Journal of Solid State Electrochemistry

https://doi.org/10.1007/s10008-024-05889-4

ORIGINAL PAPER

In situ structural characterization of ­Li3PS4 solid electrolytes

under high pressure
Atsushi Yao1 · Shogo Kadota2 · Satoshi Hiroi3 · Hiroki Yamada3,4 · Jo‑chi Tseng4 · Seiya Shimono4 · Futoshi Utsuno2 ·
Koji Ohara3,4

Received: 6 March 2024 / Revised: 3 April 2024 / Accepted: 3 April 2024

© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2024

Abstract
All-solid-state batteries are typically manufactured under high pressure to decrease the resistance of the solid interface.
However, until now, there has been a lack of research concerning changes in the structure of solid electrolytes owing to
pressurization. Our study addresses this gap by exploring the structural modifications of the sulfide solid electrolyte ­Li3PS4
under high-pressure conditions. We observed a tendency for ­PS4 molecules to converge upon each other in both β-Li3PS4
and g-Li3PS4 crystals when subjected to a pressure of 100 MPa. In g-Li3PS4, X-ray scattering and pair distribution func-
tion analyses following pressure application and subsequent return to ambient conditions remained consistent with pre-
compression measurements. Conversely, in β-Li3PS4 crystals, post-pressure X-ray scattering differed from pre-compression
measurements, suggesting pressure-induced atomic rearrangement within the crystal lattice. This underscores the importance
of accounting for pressure-induced structural changes, especially in computational simulation studies where crystal struc-
tures are often assumed to remain static pre- and post-pressurization. Our findings demonstrate that under high pressure, the
crystal structure of L
­ i3PS4 slightly changes by approximately 1~2%, rendering it a viable candidate for utilization as a solid
electrolyte in all-solid-state batteries.

Introduction optimal filling of the solid electrolyte, and ensuring the solid
electrolyte can accommodate the volume fluctuations of the
All-solid-state lithium batteries are promising energy storage active material during charge and discharge cycles [3–8].
solutions, offering high safety standards, impressive output Typically, solid electrolytes consist of particle aggre-
capabilities, and enhanced energy densities [1, 2]. Despite gates with diameters ranging from 0.1 to 10 µm, featuring
these advantages, challenges specific to solid electrolytes, numerous interstitial voids. The measured ionic conductiv-
absent in liquid counterparts, have emerged. These include ity encompasses both bulk ionic conductivity and resistance
issues related to establishing interfaces between active stemming from these voids. Consequently, reducing voids,
materials and solid electrolytes, achieving densification and which impede ionic conduction, is anticipated to enhance
overall ionic conductivity. Research by Sakuda et al. dem-
onstrated that 7­ 5Li2S-25P2S5 glass ceramics, crystallized at
* Koji Ohara
ohara@mat.shimane-u.ac.jp 200 °C, exhibited notably high ionic conductivity, with SEM
surface observations revealing minimal void presence [9].
1
Advanced Technology Research Laboratories, Idemitsu Recent findings also highlight the exceptional ionic con-
Kosan Co. Ltd., 1280, Kamiizumi, Sodegaura City, Chiba ductivity ­(10−3 S ­cm−1 at room temperature) of void-free
299‑0293, Japan
­75Li2S-25P2S5 glass prepared via melt-quenching, nearly
2
Lithium Battery Material Department, Advanced Materials matching that of liquid electrolytes [10]. However, despite
Company, Idemitsu Kosan Co. Ltd., 1280, Kamiizumi,
Sodegaura City, Chiba 299‑0293, Japan variations in void fraction across samples (approximately
3 20%), no direct correlation with ionic conduction has been
Faculty of Materials for Energy, Shimane University, 1060,
Nishikawatsu‑cho, Matsue, Shimane 690‑8504, Japan established. In the manufacturing of all-solid-state batter-
4 ies, pressurization is a common step. Analysis of morphol-
Diffraction and Scattering Division, Japan Synchrotron
Radiation Research Institute, 1‑1‑1, Kouto, ogy through cross-sectional SEM and X-ray CT has con-
Sayo‑cho, Sayo‑gun Hyogo 679‑5198, Japan firmed the achievement of high packing, deformation, and

Vol.:(0123456789)

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 Journal of Solid State Electrochemistry

favorable interface formation in solid sulfide electrolytes the detector located 841.3 mm from the sample. Measure-
[4–6]. However, investigations into the pressurization pro- ments spanned 2θ from 0.2 to 27°, resulting in a maximum
cess and its effects on solid electrolyte structure have been momentum transfer of approximately 27.2 Å−1. Utilizing the
limited, neglecting in situ studies of structural changes dur- Orochi application, the two-dimensional intensity distribu-
ing pressurization and post-release. To address this gap, our tion was summed along the vertical direction within ± 10°
study employs in situ X-ray total scattering measurements on at the beam center to derive the one-dimensional scattered
sulfide solid electrolytes, known for their excellent pressure intensity [15]. The in situ pair distribution function (PDF)
adhesion properties, to explore average and local structural was obtained via Fourier transform of the intensity. During
alterations during pressurization and subsequent release. the measurements, vertical pressure was applied to the sam-
ple, as shown in Fig. 1. Notably, the direction of the detected
structural changes in the sample aligned with the direction
Methods of the applied pressure. An accumulation time of 50 s was
employed for each pressure condition to ensure a high sig-
Sample preparation nal-to-noise ratio in the high-Q region. The powder samples
were pressurized by sandwiching them between 9-mm-diam-
To explore the structural effects induced by high pres- eter stainless steel dies within the polycarbonate cylinder.
sure, glassy ­Li3PS4 (g-Li3PS4) [11] and crystalline ­Li3PS4 They are assembled in an Ar atmosphere and the powder
(β-Li3PS4) [12] were prepared. The precursors, L­ i2S (> 99.9%, was sealed inside the cylinder in Ar. As illustrated in Fig. 1a,
Idemitsu Kosan, Japan) and ­P2S5 (> 99%, Sigma–Aldrich pressure was exerted on the stainless steel die by turning the
Japan, Japan) powders, were thoroughly mixed in a planetary handle, while pressure was continuously monitored using
ball-milling system (Fritsch, P7) utilizing zirconia balls and a pressure gauge. Figure 1b shows a schematic diagram of
a container. Subsequently, g-Li3PS4 was obtained by milling the sample’s surrounding area. Background X-ray scattering
the mixed powders at a rotation speed of 450 rpm for 40 h. intensity from an empty polycarbonate cylinder was meas-
The transition to β-Li3PS4 was accomplished by annealing ured and subtracted from the detected intensity of the pres-
g-Li3PS4 in an Ar atmosphere at 430 °C for 2 h. surized sample to obtain the specific scattering intensity.

In situ X‑ray total scattering measurements Density functional theory calculations

The in situ X-ray total scattering measurements of the pre- The structural refinement of the β-Li3PS4 crystal was evaluated
pared ­Li3PS4 samples were conducted at BL08W in SPring-8 by analyzing the Bragg peak profile of the in situ X-ray total
(Hyogo, Japan) [13, 14]. The incident X-ray beam, with a scattering through the Rietveld refinement technique [16]. The
width of 0.5 mm, a height of 0.2 mm, and an energy of refinement was performed using software PDXL 2 (Rigaku)
115 keV, was directed onto a polycarbonate cylinder con- [17]. Density functional theory (DFT) calculations were per-
taining the samples. Employing the Debye–Scherrer geom- formed utilizing the projector augmented wave method [18],
etry, the experimental setup featured a two-dimensional implemented in VASP [19, 20]. For the exchange-correlation
area detector (XRD1621 CN3). The scattered X-rays were term, the generalized gradient approximation functional by
captured by CdTe arrays covering a 40 mm × 40 mm area on Perdew, Burke, and Ernzerhof [21] was employed.

Fig. 1  A sample cell utilized for

applying pressure in the in situ
X-ray total scattering measure-
ment. a Photographs of the cell
and the pressure gauge. b A
schematic diagram of the cell

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Journal of Solid State Electrochemistry

Results was evident, attributed to the rise in density. Additionally,

the lattice parameters underwent contraction, leading to a
In situ X-ray total scattering measurements were conducted shift in the Bragg peak profile toward the wide-angle direc-
to observe the total scattering intensity of ­Li3PS4 as a tion. Figure 2b compares the X-ray total scattering at 0 and
function of pressure. Figure 2a illustrates the variation in 100 MPa normalized by the intensity of the 221 reflection.
the X-ray total scattering intensity of the β-Li3PS4 crystal An observable broadening of the Bragg peak was noted
when subjected to pressure ranging from 0 to 100 MPa. with increasing pressure, indicating potential crystallin-
As pressure increased, enhancement of the Bragg peaks ity alterations in β-Li3PS4, such as lattice distortion owing

Fig. 2  The pressure dependence of X-ray total scattering for the and 100 MPa. c The intensity-normalized total scattering intensities
β-Li3PS4 crystal. a Total scattering intensities at 0, 3, 15, 30, 60, and at atmospheric pressure before and after pressurization
100 MPa. b The intensity-normalized total scattering intensities at 0

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 Journal of Solid State Electrochemistry

Table 1  Refined lattice constants of the β-Li3PS4 crystal obtained shows the refined lattice parameters obtained from the X-ray
through Rietveld analysis total scattering at 0 MPa before and after pressurization. It
Lattice constant/Å is well known that the lattice constant of crystal in the glass
(rate of change from 0 MPa/%) ceramics varies because the fraction of glass phase contained
a b c varies with the process [22]. However, this study qualitatively
confirmed the changes in the lattice constants before and
0 MPa 12.73 8.05 6.06 after pressurizations. Results, only the lattice parameter of
100 MPa 12.66 (− 0.5) 7.95 (− 1.3) 6.01 (− 0.9) the c-axis reverted to its initial value post-pressurization. In
0 MPa after pres- 12.76 (0.3) 8.00 (− 0.6) 6.06 (0.0) contrast, the lattice parameter of the a-axis increased, and that
surized release
of the b-axis decreased, suggesting a possible involvement
of anisotropic lattice parameter alteration in a-axis ordering.
Figure 3 shows the pressure dependence of the X-ray
to variations in lattice constants. Rietveld analysis used total scattering of g-Li3PS4, with a comparison between
the X-ray total scattering of the β-Li3PS4 crystal at 0 and the results at 0 and 120 MPa normalized by the intensity
100 MPa. The refined lattice constants and their correspond- of the second peak, as shown in Fig. 3a. Notably, as pres-
ing rates of change along the a-, b-, and c-axes are sum- sure increased, the first peak corresponding to the P–P dis-
marized in Table 1. Notably, the rates of change exhibited tance between P ­ S4 molecules shifted significantly toward
orientation-dependent variations, with the strain order being the higher angle side, indicating closer proximity of adja-
b > c > a. Figure 2c illustrates the X-ray total scattering of the cent ­PS4 molecules under pressure. Figure 4a shows the
β-Li3PS4 crystal at 0 MPa before and after pressurization, PDF of g-Li3PS4 at 0 and 120 MPa, where at 120 MPa, the
with intensity normalized to the 221 reflection, as depicted peak associated with the intermolecular correlation of ­PS4
in Fig. 2a. While their Bragg peak profiles appeared similar molecules at 7–10 Å shifted toward a shorter distance. Fig-
but not identical, indicating irreversible structural changes ures 3b and 4b show the X-ray total scattering and PDF of
owing to pressurization, post-pressurization, the intensities g-Li3PS4 at 0 MPa before and after pressurization, respec-
of Bragg peaks involving the a-axis, such as the 200, 210, tively. In contrast to the results for β-Li3PS4 crystals, no
400, and 401 reflections, were enhanced, suggesting promo- discernible difference was observed in g-Li3PS4 before and
tion of a-axis ordering under pressure. Additionally, Table 1 after pressurization, indicating that g-Li3PS4 does not retain

Fig. 3  The pressure depend-

ence of X-ray total scattering
for g-Li3PS4. a Total scattering
intensities at 0 and 100 MPa.
b Total scattering intensities at
atmospheric pressure before and
after pressurization

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Journal of Solid State Electrochemistry

Fig. 4  The pressure depend-

ence of the PDF for g-Li3PS4.
a PDFs at 0 and 100 MPa. b
PDFs at atmospheric pressure
before and after pressurization

the memory of pressurization and can reversibly recover its β-Li3PS4 crystals, their structural stability under compres-
original structure at 0 MPa. sion along each lattice vector was compared. Table 2 sum-
marizes the potential energies of uncompressed structures
against those achieved by shortening the lattice vectors by
Discussion 1% along the a-, b-, and c-axis orientations. The compres-
sion along the a-axis induces structural instability, whereas
Because the compression is conducted through powder compression along the b- and c-axes results in enhanced
molding, it is unclear to what extent local stresses are gen- stability owing to the decreased potential energy of L ­ i3PS4
erated in the solid electrolyte at various volume fractions. crystals. Consequently, compression is more readily facili-
In this study, however, we focused on the refinement of the tated along the b- and c-axis orientations than the a-axis.
Bragg peaks observed by X-ray diffraction. The changes in Figure 6 compares the PDFs derived from 1% shortening
lattice parameters refined through Rietveld analysis indicate of the a, b, and c axes of the β-Li3PS4 crystal. Notably,
anisotropic shrinkage of the crystal lattice in β-Li3PS4 upon this PDF was calculated under ideal conditions, exhibiting
pressurization. Post-pressure release, the a-axis of β-Li3PS4 significantly higher real-space resolution than the PDF in
stretched more than its pre-pressurization state. Conversely, Fig. 4a. Variations in the PDF change with compression
g-Li3PS4 reverted to its original structure after pressuriza- along the a-, b-, and c-axes are evident. Typically, compres-
tion. The divergent pressure dependence observed in ­Li3PS4 sion shifts the PDF peak position toward the short-range
is ascribed to the anisotropy inherent in the β-Li3PS4 crys- region. However, specific shifts were observed: the peak at
tal. Figure 5 shows the unit cell (space group Pnma) of the 6.53 Å for a-axis compression, 7.07 Å for c-axis compres-
β-Li3PS4 crystal. To elucidate the compression behavior of sion, and both peaks for b-axis compression, indicating that

Fig. 5  The unit cell of the

β-Li3PS4 crystal (space group
Pnma). The arrows indicate
the nearest P–P distances along
the a-, b-, and c-axes. Note the
slight shift of the neighboring
P atom along the a-axis in the
b-axis direction

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 Journal of Solid State Electrochemistry

Table 2  Potential energy of Structure Original a-axis comp. b-axis comp. c-axis
the optimized and compressed comp.
β-Li3PS4 crystal
Potential energy/eV −146.1866 −146.1819 −146.2024 −146.2103

Fig. 6  A comparison of PDF

shortening along the a-, b-, and
c-axes by 1% for the β-Li3PS4
crystal. The dotted lines repre-
sent the peak positions of the
original crystal structure

b-axis compression primarily influences the PDF peak shift. Consequently, ­PS4 molecules adopted an aligned configu-
Under b-axis compression of β-Li3PS4 crystals, ­PS4 mol- ration along the a-axis, resulting in an anisotropic change
ecules in the unit cell undergo slight rearrangement, lead- of lattice parameters post-pressure application. This study
ing to lattice parameter expansion while maintaining ­PS4 underscores the potential for irreversible transformation of
molecule correlation. However, the b-axis lattice parameter crystalline solid-state electrolytes from a metastable to a dif-
does not revert owing to changes in ­PS4 molecular coordi- ferent structure through pressure application, offering a novel
nates, while the a-axis expands concurrently. As depicted in approach for synthesizing metastable structures beyond con-
Fig. 5, the nearest P atom along the a-axis orientation shifts ventional heat treatment methods alone. Future research will
slightly in the b-axis direction, ultimately aligning closer to focus on elucidating the effects of structural changes associ-
the a-axis upon b-axis shortening. This displacement aligns ated with varied pressure conditions on battery performance
the ­PS4 molecule along the a-axis, prompting the extension parameters, such as ionic conductivity.
of the a-axis lattice parameter.
Supplementary Information The online version contains supplemen-
tary material available at https://d​ oi.o​ rg/1​ 0.1​ 007/s​ 10008-0​ 24-0​ 5889-4.
Conclusion
Author contribution All authors contributed to the study conception
and design. Material preparation was performed by A. Y., S. K., and
The atomic configuration response of L ­ i3PS4 under pressure
F. U. Data collection was performed by A. Y., S. K., H. Y., J. T., F. U.,
was investigated through structural analysis of β-Li3PS4 crys- and K. O. Data analysis were performed by all authors. The first draft
tals and g-Li3PS4 using in situ X-ray total scattering measure- of the manuscript was written by A. Y., S. K., S. H., F. U., and K. O.
ments with applied pressure, along with structural optimiza- and all authors commented on previous versions of the manuscript. All
authors read and approved the final manuscript.
tion for the compressed β-Li3PS4 crystal structure using DFT
calculations. Under a pressure of 100 MPa, both β-Li3PS4
Funding Synchrotron radiation experiments were performed with the
crystals and g-Li3PS4 exhibited a tendency for ­PS4 molecules approval of the Japan Synchrotron Radiation Research Institute (JASRI)
to approach each other. Notably, when pressure was applied (Proposal Nos. 2020A1702, 2020A1703, 2021A1267, 2021B1744,
to g-Li3PS4 and subsequently released, the observed X-ray 2022A1238, and 2022B1224). This work was partially supported by
JSPS KAKENHI (Grant Number JP19H05814) and the Green Tech-
total scattering and PDFs remained consistent with pre-com-
nologies of Excellence program (Grant Number JPMJGX23S5) of the
pression measurements. Conversely, in β-Li3PS4 crystals, dis- Japan Science and Technology Agency (GteX, JST).
crepancies were observed in the X-ray total scattering post-
pressure application and release, indicating pressure-induced Declarations
atomic rearrangement in the crystal structure. Rietveld anal-
ysis using X-ray total scattering confirmed pressurization- Competing interests The authors declare no competing interests.
induced shortening of the b-axis and stretching of the a-axis
in β-Li3PS4 crystals. DFT-based structural optimization was
conducted to elucidate the origin of the observed anisotropic References
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Journal of Solid State Electrochemistry

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