Journal of Nuclear Materials 457 (2015) 118–123

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Journal of Nuclear Materials

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

XPS investigation of impurities containing boron films affected

by energetic deuterium implantation and thermal desorption
Dadong Shao a,⇑, Jiaxing Li a, Xiaoli Tan a, Zhongshi Yang a, Kenji Okuno b, Yasuhisa Oya b
a
Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei 230031, PR China
b
Radioscience Research Laboratory, Faculty of Science, Shizuoka University, 836 Ohya, Suruga-ku, Shizuoka 422-8529, Japan

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

Article history: Effect of impurities on existing states of boron, carbon and oxygen in boron films were investigated by
Received 6 September 2014 XPS technique. Carbon mainly exists as BACAB bond and BAC bond in 70% B boron films, and BAC bond
Accepted 31 October 2014 and CAC bond in 50% B boron films. The existing state of oxygen depends on impurities composition in
Available online 7 November 2014
70% B and 50% B boron films. D+ implantation and thermal desorption result in the reconstruction of
boron films, which mainly includes the elimination of B2O3, increasing of BAO bond and decreasing of
BAB bond. Implanted D+ into boron films can be trapped by carbon and oxygen, and remits as D2O
and CDx in TDS process. Comparing to carbon, oxygen can be trapped easily by BAB bond and difficult
to remit from boron films.
Ó 2014 Elsevier B.V. All rights reserved.

1. Introduction coated on the first wall [5,13], and difficult to be removed [16]. It
is unavoidable that the enrichment effect of boron films for impu-
In the present fusion devices, a lot of impurities will be contam- rities will be lost after a certain operation time due to the satura-
inated into the fusion devices [1]. Moreover, impurities (such as tion of impurities [17–19].
COx, H2O, CHxOy) are adsorbed irreversibly and accumulated on From the point of steady state operations of future fusion
material surfaces at low surface temperatures [2]. The impurities device, it is important to evaluate the trapping ability of boron
in fusion devices would induce the loss of plasma energy, and films for carbon and oxygen impurities, and the relative exiting
influence the properties of plasma confinement [1]. However, states of boron, carbon and oxygen in impurities containing boron
impurities widely present with deuterium and tritium [3], the fuel films. However, to our best knowledge, few researchers have ever
of future fusion reactor, and are unavoidable even in the samples of seriously evaluated it. Furthermore, impurities containing boron
high purity [4]. For the steady state operations of fusion devices, it films will be exposed to energy hydrogen isotopes during plasma
is important to keep the impurities low in fusion devices [5]. In operation process. It is also important to study the effect of
order to achieve effective reduction of impurities, plasma facing hydrogen isotopes on the chemical existing states of impurities
first wall conditioning has been widely applied and plays an in boron films. The related reaction processes of hydrogen isotopes
important role in fusion devices to reduce the impurities in plasma in boron films can be described as implantation process and
first wall materials [1,6,7]. thermal desorption process. Herein, we studied and compared
Boronization is widely recognized and applied as one of the the chemical existing states of boron, carbon and oxygen in boron
most effective techniques to suppress the impurities from plasma films after preheating, D+ implantation and thermal desorption.
first wall materials [6–13] because the major impurities in fusion The as-received boron films were not studied because the fusion
devices (such as Tokamak) are thought to be carbon and/or oxygen devices usually preheated for a long time to remove impurities
[13,14], and boron can easily bound to various impurities and helps as far as possible before operation.
to keep impurities at low concentration [5,15]. Moreover, it is
widely recognized that oxygen and carbon are the major impurities
2. Experimental
in the in-situ boronization process in present fusion devices and
future reactors [16], which will be contained in the boron films
2.1. Materials

⇑ Corresponding author. Tel.: +86 551 65593308; fax: +86 551 65593310. The carbon and oxygen containing boron films were prepared
E-mail addresses: [email protected] (D. Shao), [email protected] (J. Li), by plasma assisted chemical vapor deposition (p-CVD) technique
[email protected] (K. Okuno), [email protected] (Y. Oya). on Si substrate using the p-CVD apparatus at Shizuoka University.

http://dx.doi.org/10.1016/j.jnucmat.2014.10.097
0022-3115/Ó 2014 Elsevier B.V. All rights reserved.
 D. Shao et al. / Journal of Nuclear Materials 457 (2015) 118–123 119

Before preparation, the p-CVD chamber was cleaned up by using the change of chemical existing states of materials. As for B 1s
He plasma discharge at 673 K and 2.5  10 2 Pa for 30 min with spectrum, it is reasonable that boron atoms are bound to each
a He flow rate of 3.8 sccm. After He plasma cleaning process, boron other and build up the network of boron films. Many researchers
deposition was performed for 1 h by p-CVD technique to prepare [15,21–23] have reported that BAB bond as pure boron, BAC bond
carbon and oxygen containing boron films on Si substrates with as boron carbide, and BAO bond as boron oxide were located at
a size of 10  10  1.0 mm. B10H14 and He were introduced into 188 eV, 189 eV and 190 eV, respectively. Jacobsohn et al. [24] and
the p-CVD chamber at the rates of 2.5 sccm and 3.8 sccm, respec- Lyu et al. [25] finely divided BAO bond into BC2O and BCO2 at
tively. In addition, CH4 and O2 were introduced simultaneously 190.0 and 192.0 eV. They also observed B2O3 bond at 193.2 eV. In
into the p-CVD chamber as the sources of carbon and oxygen, this paper, the BAO bond includes the existing states of BC2O
respectively. By changing the flow rates of CH4 and O2, the boron and BCO2, and the B 1s spectra are deconvoluted into BAB bond
films with different carbon and oxygen concentrations were pre- (187.8 ± 0.2 eV), BAC bond (189.0 ± 0.2 eV), BAO bond (190.0–
pared (Table 1). During plasma discharge process, the temperature 192.0 eV), and B2O3 bond (193.2 ± 0.2 eV), respectively.
of substrate and pressure of p-CVD chamber were kept at 673 K In the case of C 1s spectra, the peaks at 287.6 ± 0.2 eV and
and 2.5  10 2 Pa, respectively. 288.8 ± 0.2 eV, corresponding to the species of AC@O bond (e.g.,
After boron deposition process, the boron films were heated and ketone, aldehyde) and ACOO bond (e.g., carboxylic, ester) can
held at 1173 K [20] for 10 min with a heating rate of 0.5 K s 1 in a be only found for as-received boron films, indicating that the pre-
thermal desorption chamber to remove residual hydrogen and the heating treatment can effectively remove CO2 formed during the
possible adsorbed impurities in boron films formed in the boron boron deposition process and/or adsorbed from air moisture. It
deposition process and/or adsorbed from air moisture. The thermal was clear that the C 1s XPS spectra of boron films consisted of four
desorption chamber was evacuated by using a turbo molecular chemical states, namely BACAB bond, BAC bond, CAC bond and
pump to less than 10 6 Pa. Thereafter, D+ implantation was per- CAO bond located at 281.8 ± 0.2 eV, 283.0 ± 0.2 eV, 284.5 ± 0.2 eV
formed on the boron films at room temperature with an energy and 286.3 ± 0.2 eV, respectively [26]. The O 1s spectra of boron
of 1.0 keV, an ion flux of 1.0  1018 D+ m 2 s 1, and an ion fluence films showed evidence of three chemical states at 531.5 ± 0.2 eV,
of 1.0  1022 D+ m 2, respectively. The deuterium was used as a 532.3 ± 0.2 eV and 533.2 ± 0.2 eV, which can be assigned to CAO
representative of hydrogen isotopes because deuterium would be bond, OAO bond and BAO bond [15], respectively.
one of the fuels of future fusion reactor [3]. After D+ implantation, Buzhinskij and Semenets [19] reported that the oxygen retained
the boron films were heated and held at 1173 K for 10 min with a in boron–carbon compositions was existed in the form of nonvol-
heating rate of 0.5 K s 1 in a thermal desorption chamber to study atile boron oxides (i.e. BO, BO2, B2O2 and B2O3), BACAO complexes
the chemical existing states of boron, carbon and oxygen in boron and physically trapped CO and O2. Ennaceur and Terreault [27]
films after thermal desorption. considered that the saturation concentration of oxygen in boron
films could not achieve to stoichiometric B2O3 level (related impu-
2.2. Characterization rities concentration is 60 at.%). In order to estimate the saturation
limitation of carbon and oxygen in boron films, the flow rates of
The boron films were characterized by X-ray photoelectron CH4 and O2 during boron deposition process were increased, and
spectroscopy (XPS) technique. The XPS measurements were per- 70 at.% of carbon and oxygen in boron films was achieved. Never-
formed with an ESCA1600 surface microanalysis system (ULVAC- theless, the concentrations of carbon and oxygen in boron films
PHI Inc.) equipped with a Mg Ka 400 W X-ray source (1253.6 eV) after D+ implantation-thermal desorption were reduced to 
and a hemispherical electron analyzer. The background pressure 50 at.%, suggesting that 50 at.% of carbon and oxygen closed to
and analyzed area was 10 8 Pa and 0.72  0.72 mm, respectively. its saturation concentration in boron films. Ashikawa et al. [22]
The surface charging effects were corrected with C 1s peak at observed a high BAO bond concentration of 90% (related oxygen
284.6 eV as a reference. In experiments, we found that the two rep- concentration was 45 at.%) in JT-60U after long-term operations,
resentative binding energies for Si, namely 100 eV (Si 2p) and and they considered 45 at.% is the saturation trapping capacity of
151 eV (Si 2s), cannot be observed, indicating that the boron films boron films for oxygen. In this paper, we select the boron films con-
formed on the Si surface, and Si substrate effect can be neglected. taining 50 at.% B and 50 at.% impurities (denoted as 50% B boron
films) as the representative of boron films with a high impurities
concentration, and the boron films containing 70 at.% B and
3. Results and discussions 30 at.% impurities (denoted as 70% B boron films) as the repre-
sentative of boron films with a low impurities concentration.
XPS spectrum is sensitive to the chemical environments of
materials, which is an effective technique to identify and analyze 3.1. Boron films after preheating

Table 1 It is acceptable that the concentration of impurities in boron

Chemical compositions of boron films. films is escalated during operations of fusion devices. Firstly, we
studied the relationship of carbon and oxygen compositions on
Sample no. Chemical compositions (at.%)
the chemical existing states of boron, carbon and oxygen in 70%
B C O
B boron films after preheating. According to the B 1s spectra of
70% B 70B–15C 70.1 14.7 15.2 70% B boron films after preheating (Fig. 1A and C), BAB bond is
70B–20C 70.0 19.7 10.3 the predominant existing state of boron and B2O3 bond cannot
70B–22C 70.0 22.2 7.8
70B–24C 70.1 24.1 5.8
be found due to low concentration of impurities. BAB bond also
70B–26C 69.7 26.2 4.1 slowly decrease with the increasing of carbon concentration and
50% B 50B–19C 50.3 18.7 31.0
the decreasing of oxygen in boron films.
50B–21C 49.5 20.8 29.7 According to the deconvoluted results of C 1s spectra for 70% B
50B–26C 49.9 25.9 24.2 boron films after preheating, carbon mainly exits as BACAB bond
50B–32C 50.3 31.8 17.9 (sp2 hybrid orbital) and BAC bond (sp3 hybrid orbital). The BACAB
50B–40C 49.8 40.0 10.2
bond, means boron rich bond, gradually convert into BAC bond
50B–44C 50.2 44.0 5.8
with the increasing of carbon concentration and the decreasing
120 D. Shao et al. / Journal of Nuclear Materials 457 (2015) 118–123

of oxygen concentration. Kodama et al. [14] also detected BACAB gradually converted into BAC bond with increasing of carbon con-
bond and BAC bond in the boron films with boron to carbon ratio centration in boron and carbon compositions, and they attributed
of 2.5. Moreover, the amounts of CAC and CAO bonds are negligi- it to the progressive incorporation of carbon atom and boron atom.
ble, indicating that 70% B boron films can further trap and remove It is very interesting that the percent of BAC bond increases and
carbon-containing impurity from fusion devices. the percent of CAC bond decreases with the increasing of carbon
According to the deconvoluted results of O 1s spectra for 70% B concentration in boron films. Meanwhile, CAO bond can be found
boron films after preheating, about half of the oxygen exists as only at higher oxygen concentration. It indicates that carbon atoms
OAO bond (i.e. free oxygen) in boron films [15,20]. The increases tend to bound to boron atoms rather oxygen atoms due to the high
of carbon concentration and the decreases of oxygen concentration reactivity between the elements. Similar phenomena can also be
result in the slowly decreasing of OAO bond and the slight increas- found in 50% B boron films after D+ implantation and after thermal
ing of BAO bond. It is reasonable that the trapping effect of boron desorption. The high percent of CAC bond at low carbon
films for carbon and oxygen atoms gradually decrease with concentration (high oxygen concentration) suggests the cluster of
increasing impurities concentration. Noda et al. [17] reported that free carbon at low carbon concentration because oxygen atoms
the trapping function of boron films for oxygen lost within a short tend to react with boron atoms rather than free carbon atoms
time due to the saturation of oxygen atoms at the top surface of (confirmed by O 1s XPS) [29]. Whereas, the amount and size of
boron films. Meanwhile, the compounds of carbon and oxygen clustered free carbon materials in boron films are limited because
(such as OAC bond) became to be important species in boron films carbon impurities can be effectively trapped by boron films, which
at high impurities concentration. result in the low CAC bond under the conditions of high carbon
The binding energies of B 1s (Fig. 1B and D), C 1s (Fig. 2B and D), concentration and low oxygen concentration.
and O 1s (Fig. 3B and D) for 50% B boron films after preheating dra- O 1s spectra further confirm the effect of carbon and oxygen
matically decrease with the increasing of carbon concentration to compositions on the existing states of boron and carbon in 50% B
40 at.%. Ronning et al. [28] also found that the binding energies boron films after preheating. BAO bond is the predominant
of B 1s and C 1s of boron–carbon compositions continuous existing state of oxygen in 50% B boron films after preheating when
decreased with increasing of carbon concentration in boron–car- oxygen concentration higher than 22.2 at.%. The increasing of car-
bon compositions. The binging energies of B 1s and C 1s shift bon concentration and the decreasing of oxygen concentration
toward lower energy side with the further increasing of carbon results in the decreasing of BAO bond and the increasing of CAO
concentration, which can be due to the conversion of BAB bond bond. However, BAO bond is still the primary of boron even when
to BAC bond in B 1s spectra and the conversion of CAC bond and carbon concentration (such as 32 at.%) is much higher than that
CAO bond to BAC bond in C 1s spectra, respectively. of oxygen. It means that the trapping of oxygen impurities by
Comparing to the existing states of boron, carbon and oxygen in boron films from fusion devices is much easier than that of carbon
70% B boron films after preheating, in 50% B boron films after pre- impurities.
heating, the amount of BAB bond significantly decrease, and B2O3
bond becomes to be major chemical states of boron; CAC and CAO 3.2. Boron films after D+ implantation
bonds becomes to be major chemical states of carbon, and BACAB
bond is neglectable. It can be due to the intense competition for In order to characterize the effect of D+ implantation and
active boron sites by impurity atoms at high impurities concentra- thermal desorption on boron films in fusion operation process,
tion. Ronning et al. [28] also reported that the BACAB bond the D+ implantation was performed for 70% B and 50% B boron

Fig. 1. Chemical existing states of boron in 70% B (A, C) and 50% B (B, D) boron films. The XPS spectra were ranked according to the carbon concentration, which were
increased from top to bottom, i.e. 70B–15C, 70B–20C, 70B–22C, 70B–24C, 70B–26C in Fig. 1A; and 50B–19C, 50B–21C, 50B–26C, 50B–32C, 50B–40C, 50B–44C in Fig. 1B. Fig. 2
and Fig. 3 were ranked in same order.
 D. Shao et al. / Journal of Nuclear Materials 457 (2015) 118–123 121

Fig. 2. Chemical existing states of carbon in 70% B (A, C) and 50% B (B, D) boron films.

Fig. 3. Chemical existing states of oxygen in 70% B (A, C) and 50% B (B, D) boron films.

films. As it is well known, D+ ions can be trapped by boron as for the 70% B boron films is shifted toward lower energy side with
BADAB bridge and BAD terminal bonds, and by carbon and oxygen the increasing of carbon concentration caused by D+ implantation,
as BAOAD and BACAD bonds in the carbon and oxygen containing which means that D+ implantation results in the reconstruction of
boron films [5]. It is reasonable that parts of D+ ions trapped by 70% B boron films. Kikuchi et al. [23] also found that D+ implanta-
impurities can reemit from boron films in the forms of heavy water tion lead to the reconstruction of carbon containing boron films.
(D2O) and hydrocarbons (CDx) [5]. Considering the fact that 70% B According to the deconvoluted results of B 1s, boron mainly
boron films can further effective trap impurities from fusion exists as BAO bond in the 70% B boron films after D+ implantation.
devices. It means D+ implantation will cause a serious reaction The amounts of BAC and BAB bonds are marked reduced to neg-
and conversion in 70% B boron films. The binding energies of B lectable level after D+ implantation. It further confirms that the
1s (Fig. 1A and C), C 1s (Fig. 2A and C), and O 1s (Fig. 3A and C) trapping of oxygen impurities by boron films is much easy than
122 D. Shao et al. / Journal of Nuclear Materials 457 (2015) 118–123

that of carbon impurities. Moreover, D+ implantation also result in CDx cannot be effectively re-trapped by the abundant active boron
the cluster of free carbon (CAC bond) [29] and significant decrease sites in the boron films with a low impurities concentration, and
and increase of BACAB bond and BAO bond, respectively; and a most of the formed CDx remits from boron films.
notable decreasing of OAO bond and CAO bond at high oxygen According to the deconvoluted results of C 1s spectra for 70% B
concentration because parts of the reemitted CDx and D2O would boron films after D+ implantation and after thermal desorption, a
be re-trapped by boron films in the diffusion and reemission pro- notable CAC bond converts into CABAC bond after thermal
cess. It is reasonable that the existing states of boron, carbon and desorption because the deuterium trapped by CAC bond
oxygen will be varied in the boron films containing more impuri- de-trapped quickly with forming CDx in the thermal desorption
ties, because boron bound to more impurities at higher impurities process [15] and the formed CDx can re-trapped by the abundant
concentration. However, the diffusion and remission of deuterium BAB bond. Moreover, as can be seen from Fig. 2A and D, the
trapped by impurities will be also simultaneously improved. deconvoluted results of C 1s spectra for 70% B films after preheat-
The existing states of boron, carbon and oxygen in 50% B boron ing and after thermal desorption are similar. It means that the
films after D+ implantation also fairly depend on impurities com- cycle of deuterium ions do not significant change the existing state
position because the binging energy of B 1s, C 1s and O 1s spectra of boron in the boron films with a low impurities concentration.
for 50% B boron films after D+ implantation are also dramatically The effect of deuterium ions cycle on the existing states of oxy-
decrease with the increasing of carbon concentration to 40 at.%. gen in the boron films with a low impurities concentration are
According to the deconvoluted results of B 1s spectra for, BAC bond much significant than that of carbon. As can be seen from the
and BAO bond are the major existing states of boron in 50% B deconvoluted results of O 1s spectra for 70% B boron films after
boron films after D+ implantation. BAC bond gradually increase D+ implantation (Fig. 3) and after thermal desorption (Fig. 3A and
with the increasing of carbon concentration while BAO bond grad- D), thermal desorption result in a observable decrease of OAO
ually decrease with the decreasing of oxygen concentration. B2O3 bond and a marked increase of CAO bond. It means free oxygen
bond and BAB bond, important existing states of boron in 50% B can react with CDx and/or free carbon in thermal desorption pro-
boron films after preheating (Fig. 1B and D), are neglectable in cess. Moreover, comparing to the existing states of oxygen in 70%
50% B boron films after D+ implantation. It means that B2O3 bond B boron films after preheating, the OAO bond and CAO bond in
can be reduced by D+ during implantation process [5]. Moreover, 70% B boron films after thermal desorption are also marked
the diffusion and remission of impurities can take place simulta- decrease and increase, respectably.
neously. The active boron sites caused by the remission of D2O As for the boron films with a higher impurities concentration
and CDx will re-trap oxygen and form new BAO bond. The elimina- (such as 50% B boron films), the trapping capacity of impurities
tion of B2O3, the increasing of BAO bond and the decreasing of BAB by boron films will be reduced and the emission of impurities from
bond suggest that D+ implantation can result in the reconstruction boron films will be improved because the active boron sites in
of boron films. Moreover, the distribution of boron on Si substrates boron films usually decrease with the increasing of impurities con-
is strongly affected by the morphological structure of Si substrates centration. As can be seen from Fig. 1B and D, only B 1s spectra
[30], and the local distribution of heterogeneity is improved at binging energy of 50% B boron films after thermal desorption
higher substrate temperature because the migration ability of shifted toward lower energy side with the increasing of carbon
formed particulates on Si substrates are enhanced at high temper- concentration, and BAO bond are the predominant existing state
ature [31]. According to the deconvoluted results of C 1s and O 1s of boron until carbon concentration is increased to 36.8 at.%. More-
spectra for 50% B boron films after preheating and after D+ implan- over, according to the deconvoluted results of B 1s spectra for 50%
tation, D+ implantation reduces BAC bond and enhances the for- B boron films after implantation and after thermal desorption,
mation of CAC bond; and decreases of OAO bond at high oxygen thermal desorption results in BAO bond marked decreased at car-
concentration (>18 at.%). Yoshikawa et al. [15] attributed similar bon concentration >37 at.% and moderately increased at carbon
experimental result to the fact that deuterium atoms bound to concentration <37 at.%; and BAC bond notable decreased at carbon
CAB bond with the formation of BACAD bond and new CAC bond. concentration <37 at.%. The improving of BAO bond and the
They also found that free oxygen largely decreased after D+ implan- undetectable of BAB bond at carbon concentration <37 at.% sug-
tation because a large amount of oxygen convert to volatile D2O. gests oxygen impurities can effective occupy the active boron sites
provided by the emission of CDx. Nevertheless, carbon impurities
3.3. Boron films after thermal desorption cannot effective occupy the active boron sites provided by the
emission of D2O even at high carbon concentration, which results
The deuterium trapped as BAOAD bond and BACAD bond are in the fact that BAB bond becomes to be an important existing
decomposed into BAB bond, and volatile materials (i.e. D2O and state of boron at carbon concentration >37 at.% in 50% B boron
CDx) are formed simultaneously in thermal desorption process. It films after thermal desorption. It means oxygen impurities has a
is reasonable that parts of the formed D2O and CDx will be re- significant advantage in the competing for active boron sites.
trapped by boron films during diffusion in the thermal desorption Moreover, the trapping of carbon impurities by boron films from
process, which also result in the reconstruction of boron films. The fusion devices is much difficult than that of oxygen impurities.
binding energy of B 1s spectra (Fig. 1A and C), C 1s spectra (Fig. 2A According to the deconvoluted results of C 1s spectra for 50% B
and C), and O 1s spectra (Fig. 3A and C) of 70% B boron films after boron films after implantation and after thermal desorption, TDS
thermal desorption are dramatically decrease with the increasing result in the increase and decrease of BAC bond and CAC bond,
of carbon concentration. According to the deconvoluted results of respectively. It confirms the deconvoluted results of B 1s spectra
B 1s spectra for 70% B boron films, most of BAB bond convert to for 50% B boron films after D+ implantation and after thermal
BAO bond during the D+ implantation and thermal desorption pro- desorption. Furthermore, based on the deconvoluted results of C
cess, which is further confirmed by O 1s spectra at high oxygen 1s spectra for 50% B boron films after preheating and after thermal
concentration. It reveals that a number of formed D2O can be desorption, at high carbon concentration condition, the C 1s spec-
trapped by active boron sites in the boron films with a low tra of 50% B boron films after thermal desorption similar to that of
impurities concentration in D2O remission and diffusion process. after preheating. Whereas, at low carbon concentration condition,
However, the dramatically increasing of BAB bond and BAC bond the CAC bond percent of 50% B boron films decrease markedly after
caused by thermal desorption is an unimportant existing state of TDS process. It means that just at high carbon concentration condi-
boron at high carbon concentration. It means that the formed tion, the recycle of deuterium can significant affect the existing
 D. Shao et al. / Journal of Nuclear Materials 457 (2015) 118–123 123

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