Improved length of calcium sulfate crystal seeds and whiskers via ball milling and hydration treatment

Elucidating the effect of growth periods on the quality of calcium sulfate whiskers(CSWs)prepared from calcium sulfate dihydrate(DH)is imperative.Herein,crystal seeds and whiskers were prepared from DH in a water–glycerol system.Longer whiskers were obtained from crystal seeds prepared via hydration of DH for 30 s than via ball milling for 5 min followed by hydration for 20 s.The attachment of cetyltrimethyl ammonium bromide and glycerol additives to the whisker tops promoted whisker growth.The whisker sponges exhibited good thermal barrier properties and compression cycle stability.

Morphology and optical properties of tetrapod-like zinc oxide whiskers synthesized via equilibrium gas expanding method

The zinc oxide whiskers were synthesized by the equilibrium gas expanding method at the temperature of 700 C with metallic zinc as the main raw material without any catalysts. The effects of the growth time on microstructure and photoluminescence properties were investigated. The results show that the as-grown samples are composed of uniform tetrapod-like ZnO whiskers. The length and diameter of the arms of the tetrapod-like ZnO whiskers increase obviously with the increase of the growth time. The strong single ultraviolet （UV） emission centering 385-391 nm without any accompanying deep-level emission is observed in the room temperature photoluminescence （PL） spectra of the whiskers. The intensity of UV emission increases markedly with the increase of growth time.

Effect of SiC whiskers on the oxidation protective properties of SiC coatings for carbon/carbon composites

In order to effectively employ the unique high temperature mechanical properties of carbon/carbon composite substrates, SiC coatings reinforced by SiC whiskers were prepared by pack cementation method. The effect of SiC whiskers on the oxidation resistance properties of the single-layer coating and double-layer coating was investigated. SiC whiskers in the single-layer SiC coating have little effect on the anti-oxidation property but obviously improve the thermal shock property. The double-layer coating with inner-layer reinforced coating exhibits more perfect anti-oxidation ability than the double-layer coating with SiC inner-layer coating.

Preparation of Mullite Whiskers and Their Enhancement Effect on Ceramic Matrix Composites

Mullite whiskers were facilely prepared by sintering kyanite at high temperature, with the addition of AlF3·3H20. The as-prepared whiskers have been characterized systematically in terms of phase composition, morphology, and structure. Results showed that the morphology and size of mullite whiskers were strongly depended on the content of AlF3·3H20 and sintering temperature. At temperatures in the range of 1 100 to 1 500 ℃ with 4 wt% addition of AlF3·3H20, the well-shaped mullite whiskers were obtained. For an instance, the mullite whiskers with 5-10 μm in length and 0.1-0.2 μm in cross-section could be formed at 1 400 ℃, with 4 wt% addition of A1F3·3H20. Moreover, results showed that the addition of mullite whiskers into ceramic matrix enhanced its fracture toughness significantly.

Preparation, Characterization, and Formation Mechanism of Calcium Sulfate Hemihydrate Whiskers

Calcium sulfate hemihydrate whiskers were synthesized successfully via one-step hydrothermal crystallization method using phosphogypsum at 130 °C for 240 min with an initial slurry mass fraction of 2.5 wt%. The phase compositions, microstructures, thermal properties and molecular structures of asprepared samples were analyzed by XRD, ESEM, EDS, TG-DTA, and FT-IR. The influence of raw materials’ ball-milling time on the morphologies of whiskers was investigated. The effects of impurities on crystallization morphologies and length to diameter ratio(L/D) of calcium sulfate hemihydrate whiskers were studied. The results indicated that the calcium sulfate dihydrate crystalline could be translated directly into fibrous calcium sulfate hemihydrate whiskers. It was beneficial to form fine fiber structure when the ball-milling time of the raw material was 15 min. Aspect ratio of calcium sulfate hemihydrate whiskers decreased with increasing content of impurities. Moreover, the relative growth mechanism of whisker crystals via one-step hydrothermal crystallization method was discussed in detail.

Photocatalytic performance of K2Ti6O13 whiskers to H2 evolution and CO2 photo-reduction

K2Ti6O13 whiskers were synthesized by conventional sol-gel method, sono-chemical assisted and microwave assisted sol-gel method in order to obtain catalysts with different particle sizes and to modify their optical, textural and electrochemical properties. These modifications improved their photocatalytic activity for H2 evolution and CO2 photo-reduction. Long K2Ti6O13 whiskers prepared by ultrasound assisted sol-gel method are the most active photocatalysts for the hydrogen evolution reaction using pure water as reactant (U-SG, 10,065 μmol g^-1). In contrast, an opposite behavior was observed using a mixture of ethanol-water, where the highest activity was achieved by the shortest and less crystalline K2Ti6O13 whiskers (C-SG, 3,2871 μmol g^-1). In case of CO2 photo-reduction, long whiskers that were also prepared by the sono-chemical assisted sol-gel method were the most active to transform CO2 to formaldehyde, methane, methanol and hydrogen. The EFB value of this catalyst is located very close to the potential for formaldehyde production and favors the selectivity to this organic product.

GROWTH MECHANISM OF TiC WHISKERS PREMRED BY A MODIFIED CHEMICAL VAPOR DEPOSITION METHOD

High quality TiC whiskers have been prepared by a modified chemical vapor deposition (CVD) method using TiCl4 and CH4 as reactant gases and Ni as substrate. The deposition temperature and gas flow mies have ampreciable effect on the whisker growth.The whisker orientations and morphology are determined by X-my diffraction (XRD),scanning electron micmpmph (SEM) and transmission electron microgmph (TEM).In addition to the spherical tips, spiral growth microsteps and obvious terraces are observed at the tips and side faces of whiskers in the present eoperiment. The whiskers grow mostly along (100) direction. The whisker growth mechanism is discussed in detail.

Wear properties of potassium titanate whiskers-reinforced Al-12Si alloy composites

Potassium titanate （K2O·6TIO2） whiskers-reinforced Al-12Si alloy composites were prepared by the squeeze casting technique. Wear properties of the composites were investigated by pin-on-disc tests under dry conditions. The experimental results showed that K20 ·6TiO2 whiskers can effectively reinforce the matrix alloy and improve the wear resistance of the composite when the volume fraction of whiskers is low at 10 vol%. However, the composites with a high volume fraction of whiskers showed lower wear resistance than the Al-12Si alloy. The main wear mechanism of the composites is clarified as de-lamination and abrasive wear.

IN SITU PROCESSING OF Al_(2)O_(3) WHISKERS REINFORCED Ti-Al INTERMETALLIC COMPOSITES

In situ Al2O3 whiskers reinforced Ti-Al intermetallic composites were fabricated at ~1200℃ by reaction sintering of cold-consolidated fillets consisting mainly of Ti, Al, and different additives. The phases and microstructures of the sintered composites were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS). The process of synthesis was investigated using differential thermal analysis (DTA). The effects of processing parameters and additives on the microstructures of the composites and the development of whisker were examined. It is found that the morphology of the whisker is strongly influenced by the additives, the exothermal reaction process, and the processing parameters.

Preparation of α-calcium sulfate hemihydrate whiskers with high aspect ratios in presence of a minor amount of CuCl_2·2H_2O

In order to produceα-calcium sulfate hemihydrate(α-CaSO4·0.5H2O)whiskers with high aspect ratios,a minor amount of CuCl2·2H2O was used as the modifying agent in the process of hydrothermal treatment of calcium sulfate dihydrate(CaSO4·2H2O)precursor.The presence of 2.60×10–3 mol/L CuCl2·2H2O resulted in the increase of the aspect ratios ofα-CaSO4·0.5H2O whiskers from 81 to 253.The preferential adsorption of Cu2+on the negative{110}and{100}facets ofα-CaSO4·0.5H2O crystal structures was confirmed by EDS and XPS.And ATR-FTIR demonstrated the ligand adsorption of Cu2+on the surface ofα-CaSO4·0.5H2O whiskers.The experimental results reveal that the whiskers with high aspect ratios are attributed to the adsorption of Cu2+,which promotes the 1-D growth ofα-CaSO4·0.5H2O whiskers along the c axis.

Synergistically Toughening Effect of SiC Whiskers and Nanoparticles in Al_2O_3-based Composite Ceramic Cutting Tool Material

In recent decades, many additives with different characteristics have been applied to strengthen and toughen Al2O3-based ceramic cutting tool materials. Among them, SiC whiskers and SiC nanoparticles showed excellent performance in improving the material properties. While no attempts have been made to add SiC whiskers and SiC nanoparticles together into the ceramic matrix and the synergistically toughening effects of them have not been studied. An Al2O3-SiCw-SiC np advanced ceramic cutting tool material is fabricated by adding both one-dimensional SiC whiskers and zero-dimensional SiC nanoparticles into the Al2O3 matrix with an effective dispersing and mixing process. The composites with 25 vol% SiC whiskers and 25 vol% SiC nanoparticles alone are also investegated for comparison purposes. Results show that the Al2O3-SiCw-SiCnp composite with both 20 vo1% SiC whiskers and 5 vol% SiC nanoparticles additives have much improved mechanical properties. The flexural strength of Al2O3-SiCw-SiCnp is 730＋ 95 MPa and fracture toughness is 5.6 ± 0.6 MPa.m1/2. The toughening and strengthening mechanisms of SiC whiskers and nanoparticles are studied when they are added either individually or in combination. It is indicated that when SiC whiskers and nanoparticles are added together, the grains are further refined and homogenized, so that the microstructure and fracture mode ratio is modified. The SiC nanoparticles are found helpful to enhance the toughening effects of the SiC whiskers. The proposed research helps to enrich the types of ceramic cutting tool and is benefit to expand the application range of ceramic cutting tool.

Rigid polyurethane foam reinforced with cellulosewhiskers: Synthesis and characterization

A novel nanocomposite of rigid polyurethane foam was prepared by the polymerization of a sucrose-based polyol, a glycerol-based polyol and polymeric methylene diphenyl diisocyanate in the presence of cellulose whiskers. The cell morphology of the resulting foams was examined by scanning electron microscopy which showed both the pure foam and the nanocomposite foam had homogeneous cell dispersion and uniform cell size of approximately 200 μm. Analysis of the foams by Fourier transform infrared(FT-IR) spectroscopy indicated that both samples exhibited signals attributed to the polyurethane including the NH stretching and bending vibrations at 3320 cm^(-1) and 1530 cm^(-1), the OC=O vibration at 1730 cm^(-1) and the CO-NH vibration at 1600 cm^(-1). FT-IR analysis of the nanocomposite indicated that cellulose whiskers were crosslinked with the polyurethane matrix as the signal intensity of the OH stretch at 3500 cm^(-1) was significantly reduced in comparison to the spectral data acquired for a control sample prepared from the pure polyurethane foam mixed with cellulose whiskers. According to ASTM standard testing procedures, the tensile modulus, tensile strength and yield strength of the nanocomposite foam were found to be improved by 36.8%, 13.8% and 15.2%, and the compressive modulus and strength were enhanced by 179.9% and 143.4%, respectively. Dynamic mechanical analysis results testified the improvements of mechanical properties and showed a better thermal stability of the nanocomposite foam.

Synthesis and characteristics of SiC whiskers with "rosary bead" morphology

SiC whiskers with "rosary bead" morphology were synthesized using suitable silicon source and carbon source through solid reaction at the temperature above 1537 K. The diameter and length of the SiC whiskers were about 0.1-1.0 μm and 20-100 μm, respectively. The largest diameter of their enlarged ends of the whiskers was about 0.2-1.0μm, and it gradually and smoothly decreased to the size of the plain part of the whiskers. The results of X-ray diffraction analysis show that the crystalline structure of the obtained SiC whiskers is β-SiC. It is considered that the SiC whiskers grow via a vapor-solid mechanism.

Synthesis of Mg_2B_2O_5 whiskers via coprecipitation and sintering process

Mg2B2O5 whiskers with high aspect ratio were synthesized by coprecipitation and sintering process using MgCl2-6H2O, H3BO3, and NaOH as raw materials and KCl as a flux. Their formation process was investigated by thermogravimetry and differential scanning calo- rimetry （TG-DSC）, X-ray diffraction （XRD）, and scanning electron microcopy （SEM）. It is found that the products synthesized at 832℃ are monoclinic Mg2B205 whiskers with a diameter of 200-400 nm and a length of 50-80 μm. Transmission electron microscopy （TEM） and selected area electron diffraction （SAED） analyses show that the whiskers obtained at 832℃ are single crystalline and grow along with the [010] direction. The growth mechanism of Mg2B2O5 whiskers was also presented.

Synthesis of potassium hexatitanate whiskers using hydrothermal method

High quality potassium hexatitanate whiskers were hydrothermally synthesized in one step under moderate temperature and pressure conditions. Effects of the titanium source and reaction conditions on the hydrothermal reaction rate, product phase component, and morphology of whiskers were investigated. The results show that the reactivity of hydrated titania, anatase TiO2, and rutile TiO2 with KOH decreases in turn, and with hydrated titania as titanium source, it is difficult to obtain potassium hexatitanate whiskers with good morphology. In contrast, uniform potassium hexatitanate whiskers with a length of 10-20 μm and a diameter of 200-700 nm were obtained using anatase TiO2 as titanium source. The investigation demonstrates that the initial KOH concentration, annealing temperature and time, molar ratio of K2O/TiO2, etc. significantly affect the morphology of the as-synthesized whiskers. The optimized synthesis condition is as follows： anatase as a titanium source 10 wt.% KOH solution; annealing temperature and time of 300℃ and 5 h, respectively; K2O/TiO2 molar ratio of 5, etc. A rhombic potassium hexatitanate was prepared under the optimum condition and the whisker grew along the [110] direction. The reaction mechanism was discussed.

Synthesis of ZnO whiskers via hydrothermal decomposition route

ZnO whiskers with a length of 30-40μm and a diameter of about 1μm were synthesized by co-precipitation of ZnSO 4 and Na2CO3 solution at room temperature followed by hydrothermal treatment of the as-prepared Zn5(CO3)2(OH)6 precursor at 160 ℃for 6 h.The increase of the initial solution pH promotes the hydrothermal conversion of the particulate Zn5(CO3)2(OH)6 to ZnO whiskers.The presence of minor amount of EDTA in the hydrothermal solution promotes the one dimensional growth of ZnO whiskers,leading to the formation of ZnO whiskers with a length of 50-60μm and a diameter of 1-2μm.

Fabrication and properties of aluminum silicate fibrous materials with in situ synthesized K2Ti6O13 whiskers

To improve their mechanical and thermal insulation properties, aluminum silicate fibrous materials with in situ synthesized K_2Ti_6O_(13) whiskers were prepared by firing a mixture of short aluminum silicate fibers and gel powders obtained from a sol–gel process. During the preparation process, the fiber surface was coated with K_2Ti_6O_(13) whiskers after the fibers were subjected to a heat treatment carried out at various temperatures. The effects of process parameters on the microstructure, compressive strength, and thermal conductivity were analyzed systematically. The results show that higher treatment temperatures and longer treatment durations promoted the development of K_2Ti_6O_(13) whiskers on the surface of aluminum silicate fibers; in addition, the intersection structure between whiskers modulated the morphology and volume of the multi-aperture structure among fibers, substantially increasing the fibers' compressive strength and reducing their heat conduction and convective heat transfer at high temperatures.

Removal and utilization of calcite existed in scheelite by preparation of calcium sulfate whiskers

In order to eliminate the effect of calcite associated with scheelite on the scheelite flotation, hydrochloric acid was used to dissolve the calcite, and the soaking solution was used to prepare CaSO_4 whiskers by hydrothermal reaction with sulfuric acid at ambient pressure. First, the condition experiments of preparing CaSO_4 whiskers by using CaCl_2 and H_2SO_4 were carried out to optimize reaction parameters of the crystallization process. The optimal conditions were: at 102 ℃ reaction temperature, 0,5 mol/L reactant concentration and 60 min reaction time. Then based on the condition experiments and considering keeping acid concentration stable for achieving HCl recycling, Calcium sulfate whiskers with the average diameter of 1.41 μm and the average aspect ratio of 109 were prepared by the soaking solution after evaporating to half of its volume and 1.0 mol/L H_2SO_4 at 102 ℃ for 60 min: After ion exchange processing,the filtrate could be used as HCl in the process of HCl dissolution.

Growth and Photoluminescence Properties of Tetrapod-Shaped ZnO Microcrystals-Whiskers and Microrods

Tetrapod-shaped ZnO microcrystals in forms of whiskers and microrods have been grown in the same crucible by thermal evaporation of Zn/C mixtures at a temperature of 930℃ in air without using any catalyst. The tetrapod-shaped ZnO microrods were capped by hexagonal pyramids. It is for the first time observed that the tetrapod-shaped ZnO whiskers and microrods have quite different morphologies, and this is believed to be a result of different growth behaviors associated with these two forms of ZnO microcrystals. The octa-twin model has been used to discuss their growth behaviors. Photoluminescence properties of these two forms of tetrapod-shaped ZnO microcrystals have been investigated using different excitation wavelengths. Both of the two forms of ZnO microcrystals showed strong green emission and weak ultraviolet emission behaviors. The excitation spectrum of the tetrapod-shaped ZnO whiskers showed a strong excitation peak at 395 nm, which was not observed for the tetrapod-shaped ZnO microrods.

Direct synthesis of single-phase α-CaSO4·0.5H2O whiskers from waste nitrate solution

Single-phaseα-CaSO4·0.5H2O whiskers were directly synthesized from waste Ca(NO3)2 solution using a hydrothermal method,and HNO3 was synchronously regenerated.The effects of reaction temperature and Ca^2+concentration on the phase composition and morphology of products were determined by X-ray diffraction and optical microscopy.On the basis of the experimental results,the formation diagram ofα-CaSO4·0.5H2O was plotted within the range of 5–35 g·L^-1 Ca^2+and 115°C–150°C.In addition,the conditions of the direct synthesis ofα-CaSO4·0.5H2O were determined.Well-crystallized,single-phaseα-CaSO4·0.5H2O whiskers with high aspect ratios(length,1785μm;diameter,10.63μm;aspect ratio,168)and HNO3(70.25 g·L^-1)were obtained at the optimal conditions of 25 g·L^-1 Ca^2+and 125°C.