титановий сплав, нанокристалічний матеріал,
дифракція рентгенівських променів.
Сообщается о новом методе синтеза наночастиц силицида титана
твердотельным путем в автоклаве при температуре 700 °С. Реакция силицида титана
может быть кратко записана как 5TiO2 + 3Si + 20Li = Ti5Si3 + 10Li2O. XRD-
изображение показало, что продукт является гексагональным Ti5Si3. Размер частиц
Ti5Si3 (∼ 20–40 нм) подтвержден ПЭМ-изображением. Также исследованы термоста-
бильность и сопротивление окислению частиц силицида титана.
Ключевые слова: титановый сплав, нанокристаллический материал,
дифракция рентгеновских лучей.
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ISSN 0203-3119. Сверхтвердые материалы, 2017, № 2 61
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Received 01.12.15
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| id | nasplib_isofts_kiev_ua-123456789-160107 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 0203-3119 |
| language | English |
| last_indexed | 2025-12-07T18:20:59Z |
| publishDate | 2017 |
| publisher | Інститут надтвердих матеріалів ім. В.М. Бакуля НАН України |
| record_format | dspace |
| spelling | Mao, W. Bao, K. Cao, F. Ye, L. Xie, H. Li, B. Wang, W. 2019-10-22T20:01:38Z 2019-10-22T20:01:38Z 2017 Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave / W. Mao, K. Bao, F. Cao, L. Ye, H. Xie, B. Li, W. Wang // Сверхтвердые материалы. — 2017. — № 2. — С. 56-61. — Бібліогр.: 21 назв. — англ. 0203-3119 https://nasplib.isofts.kiev.ua/handle/123456789/160107 66.091.1:669.295:543.442.3 A novel method of the synthesis of titanium silicide nanoparticles via solid-state route in an autoclave at 700 °C is reported. The reaction of titanium silicide could be described briefly as: 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD pattern indicated that the product was hexagonal Ti₅Si₃. The Ti₅Si₃ particle size (about 20–40 nm) is confirmed by the TEM images. Furthermore, the thermal stability and oxidation resistance of the titanium silicide nanoparticles were also investigated. Повідомлено про новий метод синтезу наночастинок силіциду титану твердотільним шляхом в автоклаві при температурі 700 °С. Реакція силіциду титану може бути коротко записана як 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD-зображення показало, що продукт є гексагональним Ti₅Si₃. Розмір частинок Ti₅Si₃ (∼ 20–40 нм) підтверджено ПЕМ-зображенням. Також досліджено термостабільність і опір окисленню частинок силіциду титану. Сообщается о новом методе синтеза наночастиц силицида титана твердотельным путем в автоклаве при температуре 700 °С. Реакция силицида титана может быть кратко записана как 5TiO₂ + 3Si + 20Li = Ti₅Si₃ + 10Li₂O. XRD-изображение показало, что продукт является гексагональным Ti₅Si₃. Размер частиц Ti₅Si₃ (∼ 20–40 нм) подтвержден ПЭМ-изображением. Также исследованы термостабильность и сопротивление окислению частиц силицида титана. This work is supported by the National Natural Science Foundation of China (No. U1404505), The Program for Innovative Talent in the University of Henan Province (16HASTIT010) and Henan Province Project Education Fund (14A150047). en Інститут надтвердих матеріалів ім. В.М. Бакуля НАН України Сверхтвердые материалы Получение, структура, свойства Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave Article published earlier |
| spellingShingle | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave Mao, W. Bao, K. Cao, F. Ye, L. Xie, H. Li, B. Wang, W. Получение, структура, свойства |
| title | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave |
| title_full | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave |
| title_fullStr | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave |
| title_full_unstemmed | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave |
| title_short | Facile and scalable synthesis of Ti₅Si₃ nanoparticles via solid-state route in an autoclave |
| title_sort | facile and scalable synthesis of ti₅si₃ nanoparticles via solid-state route in an autoclave |
| topic | Получение, структура, свойства |
| topic_facet | Получение, структура, свойства |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/160107 |
| work_keys_str_mv | AT maow facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave AT baok facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave AT caof facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave AT yel facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave AT xieh facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave AT lib facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave AT wangw facileandscalablesynthesisofti5si3nanoparticlesviasolidstaterouteinanautoclave |