Properties of solid hydrogen doped by heavy atomic and molecular impurities
Using powder x-ray diffraction we studied the structural characteristics of normal and para hydrogen crystals doped with Ar, Kr, N₂, and O₂ impurities over the range from 5 K to the melting point of the hydrogen matrix. It has been established that in spite of very low solubility of the dopants in s...
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України
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irk-123456789-1289282018-01-15T03:03:04Z Properties of solid hydrogen doped by heavy atomic and molecular impurities Galtsov, N.N. Prokhvatilov, A.I. Shcherbakov, G.N. Strzhemechny, M.A. Low-Temperature Thermodynamics and Structure Using powder x-ray diffraction we studied the structural characteristics of normal and para hydrogen crystals doped with Ar, Kr, N₂, and O₂ impurities over the range from 5 K to the melting point of the hydrogen matrix. It has been established that in spite of very low solubility of the dopants in solid hydrogen, these impurities appreciably affect the structural characteristics. In particular, only nitrogen impurities do not change the molar volume of the matrix, the other three make the matrix expand. The Ar and Kr impurities also change the c/a ratio of the hcp matrix. The fact that both Ar and O₂ have smaller molar volumes than hydrogen may be treated as evidence that these impurities form van der Waals complexes with the hydrogen lattice environment. 2003 Article Properties of solid hydrogen doped by heavy atomic and molecular impurities / N.N. Galtsov, A.I. Prokhvatilov, G.N. Shcherbakov, M.A. Strzhemechny // Физика низких температур. — 2003. — Т. 29, № 9-10. — С. 1036-1040. — Бібліогр.: 28 назв. — англ. 0132-6414 PACS: 67.80.Mg, 67.90.+z http://dspace.nbuv.gov.ua/handle/123456789/128928 en Физика низких температур Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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Low-Temperature Thermodynamics and Structure Low-Temperature Thermodynamics and Structure Galtsov, N.N. Prokhvatilov, A.I. Shcherbakov, G.N. Strzhemechny, M.A. Properties of solid hydrogen doped by heavy atomic and molecular impurities Физика низких температур |
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Using powder x-ray diffraction we studied the structural characteristics of normal and para hydrogen crystals doped with Ar, Kr, N₂, and O₂ impurities over the range from 5 K to the melting point of the hydrogen matrix. It has been established that in spite of very low solubility of the dopants in solid hydrogen, these impurities appreciably affect the structural characteristics. In particular, only nitrogen impurities do not change the molar volume of the matrix, the other three make the matrix expand. The Ar and Kr impurities also change the c/a ratio of the hcp matrix. The fact that both Ar and O₂ have smaller molar volumes than hydrogen may be treated as evidence that these impurities form van der Waals complexes with the hydrogen lattice environment. |
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Galtsov, N.N. Prokhvatilov, A.I. Shcherbakov, G.N. Strzhemechny, M.A. |
| author_facet |
Galtsov, N.N. Prokhvatilov, A.I. Shcherbakov, G.N. Strzhemechny, M.A. |
| author_sort |
Galtsov, N.N. |
| title |
Properties of solid hydrogen doped by heavy atomic and molecular impurities |
| title_short |
Properties of solid hydrogen doped by heavy atomic and molecular impurities |
| title_full |
Properties of solid hydrogen doped by heavy atomic and molecular impurities |
| title_fullStr |
Properties of solid hydrogen doped by heavy atomic and molecular impurities |
| title_full_unstemmed |
Properties of solid hydrogen doped by heavy atomic and molecular impurities |
| title_sort |
properties of solid hydrogen doped by heavy atomic and molecular impurities |
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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2003 |
| topic_facet |
Low-Temperature Thermodynamics and Structure |
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http://dspace.nbuv.gov.ua/handle/123456789/128928 |
| citation_txt |
Properties of solid hydrogen doped by heavy atomic and molecular impurities / N.N. Galtsov, A.I. Prokhvatilov, G.N. Shcherbakov, M.A. Strzhemechny // Физика низких температур. — 2003. — Т. 29, № 9-10. — С. 1036-1040. — Бібліогр.: 28 назв. — англ. |
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Физика низких температур |
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2025-07-09T10:14:52Z |
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| fulltext |
Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10, p. 1036–1040
Properties of solid hydrogen doped by heavy atomic and
molecular impurities
N.N. Galtsov, A.I. Prokhvatilov, G.N. Shcherbakov, and M.A. Strzhemechny
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: galtsov@ilt.kharkov.ua
Using powder x-ray diffraction we studied the structural characteristics of normal and para hy-
drogen crystals doped with Ar, Kr, N2, and O2 impurities over the range from 5 K to the melting
point of the hydrogen matrix. It has been established that in spite of very low solubility of the
dopants in solid hydrogen, these impurities appreciably affect the structural characteristics. In
particular, only nitrogen impurities do not change the molar volume of the matrix, the other three
make the matrix expand. The Ar and Kr impurities also change the c/a ratio of the hcp matrix.
The fact that both Ar and O2 have smaller molar volumes than hydrogen may be treated as evi-
dence that these impurities form van der Waals complexes with the hydrogen lattice environment.
PACS: 67.80.Mg, 67.90.+z
Solid mixtures of hydrogen with rare gas and sim-
ple molecular species are interesting for several rea-
sons. At high pressures, some of such mixtures can
form stoichiometric solid-state compounds, like
Ar(H2)2 [1] or hydrogen-methane ordered alloys [2].
At low pressures, hydrogen-containing alloys with
smaller molecular (atomic) species can be expected to
form random binary systems that would in many as-
pects resemble helium-impurity gels [3,4]. Quench
condensed Ar–H2 mixtures at sufficiently high H2
contents in the source gas show many properties that
could be treated as pertaining to gels of that kind [5].
In strongly diluted H2-based mixtures one can expect
the formation of van der Waals (VdW) complexes,
loosely bound to the crystal environment due to quan-
tum-crystal effects. Evidence of such VdW complexes
has been obtained by x-ray diffraction on Ne-doped
para hydrogen [6]. Similar results have been obtained
for other neon-doped hydrogen matrices (normal H2
and D2 , ortho deuterium) [7]. In all those crystals,
certain structural characteristics behaved in an un-
usual way, in particular, the reflection attributable to
hcp hydrogen grew considerably in intensity, the mo-
lar volume increased upon doping against natural ex-
pectations, the hcp lattice flattened on doping (the
c/a ratio decreased). Neon impurities in solid hydro-
gen cause a few effects that could be explained only
under the assumption that VdW complexes are pres-
ent in the diluted alloys. These finding are an unusual
low-temperature anomaly in the heat capacity [8], a
decrease in the thermal resistance of Ne-doped alloys
(instead of an expected increase) compared to pure
hydrogen [9], an acceleration of quantum diffusion
caused by Ne doping [10], and some others.
Behavior of atoms and smaller molecules in solid
hydrogen is important in view of the recent idea of us-
ing para hydrogen as the isolation matrix material
[11]. On the one hand, effect of the quantum-crystal
nature of solid hydrogen on optical spectra still re-
mains an open issue. On the other hand, the rotational
dynamics of molecular impurities differs essentially in
classical rare gas and quantum (hydrogen) matrices
[12–16]. Presumably, the solid hydrogen matrix is
softer, interacting less with the impurity embedded
there to. But in classical matrices, impurity molecules
(provided they do not interact) rotate quite freely
down to very low temperatures. By shear contrast to
quite reasonable expectations, rotation of impurity
molecules in a quantum-crystal matrix is substantially
hindered and even locked into a librational state along
particular crystallographic directions [16]. This fact
can be easily explained by the extreme compliability.
Thus, it was shown [15] that a SF6 molecule in a he-
lium matrix has a «coat» of 22 to 24 He atoms so that
rotation is greatly hindered even in the superfluid
phase of helium.
There is another issue in the physics of dilute impu-
rities in various matrices, which can be directly solved
© N.N. Galtsov, A.I. Prokhvatilov, G.N. Shcherbakov, and M.A. Strzhemechny, 2003
with the aid of diffraction methods. This issue is the
changes in the molar volume of the matrix material
and the relevant displacement of the closer crystal
shells, necessary to be known for crystal-field evalua-
tions and corrections.
Here we report effects of heavier atomic (Ar and
Kr) as well as molecular (N2 and O2) impurities on
the structural characteristics of the quantum crystals
of para and normal hydrogen. To facilitate under-
standing of the experimental findings for H2-based bi-
nary systems we give in Table the basic molecular and
other parameters of the species involved.
Experimental
These studies were performed on a powder x-ray
diffractometer DRON-3M equipped with a liquid-he-
lium cryostat in the Cu K� radiation. Diffractometer
control as well as data collection and processing were
done using a PC. The sample were grown by quench
condensation of gas mixtures of known composition
directly to the solid phase onto a flat copper substrate
at a temperature of 5 K. The polycrystalline samples
were typically 0.1 mm thick with grain sizes within
10–4–10–5 cm. The purity of all the source gases was
not worse that 99.9%. The source parahydrogen had
an ortho fraction of 0.23%, which is an equilibrium
value for liquid-hydrogen temperature. The concentra-
tion of the impurity species in the gas mixtures was
varied from 0.05% to 5% for Ar, 1% to 10% for Kr and
N2, and from 1% to 20% for O2. The error of the impu-
rity fraction in the gas sample was 5% of the total
amount of the impurity in the gas. X-ray examination
was carried out from 5 K up to the melting point of
the hydrogen matrix. The temperature was stabilized
to within � 0.05 K at every measurement point. Be-
cause of a partial overlap of certain reflections from
the hydrogen matrix and the impurity solid, the re-
sulting lattice parameter error was larger than for
pure cryocrystals but did not exceed � 0.04%. If
should be noted that, in contrast to what we had on
neon-doped hydrogen and deuterium [7], condensa-
tion by small spurts (the pressure drop in the mixing
chamber being 2–3 mm Hg) of the mixtures with
heavier impurities yielded, as expected, strongly
stressed samples. This was evidenced from the absence
of most of the reflections, while the observed reflec-
tion (as a rule, the 002 ones) were broad. To remove
stresses, such samples were annealed for 1 to 1.5 hours
at a temperature 2 to 3 K below the melting point.
After annealing all the reflections appear in x-ray
patterns with the intensity ratios close to normal and
the line width typical of mixtures. We think that
quench condensation onto a substrate at 5 K yields
samples with a large amount of lattice defects, finer
than usual crystallites, and stresses. The high temper-
ature annealing not only removes stresses due to fast
crystallization and cooldown but also promotes a ho-
mogenization of the impurity distribution. This argu-
mentation is corroborated by the results of experi-
ments with samples grown on the same 5 K substrate
but at a twice as fast rate (with pressure drops of 5–7
Hg mm). Under these conditions, the condensate sur-
face was momentarily heated up to the melting point,
producing immediately an equilibrium sample so that
subsequent annealing did not change the diffraction
pattern.
Results and discussions
As the impurity, two type species have been cho-
sen, considerably differing in molecular parameters
from one another and from the hydrogen matrix (see
Table). This, in particular, concerns the Lennard-
Jones parameters and the Debye temperatures. The
molar volume differences between impurity and ma-
trix were such that doping of the H2 crystal would re-
sult in dilatations of opposite signs. Thus, judging
from molar volumes (Table) of pure solids, argon and
oxygen impurities were expected to contract the hy-
drogen lattice whereas krypton and nitrogen, to ex-
pand.
Table
The relevant physical properties of nH2, pH2 as well as
impurities Ar, Kr, N2, and O2
Sub-
stance
Structure
at 5 K
Lattice
parameters, Å
Molar volume,
cm3/mole
L–J
parameters
nH
2
hcp,
P6
3
/mmc
a = 3.770,
c = 6.162
22.83
� = 36.7 K
� = 2.96 Å
pH
2
hcp,
P6
3
/mmc
a = 3.783,
c = 6.178
23.06
� = 36.7 K
� = 2.96 Å
Ne
fcc,
Fm3m
a = 4.464 13.31
� = 36.7 K
� = 2.788 Å
Ar
fcc,
Fm3m
a = 5.311 22.415
� = 119.8 K
� = 3.405 Å
Kr
fcc,
Fm3m
a = 5.646 26.932
� = 164.0 K
� = 3.624 Å
N
2
fcc,
Pa3
a = 5.649 27.13
� = 95.1 K
� = 3.708 Å
O
2
monoclinic,
C2/m
a = 5.375,
b = 3.425,
c = 4.242,
� = 117.8°
20.57
� = 117.3 K
� = 3.817 Å
It should be also taken into account that the molar
volumes of both molecular solids N2 and O2 are to an
Properties of solid hydrogen doped by heavy atomic and molecular impurities
Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10 1037
appreciable extent controlled by rather strong aniso-
tropic interactions, which tend to compress these so-
lids. In addition, the paramagnetic impurities of oxy-
gen can essentially affect the conversion process in
the normal hydrogen crystals [20–22].
Some of preliminary results of hydrogen doped
with Ar, Kr, and N2 have been reported at the 3rd
Cryocrystals Conference [23]. Later we carried out a
few complementing and more precise experiments on
the these above-mentioned systems, in particular, us-
ing normal hydrogen as matrix, as well as repeated the
entire set of measurements on oxygen-doped normal
hydrogen.
When embarking on this program, we expected to
find evidence of VdW complexes around the impurity
particles. However, our analysis shown that there are
no unambiguous confirmation of this hypothesis, at
least within the content sensitivity (about 1%) of our
method. The x-ray patterns contained reflections only
from the hcp hydrogen-rich phases (both for normal
and para H2) and, when observable, reflections from
the lattices of the respective pure substances (Fig. 1),
the monoclinic lattice of O2 and fcc lattices of all
other crystals. It should be remarked here that the de-
termination of the least concentration, at which impu-
rity-based phases used to appear, was difficult because
for krypton and nitrogen impurities the (111) reflec-
tion of the respective cubic phases overlapped in part
with the first (100) reflection of H2; for argon and oxy-
gen — with second (002) and third (101) reflection of
H2 matrix respectively (cf. Fig. 1,a to d). However,
in spite of these aggravations we have established that
reflections of the pure phases of all the dopants are de-
tectable in x-ray patterns when the normal fraction of
the impurity in the source gas mixture exceed 0.5%.
Typical powder x-ray patterns for hydrogen-based
solid mixtures with the four impurity species are
shown in Fig. 1. The position and shapes of the H2 re-
flections differ from those from pure normal and para
hydrogen. This is might be caused by the following
factors. Although the actual content (solubility) of all
impurities can be substantially less than the lower
concentration in gas mixtures (the equilibrium solu-
bility of heavy gases in solid hydrogen from thermal
conductivity measurements [24,25] is 10–4 or less),
these impurities affect perceptibly the structural char-
acteristics of doped hydrogen. Usually, when quench
depositing pure hydrogen on low temperature, it is
difficult to avoid texture [26] with the close packed
(00l) basal layers being parallel to the substrate sur-
face so that multiple reflections from these planes can
only be seen in patterns. In the experiments reported
here, even seemingly insignificant amounts of impuri-
ties (as low as 0.05% of Ar in the gas mix) essentially
suppresses preferable epitaxial crystal growth and the
intensity ratios from the hydrogen matrix is close to
that from non-textured polycrystalline samples (cf.
for example, Fig. 1,a). The part of the impurity com-
ponent that was not dissolved in solid hydrogen aggre-
gates into a separate phase producing corresponding
reflections. Above the hydrogen melting temperature,
only impurity-related reflections persist (Fig. 1). The
1038 Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10
N.N. Galtsov, A.I. Prokhvatilov, G.N. Shcherbakov, and M.A. Strzhemechny
26 28 30 32 34
200
400
600 a
14 K
5 K
2� , deg
In
te
n
si
ty
,
a
rb
. u
n
its
(1
0
0
)
(0
0
2
)
(1
1
1
)
A
r
(1
0
1
)
26 28 30 32
100
200
300
400
500
600 b
14 K
2 � , deg
5 K
In
te
n
si
ty
,
s
a
rb
. u
n
it
(1
0
0
)
(0
0
2
)
(1
1
1
)
K
r
(1
0
1
)
(2
0
0
)K
r
26 28 30 32
200
300
400
500
600
c
14 K
5 K
N
2
In
te
ns
ity
,
a
rb
. u
n
its
2�, deg
(1
0
0
),
(1
1
1
)
(0
0
2
)
(1
0
1
)
(2
0
0
)
N
2
32 34 36 38 40 42
80
120
160
200
240 dO
2
O
2O
2
5 K
In
te
ns
ity
,
a
rb
. u
n
its
2�, deg
(1
0
0
) (0
0
2
)
(1
0
1
)
(1
1
0
)
(2
0
-1
)
(1
1
-1
)
Fig. 1. Typical powder x-ray patterns for solid mixtures:
pH2 + 1% Ar (a), nH2 + 2% Kr (b), pH2 + 2% N2 (c) for
5 K and 14 K, nH2 + 2% O2 for 5 K (d).
integrated intensity of these reflections is noticeably
higher than could be expected from the nominal con-
centration in the gas. The width of the reflections af-
ter annealing-related hydrogen effusion is consider-
ably (2–2.5 times) larger than usual, which suggests a
high concentration of impurities (H2) and/or lattice
defects.
Before analyzing the structure data and giving our
arguments, we note that, when considering a molecu-
lar impurity in a solid made up of spherical particles
(like H2), one should use for scaling not the molar
volume of the pure molecular solid (in which strong
anisotropic force produce a large negative contribu-
tion) but, because in an environment of spherical par-
ticles the molecule is stripped of its anisotropic forces,
�
3 where � is the Lennard-Jones radius [27].
Argon impurities in para hydrogen increase the vol-
ume of the matrix by an amount comparable to those
observed in pH2–Ne mixtures (Fig. 2) despite the
slightly smaller volume in the bulk Ar compared to
pH2.
Oxygen impurities also expand the normal hydro-
gen lattice, approximately by the same amount as
krypton. There is, however, an important difference
because oxygen is known to accelerate ortho-para con-
version so that during sample preparation and mea-
surements oxygen impurities burn out ortho states in
their closest environment and, thus, are in fact sur-
rounded by virtually pure para hydrogen. Therefore,
the net expansion effect due to O2 impurities is less
pronounced compared to Kr impurities. Thus, the lat-
tice expansion caused by Ar and O2 impurities, both of
which are smaller than the size of vacant sites in hy-
drogen crystals, may be treated as evidence of hydro-
gen-based VdW complexes, similar to those presum-
ably found in Ne-doped hydrogen.
Nitrogen apparently does not change the volume
hydrogen matrix at any temperature up to melting
(Fig. 2). Since Lennard-Jones radius of the bare nitro-
gen molecule (3.708 Å) is close to the intermolecular
distance in solid H2 (3.784 Å for para hydrogen), one
can expect an «accurate» nesting for the N2 impurity
in H2. Since the central H2–H2 interaction constant
does not differ drastically from H2–N2 one, the almost
absent effect of N2 does not seem strange.
Krypton impurities increase the molar volume of
the normal hydrogen matrix (Fig. 3). The fact that
the excess volume and its temperature dependence are
the same for the nominal gas fractions of 1% and 10%
implies that the true Kr concentration in solid H2
must not extend 1%. Our previous evaluation [5]
yields an upper limit value of 4%, which does not con-
tradict the above reasoning. The very fact of the posi-
tive effect of Kr impurities seems to be quite natural
because of the larger impurity size.
Although Ar and Kr bring about almost equal vol-
ume changes, they deform the hexagonal H2 lattice in
a different way (Fig. 4): Ar decreases and Kr increases
Properties of solid hydrogen doped by heavy atomic and molecular impurities
Fizika Nizkikh Temperatur, 2003, v. 29, Nos. 9/10 1039
4 6 8 10 12 14
23.0
23.2
23.4
23.6
23.8
24.0
V
,
c
m
3 /m
o
le
T, K
Fig. 2. Temperature dependence of the molar volume of
solid para hydrogen with impurities: 0.05% Ar (�); 2% N2
(�); pure pH2 [26] (—); 5% Ar (�); 2% Ne [6] (- - -);
2% Ar (�).
4 6 8 10 12 14
22.8
23.0
23.2
23.4
23.6
23.8
V ,
c
m
3 /m
o
le
T. K
Fig. 3. Temperature dependence of molar volume of solid
normal hydrogen with impurities: 1% Kr (�); 10% Kr
(�); 5% Ne [7] (-�-); pure nH2 [28] (—); 5% O2 (�).
4 6 8 10 12 14
1.628
1.632
1.636
1.640
1.644
c/
a
T, K
Fig. 4. Temperature dependence of the c/a of solid hy-
drogens with impurities: pH2 + 0.05% Ar (�); nH2 + 1%
Kr (�); nH2 + 5% Ne [7] (�); pure nH2 [28] (—);
pure pH2 [26] (- - -); nH2 + 1% O2 (�); pH2 + 5% Ne
[6] (�).
the c/a ratio and both absolute deviations increase
with increasing temperature. The opposite behavior of
the c/a ratio (temperature independence close to
melting, then a fast buildup) in Ne–H2 mixtures [6]
can be due to a possible destruction of Ne(H2)n com-
plexes at higher temperatures.
All the facts listed above imply that the doping of
such a quantum crystal like hydrogen with heavier im-
purities and, especially, quantum-crystal effects in the
dynamics of substitutional impurities in quantum so-
lids cannot be described by the theory of regular solid
solutions. The experimental facts reported here might
serve as another stimulating arguments for theorists.
This work was supported by CRDF (grant
UP2-2445-KH-02). The authors thank V.G. Man-
zhelii and M.I. Bagatskii for valuable discussions.
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