This research introduces an innovative approach for evaluating the degree of densification of carbon nanotube (CNT) sheets produced through direct spinning and subsequently treated with organic solvent (specifically ethanol). Analysis of the morphological features of the CNT sheets from the FE-SEM image affirms that the sheet’s structure becomes more densified following the treatment. Based on this, the treated CNT sheet was comprehensively evaluated using Raman spectroscopy. The results indicate a downward shift in the G′ band, signifying the densification of the CNT sheet’s structure due to the C–C bond weakening by the cohesive force. Following ethanol treatment, the CNT sheet exhibited enhanced electrical conductivity and tensile strength, measuring approximately 1.7 × 105 S m− 1 and 138.7 MPa, respectively, a remarkable improvement of roughly 300% compared to the untreated CNT sheet. This study underscores the efficacy of Raman spectroscopy as a powerful tool for assessing the densification of CNT sheets.
Li1.5Al0.5Ti1.5(PO4)3 (LATP) is considered to be one of the promising solid-state electrolytes owing to its excellent chemical and thermal stability, wide potential range (~5.0 V), and high ionic conductivity (~10-4 S/cm). LATP powders are typically prepared via the sol-gel method by adding and mixing nitrate or alkoxide precursors with chelating agents. Here, the thermal properties, crystallinity, density, particle size, and distribution of LATP powders based on chelating agents (citric acid, acetylacetone, EDTA) are compared to find the optimal conditions for densely sintered LATP with high purity. In addition, the three types of LATP powders are utilized to prepare sintered solid electrolytes and observe the microstructure changes during the sintering process. The pyrolysis onset temperature and crystallization temperature of the powder samples are in the order AC-LATP > CA-LATP > ED-LATP, and the LATP powder utilizing citric acid exhibits the highest purity, as no secondary phase other than LiTi2PO4 phase is observed. LATP with citric acid and acetylacetone has a value close to the theoretical density (2.8 g/cm3) after sintering. In comparison, LATP with EDTA has a low sintered density (2.2 g/cm3) because of the generation of many pores after sintering.
The influence of MgO addition on the densification and microstructure of alumina (Al2O3) was studied. Compacted alumina specimens were manufactured using ball-milling and one-directional pressing followed by sintering at temperatures below 1700oC. Relative density, shrinkage, hardness, and microstructure were investigated using analytical tools such as FE-SEM, EDS, and XRD. When the MgO was added up to 5.0 wt% and sintered at 1500oC and 1600oC, the relative density exhibited an average value of 97% or more at both temperatures. The maximum density of 99.2% was with the addition of 0.5 wt% MgO at 1500oC. Meanwhile, the specimens showed significantly lower density values when sintered at 1400oC than at 1500oC and 1600oC owing to the relatively low sintering temperature. The hardness and shrinkage data also showed a similar trend in the change in density, implying that the addition of approximately 0.5 wt% MgO can promote the densification of Al2O3. Studying the microstructure confirmed the uniformity of the sintered alumina. These results can be used as basic compositional data for the development of MgOcontaining alumina as high-dielectric insulators.
A mixture of elemental Co50Si50 powders was subjected to mechanical alloying (MA) at room temperature to prepare a CoSi thermoelectric compound. Consolidation of the Co50Si50 mechanically alloyed powders was performed in a spark plasma sintering (SPS) machine using graphite dies up to 800 °C and 1,000 °C under 50 MPa. We have revealed that a nanocrystalline CoSi thermoelectric compound can be produced from a mixture of elemental Co50Si50 powders by mechanical alloying after 20 hours. The average grain size estimated from a Hall plot of the CoSi intermetallic compound prepared after 40 hours of MA was 65 nm. The degree of shrinkage of the consolidated samples during SPS became significant at about 450 °C. All of the compact bodies had a high relative density of more than 94 % with a metallic glare on the surface. X-ray diffraction data showed that the SPS compact produced by sintering mechanically alloyed powders for 40-hours up to 800 °C consisted of only nanocrystalline CoSi with a grain size of 110 nm.
Few studies have been performed on ZrB2- graphite platelet composite made by spark plasma sintering (SPS) technique. In this research, the influence of adding graphite platelets (Gp) with and without SiC on the fracture toughness of ZrB2 ceramic was studied. The ZrB2- 10Gp, ZrB2- 15Gp, ZrB2- 30SiC-10Gp, and ZrB2- 30SiC-15Gp specimens were sintered by the SPS method at the temperature of 1850 °C for 8 min. The fracture toughness and work of fracture (WOF) were evaluated using the Single-Edge Notched Beam (SENB) technique. It was found that the fracture toughness and WOF were improved by the alone and combined addition of Gp and SiC to the monolithic ZrB2. The maximum fracture toughness of 4.8 ± 0.1 MPa m1/ 2 was obtained for the ZrB2- 15Gp specimen. It seems that adding Gp alone was more effective in enhancing the fracture toughness of ZrB2 than the combined addition of Gp and SiC. While the addition of Gp and SiC simultaneously modified the densification behavior to reach full-densified samples.
In this study, a ZnS film of 8-mm thickness was prepared on graphite using a hot-wall-type CVD technique. The ZnS thick film was then hot isostatically pressed under different pressures (125–205 MPa) in an argon atmosphere. The effects of pressure were systematically studied in terms of crystallographic orientation, grain size, density, and transmittance during the HIP process. X-ray diffraction pattern analysis revealed that the preferred (111) orientation was well developed after a pressure of 80 MPa was applied during the HIP process. A high transmittance of 61.8% in HIPZnS was obtained under the optimal conditions (1010oC, 205MPa, 6 h) as compared with a range of approximately 10% for the CVD-ZnS thick film under a 550-nm wavelength. In addition, the main cause of the improvement in transmittance was determined to be the disappearance of the scattering factor due to grain growth and the increase in density.
The conversion of all carbon preforms to dense SiC by liquid infiltration can become a low-cost and reliable method to form SiC-Si composites of complex shape and high density. Reactive sintered silicon carbide (RBSC) is prepared by covering Si powder on top of 0.5-5.0 wt% Y2O3-added carbon preforms at 1,450 and 1,500°C for 2 hours; samples are analyzed to determine densification. Reactive sintering from the Y2O3-free carbon preform causes Si to be pushed to one side and cracking defects occur. However, when prepared from the Y2O3-added carbon preform, an SiC-Si composite in which Si is homogeneously distributed in the SiC matrix without cracking can be produced. Using the Si + C = SiC reaction, 3C and 6H of SiC, crystalline Si, and Y2O3 phases are detected by XRD analysis without the appearance of graphite. As the content of Y2O3 in the carbon preform increases, the prepared RBSC accelerates the SiC conversion reaction, increasing the density and decreasing the pores, resulting in densification. The dense RBSC obtained by reaction sintering at 1,500 oC for 2 hours from a carbon preform with 2.0 wt% Y2O3 added has 0.20% apparent porosity and 96.9% relative density.
YAG (Yttrium Aluminum Garnet, Y3Al5O12) has excellent plasma resistance and recently has been used as an alternative to Y2O3 as a chamber coating material in the semiconductor process. However, due to the presence of an impurity phase and difficulties in synthesis and densification, many studies on YAG are being conducted. In this study, YAG powder is synthesized by an organic-inorganic complex solution synthesis method using PVA polymer. The PVA solution is added to the sol in which the metal nitrate salts are dissolved, and the precursor is calcined into a porous and soft YAG powder. By controlling the molecular weight and the amount of PVA polymer, the effect on the particle size and particle shape of the synthesized YAG powder is evaluated. The sintering behavior of the YAG powder compact according to PVA type and grinding time is studied through an examination of its microstructure. Single phase YAG is synthesized at relatively low temperature of 1,000 ℃ and can be pulverized to sub-micron size by ball milling. In addition, sintered YAG with a relative density of about 98 % is obtained by sintering at 1,650 ℃.
In this paper, graphene-coated Al powders prepared by in situ reduction method were directly used for cold spraying, obtaining a graphene-reinforced Al matrix composite coating with more compact structure and better performance. Cross-sectional analysis revealed that compared with the pure Al powders, the graphene-coated Al powders were more severely deformed, and the resulting coating was denser and its porosity was reduced by over 80%. The hardness of the graphene-coated Al coating was increased by 40%, and its brine immersion time was prolonged by nearly three times. However, the graphene increases the pitting sensitivity of the Al coating; so, the enhanced corrosion resistance of the graphene-coated Al coating is mainly attributed to the improvement of its structure densification.
In this study, factors considered to be causes of promotion of densification of sintered pellets identified during phase change are reviewed. As a result, conclusions shown below are obtained for each factor. In order for MA powder to soften, a temperature of 1,000 K or higher is required. In order to confirm the temporary increase in density throughout the sintered pellet, the temperature rise due to heat during phase change was found not to have a significant effect. While examining the thermal expansion using the compressed powder, which stopped densification at a temperature below the MA powder itself, and the phase change temperature, no shrinkage phenomenon contributing to the promotion of densification is observed. The two types of powder made of Ti-silicide through heat treatment are densified only in the high temperature region of 1,000 K or more; it can be estimated that this is the effect of fine grain superplasticity. In the densification of the amorphous powder, the dependence of sintering pressure and the rate of temperature increase are shown. It is thought that the specific densification behavior identified during the phase change of the Ti-37.5 mol.%Si composition MA powder reviewed in this study is the result of the acceleration of the powder deformation by the phase change from non-equilibrium phase to equilibrium phase.
The objective of this study is to investigate the influence of powder shape and densification mechanism on the microstructure and mechanical properties of Ti-6Al-4V components. BE powders are uniaxially and isostatically pressed, and PA ones are injection molded because of their high strengths. The isostatically compacted samples exhibit a density of 80%, which is higher than those of other samples, because hydrostatic compression can lead to higher strain hardening. Owing to the higher green density, the density of BE-CS (97%) is found to be as high as that of other samples (BE-DS (95%) and P-S (94%)). Furthermore, we have found that BE powders can be consolidated by sintering densification and chemical homogenization, whereas PA ones can be consolidated only by simple densification. After sintering, BE-CS and P-S are hot isostatically pressed and BE-DS is hot forged to remove residual pores in the sintered samples. Apparent microstructural evolution is not observed in BE-CSH and P-SH. Moreover, BE-DSF exhibits significantly fine grains and high density of low-angle grain boundaries. Thus, these microstructures provide Ti-6Al-4V components with enhanced mechanical properties (tensile strength of 1179 MPa).
Infiltration is a popular technique used to produce valve seat rings and guides to create dense parts. In order to develop valve seat material with a good thermal conductivity and thermal expansion coefficient, Cu-infiltrated properties of sintered Fe-Co-M(M=Mo,Cr) alloy systems are studied. It is shown that the copper network that forms inside the steel alloy skeleton during infiltration enhances the thermal conductivity and thermal expansion coefficient of the steel alloy composite. The hard phase of the CoMoCr and the network precipitated FeCrC phase are distributed homogeneously as the infiltrated Cu phase increases. The increase in hardness of the alloy composite due to the increase of the Co, Ni, Cr, and Cu contents in Fe matrix by the infiltrated Cu amount increases. Using infiltration, the thermal conductivity and thermal expansion coefficient were increased to 29.5 W/mK and 15.9 um/moC, respectively, for tempered alloy composite.
Molybdenum (Mo) is one of the representative refractory metals for its high melting point, superior thermal conductivity, low density and low thermal expansion coefficient. However, due to its high melting point, it is necessary for Mo products to be fabricated at a high sintering temperature of over 1800-2000 oC. Because this process is expensive and inefficient, studies to improve sintering property of Mo have been researched actively. In this study, we fabricated Mo nanopowders to lower the sintering temperature of Mo and tried to consolidate the Mo nanopowders through ultra high pressure compaction. We first fabricated Mo nanopowders by a mechano-chemical process to increase the specific surface area of the Mo powders. This process includes a high-energy ball milling step and a reduction step in a hydrogen atmosphere. We compacted the Mo nanopowders with ultra high pressure by magnetic pulsed compaction (MPC) before pressureless sintering. Through this process, we were able to improve the green density of the Mo compacts by more than 20% and fabricate a high density Mo sintered body with more than a 95 % sintered density at relatively low temperature.
In this study, a thermal-gradient chemical vapor infiltration (TG-CVI) process was numerically studied in order to enhance the deposition uniformity within the preform. The computational fluid dynamics technique was used to solve the governing equations for heat transfer and gas flow during the TG-CVI process for two- and three-dimensional (2-D and 3-D) models. The temperature profiles in the 2-D and 3-D models showed good agreement with each other and with the experimental results. The densification process was investigated in a 2-D axisymmetric model. Computation results showed the distribution of the SiC deposition rate within the preform. The results also showed that using two-zone heater gave better deposition uniformity.
Recently, the material industry in the world has started appreciating the value of new materials that can overcome the limitation of steel material. In particular, new materials are expected to play a very important role in the future industry, demonstrating superior performance compared to steel in lightweight materials and ability to maintain in high temperature environments. Carbon materials have recently increased in value due to excellent physical properties such as high strength and ultra lightweight compared to steel. However, they have not overcome the limitation of productivity and price. The carbon materials are classified into various composites depending on the purpose of use and the performance required. Typical composites include carbon-glass, carbon-carbon, and carbon-plastic composites. Among them, carbon-carbon composite technology is a necessary technology in aviation and space, and can be manufactured with high investment cost and technology. In this paper, in order to find the optimal conditions to achieve productivity improvement and cost reduction of carbon material densification process, the correlation between each process parameters and results of densification is first analyzed. The main process parameters of the densification process are selected by analyzing the correlation results. And then a certain linear relationship between major process variables and density of carbon materials is derived by performing a regression analysis based on the historical production result data. Using the derived casualty, the optimal management range of major process variables is suggested. Effective process operation through optimal management of variables will have a great effect on productivity improvement and manufacturing cost reduction by shortening the lead time.
Selective laser melting (SLM) can produce a layer of a metal powder and then fabricate a three-dimensional structure by a layer-by-layer method. Each layer consists of several lines of molten metal. Laser parameters and thermal properties of the materials affect the geometric characteristics of the melt pool such as its height, depth, and width. The geometrical characteristics of the melt pool are determined herein by optical microscopy and three-dimensional bulk structures are fabricated to investigate the relationship between them. Powders of the commercially available Fe-based tool steel AISI H13 and Ni-based superalloy Inconel 738LC are used to investigate the effect of material properties. Only the scan speed is controlled to change the laser parameters. The laser power and hatch space are maintained throughout the study. Laser of a higher energy density is seen to melt a wider and deeper range of powder and substrate; however, it does not correspond with the most highly densified three-dimensional structure. H13 shows the highest density at a laser scan speed of 200 mm/s whereas Inconel 738LC shows the highest density at 600 mm/s.
In this study, the behavior of densification of copper powders during high-pressure torsion (HPT) at room temperature is investigated using the finite element method. The simulation results show that the center of the workpiece is the first to reach the true density of copper during the compressive stage because the pressure is higher at the center than the periphery. Subsequently, whole workpiece reaches true density after compression due to the high pressure. In addition, the effective strain is increased along the radius during torsional stage. After one rotation, the periphery shows that the effective strain is increased up to 25, which is extensive deformation. These high pressure and severe strain do not only play a key role in consolidation of copper powders but also make the matrix harder by grain refinement.
The prime objective of this research was to study the influence of hot-pressing pressure and matrix-to-reinforcement ratio on the densification of short-carbon-fiber-reinforced, randomly oriented carbon/carbon-composite. Secondary objectives included determination of the physical and mechanical properties of the resulting composite. The ‘hybrid carbon-fiberreinforced mesophase-pitch-derived carbon-matrix’ composite was fabricated by hot pressing. During hot pressing, pressure was varied from 5 to 20 MPa, and reinforcement wt% from 30 to 70. Densification of all the compacts was carried at low impregnation pressure with phenolic resin. The effect of the impregnation cycles was determined using measurements of microstructure and density. The results showed that effective densification strongly depended on the hot-pressing pressure and reinforcement wt%. Furthermore, results showed that compacts processed at lower hot-pressing pressure, and at higher reinforcement wt%, gained density gradually during three densification cycles and showed the symptoms of further gains with additional densification cycles. In contrast, samples that were hot-pressed at moderate pressure and at moderate reinforcement wt%, achieved maximum density within three densification cycles. Furthermore, examination of microstructure revealed the formation of cracks in samples processed at lower pressure and with low reinforcement wt%.
This study investigated the densification behavior of rhenium alloys including W-25 wt.%Re and Re-2W-1Ta (pure Re) during sintering. The dilatometry experiments were carried out to obtain the in-situ shrinkage in H2 atmo-sphere. The measured data was analyzed through shrinkage, strain rate and relative density, and then symmetricallytreated to construct the linearized form of master sintering curve (MSC) and MSC as a well-known and straightforwardapproach to describe the densification behavior during sintering. The densification behaviors for each material were ana-lyzed in many respects including apparent activation energy, densification parameter, and densification ratio. MSC witha minimal set of preliminary experiments can make the densification behavior to be characterized and predicted as wellas provide guideline to sinter cycle design. Considering the results of linearized form and MSC, it was confirmed thatthe W-25 wt.%Re compared to Pure Re is more easily densified at the relatively low temperature.
In order to increase the toughness of ZTA(zirconia toughened alumina) ceramics, the present study focused on rearrangement and densification of particles according to the particle size of the parent material. When rough alumina was used for production of ZTA, densification behavior was observed in the specimen sintered at a temperature over 1550˚C. However, it was found that the densification behavior was occurred in the specimen sintered at 1450˚C when fine alumina powder was used. High relative density exceeding 98% was obtained when fine alumina powder was mixed with 15 wt% of 3Y-TZP and sintered at 1600˚C. Also, a hardness of 1820.2 Hv was obtained when a specimen containing 10 wt% of 3Y-TZP was sintered at 1600˚C. In the case of 3Y-TZP containing rough alumina powder that had been sintered the hardness value was around 1720.3 Hv. It was predicted that an improved toughening effect in ZTA could be achieved by using finer alumina powder as the parent material.