Research of a vacuum diffusion boron silicification process for constructional materials
In this work process of vacuum diffusion boron silicification of materials in sodium chloride vapour were researched. Gaseous medium composition was found by using the thermodynamic calculations of chemical reactions between NaCl vapour and the components of saturating powder mixture in the proce...
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| Опубліковано в: : | Физическая инженерия поверхности |
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| Дата: | 2013 |
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Науковий фізико-технологічний центр МОН та НАН України
2013
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| Цитувати: | Research of a vacuum diffusion boron silicification process for constructional materials / V.I. Zmij, S.G. Rudenkiy // Физическая инженерия поверхности. — 2013. — Т. 11, № 1. — С. 18–21. — Бібліогр.: 7 назв. — англ. |
Репозитарії
Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1859620460292997120 |
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| author | Zmij, V.I. Rudenkiy, S.G. |
| author_facet | Zmij, V.I. Rudenkiy, S.G. |
| citation_txt | Research of a vacuum diffusion boron silicification process for constructional materials / V.I. Zmij, S.G. Rudenkiy // Физическая инженерия поверхности. — 2013. — Т. 11, № 1. — С. 18–21. — Бібліогр.: 7 назв. — англ. |
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| description | In this work process of vacuum diffusion boron silicification of materials in sodium chloride vapour
were researched. Gaseous medium composition was found by using the thermodynamic calculations
of chemical reactions between NaCl vapour and the components of saturating powder mixture in the
process for the temperature T = 1400 − 1600 K and pressure P = 1.33 − 1333 Pa, when the content of
boron is 1 weight percent and 10 weight percent in backfilling. Formation mechanism of diffusion
layer оn example of the vacuum activated boron silicification of graphite was determined.
Keywords: boron silicification, diffusion saturation, activator, vacuum, graphite.
В работе были проведены исследования механизма процесса вакуумного диффузионного боросилицирования материалов в парах хлористого натрия. Используя термодинамический расчет
химических реакций между парами активатора и компонентами насыщающей порошковой
смеси был определен состав газовой среды в этом процессе для температур Т = 1400 – 1600 К
и давлений Р = 1.33 – 1333 Па, при содержании бора 1 и 10 вес.% в засыпке. На примере вакуумного активированного боросилицирования графита установлен механизм образования диффузионного слоя.
В роботі були проведені дослідження механізму процесу вакуумного дифузійного боросиліціювання матеріалів у парах хлористого натрію. Використовуючи термодинамічний розрахунок
хімічних реакцій між парами активатора та компонентами насичуючої порошкової суміші був
визначений склад газового середовища у цьому процесі для температур Т = 1400 – 1600 К та
тисків Р = 1.33 – 1333 Па, при вмісті бору 1 та 10 ваг.% в засипці. На прикладі вакуумного активованого боросиліціювання графіту встановлено механізм утворення дифузійного шару
|
| first_indexed | 2025-11-29T03:19:25Z |
| format | Article |
| fulltext |
18
INTRODUCTION
The performance characteristics of constructional
materials must meet high requirements, if the ma-
chinery working in harsh environments. It is possible
to apply a different coatings for the development
and deriving of such materials. There are different
methods of formation of such coatings. Structure
and physical-chemical features of each of these
coatings are formed by the composition, manner
and mode of receipt of this protective layer. A team
of specialists at the National Science Center “Khar-
kov Institute of Physics and Technology” (NSC
KIPT) has developed a method of vacuum activated
diffusion saturation [2, 3]. This method is environ-
mentally friendly, provides a strong adhesion of the
coating to the surface of the processed materials of
construction and allows you to create effective integ-
rated multipurpose protective layers. Such diffusion
coatings protect the surface of construction materials
from wear, i.e. they are durable. Also, these coatings
are corrosion resistant. The coatings prevent the des-
truction of refractory metals and carbon materials
from oxidising. Corrosion resistance of the coating
is persistent in the temperature range from room
temperature up to 2000 °С. Silicification or boron
silicification of metals and carbon materials is one of
the stages of a chemical-thermal treatment for cre-
ation of these protective coatings. Layer of silicide’s
UDC 621.793.6:620.181.4
RESEARCH OF A VACUUM DIFFUSION BORON SILICIFICATION PROCESS FOR
CONSTRUCTIONAL MATERIALS
V.I. Zmij, S.G. Rudenkiy
National Science Center “Kharkov Institute of Physics and Technology”
Ukraine
Received 21.01.2013
In this work process of vacuum diffusion boron silicification of materials in sodium chloride vapour
were researched. Gaseous medium composition was found by using the thermodynamic calculations
of chemical reactions between NaCl vapour and the components of saturating powder mixture in the
process for the temperature T = 1400 − 1600 K and pressure P = 1.33 − 1333 Pa, when the content of
boron is 1 weight percent and 10 weight percent in backfilling. Formation mechanism of diffusion
layer оn example of the vacuum activated boron silicification of graphite was determined.
Keywords: boron silicification, diffusion saturation, activator, vacuum, graphite.
ИССЛЕДОВАНИЕ ПРОЦЕССА ВАКУУМНОГО АКТИВИРОВАННОГО
БОРОСИЛИЦИРОВАНИЯ КОНСТРУКЦИОННЫХ МАТЕРИАЛОВ
В.И. Змий, С.Г. Руденький
В работе были проведены исследования механизма процесса вакуумного диффузионного боро-
силицирования материалов в парах хлористого натрия. Используя термодинамический расчет
химических реакций между парами активатора и компонентами насыщающей порошковой
смеси был определен состав газовой среды в этом процессе для температур Т = 1400 – 1600 К
и давлений Р = 1.33 – 1333 Па, при содержании бора 1 и 10 вес.% в засыпке. На примере ва-
куумного активированного боросилицирования графита установлен механизм образования диф-
фузионного слоя.
Ключевые слова: боросилицирование, активатор, вакуум, графит, диффузионное насыщение
ДОСЛІДЖЕННЯ ПРОЦЕСУ ВАКУУМНОГО АКТИВОВАНОГО
БОРОСИЛІЦІЮВАННЯ КОНСТРУКЦІЙНИХ МАТЕРІАЛІВ
В.І. Змій, С.Г. Руденький
В роботі були проведені дослідження механізму процесу вакуумного дифузійного боросилі-
ціювання матеріалів у парах хлористого натрію. Використовуючи термодинамічний розрахунок
хімічних реакцій між парами активатора та компонентами насичуючої порошкової суміші був
визначений склад газового середовища у цьому процесі для температур Т = 1400 – 1600 К та
тисків Р = 1.33 – 1333 Па, при вмісті бору 1 та 10 ваг.% в засипці. На прикладі вакуумного ак-
тивованого боросиліціювання графіту встановлено механізм утворення дифузійного шару.
Ключові слова: боросиліціювання, активатор, вакуум, графіт, дифузійне насичення.
V.I. Zmij, S.G. Rudenkiy, 2013
19ФІП ФИП PSE, 2013, т. 11, № 1, vol. 11, No. 1
is formed on the surface of the material after the
chemical-thermal treatment. Many of this silicide’s
are corrosion resistant. Coating of silicon carbide
SiC is formed on the carbon materials after the che-
mical-thermal treatment. This coating has high har-
dness and heat resistance. Molybdenum silicide and
tungsten silicide can be got by silicification method
of these refractory metals. These silicide’s are widely
used to protect products from high-temperature
oxidation. During the boron silicification process a
boron is injected simultaneously with the silicon
saturation of the surface. Boron atoms have a small
size and prevent the degradation of the coating. This
boron silicide coating is heat resistant at high tempe-
ratures. The process of vacuum diffusion silicification
in vapour of sodium chloride was investigated in [4,
5]. However, the process of boron silicification is
not yet sufficiently studied.
VACUUM DIFFUSION BORON SILIFI-
CATION PROCESS AND COMPOSITION
OF GASEOUS SATURATION MEDIUM
In this work we investigated the mechanism of va-
cuum diffusion boron silicification in the presence of
a vapour of sodium chloride. We have established
the dependence of a composition of the gaseous
saturation medium from temperature and pressure
during the process. And the influence of the com-
position of the gaseous saturation medium on the
composition of the resulting diffusion layer.
Vacuum activated diffusion boron silicification of
materials occurs by reaction of sodium chloride va-
pour with boron and silicon. This process takes place
under reduced pressure. The result is a saturating
gaseous medium. Gaseous activator interacts with
saturating elements. This interaction is described by
chemical reactions:
NaCl(g) + B(s) X BCl(g) + Na(g), (1)
NaCl(g) + (1/2)B(s)X(1/2)BCl2(g) + Na(g), (2)
NaCl(g) + (1/3)B(s)X(1/3)BCl3(g) + Na(g), (3)
NaCl(g) + Si(s) X SiCl(g) + Na(g), (4)
NaCl(g) + (1/2)Si(s)X(1/2)SiCl2(g) + Na(g),
(5)
NaCl(g) + (1/3)Si(s)X 1/3)SiCl3(g) + Na(g),
(6)
NaCl(g) + (1/4)Si(s)X(1/4)SiCl4(g) + Na(g). (7)
The formation of the gaseous saturation medium
occurs in accordance with the chemical reactions
(1) – (7). The degree of progress of chemical rea-
ctions determine the composition of the gaseous
medium. In order to define the composition of the
gaseous medium in the vacuum activated diffusion
boron silicification we need to choose initial
conditions: quantity of vapours of sodium chloride,
silicon and boron. Also it is necessary to establish
the degree of chemical reactions (1) – (7). It is
possible by solving set of equations which are
prepared in accordance with the law of mass action
for these reactions. Set of equations is based on the
fact that the initial amount of gaseous sodium chloride
is 1 mole and saturating powder mixture is 1 mole.
Saturating powder mixture is composed from boron
and silicon. We established that the percentage of
sodium chloride, which reacted by chemical
reactions (1) – (7), respectively, will be x, y, z, k, l,
m, n.
Using the law of mass action we can establish a
connection between the equilibrium constants for
reactions (1) – (7) and the equilibrium partial
pressure of substances that are present in the system
NaСl-В-Si.
( )1
1 7exp
1
2 3 2 3 4
x x y z k l m nGK G
y z l m nR T x k
⋅ + + + + + +∆ = − ∆ = × ⋅ + + + + + + +
( )1 B
P
x y z k k m n a
×
− + + + + + + ⋅
; (8)
( ) ( )1 2
2
2 1 2
2
exp
1
2 3 2 3 4
y x y z k l m nGK
R T y z l m nx k
⋅ + + + + + +∆ = − = × ⋅ + + + + + + +
( )
1 2
1 21 B
P
x y z k k m n a
×
− + + + + + + ⋅
; (9)
( ) ( )1 3
3
3 1 2
3
exp
1
2 3 2 3 4
z x y z k l m nGK
R T y z l m nx k
⋅ + + + + + +∆ = − = × ⋅ + + + + + + +
( )
1 3
1 31 B
P
x y z k l m n a
×
− + + + + + + ⋅
; (10)
( )4
4 exp
1
2 3 2 3 4
k x y z k l m nGK
y z l m nR T x k
⋅ + + + + + +∆ = − = × ⋅ + + + + + + +
( )1 Si
P
x y z k k m n a
×
− + + + + + + ⋅
; (11)
V.I. ZMIJ, S.G. RUDENKIY
20
( ) ( )1 2
5
5 1 2
2
exp
1
2 3 2 3 4
l x y z k l m nGK
R T y z l m nx k
⋅ + + + + + +∆ = − = × ⋅ + + + + + + +
( )
1 2
1 2
Si1
P
x y z k k m n a
×
− + + + + + + ⋅
; (12)
( ) ( )1 3
6
6 1 3
3
exp
1
2 3 2 3 4
m x y z k l m nGK
R T y z l m nx k
⋅ + + + + + +∆ = − = × ⋅ + + + + + + +
( )
1 3
1 3
Si1
P
x y z k l m n a
×
− + + + + + + ⋅
; (13)
( ) ( )1 4
7
7 1 4
4
exp
1
2 3 2 3 4
n x y z k l m nGK
R T y z l m nx k
⋅ + + + + + +∆ = − = × ⋅ + + + + + + +
( )
1 4
1 4
Si1
P
x y z k l m n a
×
− + + + + + + ⋅
; (14)
Here K1, K2, K3, K4, K5, K6, K7 and ∆G1,
∆G2, ∆G3, ∆G4, ∆G5, ∆G6, ∆G7 – respectively,
are the equilibrium constant and Gibbs energy for
reactions (1 – 7); R – universal gaseous constant;
aB and aSi – activity of boron and silicon.
Solution of this system was carried out for the
temperature Т = 1400 ÷ 1600 К and pressure
Р = 1333 ÷ 1.33 Pa and is presented in tabl. 1.
The values of the Gibbs energy was calculate
using thermodynamic data from sources [6, 7].
Tabl. 1 shows the structure of the gaseous
saturation medium in the system environment
NaCl – B – Si during boron silicification process.
These data are expressed in moles, depending
on the ratio of the components of powder filling,
temperature and pressure. After analysis of these
data we concluded that the main products involved
in the formation of the diffusion layer through
disproportionation reactions are those BCl, BCl2,
SiCl, SiCl2. Gaseous mixture contains boron tri-
chloride in large quantities. It may participate in the
etching of the substrate material depending on a
temperature and pressure in the reaction zone. For
a more complete understanding of the mechanism
of vacuum activated diffusion boron silicification we
also investigated the interaction of the lower
chlorides of boron and silicon with the treated ma-
terial, for example, graphite. Boron and silicon with
carbon forms B4C and SiC. We conducted a
thermodynamic calculation of possible chemical
disproportionation reactions, which describe the
interaction of the lower chlorides of boron and silicon
with carbon. The results of these calculations are
presented in tabl. 2.
The data presented in tabl. 2 shows that the
conversion reactions rate of borides and silicides is
close to one. Based on the composition of the
saturating gaseous mixture we established that the
preferred is the formation of silicon carbide com-
pared with boron carbide. Also heat-resistant of bo-
ron carbide is lower than heat-resistant of silicon
carbide. Because of this using of boron as a dopant
is preferred than using it as a primary component of
Table 1
Equilibrium composition of the gaseous mixture in
the system NaCl-B-Si
Sub-
stan-
ce
T = 1400 K
Composition of powder mixture
10 atomic percent of
B+90 atomic percent of Si
1 atomic percent of
B+99 atomic percent of Si
Pressure Р, Pа Pressure Р, Pа
1333 1333 1.331.33
7.253⋅10–8 7.067⋅10–9 5.732⋅10–75.953⋅10–6BCl
1.734⋅10–7 1.647⋅10–8 1.070⋅10–71.154⋅10–6BCl2
1.0211⋅10–5 9.456⋅10–7 4.912⋅10–75.511⋅10–6BCl3
1.083⋅10–4 1.161⋅10–4 9.412⋅10–38.886⋅10–3SiCl
6.502⋅10–4 6.792⋅10–4 4.412⋅10–34.328⋅10–3SiCl2
2.805⋅10–6 2.855⋅10–6 1.485⋅10–61.514⋅10–6SiCl3
1.703⋅10–8 1.689⋅10–8 7.039⋅10–107.453⋅10–10SiCl4
1.448⋅10–3 1.486⋅10–3 1.824⋅10–21.757⋅10–2Na
9.986⋅10–1 9.985⋅10–1 9.818⋅10–19.824⋅10–1NaCl
T = 1500 K
4.815⋅10–7 4.673⋅10–8 2.968⋅10–63.122⋅10–5BCl
6.406⋅10–7 6.034⋅10–6 2.502⋅10–72.731⋅10–6BCl2
1.223⋅10–5 1.118⋅10–6 3.027⋅10–73.428⋅10–6BCl3
5.622⋅10–4 6.002⋅10–4 3.812⋅10–23.645⋅10–2SiCl
1.345⋅10–3 1.394⋅10–3 5.780⋅10–35.736⋅10–3SiCl2
3.515⋅10–6 3.534⋅10–6 9.570⋅10–79.853⋅10–7SiCl3
1.058⋅10–8 1.033⋅10–8 1.820⋅10–101.851⋅10–10SiCl4
3.302⋅10–3 3.402⋅10–3 4.968⋅10–24.797⋅10–2Na
9.967⋅10–1 9.966⋅10–1 9.503⋅10–19.520⋅10–1NaCl
T = 1600 K
2.428⋅10–6 2.347⋅10–7 1.030⋅10–51.102⋅10–4BCl
1.864⋅10–6 1.742⋅10–7 4.184⋅10–74.600⋅10–6BCl2
1.266⋅10–5 1.145⋅10–6 1.505⋅10–71.700⋅10–6BCl3
2.286⋅10–3 2.432⋅10–3 1.067⋅10–11.037⋅10–1SiCl
2.356⋅10–3 2.423⋅10–3 5.819⋅10–35.816⋅10–3SiCl2
3.814⋅10–6 3.793⋅10–6 4.986⋅10–75.122⋅10–7SiCl3
2.035⋅10–12 5.741⋅10–9 4.130⋅10–114.362⋅10–11SiCl4
7.054⋅10–3 7.293⋅10–3 1.183⋅10–11.155⋅10–1Na
9.928⋅10–1 9.927⋅10–1 8.816⋅10–18.845⋅10–1NaCl
RESEARCH OF A VACUUM DIFFUSION BORON SILICIFICATION PROCESS FOR CONSTRUCTIONAL MATERIALS
ФІП ФИП PSE, 2013, т. 11, № 1, vol. 11, No. 1
21ФІП ФИП PSE, 2013, т. 11, № 1, vol. 11, No. 1
the protective coating. Therefore, the process of
boron silicification of carbon must be carried out in
appropriate conditions. Based on tabl. 1 we can
see that the equilibrium partial pressure of the lower
chlorides of boron is about three orders of magnitude
lower than the corresponding value for the silicon
chloride. And the concentration of boron in the
resulting diffusion layer is much smaller than silicon.
This should facilitate to boron carbide doping of
heat-resistant diffusion coating based on silicon
carbide. Below, on fig. 1, a microstructure of boron
silicificated graphite is shown.
CONCLUSIONS
1. We carried out calculation of gaseous medium
for the process of vacuum diffusion boron
silicification in vapours of sodium chloride for
the temperature T = 1500 K and pressure of
1.33 Pa and 1333 Pa.
2. We found that the main components of the ga-
seous saturation medium in the process of vacu-
um boron silicification are lower chlorides of
boron and silicon. These chlorides are a cause
of the diffusion layer formation.
3. We defined the chemical reaction conversion
degree of boron carbide and silicon carbide for-
mation during diffusion boron silicification of
graphite surface.
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Table 2
The conversion rate of α reactions of the lower
chlorides of boron and silicon with carbon at a
temperature Т = 1500 К
Chemical reaction equation Pressure Р, Pа
1333 1.33
BCl(g) + (1/6)C(s) X
X (1/6)B4C(s) + (1/3)BCl3(g)
0.995 0.388
BCl2(g) + (1/12)C(s) X
X (1/12)B4C(s) + (2/3)BCl3(g)
0.999 0.99
SiCl(g) + (3/4)C(s) X
X (3/4)SiC(s) + (1/4)SiCl4(g)
0.999 0.986
SiCl2(g) + (1/2)C(s) X
X (1/2)SiC(s) + (1/2)SiCl4(g)
0.80 0.012
Fig. 1. The microstructure of graphite with coating after
vacuum activated boron silicification at a temperature
Т = 1280 °С during 7 hours (×400).
V.I. ZMIJ, S.G. RUDENKIY
|
| id | nasplib_isofts_kiev_ua-123456789-99266 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1999-8074 |
| language | English |
| last_indexed | 2025-11-29T03:19:25Z |
| publishDate | 2013 |
| publisher | Науковий фізико-технологічний центр МОН та НАН України |
| record_format | dspace |
| spelling | Zmij, V.I. Rudenkiy, S.G. 2016-04-25T17:32:39Z 2016-04-25T17:32:39Z 2013 Research of a vacuum diffusion boron silicification process for constructional materials / V.I. Zmij, S.G. Rudenkiy // Физическая инженерия поверхности. — 2013. — Т. 11, № 1. — С. 18–21. — Бібліогр.: 7 назв. — англ. 1999-8074 https://nasplib.isofts.kiev.ua/handle/123456789/99266 621.793.6:620.181.4 In this work process of vacuum diffusion boron silicification of materials in sodium chloride vapour were researched. Gaseous medium composition was found by using the thermodynamic calculations of chemical reactions between NaCl vapour and the components of saturating powder mixture in the process for the temperature T = 1400 − 1600 K and pressure P = 1.33 − 1333 Pa, when the content of boron is 1 weight percent and 10 weight percent in backfilling. Formation mechanism of diffusion layer оn example of the vacuum activated boron silicification of graphite was determined. Keywords: boron silicification, diffusion saturation, activator, vacuum, graphite. В работе были проведены исследования механизма процесса вакуумного диффузионного боросилицирования материалов в парах хлористого натрия. Используя термодинамический расчет химических реакций между парами активатора и компонентами насыщающей порошковой смеси был определен состав газовой среды в этом процессе для температур Т = 1400 – 1600 К и давлений Р = 1.33 – 1333 Па, при содержании бора 1 и 10 вес.% в засыпке. На примере вакуумного активированного боросилицирования графита установлен механизм образования диффузионного слоя. В роботі були проведені дослідження механізму процесу вакуумного дифузійного боросиліціювання матеріалів у парах хлористого натрію. Використовуючи термодинамічний розрахунок хімічних реакцій між парами активатора та компонентами насичуючої порошкової суміші був визначений склад газового середовища у цьому процесі для температур Т = 1400 – 1600 К та тисків Р = 1.33 – 1333 Па, при вмісті бору 1 та 10 ваг.% в засипці. На прикладі вакуумного активованого боросиліціювання графіту встановлено механізм утворення дифузійного шару en Науковий фізико-технологічний центр МОН та НАН України Физическая инженерия поверхности Research of a vacuum diffusion boron silicification process for constructional materials Исследование процесса вакуумного активированного боросилицирования конструкционных материалов Дослідження процесу вакуумного активованого боросиліціювання конструкційних матеріалів Article published earlier |
| spellingShingle | Research of a vacuum diffusion boron silicification process for constructional materials Zmij, V.I. Rudenkiy, S.G. |
| title | Research of a vacuum diffusion boron silicification process for constructional materials |
| title_alt | Исследование процесса вакуумного активированного боросилицирования конструкционных материалов Дослідження процесу вакуумного активованого боросиліціювання конструкційних матеріалів |
| title_full | Research of a vacuum diffusion boron silicification process for constructional materials |
| title_fullStr | Research of a vacuum diffusion boron silicification process for constructional materials |
| title_full_unstemmed | Research of a vacuum diffusion boron silicification process for constructional materials |
| title_short | Research of a vacuum diffusion boron silicification process for constructional materials |
| title_sort | research of a vacuum diffusion boron silicification process for constructional materials |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/99266 |
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