Using PIGE for analysis of boron carbide of received by CVD method
The method PIGE was used for determination of stoichiometry and isotopic content of boron carbide in one measurement. The optimal conditions of experimental measurement were determined. The possibility was shown of obtaining of boron carbide enriched according to boron using CVD-method. Метод ядерни...
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| Zitieren: | Using PIGE for analysis of boron carbide of received by CVD method / V. Levenets, A. Omelnyk, A. Shchur, B. Shirokov // Вопросы атомной науки и техники. — 2008. — № 1. — С. 181-184. — Бібліогр.: 11 назв. — рос. |
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| author | Levenets, V. Omelnyk, A. Shchur, A. Shirokov, B. |
| author_facet | Levenets, V. Omelnyk, A. Shchur, A. Shirokov, B. |
| citation_txt | Using PIGE for analysis of boron carbide of received by CVD method / V. Levenets, A. Omelnyk, A. Shchur, B. Shirokov // Вопросы атомной науки и техники. — 2008. — № 1. — С. 181-184. — Бібліогр.: 11 назв. — рос. |
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| description | The method PIGE was used for determination of stoichiometry and isotopic content of boron carbide in one measurement. The optimal conditions of experimental measurement were determined. The possibility was shown of obtaining of boron carbide enriched according to boron using CVD-method.
Метод ядерних реакцияй на протонах с реєстрацією гама-випромінювання було використано для визначення стехіометриї і ізотопного складу карбіду бора за одне вимірення. Визначені оптимальні умови проведення вимірювань. Показана можливість аналізу карбіду бора з збагаченням по бору, отриманим газофазним методом.
Метод ядерных реакций на протонах с регистрацией гамма-излучения был использован для определения стехиометрии и изотопного состава карбида бора за одно измерение. Определены оптимальные условия проведения измерений. Показана возможность анализа карбида бора с обогащением по борe, полученному газофазным методом.
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УДК 539.1.
USING PIGE FOR ANALYSIS OF BORON CARBIDE OF RECEIVED
BY CVD METHOD
V. Levenets, A. Omelnyk, A. Shchur, B. Shirokov
Institute of solid-state physics, materials science and technologies NSC KIPT,
Kharkiv, Ukraine; E-mail:levenets@kipt.kharkov.ua
The method PIGE was used for determination of stoichiometry and isotopic content of boron carbide in one
measurement. The optimal conditions of experimental measurement were determined. The possibility was shown of
obtaining of boron carbide enriched according to boron using CVD-method.
INTRODUCTION
The boron carbide is semiconductor with high tem-
perature of melting. This substance is of interest for de-
velopment of materials for high-temperature thermoelec-
tric converters. The variation of concentrations of impuri-
ties and also stoichiometry out of the way increasing of
boron content sufficiently influence on main thermoelec-
tric features of boron carbide. This material consist of
atoms of four stable isotopes which have in natural mix-
ture the such concentrations: 10В-19.9 %; 11В-80.1 %,
12С-98.9 %, 13С-1.1 %. The cross-sections of capture of
thermal neutrons by nuclear of atoms of isotope 11В is
equal 0.005 b, carbon – 0.0035 b, and by isotope 10В is
equal 3837 b. Because of this the increasing of content
isotope of boron with low cross-section of the absorbing
of neutrons influences on radioactive resistance of mate-
rial, if thermoconverter made from boron carbide is used
to convert the thermal energy to electrical in nuclear reac-
tors or isotopic sources.
It is possible to obtain the ceramics on base of boron
carbide by means of agglomeration or hot-pressing of
powdered boron carbide in vacuum. Nevertheless, mate-
rials made with application of these techniques do not
have necessary densities. It is known, that thermoelectri-
cal features of boron carbide depend on its porosity suffi-
ciently. The possibilities were studied to obtain boron
carbide using gas-phase deposition. During of it produc-
tion the stoichiometry and isotopic content was checked.
Boron uses extensively in nuclear energetic,
medicine, geology, ecology, where namely its isotopic
content is important. Carbon from this point of view is in-
teresting for the studying of chains of feeding and it cyc-
licity in ecosystems and the age dating using isotope 14C.
However, despite wide application, the determination of
isotopic content these elements are difficult analytical
problem. It gives much more articles to analysis of iso-
topic content of boron in comparison with determination
of isotopic content of carbon.
A number of analytical methods of isotopic content
boron determination are presented in review [1]. The var-
ious ways of analysis and problem arising at they realiza-
tion were discussed. The cross-sections of capture of
thermal neutrons for 10B and 11B are different on six or-
ders of magnitude, that makes difficult the application of
neutron activation analysis to determination of isotopic
content. In work [2] the neutron flux was optimized by
the using of cadmium foil and analytical technique was
applied on base studying of tracks of α-particles from re-
action (n, α) for determination of enrichment relative to
isotope 10B. Mass-spectrometry is one of main methods
of determination of isotopic content of boron. The vari-
ous ways of exiting of sample and obtaining of plasma
may be used. The laser exiting of analyzed sample was
used in ref. [3] at determination boron isotopes in boron
carbide. In ref. [4] it was obtained sufficiently low limits
of detection (less then 5 ppm) for boron isotopes using
method resonant laser secondary neutral mass spectrome-
try (r-laser-SNMS). In this case a system of tunable dye-
lasers for resonantly ionizing the neutral atoms and time-
of-flight mass-spectrometer was use for registration of
emission. The high sensitivity at measurement ratio of
content of boron isotopes was reached in [5] with the us-
ing of mass-spectrometry with inductive connected plas-
ma. The distribution of boron isotopes in absorbing rods
was determined by method of second ions mass-spec-
trometry in [6].
The most general method of determination of stable
isotopes of carbon based on transfer of carbon to carbon
dioxide and consequent application of mass-spectrometry
(Gas Source Isotope Ratio Mass Spectrometry (IRMS).
The accelerating mass-spectrometry (AMS) applied gen-
erally to determine the content of carbon isotope 14C for
age dating.
Mass-spectrometric methods require long and labori-
ous previous sample preparation. Therefore it is naturally
to develop simple, suitable and sensitive method of iso-
topic content determination of boron and carbon. Nuclear
reactions induced by charged particles have the wide pos-
sibility for these purposes. They have high selectivity, the
matrix influence is rather weak, and their limits of detec-
tion are low and practically do not need previous
sampling. In work [7] the typical application was shown
of analytical methods based on particles beams. The film
from boron carbide on the mirror for X-rays emission
made from Мо/Si was studied. Stoichiometry and surface
density of film were determined using Rutherford back
scattering and nuclear reactions 11В(р,α)8Ве, 11В(d,α0)9Be,
12C(d,p)13C. But in example given and in a number anoth-
er ones the reactions chosen require the execution some
measurements on one sample with variation of particles
type or registration system.
After studying of available literary data the proton in-
duced nuclear reaction were selected which made it pos-
sible to determine simultaneously the stoichiometry and
isotopic content of boron carbide in one measurement,
without previous sampling.
ВОПРОСЫ АТОМНОЙ НАУКИ И ТЕХНИКИ. 2008. № 1.
Серия: Вакуум, чистые материалы, сверхпроводники (17), с.181– 184
181
http://www.kipt.kharkov.ua/en/isspmst.html
EXPERIMENTAL
THE STUDYING AND STANDARD SAMPLES
Samples of boron carbide were prepared using tech-
niques of gas-phase and plasma-chemical hydrogen
reduction of tree-chloride boron in vapors of toluene un-
der streamline flow of the surface of backing by laminar
non-skid stream without convection.
The deposition of boron carbide was made in cylin-
drical flowing-type reactor on graphite substrate. The
unit was described in detail, previously [8]. The graphite
substrate was previously saturated with pyrolytic carbon
for the better separation of deposited boron carbide from
the substrate. In reaction volume the substrate was
placed in zone of inductor of rf generator at the ohmic
heater made from tungsten. The pumping of reaction
volume was made by the vacuum pump using the freez-
ing nitrogen trap. After the pumping of reaction cham-
ber up to pressure 1.33 Pa hydrogen was conducted to
chamber up to required pressure, and, after warming up
the substrate up to given temperature, thee-chloride
boron and vapors of toluene were conducted in various
relationships. The hydrogen reduction of thee-chloride
boron was realized using the reaction
28BCl3 + C6H5CH3 + 38H2 ⇔ 7B4C + 84 HCl
both gas-phase and plasma-chemical methods, exiting
high-frequency charge in vapor-gaseous mixture. The
thicknesses of deposited films vary from 30 µm to
2 mm. The diameter of samples prepared for analysis
was equal 20 mm.
To make quantitative analysis samples of interest
were placed in irradiated chamber together with stan-
dard samples. Carbon (99.99 %), boron (99.99 %) and
boron carbide powder were used as standards.
FEATURES OF NUCLEAR REACTIONS USED
FOR ANALYSIS
It was determined, after previous research, that it is
appropriate to use for elemental and isotopic analysis of
binary compounds on base of carbon and boron, the
protons induced nuclear reactions with registration of γ-
quanta. The features of proton induced nuclear reactions
of radiative capture which were used to determine the
isotopes 11B, 12С, 13С are shown in table 1. The isotope
10В was determined using reaction 10В(р,αγ)7Ве.
The γ-lynes with energy 429 keV from reaction
10В(р,αγ)7Ве, 2.36 MeV - 12C(p,γ)13N; 4.43 MeV -
11B(p,γ)12C; 8 – 8.7 MeV- 13C(p,γ)14N were chosen for
analysis.
EXPERIMENTAL SET
The experimental measurements were made on ana-
lytical complex "Sokol" NSC KIPT [9]. Experimental
set includes electrostatic accelerator with outputting fa-
cilities; experimental chambers for fulfillment of set of
nuclear-physical methods of analysis; spectrometric and
computing devices designed for the handling of opera-
tion of experimental set and automation of processing of
experimental results. The general form of complex is
viewed in Fig.1.
The accelerator provides to obtain the beam of one-
charged ions with energy up to 2 MeV and energy reso-
lution up to 0.04 %. The measurements were executed
in channel number trees. The all studying samples were
placed in irradiated chamber simultaneously. The pro-
tons beam was oriented at normal to surface of target.
The size of beam on a target was about 3 mm.
Table I
Features of nuclear reactions used for determination
of content of boron and carbon [10]
Energy
of reso-
nance,
keV
Reaction
Cross-
section,
mb
Width
of reso-
nance,
keV
Eγ,
MeV
163 11B(p,γ)12C 0,157 7
4.43
11.68
16.11
675 11B(p,γ)12C 0,050 322 4,43
12.15
459
12C(p,γ)
13N 0,127 39,5 2,36
550
13C(p,γ)
14N 1,44 32,5 8,06
1160
13C(p,γ)
14N 0,56 6
2,39
3,07
4,11
8,62
To register γ-emission scintillation NaI(Tl) detector
with volume of crystal 150×100 mm and Ge(Li)-detec-
tor with volume of crystal 160 and energy resolution of
2.5 keV at 1332 keV were used. Both detectors were
placed outside the chamber. The distances from target to
detectors were 5 cm and the angles between beam direc-
tion and axes of detectors were 55° for Ge(Li) and 45° -
for NaI(Tl). To decrease the natural background and ra-
diation background induced by operating units the sen-
sitive volumes of detectors were shielded by cases made
from lead 15 mm in thickness. Ge(Li) detector was
used to register γ-emission in range from 200 to 5000
keV. NaI(Tl) detector was applied to register high ener-
gy γ-emission with energy 8…10.5 MeV by reason it
high efficiency. The standard spectrometric equipment
was used. The charge of protons stored on target was
measured by current integrator.
THE MEASUREMENTS AND RESULTS
At the development of method of quantitative evalu-
ation of basic components of boron carbide the general
efforts were directed on studying of possibility of simul-
taneous determination carbon and boron in one mea-
surement. The energy and current of beam were
changed and absorbers from lead in thickness from 1 to
5 cm in front of Ge(Li) detector for suppressing of high-
intensity 429 keV γ-emission were used to find the opti-
mal conditions of analysis. The spectrometric channel
including the NaI(Tl) detector was tuned to register γ-
emission in energy range 8.0…8.7 MeV in such a way
as to except the interferences with emission from other
protons induced reactions proceeding on nuclear of
atoms isotopes 10B, 11B, 12C.
ВОПРОСЫ АТОМНОЙ НАУКИ И ТЕХНИКИ. 2008. № 1.
Серия: Вакуум, чистые материалы, сверхпроводники (17), с.181– 184
182
Fig.1. Analytical nuclear-physical complex "Sokol":
1 - electrostatic accelerator; 2 - deflecting magnet;
3 – 7 the channels of outgoing ions beam
For example, in Fig.2 the spectrum was shown of γ-
emission from nuclear reactions induced on nuclear of
atoms for tree isotopes. This spectrum was measured at
energy and current of protons beam 0,57 MeV and 2.7 µ
A and charge of protons stored on target was 3000 µC.
It was possible to increase yields of high-energy γ-emis-
sion and decrease the duration of analysis by the in-
creasing of protons energy if the absorber from lead in
front of Ge(Li) detector to place.
The range of lower-energy protons used for analysis
of samples of boron carbide is rather small. On this ba-
sis it can be neglected absorption of γ-rays in a target,
and, if atoms of analyzed elements are distributed uni-
formly in a sample, we can draw on for content determi-
nation the formula
Y smpl SstC Csmpl st SY st smpl
= , (1)
where C smpl , C st – contents of in analyzed and
standard samples accordingly; Y smpl ,Y st - yields of
analytical γ-rays from analyzed and standard samples
accordingly; S smpl , S st - the stopping power of sub-
stance about protons with energy Еp for analyzed and
standard.
It was found after determination of elemental con-
tent of samples by external standard methods, that the
main error of concentration determination was associ-
ated with the error of charge measurement. The method
of evaluating of content proposed in ref [11] was used to
maintain high accuracy of computation. As is shown by
authors in case of the sum of contents of determined ele-
ments in analyzed samples and standard is equal 100 %,
and difference in matrix composition doesn't influence
significantly on intensities of analytical lines, the con-
tent each of elements may be determined from the for-
mula
1
smplYsmpl iCi st stn CY i jsmplY j st stCYj j i
=
е
=
, (2)
where smplCi - content of i-th determining element in
analyzed sample; smplY i smplY j - yields of γ-rays, ac-
cordingly, i-th и j-th element from analyzed sample.
The same symbols with superscript "st" denote accord-
ing quantities for standard sample. The error contributed
by inaccurate measurement of charge is excluded if ele-
mental contents are calculated by some means, as far as
ratios of yields depending only on statistical accuracy of
definition of sum of counts in analytical peak.
0 400 800 1200 1600 2000
Channel number
10
100
1000
10000
100000
N
um
be
r o
f
pu
ls
es
10B(p,α γ )7Be
429 keV
511 keV
12C(p,γ )13N
2365 keV
11B(p,γ ) 1 2 C
4439 keV
Fig. 2. The spectrum of γ-emission induced in (p,γ) re-
actions on nuclear of atoms of isotopes 10B, 11B, 12C
The results of analysis a number of samples made in
various conditions (temperature, flow, duration) by
CVD method are presented in Table 2.
The measurements of isotopic content of boron car-
bide in various stoichiometry don't reveal of its varia-
tion in process of deposition of boron carbide on the
backing. The ratio of content of isotopes was 0.24±0.01
for 10B/11B and – 0.0111±0.0005 for 13C/12C.
Table 2
The results of determination of stoichiometry
of boron carbide by PIGE
Sample
Concentration,
mass %
B C
Stechiomery
(per one atom of С)
# 254 0.01 99.99 C
# 235 45.89 54.11 BC
# 221 90.64 9.36 B11,5 C1
# 191 94.48 5.52 B20,3 C1
# 121 97.48 2.52 B45,8 C1
# 113 98.62 1.38 B84,5 C1
# 103 99.04 0.96 B122,3 C1
ВОПРОСЫ АТОМНОЙ НАУКИ И ТЕХНИКИ. 2008. № 1.
Серия: Вакуум, чистые материалы, сверхпроводники (17), с.181– 184
183
CONCLUSIONS
It has been found that CVD method may be used to
obtain the boron carbide with given stoichiometry en-
riched about boron.
The developed technique of boron carbide composi-
tion analysis makes it possible on base of nuclear reac-
tions to determine in one measurement the stoichiome-
try and isotopic content of analyzed product express-
ively, without previous sampling, with required metro-
logical features.
REFERENCES
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Chem. Soc. 2006, v.27, p.1609.
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ПРИМЕНЕНИЕ ЯДЕРНЫХ РЕАКЦИЙ ДЛЯ АНАЛИЗА КАРБИДА БОРА, ПОЛУ-
ЧЕННОГО ГАЗОФАЗНЫМ МЕТОДОМ
В. Левенец, А. Омельник, А. Щур, Б. Широков
Метод ядерных реакций на протонах с регистрацией гамма-излучения был использован для определения
стехиометрии и изотопного состава карбида бора за одно измерение. Определены оптимальные условия про-
ведения измерений. Показана возможность анализа карбида бора с обогащением по борe, полученному газо-
фазным методом
ВИКОРИСТАННЯ ЯДЕРНИХ РЕАКЦІЙ ДЛЯ АНАЛІЗУ КАРБІДУ БОРА,
ОТРИМАНОГО ГАЗОФАЗНИМ МЕТОДОМ
В. Левенець, О. Омельник, А. Щур, Б. Широков
Метод ядерних реакцияй на протонах с реєстрацією гама-випромінювання було використано для
визначення стехіометриї і ізотопного складу карбіду бора за одне вимірення. Визначені оптимальні умови
проведення вимірювань. Показана можливість аналізу карбіду бора з збагаченням по бору, отриманим
газофазним методом.
ВОПРОСЫ АТОМНОЙ НАУКИ И ТЕХНИКИ. 2008. № 1.
Серия: Вакуум, чистые материалы, сверхпроводники (17), с.181– 184
184
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| id | nasplib_isofts_kiev_ua-123456789-110847 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1562-6016 |
| language | Russian |
| last_indexed | 2025-12-07T18:47:23Z |
| publishDate | 2008 |
| publisher | Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| record_format | dspace |
| spelling | Levenets, V. Omelnyk, A. Shchur, A. Shirokov, B. 2017-01-06T15:24:26Z 2017-01-06T15:24:26Z 2008 Using PIGE for analysis of boron carbide of received by CVD method / V. Levenets, A. Omelnyk, A. Shchur, B. Shirokov // Вопросы атомной науки и техники. — 2008. — № 1. — С. 181-184. — Бібліогр.: 11 назв. — рос. 1562-6016 https://nasplib.isofts.kiev.ua/handle/123456789/110847 539.1. The method PIGE was used for determination of stoichiometry and isotopic content of boron carbide in one measurement. The optimal conditions of experimental measurement were determined. The possibility was shown of obtaining of boron carbide enriched according to boron using CVD-method. Метод ядерних реакцияй на протонах с реєстрацією гама-випромінювання було використано для визначення стехіометриї і ізотопного складу карбіду бора за одне вимірення. Визначені оптимальні умови проведення вимірювань. Показана можливість аналізу карбіду бора з збагаченням по бору, отриманим газофазним методом. Метод ядерных реакций на протонах с регистрацией гамма-излучения был использован для определения стехиометрии и изотопного состава карбида бора за одно измерение. Определены оптимальные условия проведения измерений. Показана возможность анализа карбида бора с обогащением по борe, полученному газофазным методом. ru Національний науковий центр «Харківський фізико-технічний інститут» НАН України Вопросы атомной науки и техники Физика и технология конструкционных материалов Using PIGE for analysis of boron carbide of received by CVD method Використання ядерних реакцій для аналізу карбіду бора, отриманого газофазним методом Применение ядерных реакций для анализа карбида бора, полученного газофазным методом Article published earlier |
| spellingShingle | Using PIGE for analysis of boron carbide of received by CVD method Levenets, V. Omelnyk, A. Shchur, A. Shirokov, B. Физика и технология конструкционных материалов |
| title | Using PIGE for analysis of boron carbide of received by CVD method |
| title_alt | Використання ядерних реакцій для аналізу карбіду бора, отриманого газофазним методом Применение ядерных реакций для анализа карбида бора, полученного газофазным методом |
| title_full | Using PIGE for analysis of boron carbide of received by CVD method |
| title_fullStr | Using PIGE for analysis of boron carbide of received by CVD method |
| title_full_unstemmed | Using PIGE for analysis of boron carbide of received by CVD method |
| title_short | Using PIGE for analysis of boron carbide of received by CVD method |
| title_sort | using pige for analysis of boron carbide of received by cvd method |
| topic | Физика и технология конструкционных материалов |
| topic_facet | Физика и технология конструкционных материалов |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/110847 |
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