Research Center for All-Solid-State Battery
Institute of Innovative Research, Tokyo Institute of Technology

Lab Tour

On this page, we will introduce you some of the main equipments we use in our laboratory. We also use neutron and radiation facilities as needed.

Material Synthesis Equipment

Electric Furnaces

There are tube furnaces and muffle furnaces to synthesize inorganic materials. We synthesize them at the reaction temperatures ranging from 100 to 1750 °C. All tube furnaces are equipped with a flange to control the synthesis atmosphere.

High Energy Ball Mill Equipment

To synthesize materials by solid phase method, reagents need to be ground and mixed. In particular, some materials cannot be synthesized without amorphization by mechanical mixing and mechanochemical reactions. For this reason, we have installed multiple ball mill equipment to ensure that experiments can proceed smoothly.

High Quality Thin Film Synthesis System

A laser ablation device is a synthesis device that is actively used to create epitaxial thin films, which are the materials of lithium batteries and fuel cells. The RHEED devices installed inside the chambers make it possible to monitor the conditions of each layer during the synthesis. One of film formation chambers is directly connected to an Ar-filled glove box, which makes it possible to create batteries without exposing the materials to the air. In our group, there are two laser oscillators and five film formation chambers.

Supttering Equipment

Magnetron sputtering systems (3 units) are used for the synthesis of electrodes and solid electrolyte membranes for thin film batteries. Two units are connected to glove boxes and one unit is connected to a laser ablation system via a load lock chamber. The system is designed for non-atmospheric exposure and continuous film formation. Since the system can be used for various thin film syntheses, it is in full operation.

High-Pressure Synthesis Equipment

The cubic-anvil type high-pressure apparatus is used to synthesize materials under high pressures of 30,000 to 70,000 atmospheres. 180, 250, and 400 ton units are in operation. There are many advantages, such as the ability to synthesize new materials that cannot be obtained by normal pressure synthesis, and the ability to complete the synthesis in a short time.

 

Glove Box

In solid-state battery materials research, glove boxes are essential to handle various materials with argon atmosphere. We have various type glove boxes to use different materials and for different purposes.

 

Structural Analysis Equipment

X-ray Diffraction

We have various powder X-ray diffractometers and thin film X-ray diffractometers. It is our routine work to identify the materials by X-rays after synthesis, because our main research theme is inorganic material synthesis. All of our work will be suspended in case any of the machines break down.
Four powder X-ray diffractometers are installed, two of which can perform measurements while controlling the temperature and atmosphere. There are two thin-film X-ray diffractometers, one with a Cu source and the other with a Mo source, and they are used for different purposes.

Electron Microscope

2 units of scanning electron microscopes (SEM/EDX) are used to evaluate the morphology and mixing state, and compositional distribution of samples. As a composite material consisting of an active electrode and a solid electrolyte is used in all solid-state batteries, the SEM/EDX system has become indispensable to investigate whether the reaction area is sufficient. We have introduced instruments with different resolutions and use them together according to the sample to be observed. Batteries can be introduced directly into the vacuum chamber for SEM observation during charging and discharging.

Probe Microscope

2 units of scanning probe microscopes are used to investigate nanoscale morphology of epitaxial film surfaces. We evaluate whether the films have sufficient smoothness and uniformity as a model reaction field for interfacial reaction analyses. Recently, we have introduced a cross-sectional polisher, which enables us to evaluate the morphology and physical properties of pellet-type materials.

Raman Spectroscopy

The Raman spectrometer was introduced to investigate the local structure of materials, and when used in conjunction with X-ray diffraction measurements, it allows us to understand both the average and local structures of materials.

Particle Size Distribution Analyzer

We introduced this system to study the particle size of various materials. Understanding particle size distribution is very important because battery performance can vary tremendously depending on particle size and its distribution.

Physical Property Evaluation Equipment

Electrochemistry

We have electrochemical charge/discharge devices and potentio-galvanostat systems with AC impedance analyzer. They are very common equipment used in electrochemistry laboratories.

With many channels available, we evaluate the performance of materials and devices while controlling various parameters such as temperature, atmosphere, and pressure.

Low Temprature Impedance Measurment System

Sulfide solid electrolytes have low grain-boundary resistance, so it is difficult to separate the bulk contribution from the impedance spectra. To solve this problem, we combine an impedance analyzer that can measure from a high frequency of 100 MHz with a cryostat to perform precise measurements in the low temperature range and separate the resistance components.

SQUID

A SQUID is used to evaluate the magnetism of materials. Because of the high cost of liquid helium, it is painful that we have to limit the usage of this device.

TG-DTA

Differential thermal analysis is used to investigate the phase transition behavior of crystals, which is one of the basic information of material synthesis, by observing the heat flow and the weight changes of materials when the temperature goes up and down.  By viewing the data in combination with high temperature X-ray diffraction measurements, we can deepen our understanding of the behavior for developed materials.

Joint-Use Facilities

SPring8

SPring-8 is a large synchrotron radiation facility, which delivers the most powerful synchrotron radiation currently available. We use several beamlines several times a year.
・Large-scale synchrotron radiation facility SPring-8  BL14B1, BL22XU Kappa-type multi-axis diffractometer.
・Direct observation of the interfacial structure is extremely important for elucidating the electrochemical reactions in batteries.  Surface diffraction and reflectivity measurements are used to investigate changes in crystal structure and morphology.

・Large-scale synchrotron radiation facility SPring-8  BL02B2, BL19B2 Powder X-ray diffractometer.
・Understanding the crystal structure is essential for materials development. High intensity X-ray diffraction data using monochromatic X-ray can be analyzed for revealing the detailed crystal structure, which shows important guidelines for the next material design.

・Large-scale synchrotron radiation facility SPring-8 BL28XU Hard X-ray photoelectron spectrometer
・By understanding the electronic structure of materials and interfaces, we can elucidate reaction mechanisms and obtain guidelines for improving performance. Since hard X-rays can provide information on buried interfaces, we are conducting experiments to directly observe the changes of electronic structure at the electrochemical interfaces during charging and discharging.

J-PARC

・J-Parc is a neutron facility (J-PARC) with TOF-type powder diffractometer [Super HRPD(BL08), SPICA (BL09), iMateria (BL20)] and Soft Interface Analyzer [SOFIA (BL16)]. With a neutron diffractometer, the locations and the amount of Li and H in crystals can be identified, while they are difficult to be investigated by X-ray.

Tokyo Institute of Technology the Institute of Innovate Research (IIR) School of Materials and
Chemical Technology
Department of Chemical Science
and Engineering
FACES Tokyo Tech Researchers
Ryoji Kanno
The Electrochemical Society of Japan The Ceramic Society of Japan The Chemical Society of Japan Solid State Ionics of Japan THE COMMITTEE OF
BATTERY TECHNOLOGY
Japan Society of Powder and
Powder Metallurgy
化学電池材料研究会