Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments
A phenomenon of termination of sputtering of protonated water clusters (H2O)nH⁺ in low-temperature secondary emission mass spectrometric studies of solid water was observed in the temperature range of crystallization of amorphous solid water (ASW). In this range the mass spectra contained only H₃O⁺,...
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Kosevich, M.V. Boryak, O.A. Shelkovsky, V.S. Orlov, V.V. 2018-01-14T13:08:47Z 2018-01-14T13:08:47Z 2003 Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments / M.V. Kosevich, O.A. Boryak, V.S. Shelkovsky, V.V. Orlov // Физика низких температур. — 2003. — Т. 29, № 9-10. — С. 1061-1064. — Бібліогр.: 30 назв. — англ. 0132-6414 PACS: 68.49.Sf, 64.70.Kb, 61.43.-j, 36.40.Wa https://nasplib.isofts.kiev.ua/handle/123456789/128931 A phenomenon of termination of sputtering of protonated water clusters (H2O)nH⁺ in low-temperature secondary emission mass spectrometric studies of solid water was observed in the temperature range of crystallization of amorphous solid water (ASW). In this range the mass spectra contained only H₃O⁺, H₂O⁺•, and OH⁺ ions. The following explanation of the revealed phenomenon is suggested: the heat supplied to the ASW sample by the bombarding particles is spent on initiation of an amorphous–crystalline transition within the condensed sample but not for the transfer of the sample matter to the gas phase. At the same time heat released on crystallization causes a local rise in temperature of the crystallizing sample surface, which enhances the rate of sublimation of ice. The resulting increased concentration of subliming water molecules over the sample surface is reflected in the growth of abundance of H₂O⁺• molecular ion-radical, produced by gas-phase ionization mechanism. The appearance of a set of low-mass peaks in the course of crystallization observed for some types of ASW samples is explained by the release of gases trapped in the ASW film during its growth. This work was partially supported by the grant INTAS-99-00478. en Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України Физика низких температур Biological Systems at Low Temperatures Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments Article published earlier |
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Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments |
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Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments Kosevich, M.V. Boryak, O.A. Shelkovsky, V.S. Orlov, V.V. Biological Systems at Low Temperatures |
| title_short |
Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments |
| title_full |
Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments |
| title_fullStr |
Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments |
| title_full_unstemmed |
Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments |
| title_sort |
observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments |
| author |
Kosevich, M.V. Boryak, O.A. Shelkovsky, V.S. Orlov, V.V. |
| author_facet |
Kosevich, M.V. Boryak, O.A. Shelkovsky, V.S. Orlov, V.V. |
| topic |
Biological Systems at Low Temperatures |
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Biological Systems at Low Temperatures |
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2003 |
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English |
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Физика низких температур |
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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Article |
| description |
A phenomenon of termination of sputtering of protonated water clusters (H2O)nH⁺ in low-temperature secondary emission mass spectrometric studies of solid water was observed in the temperature range of crystallization of amorphous solid water (ASW). In this range the mass spectra contained only H₃O⁺, H₂O⁺•, and OH⁺ ions. The following explanation of the revealed phenomenon is suggested: the heat supplied to the ASW sample by the bombarding particles is spent on initiation of an amorphous–crystalline transition within the condensed sample but not for the transfer of the sample matter to the gas phase. At the same time heat released on crystallization causes a local rise in temperature of the crystallizing sample surface, which enhances the rate of sublimation of ice. The resulting increased concentration of subliming water molecules over the sample surface is reflected in the growth of abundance of H₂O⁺• molecular ion-radical, produced by gas-phase ionization mechanism. The appearance of a set of low-mass peaks in the course of crystallization observed for some types of ASW samples is explained by the release of gases trapped in the ASW film during its growth.
|
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0132-6414 |
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https://nasplib.isofts.kiev.ua/handle/123456789/128931 |
| citation_txt |
Observation of crystallization of amorphous solid water under the conditions of secondary emission mass spectrometric experiments / M.V. Kosevich, O.A. Boryak, V.S. Shelkovsky, V.V. Orlov // Физика низких температур. — 2003. — Т. 29, № 9-10. — С. 1061-1064. — Бібліогр.: 30 назв. — англ. |
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AT kosevichmv observationofcrystallizationofamorphoussolidwaterundertheconditionsofsecondaryemissionmassspectrometricexperiments AT boryakoa observationofcrystallizationofamorphoussolidwaterundertheconditionsofsecondaryemissionmassspectrometricexperiments AT shelkovskyvs observationofcrystallizationofamorphoussolidwaterundertheconditionsofsecondaryemissionmassspectrometricexperiments AT orlovvv observationofcrystallizationofamorphoussolidwaterundertheconditionsofsecondaryemissionmassspectrometricexperiments |
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2025-11-26T01:42:50Z |
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| _version_ |
1850605380822892544 |
| fulltext |
Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10, p. 1061–1064
Observation of crystallization of amorphous solid water
under the conditions of secondary emission
mass spectrometric experiments
M.V. Kosevich, O.A. Boryak, V.S. Shelkovsky, and V.V. Orlov
B. Verkin Institute for Low Temperature Physics and Engineering of the National Academy of
Sciences of Ukraine, 47 Lenin Ave., Kharkov 61103, Ukraine
E-mail: mvkosevich@ilt.kharkov.ua
A phenomenon of termination of sputtering of protonated water clusters (H2O)nH
+ in low-tem-
perature secondary emission mass spectrometric studies of solid water was observed in the tempera-
ture range of crystallization of amorphous solid water (ASW). In this range the mass spectra con-
tained only H3O
+, H2O
+�, and OH+ ions. The following explanation of the revealed phenomenon
is suggested: the heat supplied to the ASW sample by the bombarding particles is spent on initia-
tion of an amorphous–crystalline transition within the condensed sample but not for the transfer
of the sample matter to the gas phase. At the same time heat released on crystallization causes a lo-
cal rise in temperature of the crystallizing sample surface, which enhances the rate of sublimation
of ice. The resulting increased concentration of subliming water molecules over the sample surface
is reflected in the growth of abundance of H2O
+� molecular ion-radical, produced by gas-phase ion-
ization mechanism. The appearance of a set of low-mass peaks in the course of crystallization ob-
served for some types of ASW samples is explained by the release of gases trapped in the ASW film
during its growth.
PACS: 68.49.Sf, 64.70.Kb, 61.43.–j, 36.40.Wa
1. Introduction
Investigations of solid water by means of secondary
emission mass spectrometry [1–14] have used either
amorphous solid water (ASW) obtained by vapor de-
position on some surface cooled below the temperature
of the glass transition of water Tg = 136 K [15–17] or
crystalline ice. Under bombardment by energetic par-
ticles — by neutral atoms of Aro or Xeo in a fast atom
bombardment (FAB) mode, or ions of Cs+or Ar+ in
secondary ion mass spectrometry (SIMS), with the
energy varied in the 5–30 keV range — sets of
protonated water clusters (H2O)nH
+ with n up to
30–50 are sputtered both from ASW and crystalline
ice. The distribution of clusters in the secondary emis-
sion mass spectra of the both forms of water is qualita-
tively very similar, with a slight quantitative dif-
ference in the abundances of some clusters. The
measurements were usually conducted at some con-
stant temperature. Secondary emission mass spectro-
metric experiments were not performed, however, on
gradual variation of the sample temperature in the
range around the temperature of crystallization of
ASW, which, according to the data of Ref.15, can
start at 140–160 K and proceed in some temperature
range up to 166 K.
It was revealed in our previous works on LT FAB
and SIMS of a number of organic and inorganic com-
pounds that phase transitions in the sample matter are
reflected in characteristic changes in cluster patterns of
the secondary emission mass spectra [13, 14, 18–20].
The aim of the present work was to obtain second-
ary emission mass spectra of vapor-deposited solid wa-
ter in the temperature range of crystallization of ASW
with the expectation of observing and investigating
changes in the mass spectral pattern resulting from
this type of transition.
2. Low-temperature secondary emission mass
spectrometric experiments
Mass spectrometric experiments were performed us-
ing the magnetic sector mass spectrometer MI-1201E
(Sumy, Ukraine) equipped with primary FAB ion
source for generating a bombarding beam of argon at-
© M.V. Kosevich, O.A. Boryak, V.S. Shelkovsky, and V.V. Orlov, 2003
oms; the energy of the primary ion beam before neu-
tralization was 4–5 keV. The secondary ion source
contained a cryogenic unit described in detail else-
where [12]. The cryogenic unit, cooled by liquid ni-
trogen, had a recess for a removable copper sample
holder which could be cooled either externally or di-
rectly in the ion source. A thermistor inserted into the
unit served for temperature measurements. The cryo-
genic unit was surrounded by a toroidal cryogenic
shield cooled by liquid nitrogen, which provided effi-
cient adsorption of residual gases inside the ion source.
The pressure in the FAB secondary ion source ahead of
the bombarding argon inlet was about 10–6 Pa.
Polycrystalline ice samples were produced by freez-
ing of deionized water in vapors of liquid nitrogen.
Layers of ASW were produced in two ways. Vapors of
water were deposited onto the substrate pre-cooled to
the liquid nitrogen temperature from residual gases in
the evacuation chamber of the direct sample inlet sys-
tem. During the deposition the temperature of the
sample holder did not rise above the one recommended
for the procedure 140 K [15], which was controlled by
direct temperature measurement after the insertion of
the sample holder to the cryogenic block. Alterna-
tively, water vapor was deposited on the cold sample
holder directly in the secondary ion source. The source
of low-pressure flux of water molecules was crystal-
line hydrate CuSO4·5H2O kept in a heated ceramic
ampoule near the sample holder. Substrates for ASW
deposition were the bare copper sample holder, frozen
crystalline H2O and D2O, and frozen solutions of in-
organic salts.
3. Results and discussion
In the FAB mass spectra of layers of ASW depos-
ited by various methods on various substrates, as
described in the Experimental Section, a set of
protonated water clusters (H2O)nH
+ (n = 1–10) was
present (Fig. 1,a). The spectral pattern, that is the
types of clusters and distribution of their abundances,
did not undergo any substantial changes on tempera-
ture variation in the 77–140 K temperature range. On
warming the sample up to 140–150 K a rather unex-
pected and pronounced effect was observed: all cluster
ions of water (H2O)nH
+ except for those with n = 1
(that is H3O
+) decreased in abundance rather rapidly
(during one spectrum scan) and disappeared from the
spectrum. At the same time the absolute intensity of a
peak at m/z 18 which can be attributed to water radi-
cal-cation H2O
+� increased by one to two orders of
magnitude (Fig. 1,b). The intensity of a peak of the
ion at m/z 17, which is known to be an OH+ fragment
of H2O
+�, increased similarly to that of its parent ion.
Thus, the FAB mass spectrum contained only three in-
tense peaks of H3O
+, H2O
+�, OH+ (Fig. 1,b). For
some types of samples at somewhat higher tempera-
tures of about 150–160 K a noisy spectrum with a
peak at every mass started to interfere with the above
three peaks in the low-mass range. It lasted for some
time and then vanished, giving way to a recovered
normal spectrum of ice containing a (H2O)nH
+ cluster
set at temperatures of about 160–170K . The latter, in
turn, after completion of rather rapid sublimation of
the crystallized ice layer on further warming was
replaced by the spectrum characteristic of an un-
der-layer (substrate). Once happened on warming,
the described transformations were not repeated on
subsequent cyclic cooling-warming of the ice formed.
The reported changes of mass spectra were qualita-
tively reproducible with slight quantitative variations
in several tens of independent experiments.
The most remarkable feature of these changes is a
temporary termination of production of all the ions
except H3O
+ and H2O
+� when a solid water sample is
still definitely present on the sample holder. Even in
1062 Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10
M.V. Kosevich, O.A. Boryak, V.S. Shelkovsky, and V.V. Orlov
Fig. 1. FAB mass spectra of solid water: spectral pattern of
ASW, characteristic in the temperature range 77–110 K (a);
peaks corresponding to protonated water clusters in the set
(H2O)nH
+ (n = 1–10) are marked by ✽; (the unmarked pe-
ak at m/z 30 corresponds to NO adsorbed from the residual
gas at T < 110 K); mass spectrum recorded at � 150 K (b).
the case of complete exhaustion of the water layer the
spectra of the exposed under-layer should appear, but
they did not.
To explain the phenomena observed, the answers to
at least two questions are to be searched for: what are
the reasons for termination of the production of
(H2O)nH
+ clusters with n > 1 and continuation of the
production of the H3O
+ ion, and what is the origin of
the abundant H2O
+� ion. First of all, it is obvious that
the temperature range of anomalous changes in the
mass spectra is very close to the temperature range of
spontaneous crystallization of ASW, which, according
to the results of the relevant studies [15], can start on
slow warming at 140–160 K and be completed at
166 K. The action of some external factors, including
energetic particle impact, initiates the so-called explo-
sive crystallization, which can start at 15 K lower
than the spontaneous crystallization [15]. This allows
us to suggest that any effect observed in this tempera-
ture range may be connected with an amorphous–crys-
talline transition in the sample.
It is generally recognized that excitation caused by
a bombarding particle in a condensed sample is
ultimately converted to thermal energy [21]. It is
known also that all heat deposited in a system in the
phase transition state is consumed on carrying out the
transition to its completion. In this light, it may be
suggested that in the present experiments practically
all the energy supplied by a bombarding particle to an
ASW sample at 140–166 K is spent on performing the
amorphous–crystalline transition. In the zone heated
by a bombarding particle water molecules in the amor-
phous layer acquire some degrees of freedom which al-
lows them to rearrange in a regular crystalline struc-
ture. Thus, heat is spent on initiation and support of
the crystallization process within the condensed sam-
ple but not for evaporation (sublimation) of molecules
to the gas phase. This can explain the absence of
«sputtering» of sample matter to the gas phase (the
latter usually being revealed by registering charged
water clusters). The effects described are valid both
for spontaneous and particle-initiated scenarios of
crystallization. The low flux of bombarding particles
used in FAB experiments provides incidence of parti-
cles to the surface areas undamaged by preceding im-
pacts for at least 5 minutes, which means that the
probability of a new particle impact to the zone crys-
tallized after a previous particle impact (from which
cluster sputtering becomes possible) is rather low in
the time frame of the experiment.
Concerning the origin of H3O
+ ions under the
above described conditions, it is known that the very
first event on contact of a bombarding particle with
the condensed sample surface can consist in direct
mechanical knock-out by direct momentum transfer or
by recoil atoms of one or a few surface atoms or mole-
cules, either in the neutral or charged forms [22–24].
The H3O
+ ion can be produced by this surface mecha-
nism, which is independent of further events caused
by the bombarding particle in the bulk sample [25].
The difference in the origin of the H3O
+ ion and
(H2O)nH
+ clusters with n > 1 is supported by the re-
sults of early experiments on the determination of the
kinetic energy of the sputtered species, which appeared
to be higher for H3O
+ in comparison with larger water
cluster ions [2].
This mechanism, however, could not be responsible
for the appearance of the abundant molecular radical
ion H2O
+�, since its abundance in ordinary secondary
ion emission mass spectra of both ASW and crystalline
ice is relatively small. The appearance of H2O
+� is
usually conditioned by the increase of water concen-
tration in the gas phase over the sample surface [7],
since it was proved that H2O
+� ion is formed by the
so-called gas-phase FAB mechanism [7,26]. The in-
crease of absolute and relative intensity of the peak
corresponding to H2O
+� in the FAB mass spectra of
ice was observed earlier [13,14,25] under conditions
of high-rate sublimation of ice samples at a tempera-
ture of about 200–220 K [27] preceding complete
rapid exhaustion of the sample. This suggests that in
the experiments under discussion (Fig. 1,b) the con-
centration of water molecules in the gas phase be-
comes relatively high apparently for the same reason,
that is, due to active sublimation. Although the tem-
perature of the sample holder and bulk sample is kept
rather low (140–160 K), the temperature of the sam-
ple surface can become noticeably higher due to the
known thermal effect characteristic of ASW crystalli-
zation. It was found earlier that the heat released on
rapid crystallization can cause a rise in the tempera-
ture of the sample surface in the crystallizing region of
about 60–80 K [15]. Assuming that the starting tem-
perature of the sample is above 140 K, its increase by
60–80 K will raise the local temperature to a value of
200–220 K, at which the rate of sublimation is high
and sufficient for recording abundant H2O
+� ions.
As to the temporary appearance of a noisy spec-
trum, this effect can be explained by ionization of
gaseous species trapped within ASW on its deposition
and released on its structural rearrangement during
crystallization [17,28]. Some data on ASW deposition
show that the amount of gases trapped by ASW can
exceed by a factor of three the weight of the ASW
sample [29]. The intense release of gases at a certain
stage of ASW crystallization has been named the «mo-
lecular volcano» effect [30].
Observation of crystallization of amorphous solid water under the conditions of secondary emission
Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10 1063
Thus, the chain of events leading to the changes in
the spectra presented in Fig. 1 can be summarized as
follows. In the temperature range of ASW crystalliza-
tion the energy deposited by a bombarding particle
contributes to carrying out the crystallization. This al-
ternative channel of heat dissipation prevents transfer
of the sample matter to the gas phase on the interac-
tion of the bombarding particle with the sample. Only
relatively simple H3O
+ species are released by direct
sputtering from the surface. Upon both spontaneous
and initiated crystallization the latent heat of crystal-
lization is released and the temperature of the sample
surface rises to values at which the sublimation rate is
rather high and provides a concentration of water va-
por over the sample surface sufficient for abundant
production of H2O
+� by gas-phase FAB ionization.
The effects described should be taken into account
in the models of the interaction of accelerated parti-
cles with amorphous ices in outer space [11].
3. Conclusions
In FAB mass spectrometric studies of solid water in
the temperature range of ASW crystallization a phe-
nomenon of the termination of sputtering of clusters
(H2O)nH
+, which are always the main constituents of
mass spectra of both amorphous solid and crystalline
water, was revealed. The spectra contained only
H3O
+, H2O
+� and OH+ ions. An explanation of the
observed phenomenon is suggested: the heat supplied
to the sample by the bombarding particles is spent on
carrying out the amorphous–crystalline transition but
not for the transfer of the sample matter to the gas
phase. At the same time heat released on crystalliza-
tion causes a rise of the sample surface temperature,
which enhances ice sublimation. The increased con-
centration of subliming water over the sample surface
is reflected in the increase of the abundance of the
H2O
+� molecular ion-radical, produced by gas-phase
ionization.
Acknowledgment.
This work was partially supported by the grant
INTAS-99-00478 .
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M.V. Kosevich, O.A. Boryak, V.S. Shelkovsky, and V.V. Orlov
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