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At least 1,135 records · Page 63
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Preparation and characterization of novel foamed porous glass-ceramics

Foamed glass-ceramics without using foaming agent have been synthesized in a novel glass system of SrO-CaO-Al{sub 2}O{sub 3}-TiO{sub 2}-B{sub 2}O{sub 3}-SiO{sub 2}-P{sub 2}O{sub 5}-M{sub x}O{sub y} (where M = Ba, Mg, La, Ce and Ni) by a simple process of powder sintering. The glass and glass-ceramics are characterized by dilatometry, differential scanning calorimetry (DSC), heating stage microscopy (HSM), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), optical microscopy and Fourier transformed infrared spectroscopy (FTIR). All the glasses formed are amorphous and the glass transition temperature and dilatometric softening temperature of these glasses are found to be in the range 673–678 °C and 706–728 °C respectively. The glasses are highly stable as indicated by the DSC evaluated glass stability parameters of the range 195–240 °C. Quantitative sintering study of glass powder compacts revealed swelling in the samples with NiO and CeO{sub 2} corresponding to a geometry change of 75 and 108% around 900 °C respectively. With reference to this finding the glass powder compacts are heated to 900 °C and the foamed glass-ceramics are obtained. Characteristic crystalline silicate phases have been identified in the XRD studies and their microstructures are recorded by FESEM. Optical microscope study of the foamed samples revealed formation of bigger foamed cavity with residual pores in samples with NiO and CeO{sub 2} in comparison to samples with BaO, MgO and La{sub 2}O{sub 3}. The mean pore diameters of the samples with NiO and CeO{sub 2} are determined to be 43 and 32 μm, and their respective porosities are 2.34 and 1.82 cm{sup 3}/g respectively. Thus NiO and CeO{sub 2} are found to be very effective to obtain foamed glass-ceramics without using foaming agent by the viscous flow sintering of fine glass powder compacts along with the reduction of the respective polyvalent ions. - Highlights: • Synthesis of foamed porous glass-ceramics without foaming agent by sintering method • Only powder compact yielded foamed porous glass-ceramics but bulk glass did not. • Glasses containing NiO and CeO{sub 2} exhibited significant foaming efficiency. • Bloating of entrapped gas during viscous flow sintering is the origin of foaming. • Residual void created pores in the sintered glass-ceramics as evidenced in FESEM.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Understanding the effects of fabrication process on BaZr 0.9 Y 0.1 O 3– δ grain-boundary chemistry using atom probe tomography

Proton-conducting oxides, such as BaZr 0.9 Y 0.1 O 3–δ (BZY10), are receiving significant scientific attention for application in a variety of electrochemical applications. It has been shown that the synthesis route has a significant effect on the ionic behavior of these materials, especially the grain boundaries (GB). In this study, laser-pulsed atom probe tomography (APT) is used to characterize the GB chemistry of BZY10 samples prepared by four different methods: (1) spark plasma sintering (SPS), (2) conventional sintering followed by high-temperature annealing (HT), (3) conventional sintering with NiO used as a sintering aid (SSR-Ni), and (4) solid-state reactive sintering of oxide precursor powders with NiO as a reactive sintering aid (SSRS-Ni). Oxygen depletion (corresponding to oxygen vacancy accumulation) was observed at every GB in this study, consistent with the positive space-charge GB region commonly assigned to these materials. In contrast to the consistent trends associated with oxygen depletion, cation constituents showed varying segregation/depletion behaviors. The samples that used NiO revealed Ni preferentially segregating to the GB. The most common impurities in BZY10 are Al, Fe, Mg, Si, and Sr, all of which generally accumulate at GBs. In order to quantify these chemical trends, the APT method was optimized for this material supplemented with understanding from density functional theory (DFT). Finally, this APT study reveals the complexity of BZY10 GB chemistry and shows that even adjacent GBs in the same material can sometimes show surprisingly different GB chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

An Assessment of Additively Manufactured Bonded Permanent Magnets for a Distributed Wind Generator

In this paper, we examine and compare the performance of a generator design optimized using additively manufactured NdFeB-SmFeN in nylon-polymer-bonded permanent magnets (PMs) against a generator design with conventional NdFeB sintered PMs. To realize this, a commercially available 15-kW wind generator's rotor is re-optimized using both additively manufactured and sintered NdFeB magnets using simple geometric parameterization that allowed for two specific magnet shapes, namely, arc-shaped and crown-shaped designs. Results showed that for a similar generator performance, the designs with additively manufactured bonded PMs are more cost-competitive in terms of the estimated PM material cost and also have negligible eddy current magnet losses.

additive manufacturing↗
DOE OSTI2020

VTO FY20Q4 quarterly report

Project Objective.This project has three objectives: (1) tuning microstructures of 3D-printed SSE separators,(2) determining material and processing compatibilities with cathode printing,and (3)3D printing of sintering-free SSE separators.Project Impact.All-solid-state lithium batteries are difficult to process due to the brittleness of ceramic materials, poor solid-solid contact, and electrolyte-electrode stability issues. As a result, the energy and power density and also cycling stability are far from satisfying. This project will address fabrication difficulties by using state-of-the-art 3D-printing techniques that can introduce 3D interfaces and architectures to enhance solid-solid contact and reduce charge transfer resistance. Success will benefit the DOE by establishing the best manufacturing methods for ASSBsto achieve VTO goals on the performance of beyond Li-ion batteries. Approach.The project employs 3D-printing techniques to manufacture SSEs and related components for ASSBs. The team starts with direct ink writing (DIW) to develop ink recipes with desired rheological properties and explore post-sintering approaches to achieve high densification. In parallel with DIW3D printing, the team also explores other 3D printing options, such as projection microstereolithography (PuSL). Both sintering and sintering-free approaches can gain benefit from 3D printing and therefore will be investigated.Out-Year Goals.The team will determine particle sizes and morphologies as well as post-processing conditions that deliver good ionic conductivity and charge transfer properties of LLZTO separators. They will examine co-sintering of LLZTO/cathode and determine the effects of material, particle size, surface coating, and sintering conditions.Collaborations.Microstructures, ionic conductivities, and mechanical properties will be provided to the LLNL simulation team, led by PI B. Wood, for establishing and validating phase-field modeling methods.

36 MATERIALS SCIENCE↗
NASA NTRS1976

Improved toughness of silicon carbide

Impact energy absorbing layers (EALs) comprised of partially densified silicon carbide were formed in situ on fully sinterable silicon carbide substrates. After final sintering, duplex silicon carbide structures resulted which were comprised of a fully sintered, high density silicon carbide substrate or core, overlayed with an EAL of partially sintered silicon carbide integrally bonded to its core member. Thermal cycling tests proved such structures to be moderately resistant to oxidation and highly resistant to thermal shock stresses. The strength of the developed structures in some cases exceeded but essentially it remained the same as the fully sintered silicon carbide without the EAL. Ballistic impact tests indicated that substantial improvements in the toughness of sintered silicon carbide were achieved by the use of the partially densified silicon carbide EALs.

Palm, J. A.↗
NASA NTRS1991

Development of high Tc (greater than 110K) Bi, Tl and Y-based materials as superconducting circuit elements

This report is presented in two parts. Part 1 deals primarily with Bi-based materials and a small amount of work on a Y-based composition while Part 2 covers work on Tl-based materials. In Part 1, a reliable and reproducible process for producing bulk bismuth-based superconductors has been developed. It is noted however, that a percentage of the tapecast material experiences curling and fracturing after a 30 hour sintering period and is thus in need of further examination. The Bi-Sr-Ca-Cu-O (BSCCO) material has been characterized by critical temperature data, X-ray diffraction data, and surface morphology. In the case of T sub c, it is not critical to anneal the material. It appears that the BSCCO material has the possibility of producing a better grounding strap than that of the 123 material. Attempts to reproduce near room temperature superconductors in the Y-Ba-Cu-O system were unsuccessful. In Part 2, several methods of processing the high temperature superconductor Tl2Ba2Ca2Cu3O10 were investigated; i.e., different precursor compositions were sintered at various sintering times and temperatures. The highest superconductig temperature was found to be 117.8K when fired at 900 C for three hours. Higher sintering temperatures produced a melted sample which was nonsuperconducting at liquid nitrogen temperature. Also, a preliminary study found Li2O substitutions for copper appeared to increase the transition temperature and create fluxing action upon sintering. It was suggested that lower sintering temperatures might be obtained with lithium additions to produce reliable Tl2Ba2Ca2Cu3O10 processing methods.

Haertling, Gene H.↗
NASA NTRS2004

Processing Techniques Developed to Fabricate Lanthanum Titanate Piezoceramic Material for High-Temperature Smart Structures

Piezoelectric ceramic materials are potential candidates for use as actuators and sensors in intelligent gas turbine engines. For piezoceramics to be applied in gas turbine engines, they will have to be able to function in temperatures ranging from 1000 to 2500 F. However, the maximum use temperature for state-of-the-art piezoceramic materials is on the order of 300 to 400 F. Research activities have been initiated to develop high-temperature piezoceramic materials for gas turbine engine applications. Lanthanum titanate has been shown to have high-temperature piezoelectric properties with Curie temperatures of T(sub c) = 1500 C and use temperatures greater than 1000 C. However, the fabrication of lanthanum titanate poses serious challenges because of the very high sintering temperatures required for densification. Two different techniques have been developed at the NASA Glenn Research Center to fabricate dense lanthanum titanate piezoceramic material. In one approach, lower sintering temperatures were achieved by adding yttrium oxide to commercially available lanthanum titanate powder. Addition of only 0.1 mol% yttrium oxide lowered the sintering temperature by as much as 300 C, to just 1100 C, and dense lanthanum titanate was produced by pressure-assisted sintering. The second approach utilized the same commercially available powders but used an innovative sintering approach called differential sintering, which did not require any additive.

Goldsby, Jon C.↗
NASA NTRS2006

Pulsed Laser Deposition of High Temperature Protonic Films

Pulsed laser deposition has been used to fabricate nanostructured BaCe(0.85)Y(0.15)O3- sigma) films. Protonic conduction of fabricated BaCe(0.85)Y(0.15)O(3-sigma) films was compared to sintered BaCe(0.85)Y(0.15)O(3-sigma). Sintered samples and laser targets were prepared by sintering BaCe(0.85)Y(0.15)O(3-sigma) powders derived by solid state synthesis. Films 1 to 8 micron thick were deposited by KrF excimer laser on porous Al2O3 substrates. Thin films were fabricated at deposition temperatures of 700 to 950 C at O2 pressures up to 200 mTorr using laser pulse energies of 0.45 - 0.95 J. Fabricated films were characterized by X-ray diffraction, electron microscopy and electrical impedance spectroscopy. Single phase BaCe(0.85)Y(0.15)O(3-sigma) films with a columnar growth morphology are observed with preferred crystal growth along the [100] or [001] direction. Results indicate [100] growth dependence upon laser pulse energy. Electrical conductivity of bulk samples produced by solid state sintering and thin film samples were measured over a temperature range of 100 C to 900 C. Electrical conduction behavior was dependent upon film deposition temperature. Maximum conductivity occurs at deposition temperature of 900 oC; the electrical conductivity exceeds the sintered specimen. All other deposited films exhibit a lower electrical conductivity than the sintered specimen. Activation energy for electrical conduction showed dependence upon deposition temperature, it varied

Dynys, Fred W.↗
NASA NTRSDate not supplied

Print-Consistency and Process-Interaction for Inkjet-Printed Copper on Flexible Substrate

Printed electronics is a fastest growing and emerging technology that have shown much potential in several industries including automotive, wearables, healthcare, and aerospace. Its applications can be found not only in flexible but also in large area electronics. The technology provides an effective and convenient method to additively deposit conductive and insulating materials on any type of substrate. Comparing with traditional manufacturing processes, which involves chemical etching, this technology also comes to be relatively environmental friendly. Despite its status, it is not without its challenges. Starting from the material being compatible in the printer equipment to the point of achieving fine resolutions, and with excellent properties are some of the challenges that printed electronics face. Among the myriad of printing technologies such as Aerosol Jet, micro-dispensing, gravure printing, screen printing, Inkjet printing, Inkjet has gained much attention due to its low-cost, low material consumption, and roll-to-roll capability for mass manufacturing. The technology has been widely used in home and office, but recently gained interest in printed electronics in a research and development setting. Conductive materials used in Inkjet printing generally comprises of metal Nanoparticles that need to be thermally sintered for it to be conductive. The preferred metal of choice has been mostly silver due to its excellent electrical properties and ease in sintering. However, silver comes to be expensive than its counterpart copper. Since copper is prone to oxidation, much focus has been given towards photonic sintering that involves sudden burst of pulsed light at certain energy to sinter the copper Nanoparticles. With this technique, only the printed material gets sintered in a matter of seconds without having a great impact on its substrate, due to which it is also preferred in low temperature applications. With all the knowledge, there is still a large gap in the process side with copper where it is important to look how the print process affects the resolution of the print along with the effect of post-print processes on electrical and mechanical properties. In this paper, a copper Inkjet ink is utilized for understanding the effect of Inkjet print parameters on the ejected droplet and its resolution. Post-print process is also quantified using a photonic sintering equipment for excellent electrical and mechanical properties. To demonstrate the complete process, commercial-off-the-shelf components will also be mounted on the additively printed pads via Inkjet. Statistically, control charting technique will be utilized to understand the capability of the Inkjet process.

printed electronics↗
NASA NTRSDate not supplied

Ceramic Heat Pipe for Thermal Management of a High Frequency Inductor

As the power density of electric machines and power electronics continues to increase to meet the demands of more electric aircraft, the thermal management of these devices becomes increasingly important. Ideally, the thermal management solution of the device should have high thermal conductivity and be electrically insulating so that it can be directly integrated with the device in question. Technical ceramics are a class of materials that meet these two requirements. Direct liquid cooling by submerging electric components in a dielectric fluid is an alternate option, but adds system complexity and may incur pumping loss. In this work, the thermal management solution for a high frequency inductor is presented. A conventional wicked heat pipe is designed that is made from a solid ceramic case with a sintered ceramic wick. This heat pipe can provide structural support for the core and windings and is electrically insulating, so it does not incur any additional eddy current losses from the high frequency magnetic fields. It does not require additional pumping power, because conventional wicked heat pipes are passive devices. In this paper, the manufacturing process of the ceramic heat pipe is also presented. It is shown that the sintering of large diameter spherical ceramic particles is difficult due to their high specific surface area and low surface free energy. To overcome this difficulty, a flux material was used to initiate liquid phase sintering. The results of the sintering trials show that for the 120 μm diameter α-Al2O3powder selected for the wick, the combination of 1650°C sintering temperature and the addition of 5 wt% talc sintered the porous matrix together sufficiently for use as a heat pipe wic

High-frequency Inductor↗
NASA NTRSDate not supplied

Ceramic Heat Pipe for Thermal Management of a High Frequency Inductor

As the power density of electric machines and power electronics continues to increase to meet the demands of more electric aircraft, the thermal management of these devices becomes increasingly important. Ideally, the thermal management solution of the device should have high thermal conductivity and be electrically insulating so that it can be directly integrated with the device in question. Technical ceramics are a class of materials that meet these two requirements. Direct liquid cooling by submerging electric components in a dielectric fluid is an alternate option, but adds system complexity and may incur pumping loss. In this work, the thermal management solution for a high frequency inductor is presented. A conventional wicked heat pipe is designed that is made from a solid ceramic case with a sintered ceramic wick. This heat pipe can provide structural support for the core and windings and is electrically insulating, so it does not incur any additional eddy current losses from the high frequency magnetic fields. It does not require additional pumping power, because conventional wicked heat pipes are passive devices. In this paper, the manufacturing process of the ceramic heat pipe is also presented. It is shown that the sintering of large diameter spherical ceramic particles is difficult due to their high specific surface area and low surface free energy. To overcome this difficulty, a flux material was used to initiate liquid phase sintering. The results of the sintering trials show that for the 120 μm diameter α-Al2O3 powder selected for the wick, the combination of 1650°C sintering temperature and the addition of 5 wt% talc sintered the porous matrix together sufficiently for use as a heat pipe wick.

High frequency inductor↗
DOE OSTI2020

Tape casting and characterizations of MgO ceramics

Herein we report a high density MgO ceramic substrate produced by the tape casting technology. The tape casting formulation and process produced a uniform tape free of cracking. Y 2 O 3 and SiO 2 were used as the sintering aid for the pressureless sintering of the green tape. X-ray diffraction phase identification indicates that MgO is the main phase, while both Y 2 O 3 and SiO 2 sintering aids react with MgO to form MgY 4 Si 3 O 13 as the second phase. Liquid phase sintering occurs in the temperature range from 1030°C to ~1500°C, which is confirmed by the simultaneous Thermal Gravitation Analysis/ Differential Scanning Calorimeter (TGA/DSC) and the percent linear shrinkage and densification. A 96.5% theoretical density was achieved by presureless sintering at 1650°C for 2 hours, which was further increased to a fully dense structure using hotisostatic- pressing(HIP) at 1650°C and 207 MPa in argon. Scanning electron microscopy (SEM) and energy dispersive(EDS) spectroscopic analysis on the HIP’ed sample show that MgY 4 Si 3 O 13 is located at the MgO grain boundary and the sample has a fully dense structure. The refractive indices and extinction coefficient were measured on the HIP’ed sample along with thermal properties and dielectric properties. Thermal diffusivity and heat capacity were measured to calculate the thermal conductivity.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Influence of Ba Substitutions on Microstructure and Magnetic Properties of La–Ca–Co System Permanent Ferrite

La{sub 0.6}Ca{sub 0.4−x}Ba{sub x}O⋅n/2(Fe{sub 1−y}Co{sub y}){sub 2}O{sub 3}(x = 0, 0.05, 0.1, 0.15 and 0.2) permanent ferrite materials were prepared by ceramic technique. The topography and the structure were characterized by scanning electron microscopy (SEM) and x-ray diffraction (XRD), respectively. The magnetic properties were measured using vibrating sample magnetometer (VSM) and digital magnetometer. Single M-phase and flake-like grains were obtained for samples without Ba substitution(x = 0), and the magnetic properties of the pre-sintering La–Ca–Co ferrite were as follows: B{sub r} = 440 mT, H{sub cb} = 296 kA/m, H{sub cj} = 426 kA/m, (BH){sub max} = 36.6 kJ/m{sup 3} and H{sub k}/H{sub cj} = 0.83. When Ca was substituted by Ba, pre-sintered powder presents single M-phase structure and close three-dimensional size of grains, resulting in an improved rectangle ratio of sintered magnet. The rectangle ratio of sintered magnet reaches a maximum of 0.93 when x = 0.1. By optimizing process parameters, M-type La–Ca–Ba–Co sintered magnet was prepared with B{sub r} = 445 mT, H{sub cb} = 337 kA/m, H{sub cj} = 420 kA/m, (BH){sub max} = 38.6 kJ/m{sup 3} and H{sub k}/H{sub cj} = 0.95.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Microstructure evolution during binder jet additive manufacturing of H13 tool steel

H13 is one of the most used tool steels for both hot and cold work tooling applications. Binder jet additive manufacturing offers the potential to deposit complex tools at scale due to larger powder bed sizes and faster deposition rates. However, to date there is no published literature on the sintering of H13 to full densification. Here, we discuss the pressureless sintering of binder jet AM H13 steel to full densification via supersolidus liquid phase sintering (SLPS) while presenting appropriate process windows (1360 °C – 1380 °C) for densification without distortion. The process windows have been rationalized based on thermodynamic calculations of liquid volume fractions with temperature. We show that higher binder saturation results in higher carbon retention and subsequently early liquid formation that can initiate the sintering process at lower temperatures. We report abnormal grain growth during sintering and found that the solidification phase transformations play a critical role on microstructural evolution and must be considered to accurately model the kinetics of SLPS.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Tuning transition metal nanoparticles on a non-traditional support via experimental design

The ability to control metal nanoparticle size and morphology on supported catalysts is crucial for optimizing catalytic performance in targeted applications. Here, this work presents a systematic approach for tuning Ni particle and crystallite size on an unconventional, low-porosity silica fume support through select thermal treatments. The catalyst was synthesized via the deposition of nickelocene onto silica fume, resulting in well-dispersed Ni nanoparticles. A face-centered central composite design was employed to systematically assess the effects of time, temperature, and sintering gas environment on metal particle growth. The results demonstrate that the sintering gas environment is the primary factor governing particle and crystallite evolution, with temperature as the next most significant influence. Nickel nanoparticles sintered at temperatures of 650 °C and above under inert conditions exhibited substantial growth and polycrystalline structures, whereas samples treated in oxidative environments formed NiO, restricting particle mobility. Minimally oxidative (500 ppm O₂) environments facilitated rapid sintering while effectively removing residual ligands from the one-step nickelocene deposition process. Extensive structural characterization via a combination of scanning transmission electron microscopy, X-ray diffraction, hydrogen temperature programmed reduction, and small-angle X-ray scattering revealed that oxidative treatments enhanced metal-support interactions, as evidenced by increased reduction temperatures and narrower particle size distributions. These findings establish quantitative relationships between sintering parameters and Ni nanoparticle characteristics, providing a framework for rational catalyst design through controlled thermal treatments. This methodology is broadly applicable to other catalytic systems and provides a quantitative foundation for catalyst design.

CVD↗
DOE OSTI2015

Relating adatom emission to improved durability of Pt-Pd diesel oxidation catalysts

Sintering of nanoparticles is an important contributor to loss of activity in heterogeneous catalysts, such as those used for controlling harmful emissions from automobiles. But mechanistic details, such as the rates of atom emission or the nature of the mobile species, remain poorly understood. Herein we report a novel approach that allows direct measurement of atom emission from nanoparticles. We use model catalyst samples and a novel reactor that allows the same region of the sample to be observed after short-term heat treatments (seconds) under conditions relevant to diesel oxidation catalysts (DOCs). Monometallic Pd is very stable and does not sinter when heated in air (T ≤ 800 °C). Pt sinters readily in air, and at high temperatures (≥800 °C) mobile Pt species emitted to the vapor phase cause the formation of large, faceted particles. In Pt–Pd nanoparticles, Pd slows the rate of emission of atoms to the vapor phase due to the formation of an alloy. However, the role of Pd in Pt DOCs in air is quite complex: at low temperatures, Pt enhances the rate of Pd sintering (which otherwise would be stable as an oxide), while at higher temperature Pd helps to slow the rate of Pt sintering. DFT calculations show that the barrier for atom emission to the vapor phase is much greater than the barrier for emitting atoms to the support. Thus, vapor-phase transport becomes significant only at high temperatures while diffusion of adatoms on the support dominates at lower temperatures.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2025

Densification, microstructure, and mechanical properties of Mo–30W alloys fabricated from conditioned powders

Refractory alloys, such as molybdenum-based systems, are attracting growing interest for applications in extreme environments, such as in the nuclear and aerospace industries. Recent advances in sintering technologies, coupled with mechanical alloying, have enabled the tailored design of these alloys by leveraging powder characteristics to control final microstructures and mechanical properties. In this study, Mo-30W alloys were fabricated using electric field-assisted sintering (EFAS) from ball-milled powders with and without hydrogen treatment to investigate the influence of surface oxides on material properties and sintering behavior. The results revealed that samples processed from as-ball-milled powder contained a high density of oxides within the microstructure, whereas oxide presence was significantly reduced in samples fabricated from hydrogen-treated powders. Interestingly, the two powder types led to opposite trends in grain size distribution: samples from untreated powders exhibited grain refinement from sample periphery to the center, while samples from hydrogen-treated powders showed grain coarsening toward the center. This behavior is attributed to temperature gradients present during sintering due to electrical percolation pathway differences during Joule heating. The powder surface oxides may have influenced the temperature distribution and grain evolution. Microhardness profiles measured along both axial and thickness directions were consistent with the grain size distribution. Furthermore, oxide films on powder surfaces have delayed densification by hindering particle necking and atomic diffusion during sintering.

36 - MATERIALS SCIENCE↗
DOE OSTI2013

Hole mobility enhancement of Cu-deficient Cu{sub 1.75}Zn(Sn{sub 1−x}Al{sub x})Se{sub 4} bulks

Cu-deficient Cu{sub 1.75}ZnSn{sub 1−x}Al{sub x}Se{sub 4} (x=0–0.6) bulks were prepared by a liquid-phase reactive sintering method at 600 {sup °}C with soluble sintering aids of Sb{sub 2}S{sub 3} and Te. Defect chemistry was studied by measuring electrical properties of Al-doped CZTSe as a function of dopant concentration. Al-CZTSe pellets at x=0.4 with electrical conductivity of 57.2 S cm{sup −1} showed the highest hole mobility of 32.5 cm{sup 2} V{sup −1} s{sup −1}. The high mobility is mainly contributed from the low atomic scattering factor of Al. The high carrier concentration and slightly changed lattice parameter of Al-CZTSe are related to the types of its defects. - Graphical abstract: The controls in electrical properties and the changes in lattice parameters of Cu-deficient Cu{sub 2}ZnSnSe{sub 4} by doping Al{sup 3+} on the Sn{sup 4+} site. Display Omitted - Highlights: • Cu-deficient Cu{sub 1.75}Zn(Sn{sub 1−x}Al{sub x})Se{sub 4} was prepared by liquid-phase sintering at 600 °C. • Sintering aids of Sb{sub 2}S{sub 3} and Te were used for reactive sintering. • Al-CZTSe at x=0.4 showed the extremely high mobility of 32.5 cm{sup 2} V{sup −1} s{sup −1}. • Al-CZTSe reached large grains of 2−3 μm, while it was <1.0 μm for the undoped. • Electrical properties of Al-CZTSe pellets changed with the Al content.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗