Synthesis of hydrogen storage materials in a Ti-Zr-Ni system using the hydride cycle technology during dehydrogenation by an electron bean in a vacuum

The synthesis of intermetallic material was carried out by means of dehydrogenating annealing of a (TiH 2) 30 Zr 45 Ni 25 sample in vacuum by an electron beam. The properties of the obtained material were studied for establishing the structural phase composition by scanning electron microscopy and X-ray structural analysis. It was found that prolonged exposure of an electron beam to a sample containing titanium hydride leads to a number of structural transformations in the material, accompanied by a redistribution of hydrogen from titanium to zirconium and culminating in the synthesis of a ternary alloy with characteristic growth structures. The processes of hydrogen sorption-desorption by a synthesized sample were studied, the temperature ranges of these processes and the absorption capacity of the obtained material were established. It was shown that the structure of the sample formed upon heating by an electron beam promotes the absorption of hydrogen at room temperature up to 1.41 wt.%.
About Klee Irwin

Klee Irwin is an author, researcher and entrepreneur who now dedicates the majority of his time to Quantum Gravity Research (QGR), a non-profit research institute that he founded in 2009. The mission of the organization is to discover the geometric first-principles unification of space, time, matter, energy, information, and consciousness.
As the Director of QGR, Klee manages a dedicated team of mathematicians and physicists in developing emergence theory to replace the current disparate and conflicting physics theories. Since 2009, the team has published numerous papers and journal articles analyzing the fundamentals of physics.
Klee is also the founder and owner of Irwin Naturals, an award-winning global natural supplement company providing alternative health and healing products sold in thousands of retailers across the globe including Whole Foods, Vitamin Shoppe, Costco, RiteAid, WalMart, CVS, GNC and many others. Irwin Naturals is a long time supporter of Vitamin Angels, which aims to provide lifesaving vitamins to mothers and children at risk of malnutrition thereby reducing preventable illness, blindness, and death and creating healthier communities.
Outside of his work in physics, Klee is active in supporting students, scientists, educators, and founders in their aim toward discovering solutions to activate positive change in the world. He has supported and invested in a wide range of people, causes and companies including Change.org, Upworthy, Donors Choose, Moon Express, Mayasil, the X PRIZE Foundation, and Singularity University where he is an Associate Founder.
sample HYDROGEN temperature ELECTRON BEAM heat Ti Zr Ni
About Klee Irwin

sample HYDROGEN temperature ELECTRON BEAM heat Ti Zr Ni
 
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      ISSN 1562-6016. ВАНТ. 2020. №1(125) 
UDC 544.723; 669.788 
 
SYNTHESIS OF HYDROGEN STORAGE MATERIALS IN A Ti-Zr-Ni 
SYSTEM USING THE HYDRIDE CYCLE TECHNOLOGY DURING 
DEHYDROGENATION BY AN ELECTRON BEAM IN A VACUUM 
 
O.E. Dmytrenko, V.I. Dubinko, V.M. Borysenko, K. Irwin* 
National Science Center “Kharkоv Institute of Physics and Technology”, Kharkiv, Ukraine; 
*Quantum Gravity Research, Los Angeles, CA 
E-mail: dmitrenko@kipt.kharkov.ua 
 
The synthesis of intermetallic material was carried out by means of dehydrogenating annealing of a 
(TiH2)30Zr45Ni25 sample in vacuum by an electron beam. The properties of the obtained material were studied for 
establishing the structural phase composition by scanning electron microscopy and X-ray structural analysis. It was 
found that prolonged exposure of an electron beam to a sample containing titanium hydride leads to a number of 
structural transformations in the material, accompanied by a redistribution of hydrogen from titanium to zirconium 
and culminating in the synthesis of a ternary alloy with characteristic growth structures. The processes of hydrogen 
sorption-desorption by a synthesized sample were studied, the temperature ranges of these processes and the 
absorption capacity of the obtained material were established. It was shown that the structure of the sample formed 
upon heating by an electron beam promotes the absorption of hydrogen at room temperature up to 1.41 wt.%. 
 
INTRODUCTION 
The 
possibility 
of 
synthesizing 
complex 
intermetallic and quasicrystalline materials based on 
refractory metals of the zirconium group using hydride 
technology was shown in [1–8]. These materials are 
capable of reversibly absorbing hydrogen in significant 
quantities over 2 wt.% [9–11], which allows us to 
consider them as materials for the storage of hydrogen. 
The studies conducted earlier [12, 13] showed that 
materials of the Ti-Zr-Ni system obtained by the rapid 
quenching method and containing the Laves phase C14 
(L-TiZrNi) absorb hydrogen in the temperature range 
450550 °С. The maximum amount of hydrogen when 
saturated from the gas phase occurs at 450 °C and is 
characterized by slow sorption to values of about 
1.8 wt.%. For the industrial use of these materials as 
hydrogen storage devices, it is necessary to increase the 
absorption coefficient and 
reduce 
the sorption-
desorption temperatures. In addition, the synthesis of 
samples by spinning is inefficient and technically 
complex, requires the use of expensive vacuum 
equipment. Therefore, it is necessary to develop more 
productive techniques that allow the synthesis of bulk 
samples with a given structure and properties. In this 
work, we studied the structure and properties of the 
(TiH2)30Zr45Ni25 
sample during 
its 
layer-by-layer 
dehydrogenation in a vacuum under the influence of an 
electron beam. The technology of the “hydride cycle”, 
based on the interaction of the decomposition products 
(dissociation) of the hydrides of the initial components 
with the formation of systems and phases characteristic 
of these materials with significantly less energy 
consumption. Hydrogen, in this case, plays the role of a 
temporary alloying impurity to titanium and zirconium, 
leaving the sample when heated in a vacuum, but 
having a positive effect on the process of converting the 
system of starting dispersed particles into a massive 
(consolidated) alloy. Titanium and zirconium, as 
elements of one group of the periodic system, have 
similar characteristics of interaction with hydrogen, in 
particular, they have similar binary phase diagrams with 
hydrogen 
(both 
metals 
form 
hydrides). 
Dehydrogenation with an electron beam will allow 
gradient heating of the sample and, therefore, obtain a 
sample with all intermediate structural states from 
hydride to ternary alloy. And, therefore, with a cross-
section, it will allow studying/observe these processes 
of structural transformations, which in turn will expand 
the possibilities of synthesis of materials of the Ti-Zr-Ni 
system with predetermined properties. 
 
MATERIALS AND METHODS 
To prepare the sample (TiH2)30Zr45Ni25 (wt.%), the 
powders of the starting components were used: TiH2 
(with a hydrogen content of 3.8 wt.%, Zr powder 
(ПЦРК-1) Ni powder (ПНЭ-1)). The powders were 
mixed by grinding in an alundum mortar for 10 min. 
The resulting mixture powders were pressed into a 
briquette of Ø 30 mm and a height of 15 mm with a load 
of 77 t. 
Annealing/dehydrogenation of the sample was 
carried out by an electron beam in a high vacuum at the 
EBM-1 facility [14]. Electron beam treatment of the 
sample (TiH2)30Zr45Ni25 was carried out in vacuum 
(1…5)·10
-2
 Pa. The structure and composition of the 
samples were studied by scanning electron microscopy 
(SEM) and X-ray energy-dispersive microanalysis 
(EDX), using a SEM JSM 7001F with an accelerating 
voltage of 20 kV. Observation of the structure was 
carried out both in the secondary electron (SEI) mode 
and in the backscattered electron (COMPO) mode 
forming the composite image contrast. The composition 
was analyzed using the INCA PentaFET*3 detector and 
the Oxford 
Instruments 
INCA 4.11 program. 
Diffractometric studies of the samples were carried out 
on a DRON-4-07 X-ray diffractometer in copper Cu-Kα 
radiation using a selectively absorbing β-filter. 
Diffracted radiation was recorded by a scintillation 
detector. The diffraction patterns were taken in step 
mode. The 
following 
samples of 
composition 
(TiH2)30Zr45Ni25 were taken for research:   a) the melted 
 
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part; b) not melted part. The samples were saturated 
with hydrogen from the gas phase in two different 
chambers: a) a metal chamber with a vacuum pumping 
system and a hydrogen/deuterium supply system with a 
pressure of up to 3 atm; b) in an installation with an 
MX7203 mass spectrometer at a hydrogen pressure of 
10 mm Hg and heating in the range of 20450 °C for 3 
h. The temperature increased at a rate of 5 °C/min in a 
hydrogen atmosphere. The temperature difference at the 
boundaries of the heat treatment region is ± 20 °C. The 
cooling of the furnace to 20 °C took place in a hydrogen 
atmosphere. Hydrogen-saturated samples of Ti-Zr-Ni 
alloys were investigated for desorption by heating in a 
vacuum in the temperature range 0900 °C using a 
setup with an MX7203 mass spectrometer. The 
MX7203 mass spectrometer is designed to determine 
the hydrogen in the alloys and the composition of the 
gas phase released from the material when heated in a 
vacuum. 
 
RESULTS AND DISCUSSION 
The sample obtained after electron beam melting 
was partially melted: the upper part of the briquette was 
melted to a depth of 4 mm. The rest of the briquette is 
not fused, it easily crumbles with little effort. For 
analysis of XRD, the upper (melted) and lower (non-
melted) parts of the sample were taken, which were 
mechanically fragmented 
into several parts 
(the 
resulting sample is extremely fragile and easily 
collapses upon impact). For SEM/EDX studies, a 
transverse kink of the sample was used, thus the 
structure from the molten surface to the unsintered 
powders was analyzed. Electron microscopy showed 
that there is a significant structural heterogeneity along 
with the depth of the sample. 
Under the influence of an electron beam, the gradual 
heating of the sample begins. Since the sample is 
located on a copper water-cooled crystallizer, and the 
electron beams are focused on the upper surface of the 
sample, a heat gradient arises from the top-down of the 
sample. With further heating of the upper surface and 
reaching the dissociation temperature of titanium 
hydride, the process of sequential decomposition of 
TiH2 begins according to the scheme [15]: TiH2(ε) → 
TiH2(δ) → Ti(β) → Ti(α). However, 
as 
it was 
established during a preliminary study of the thermal 
desorption of TiH2 shown in Fig. 1, the active 
decomposition of 
titanium hydride occurs at a 
temperature of 500550 °C, at the same time, at this 
temperature, 
zirconium powder actively absorbs 
hydrogen, since the decomposition temperature of ZrH2 
is higher than that of TiH2 at 100150 °С (see Fig. 1). 
Thus, the heating of the (TiH2)30Zr45Ni25 sample by 
an electron beam is accompanied by a series of 
structural 
transformations 
that occur during 
the 
redistribution of hydrogen from TiH2 to ZrH2 and the 
subsequent decomposition of ZrH2(ε) → ZrH2(δ) → 
Zr(β) → Zr(α) with increasing temperature [16]. Since 
the beam power is set necessary for slow heating of the 
sample and does not change further, a stationary 
dehydrogenation process is established in the chamber 
in which the above transformations occur layer by layer, 
as the sample is heated from top to bottom. During 
dissociation during annealing in vacuum, TiH2 and ZrH2 
emit hydrogen, gradually turning into metals, and a 
decrease in the concentration of hydrogen in their 
crystal 
lattices 
leads 
to a sequence of phase 
transformations. Due to the presence of bonds broken 
during dissociation, the obtained metal titanium and 
zirconium actively interact with each other and with 
nickel at temperatures well below their melting points. 
An additional factor contributing to the interaction is the 
cleaning of the surfaces of the powders from oxide films 
by active hydrogen released during the decomposition 
of hydrides, as shown in [17]. 
0
10
20
30
40
50
60
70
80
90
100
0
100
200
300
400
500
600
700
800
Temperature, °С
Pressure, mm.Hg.TiH2
ZrH2
 
Fig. 1. Thermal desorption TiH2 and ZrH2 
 
The fusion process begins with the local melting of 
individual Ti, Zr, Ni particles at the contact boundary 
with the formation of the eutectic (Fig. 2,a). As the 
sample is heated and the temperature rises in volume, 
the local boundary fusion passes into the melt zones 
with the involvement of a larger number of initial 
components. The resulting eutectic type melt (since a 
composition close to the eutectic is taken) penetrates 
deep into the sample, the melt zone expands (see 
Fig. 2,b). When an equilibrium annealing process is 
established (all heat transferred to the upper part of the 
sample by an electron beam is removed through the 
lower part of the sample located on a copper water-
cooled tray), a new/gradual formation of a new structure 
in the melt zone occurs. 
At a certain point in time (at a certain temperature, 
composition, temperature gradient), more refractory 
crystallization centers form in the melt (see Fig. 2,c). 
Since this composition of the Ti-Zr-Ni melt corresponds 
to eutectic, and the temperature at the beginning of 
crystallization, we obtain a mixture of more refractory 
crystals, 
presumably 
enriched with 
zirconium, 
surrounded by more fusible melts with a high content of 
titanium and nickel (see Fig. 2,d). This was confirmed 
by the EDX analysis data presented in Table. The Zr 
content in the growth structures is 56 wt.%, in contrast 
to 4345 wt.% in the eutectic matrix surrounding them. 
Classical eutectic precipitation will not occur since the 
sample continues to be heated by the electron beam and 
the melt zone continues to propagate down the sample. 
 
 
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a 
b 
 
 
c 
d 
 
 
e 
f 
Fig. 2. Formation of growth patterns characteristic of the given system with gradual melting of the sample 
After the equilibrium process is established, with a 
constant beam power that corresponds to the melting 
point of the eutectic and a constant heat removal rate, 
i.e., we have a constant temperature gradient, the melt 
and crystallization centers create optimal conditions for 
polycrystalline grain growth. As can be seen from 
Fig. 2,e,f the growth patterns characteristic of this 
system are formed. As these formations grow, the 
amount of surrounding eutectic decreases accordingly. 
At a distance of less than 1 mm from the heated upper 
surface of the sample, the crystals completely “absorb” 
the surrounding eutectic and grow to the maximum size 
limited by neighboring formations. Considering the 
duration of the annealing process (about 3 h), significant 
formations up to 500 m in size are formed (Fig. 3). 
Since the gradual melting of the sample occurs, all 
of the above processes occur in layers as the sample is 
melted, i.e. simultaneously: in a layer located 3 mm 
 
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from the upper part of the sample, crystallization centers 
surrounded by a eutectic only appear (see Fig. 2,c,d); in 
a layer of 2 mm (from the upper part of the sample) 
crystalline multilayer formations (growth figures) have 
already formed, partially surrounded by a eutectic (see 
Fig. 2,e,f); in a 1 mm layer, crystals completely 
absorbing the surrounding eutectic, grow to maximum 
sizes (limited by adjacent formations) form spherical 
formations consisting of square pyramids and octahedra 
(see Fig. 3,a,b); on the surface of the sample (directly 
under the electron beam) the previously formed 
spherical formations begin to melt due to the gradual 
heating of the entire sample (see Fig. 3,c,d). 
 
 
Data from EDX analysis of growth patterns and surrounding eutectics 
Element 
Ti K 
Ni K 
Zr L 
Hf L 
Totals 
Growth patterns 
21.73 
19.41 
56.66 
2.20 
100.00 
Surrounding matrix 
31.70 
26.07 
42.23 
 
100.00 
 
 
 
a 
b 
 
 
c 
d 
Fig. 3. Spherical formations consisting of square pyramids and octahedrons (a, b); reflow of previously formed 
spherical formations consisting of square pyramids and octahedrons (c, d) 
 
Thus, 
the obtained sample contains various 
structural elements that are formed during the long-term 
exposure of the initial sample (TiH2)30Zr45Ni25 electron 
beam. The stages characteristic for each stage can be 
distinguished: fusion of the initial components Ti, Zr, 
Ni → formation of growth structures surrounded by 
eutectics → conglomerates of 
square pyramids → 
fusion of previously formed square pyramids and 
octahedrons. An additional factor for the formation of 
structural features in this sample is the dissociation of 
titanium hydride into hydrogen and titanium. And 
accordingly, the active diffusion of released hydrogen in 
a sample heated to a pre-melting temperature. 
 
PHASE ANALYSIS OF SAMPLES Ti30Zr45Ni25 
X-ray diffraction patterns of the samples are shown 
in Fig. 4. The results of studies of the phase 
composition of the samples showed that 4 phases were 
identified in the melted upper part of the sample (see 
Fig. 4,a): (Ti,Zr)2Ni, Laves phase L-TiZrNi, Ti-α, and 
Zr-α. The lattice parameter of the (Ti,Zr)2Ni phase is 
a = 11.761 Å. The lattice parameters of the Laves phase 
are a = 5.222 Å; c = 8.558 Å. The lattice parameters of 
titanium are a = 2.964 Å; c = 4.618 Å. The lattice 
 
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parameters of zirconium are a = 3.242 Å; c = 5.156 Å. 
Due to the superposition of some diffraction lines on 
each other, some phases are not identified, including the 
quasicrystalline phase. 
The presence of three phases was revealed in the 
unmelted lower part of the sample (see Fig. 4,b): 
tetragonal zirconium hydride ε-ZrH2-x, cubic titanium 
hydride TiH2, and nickel Ni. The lattice parameters of 
the ε-ZrH2-x phase are: a = 3.496 Å; c = 4.493 Å. The 
lattice parameter of 
titanium hydride TiH2 
is 
a = 4.411 Å. The lattice parameter of nickel Ni is 
a = 3.524 Å. In addition, the sample contains diffraction 
lines that could not be indicated. 
 
 
a 
 
b 
Fig. 4. Diffraction pattern of the sample 
(TiH2)30Zr45Ni25: upper melted part (a);  
lower not melted part (b) 
 
Since there was no zirconium hydride in the initial 
sample, therefore, the presence of ZrH2(δ) in the lower 
non-melted part of the sample confirms that the 
hydrogen formed during the decomposition of titanium 
hydride is absorbed by zirconium. And only then, with a 
further increase in temperature, does the sample leave. 
The presence in the sample of unusual structural 
formations shown in Figs. 2, 3 gave a prerequisite for 
research on the interaction of this material with 
hydrogen. 
THE STUDY OF SORPTION-DESORPTION 
For conducting research, a sample of the upper 
molten portion weighing 2.8 g was previously ground 
by grinding in an alundum mortar. Grinding was carried 
out immediately before the experiment. After loading 
the sample into the reaction chamber, the chamber was 
evacuated to a pressure of 510
-6
 bar. After the 
evacuation, hydrogen was introduced into the reaction 
chamber. The initial hydrogen pressure in the reaction 
chamber was 198 kPa. About 500 s after the hydrogen 
was introduced into the reaction chamber, intense heat 
evolution began, which led to an increase in the 
temperature of the sample (Fig. 5,a). The rate of heat 
evolution was proportional to the rate of change in 
pressure in the reaction chamber Fig. 5,b. The heat was 
generated by pulses. The heat generation impulsivity is 
especially pronounced at the initial stage of hydrogen 
absorption. When saturated, the sample absorbed about 
1.41% by weight of hydrogen for 1.5 h. The relatively 
small amount of absorbed hydrogen can be explained by 
the predominance of the (Ti,Zr)2Ni phase over the 
Laves phase of L-TiZrNi. As was established earlier 
[10], the absorption potential of the (Ti,Zr)2Ni phase is 
much lower than that of the Laves phase. However, in 
contrast to rapidly quenched tapes of the same 
composition starting to absorb hydrogen when heated 
above 400 °C, this sample began to absorb hydrogen at 
12 °C after a short incubation period.  
 
a 
 
b 
Fig. 5. Dependences of the temperature of sample (a) 
and the pressure in the reaction chamber (b) on time, 
when the Ti30Zr45Ni25 sample is saturated with hydrogen 
at room temperature 
After saturation with hydrogen at room temperature, 
the sample was subjected to thermal desorption by 
heating to 900 °C and cooling to room temperature with 
 
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         203 
continuous vacuum pumping. Fig. 6,a shows the 
dependence of the pressure in the reaction chamber on 
the temperature of the sample during monotonous 
heating of the sample at a constant rate of pumping the 
reaction chamber to a low vacuum after a heating cycle. 
Intensive gas evolution from the sample began at about 
40 °C and lasted with variable intensity up to a 
temperature of 800 °C. The presence of several peaks of 
gas evolution indicates the evolution of hydrogen from 
various phases present in the sample, which corresponds 
to XRD analysis. 
 
a 
 
b 
Fig. 6. The dependence of the pressure in the reaction 
chamber on the temperature of the sample when the 
sample is heated at a constant rate of evacuation of the 
reaction chamber to vacuum after the first 
saturation (a), after re-saturation (b) 
 
After degassing, the sample was re-saturated with 
hydrogen at room temperature Fig. 7. The initial 
hydrogen pressure in the reaction chamber was 260 kPa. 
Upon repeated saturation, the absorption of hydrogen by 
the sample began with approximately the same delay as 
at the first saturation. The heat generation impulsivity 
was also observed. The intensity of the heat during the 
second saturation was significantly lower, but it took a 
longer time. The amount of heat was proportional to the 
magnitude of the change in pressure in the reaction 
chamber. Upon re-saturation, the sample absorbed 
0.34 wt.% hydrogen for 4 h. Thus, it was found that this 
material is capable of absorbing hydrogen at room 
temperature after a dehydrogenation cycle. Subsequent 
dehydrogenation showed identical kinetics of thermal 
desorption (see Fig. 6,b). 
The next stage of studies on the interaction with 
hydrogen was carried out on the subject of the influence 
of passivation/oxidation of the surface of the sample by 
air. Between grinding material and loading the sample 
into the reaction chamber, the crushed material of the 
sample (upper melted portion) Ti30Zr45Ni25 was in the 
air for 7 days. After loading the sample into the reaction 
chamber, the chamber was evacuated to a pressure of 
510
-6
 bar. After 
the evacuation, hydrogen was 
introduced into the reaction chamber. The initial 
hydrogen pressure in the chamber was 268 kPa. As a 
result of the exposure of the sample at room temperature 
for 60 min, hydrogen uptake was not observed. During 
monotonous heating of the sample, active absorption of 
hydrogen by the sample began after reaching a 
temperature of 300 °C (Fig. 8). The active phase of 
hydrogen absorption continued to a temperature of 
about 400 °C. At a sample temperature above 450 °C, 
the absorption practically ceased. In the temperature 
range 300400 °C, the sample absorbed about 0.95% 
by weight of hydrogen. Hydrogen evolution during 
thermal desorption from this sample occurred in the 
range 350600 °С with max at 450 °С, which 
significantly differs from the kinetics of desorption of a 
hydrogen-saturated small particle at room temperature. 
 
a 
 
b 
Fig. 7. Dependences of the temperature of the sample 
and heater (a), the pressure in the reaction chamber (b) 
on time upon re-saturation of the Ti30Zr45Ni25 sample 
with hydrogen at room temperature 
To confirm the obtained data, duplicate experiments 
on hydrogen sorption-desorption were carried out with a 
 
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Ti30Zr45Ni25 sample in a setup with an MX7203 mass 
spectrometer. The sample was studied in the air for 
7 days after grinding. Absorption at room temperature 
was not observed upon exposure to hydrogen for more 
than 2 h. Hydrogen sorption began only when heated 
above 200 °C. Active absorption took place in the range 
of 250350 °C, plots of hydrogen sorption and thermal 
desorption after saturation of the samples with hydrogen 
are shown in Fig. 8. 
 
 
a 
0
10
20
30
40
50
60
70
80
90
100
110
120
0
100
200
300
400
500
600
700
800
Temperature, °С
Pressure, mm.Hg. 
b 
Fig. 8. Dependence of the pressure in the reaction 
chamber on the temperature of the Ti30Zr45Ni25 sample 
(7 days in the air) for: sorption (a) and thermal 
desorption (b) of hydrogen 
 
Thus, it can be argued that the presence of the 
ground Ti30Zr45Ni25 sample in air leads to a gradual 
increase in the incubation period before the absorption 
of hydrogen at room temperature and subsequently 
completely eliminates this process. Nevertheless, the 
detected temperature ranges of sorption-desorption and 
the corresponding sorption capacity are unique for the 
Ti-Zr-Ni system and most other known metal hydride 
systems. This material can be an extremely promising 
hydrogen accumulator, research is ongoing. 
 
CONCLUSION 
The Ti30Zr45Ni25 
intermetallic material was 
synthesized using the hydride cycle technology with 
dehydrogenation of a portion of the (TiH2)30Zr45Ni25 
sample by an electron beam in vacuum. The 
establishment of a stationary process of gradient heating 
of a sample by an electron beam made it possible to 
form a layered structure in the sample and fix all stages 
of transformations, from the initial hydrides to the 
formation of a ternary alloy. Using scanning electron 
microscopy and X-ray diffraction analysis, it was 
established that under the influence of an electron beam, 
structural 
transformations occur 
in 
the sample, 
associated with the decay of titanium hydride and 
accompanied by a redistribution of hydrogen between 
the components of the sample. As a result of synthesis, 
the growth structures characteristic of the given system 
are formed in the sample, which are a mixture of 
(Ti,Zr)2Ni phases, Laves phases C14 L-TiZrNi,             
α-(Ti,Zr). The study of hydrogen sorption and 
desorption processes by a synthesized sample showed 
that the structure of the sample formed upon heating by 
an electron beam promotes reversible absorption of 
hydrogen at room temperature up to 1.41 wt.% with 
heat evolution. Subsequent thermal desorption of 
hydrogen begins when the sample is heated above 40 °C. 
It was also found that after grinding a sample of 
Ti30Zr45Ni25 and being in a ground state for more than 
7 days in the air, the material loses its ability to absorb 
hydrogen at room temperature. 
ACKNOWLEDGEMENTS 
Authors thank gratefully to R. Vasilenko for the 
sample SEM/EDX investigations and I.V. Kolodiy for 
XRD 
investigations. Also, 
special 
thanks 
to 
M.M. Pylypenko and O.M. Bovda for the help in 
discussing the results. 
 
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Статья поступила в редакцию 27.11.2019 г. 
 
СИНТЕЗ МАТЕРИАЛОВ НАКОПИТЕЛЕЙ ВОДОРОДА В СИСТЕМЕ Ti-Zr-Ni  
ПО ТЕХНОЛОГИИ ГИДРИДНОГО ЦИКЛА ПРИ ДЕГИДРИРОВАНИИ ЭЛЕКТРОННЫМ 
ПУЧКОМ В ВАКУУМЕ 
А.Е. Дмитренко, В.И. Дубинко, В.Н. Борисенко, К. Ирвин 
Проведен синтез интерметаллического материала посредством дегидрирующего отжига образца 
(TiH2)30Zr45Ni25 в вакууме электронным пучком. Методом сканирующей электронной микроскопии и 
рентгеноструктурного анализа исследованы свойства полученного материала для установления структурно-
фазового состава. Установлено, что длительное воздействие электронного пучка на образец, содержащий 
гидрид титана, приводит к ряду структурных превращений в материале, сопровождающихся 
перераспределением водорода из титана в цирконий и завершающихся синтезом тройного сплава с 
характерными структурами роста. Исследованы процессы сорбциидесорбции водорода синтезированным 
образцом, установлены температурные диапазоны данных процессов и поглотительная способность 
полученного материала. Показано, что сформировавшаяся при нагреве электронным пучком структура 
образца способствует поглощению водорода при комнатной температуре до 1,41 вес.%. 
 
 
СИНТЕЗ МАТЕРІАЛІВ НАКОПИЧУВАЧІВ ВОДНЮ В СИСТЕМІ Ti-Zr-Ni  
ЗА ТЕХНОЛОГІЄЮ ГІДРИДНОГО ЦИКЛУ ПРИ ДЕГІДРУВАННІ ЕЛЕКТРОННИМ 
ПУЧКОМ У ВАКУУМІ 
О.Є. Дмитренко, В.І. Дубінко, В.М. Борисенко, К. Ірвін 
Проведено синтез інтерметалічного матеріалу за допомогою дегідруючого відпалу зразка (TiH2)30Zr45Ni25 
у вакуумі електронним пучком. Методом скануючої електронної мікроскопії і рентгеноструктурного аналізу 
досліджені властивості отриманого матеріалу для встановлення структурно-фазового складу. Встановлено, 
що тривала дія електронного пучка на зразок, що містить гідрид титану, призводить до ряду структурних 
перетворень у матеріалі, що супроводжуються перерозподілом водню з титану в цирконій і завершуються 
синтезом потрійного сплаву з характерними структурами зростання. Досліджено процеси сорбціїдесорбції 
водню синтезованим зразком, встановлені температурні діапазони даних процесів і поглинальна здатність 
отриманого матеріалу. Показано, що сформована при нагріванні електронним пучком структура зразка 
сприяє поглинанню водню при кімнатній температурі до 1,41 ваг.%. 
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