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[Lihong Liu](https://orcid.org/0000-0002-8964-5512), [Jiguang Li](https://orcid.org/0000-0002-5625-7361), [Koji Morita](https://orcid.org/0000-0001-6040-7054), [Byung-Nam Kim](https://orcid.org/0000-0003-4302-462X), [Tohru S. Suzuki](https://orcid.org/0000-0001-9458-6863)

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[Enhanced optical properties of translucent YVO<sub>4</sub> ceramic fabricated by spark-plasma-sintering (SPS) via texture-controlled microstructure](https://mdr.nims.go.jp/datasets/458dc0e8-995b-429d-a4bd-02c41146e430)

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Enhanced optical properties of translucent YVO4 ceramic fabricated by spark-plasma-sintering (SPS) via texture-controlled microstructureResearch Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16976Enhanced optical properties of translucent YVO4ceramic fabricated by spark-plasma-sintering(SPS) via texture-controlled microstructureLIHONG LIU,1 JIGUANG LI,2 KOJI MORITA,2 BYUNG-NAM KIM,2 ANDTOHRU S. SUZUKI1,*1Optical Ceramics Group, Research Center for Electronic and Optical Materials, National Institute forMaterials Science, Tsukuba, Ibaraki 305-0047, Japan2Polycrystalline Optical Material Group, Research Center for Electronic and Optical Materials, NationalInstitute for Materials Science, Tsukuba, Ibaraki 305-0047, Japan*Suzuki.tohru@nims.go.jpAbstract: Achieving an (001) orientation-aligned structure in the YVO4 green bodies bycolloidal processing with a strong magnetic field can enhance the optical properties of translucentYVO4 ceramics fabricated by a spark-plasma-sintering (SPS) technique. YVO4 green bodies withorientation along the (001) direction are successfully attained from a well-dispersed and highlystable YVO4 slurry containing 15 vol% YVO4 nanopowders prepared at 1 wt% of dispersantunder a pH> 9. By designing the (001) texture of YVO4 with aligning the slip casting directionparallel to the magnetic field B during the slip casting, the YVO4 SPSed at a temperature ofT = 1300 °C gained much higher transmittance than that of non-textured random YVO4, indicatingthat controlling the microstructure by colloidal processing with a strong magnetic field is aneffective approach to improving the optical properties of YVO4 ceramics.© 2025 Optica Publishing Group under the terms of the Optica Open Access Publishing Agreement1. IntroductionYttrium-orthovanadate (YVO4), which crystallizes in a tetragonal structure and belongs to aspace group D4 h, is a highly versatile crystalline material widely used in diverse fields such aspolarization optics [1], phosphors [2], and laser host material [3]. In solid-state laser application,YVO4 is a very known transparent host material for the rare earth ions, such as Nd3+, fordeveloping micro-chip lasers with laser diode pumping due to its high absorption coefficient, highoptical transparency in the 400-5000 nm range, large emission cross section. These propertiesallow YVO4:Nd to achieve high optical efficiency even at small size, [4] which has driven interestin developing larger-sized YVO4:Nd crystals to support high-power, high-efficiency laser designs.However, the traditional single-crystal growth method for producing high quality and large-sizedcrystals is costly, and the process is complex and difficult to control. As an alternative approach,the fabrication of transparent YVO4:Nd laser ceramics offers a promising route to producinglarge-sized YVO4:Nd materials. Previously, YVO4:Nd was considered unsuitable for high-poweroperation because its thermal conductivity was thought to be only half that of Y3Al5O12:Nd(YAG:Nd) [5], and it was believed that highly Nd-doped YAG ceramics could replace YVO4:Ndin such applications. This perspective changed when Taira et al. [6] discovered that the thermalconductivity of c-cut YVO4 is higher than that of YAG. This breakthrough has since spurredthe development of large-sized YVO4 laser ceramics. However, fabricating a transparent YVO4ceramic is a big challenge because the birefringent scattering at the grain boundaries is large dueto the non-cubic crystal structure causing the large refractive index anisotropy between its crystalaxes. This scattering can lead to significant light losses and reduce the transparency and opticalquality of the material. To minimize light scattering losses in non-cubic structured materials,controlling microstructures through grain size and textured structures is a promising approach#538699 https://doi.org/10.1364/OE.538699Journal © 2025 Received 16 Aug 2024; revised 28 Dec 2024; accepted 3 Jan 2025; published 9 Apr 2025https://orcid.org/0000-0001-9458-6863https://doi.org/10.1364/OA_License_v2#VOR-OAhttps://crossmark.crossref.org/dialog/?doi=10.1364/OE.538699&amp;domain=pdf&amp;date_stamp=2025-04-09Research Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16977[7–12]. In addition to porosity, these microstructural factors have a significant impact on theoptical properties of materials [13,14]. However, achieving smaller grain sizes often requireslower temperature processing, which can make it difficult to obtain pore-free dense bulks foroptical applications.The textured structure has recently attracted many attentions for the non-cubic crystal ceramicsystems; the birefringent scattering at the grain boundaries can be reduced by aligning the crystalorientation of each grain. This method is particularly effective for non-cubic crystal ceramicsystems because they exhibit birefringent scattering at the grain boundaries, which can negativelyimpact their optical properties. As a fabrication process of the textured ceramics, severalapproaches have been developed; for example, templated grain growth (TGG), [15] hot-forging[16] and magnetic field alignment methods [17,18]. Among them, the texture controlling throughthe magnetic field alignment technique is one of the most widely utilized methods not onlyfor optical applications, but also for other fields of ceramic materials. Since template graingrowth can be limited by the quality of the templates and the precise control over the alignmentprocess. And the hot forging normally requires high temperatures and pressures that can introduceunwanted defects or stresses in the material, reducing the material quality. Whereas, the magneticfield alignment method is cost-effective, scalable, and easy to control over the above two methods.The principle of the magnetic field alignment process is as follows [19]. For the ceramics withanisotropic crystal structure, magnetic susceptibility is slightly different along different crystalaxes. The strong magnetic field can align the crystal axis of ceramic particles dispersed in slurryand the strong texture can be developed during subsequent sintering [19–21]. For the YVO4particles with a tetragonal crystal structure, since the magnetic susceptibility should be differentamong the axes, if the strong magnetic field is applied to the YVO4 slurry during slip castingprocessing, it is expected that the textured YVO4 bulk materials can be synthesized after sinteringto reduce the birefringent scattering loss at the grain boundaries.For achieving the homogenous textured-microstructures, it is important to control the nanopow-der slurry preparation to refrain from the agglomeration of fine particles. Colloidal techniqueis such a simple and cost-effective technique, which offers significant advantages to avoidagglomerates of fine particles by using electrostatic repulsive forces and/or steric stabilization.[7–10,22] During the colloidal processing, dispersant, solvent, pH adjustment and viscosityshould be controlled. Among them, the dispersant will help to induce the electrostatic chargeto enhance the stability of slurries through the electrostatic repulsion between particles. Thesuitable viscosity of the slurry, on the other hand, will help to keep kinetic stability by slowingdown the particle aggregation and sedimentation which helps the particles having enough time torotate under strong magnetic field, and finally, a homogeneous well-textured green body can beobtained under the strong magnetic field by using slip casting method via colloidal technique forslurry preparation.In this work, therefore, the colloidal technique was utilized to prepare a YVO4 nanopowderslurry with good dispersion and high stability. A magnetic field alignment technique wasproposed, using the slip casting method, to fabricate a textured-YVO4 green body. The greenbody was subsequently sintered using the SPS technique, which is a powerful sintering tool forachieving dense materials at relatively low temperatures to obtain the translucent YVO4 ceramics.2. Experimental procedure2.1. YVO4 nanopowders synthesisThe YVO4 nanopowders were prepared using the same procedure as described elsewhere [23].Briefly, NH4VO3 (Kanto Chemical Co., Japan, purity: analytical grade) was dissolved in aNaOH (Kanto Chemical Co., Japan, purity:> 99%) solution to produce a colorless solution witha concentration of 0.1 mol·L−1 (pH∼12), during which VO3− was converted to VO43−. Thisvanadate solution was then mixed with 2 mmol of Na2C4H4O5 (Kanto Chemical Co., Japan,Research Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16978purity:> 99%), which was dissolved in 30 mL of an aqueous solution, followed by pH adjustmentto ∼12. Secondly, the resultant transparent solution was homogenized via magnetic stirring andthen transferred to a stainless-steel autoclave for 30 h of hydrothermal reaction in an electric ovenpreheated to 200 °C. After the reaction, the hydrothermal YVO4 nanopowders were collected viacentrifugation, washed with water, and dried in air at 70 °C for 24 h.2.2. Preparation of YVO4 nanopowder slurryThe 15 vol% YVO4 nanopowders were dispersed into distilled water with polyelectrolyte(poly(ammonium)acrylate A-6114, Toaghosei Co., Japan) as a dispersion media to obtainwell dispersed YVO4 slurry. The pH value of the YVO4 slurries was adjusted to> 9 byTetramethylammonium Hydroxide (TMAH). The adding amount of A-6114 was referred to 1wt%mass amount of YVO4 in slurry. The slurry was then deagglomerated using a homogenizer for10 minutes, followed by continuous stirring under ultrasonic dispersion for another 10 minutes.2.3. Fabrication of textured-YVO4 ceramicThe YVO4 green body was fabricated from the slurry obtained as described above using slipcasting in a strong magnetic field of B= 12 T by aligning the slip casting direction S parallel to themagnetic field B (Fig. 1). The resulting slip-cast YVO4 green compacts were subjected to coldisostatic pressing (CIP) at 350 MPa for 10 min and were then densified in a graphite mold using aSPS machine (SPS, LABOX-315, Sinterland Co., Ltd., Japan) at the sintering temperatures ofT = 1100-1300 °C with heating rates of 100 °C/min under a constant uniaxial pressure of 90 MPa.The pressure was increased to the target pressure of 90 MPa as the temperature rises from 1000to 1100 °C. The temperature during sintering was monitored by measuring the temperature ofhole on the mold using an optical pyrometer.Fig. 1. Schematic illustrations of the preparation of (001) textured-YVO4 green body withthe slip casting direction S parallel to the magnetic field B during the slip casting under thestrong magnetic field.2.4. Characterization techniquesSlurry viscosities and Rheological behavior were measured as a function of the shear rate of theslurry by using a cone-plate viscometer (Re-215 Model, Toki Sangyo Co., Ltd., Tokyo, Japan).Zeta-potential measurement of the slurry was performed as a function of pH using zetasizer nanoessentials (Malvern Instruments Ltd., United Kingdom). Particle size distribution was examinedby a dynamic light scattering (DLS) analyzer (model Nanotrac UPA-UT 151, Nikkiso Co. Ltd.,Tokyo, Japan).X-ray diffraction (XRD) analysis of the YVO4 nanopowders and sintered bodies were performedby RINT-TTR III diffractometer (Rigaku Co., Ltd, Tokyo, Japan, 40 kV 150 mA) using Cu KαResearch Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16979radiation. Electron backscatter diffraction (EBSD, EDAX-TSL OIM EBSD system, EDAXInc., USA) characterization was conducted for texture analysis, which was performed using afield-emission scanning electron microscope (JSM7000F, JEOL Ltd., Tokyo, Japan). OrientationImaging Microscopy TM (TexSEM Laboratories, Inc., Draper, UT, United States of America) wasused for collecting and analyzing the EBSD data. Microstructures of the nanopowders/ceramicswere observed with a field emission scanning electron microscope (FE-SEM, JSM-7000, JEOL,Tokyo, Japan). Distribution of the grain size was calculated from EBSD data.The transmittance in the wavelength range of λ= 0.4-1.4 µm were measured by using adouble-beam spectrophotometer (SolidSpec-3700DUV, Shimadzu) equipped with an integratingsphere.3. Results and discussion3.1. Preparation and characterization of YVO4 nanopowders and slurryThe XRD pattern of the nanopowders can only be indexed by tetragonal YVO4 phase (Fig. 2(a)),and no any other impurity phases were identified. The morphology was further examined indetail using SEM, which revealed that the YVO4 nanopowders exhibit a uniform morphologyand excellent dispersion, as shown in Fig. 2(b). A narrow particle size distribution was achievedwith a particle size of d50 = 126 nm, according to the particle size distribution measurement inFig. 2(c).Fig. 2. XRD patterns (a), SEM image (b), and particle size distribution (c) of the YVO4nanopowders synthesized by using hydrothermal method.The effect of pH on the zeta potential was considered for the YVO4 slurry with the A6114amount of 1wt%. As shown in Fig. 3(a), isoelectric point (pHIEP) is about 5 for YVO4 slurry.With increasing the pH value (pH> pHIEP), the negative zeta potential increases accordingly. Atthe pH range of >9, the zeta potential value exceeds −40 mV, which is sufficient to prevent theparticle aggregation by generating the repulsive force between the particles [24], indicating thatthe slurries with pH at this range (>9) can provide much better colloidal stability.The rheological behavior, which evaluates powder dispersity in the slurries, was analyzed forthe slurry containing 15 vol% YVO4, 1 wt% of A6114 additive, and pH >9. The rheologicalResearch Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16980Fig. 3. (a) The effect of pH on the zeta potential of YVO4 slurries with 1 wt% A6114, and(b) the shear rate dependence of the viscosities of the slurries with 15 vol% YVO4.Fig. 4. XRD patterns of (001) textured-YVO4 green body. For comparation, the XRDpattern of random YVO4 green body is also presented.behavior was assessed by measuring the effect of shear rate on the viscosity of the slurry. Asshown in Fig. 3(b), the YVO4 slurry exhibited relatively constant viscosities regardless of theshear rate, indicating a Newtonian response consistent with a well-dispersed powder slurry. Therheological measurements suggest that a well-dispersed and stable YVO4 slurry can be obtainedunder the conditions investigated in this study.3.2. Characterization of crystalline orientation in YVO4XRD patterns of YVO4 green body, which was fabricated via slip casting in a strong magneticfield of B= 12 T with the slip casting direction S parallel to the magnetic field B are shown inFig. 4. For comparison, the XRD pattern of random YVO4 green body prepared outside of themagnet is also presented. The peak intensity ratio is slightly varies depending on the structureof YVO4 prepared in a magnetic field. The reflection intensity of (004) plane at 2θ = 58.64° islarger than that of the random YVO4. The reflection intensities of (004) and (220) correspondto (001) plane and a,b-plane of YVO4, respectively. Hence, the degree of (001) texture can beroughly estimated from the peak ratio PXRD of the reflection intensities I(004) and I(220) of (004)and (220) planes, respectively. The PXRD value is approximately 7.73 for textured-YVO4 andResearch Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16981Fig. 5. XRD pattern of the random YVO4 sintered at 1300 °C with a fixed dwelling time of10 min and heating rate of 100 °C/min.0.634 for the random sample, indicating that a well (001) textured-YVO4 green body can beachieved under the strong magnetic field of B= 12 T. It was revealed that the c-axis was alignedparallel to the magnetic field and is easy magnetization axis.The well-textured green bodies obtained above were then sintered by SPS under varioustemperatures with a fixed dwelling time of 10 min and heating rate of 100 °C/min, respectively.For comparison, the random YVO4 sintered at 1300 °C with the same heating rate and dwellingtime mentioned above is also fabricated. To accurately determine the impurity content in thesintered samples, XRD was only performed on random YVO4 sample (Fig. 5), since the intensitiesof peaks (112), (103), and (004) with the tilting angle (θ)< 45° are enhanced in oriented samples,potentially affecting the precise determination of impurity content. The XRD reflection peaks inFig. 5 are mainly indexed by the YVO4 phase (PDF No.: 01-082-1968), and a small amount ofY10V2O20-related peaks are detected in the sample, possibly due to the V-O evaporation duringthe sintering [25].Texture structure of the SPSed samples were considered by SEM-EBSD for YVO4 sinteredunder various temperatures. Figure 6 shows the EBSD inverse pole figure (IPF) map for thesample sintered at 1300 °C. The IPF map was colored against the vertical direction of the images,according to the color key on the standard stereographic triangle shown in Fig. 6. Most ofthe grains clearly show red and orange colors, indicating that the c-axis of most grains alignsperpendicular to the surface in the sample. This result demonstrates that by controlling the slipcasting and the magnetic field set-up, the (001) textured structure can be successfully designed toalign parallel to the YVO4 surface.The distributions of the tilt angle between the c-axis and the vertical direction in the YVO4sintered with various temperatures are calculated by using the multiples of a random distributions(MRD) from the EBSD data shown in Fig. 7(a). For comparation, MDR of random YVO4sintered with 1300 °C is also presented. For the random YVO4, MDR is almost constant of≈1 and no typical (001) orientation can be observed, whereas for the (001) textured samples,MRD shows a peak around θ = 0°. The (001) planes of ∼ 82%, ∼86%, and ∼91% grains areResearch Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16982Fig. 6. EBSD inverse pole figure (IPF) mapping of the textured SPSed-YVO4 sinteredunder 1300 °C.aligned within the tilting range of θ = 0-10° for textured YVO4 fabricated with the temperaturesof 1100 °C, 1200 °C, and 1300 °C, respectively. These results suggest that well-aligned (001)texture structure was obtained in textured YVO4. Additionally, texture degree was enhancedwith increasing sintering temperature from 1100 to 1300 °C for the samples fabricated from thetextured green bodies. The development of texture degree with sintering temperature is generallyattributed to grain coarsening [26]. According to Suzuki et al. [19], an increase in the texturedegree due to the grain coarsening can be explained by the preferential growth of well-alignedlarger grains over adjacent small grains with low orientation during sintering. The distribution ofgrain size which calculated from the EBSD data in Fig. 7(b) shows that the d50 increases from∼0.7 µm at T = 1100 °C to ∼ 2.44 µm at T = 1300 °C. This result can be inferred that the initialwell-aligned grain structure of the sample before sintering may contribute to the development offinal texture at higher sintering temperatures.Temperature dependent microstructures in Fig. 8 show that many residual pores are observedat multiple grain junctions at a lower temperature of T = 1100 °C and those apparently decreasewith increasing the sintering temperature. For comparison, the microstructure of random YVO4ceramic sintered at 1300 °C is given in Fig. 8(d). Similar to the textured-YVO4 sintered at thesame sintering temperature, a few of residual pores can be observed at the multiple grain junctionsas well (Fig. 8(c, d)), the grain size of random YVO4 ceramic, however, is slightly larger than thatof the textured-sample, with an average grain size of ∼3.67 µm for the random sample comparedto ∼2.88 µm for the textured sample (Fig. 8(c, d)). This is because the grain boundary energywas influenced by the misorientation angle between adjacent grains. When the misorientationangle is large, as in the random sample, the grain boundary energy tends to be higher, whichencourages grain coarsening. Whereas, in the oriented YVO4 sample, the grains are aligned in aspecific direction, which reduces the grain boundary misorientation angles between neighboringgrains, leading to lower grain boundary energy and thus less grain coarsening. This can bedemonstrated by the distribution of misorientation angles shown in Fig. 9. The misorientationangles in the random sample are much larger than those in the textured sample, indicating thatmany more high-angle boundaries can be observed in the random sample. Since grain boundariesResearch Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16983Fig. 7. (a) c-axis distribution, and (b) grain size distribution in the textured SPSed-YVO4sintered under various temperatures, which is calculated from the EBSD data.act as barriers to grain growth, these higher energy grain boundaries are less effective barriers,ultimately leading to a larger grain size in the random sample. Additionally, the misorientationangle distribution curve for the random sample is very similar to the Mackenzie ideal line, whichis normally used to represent the theoretical distribution of grain boundary misorientation anglesfor an ideal random texture in polycrystalline materials [27]. Whereas a significant deviationcan be observed between the misorientation distribution of textured sample and Mackenziedistribution, further confirming that textured structure was successfully designed in the sampleprepared under the magnetic field.3.3. Optical properties of (001) textured-YVO4 ceramicsFigure 10 gives the transmittance efficiencies of both textured- and random YVO4 sintered at1300 °C in the wavelength range from the visible to near-IR wavelength of λ= 0.4 -1.4 µm. Theuneven profile around the wavelength of 900 nm is due to the equipment and does not reflect theproperties of the sample. The transmittance is sensitive to textured structure of YVO4, whichexhibits much higher transmittance value than that of the random sample for the same sinteringconditions at the whole measurement wavelength range. For the YVO4 with non-cubic structure,the transmittance is known to be highly sensitive to all the microstructural factors of texture,grain size and porosity. Compared to the random YVO4 sample, YVO4 with (001) orientationcan improve the transmittance by reducing the birefringence at the grain boundary throughdevelopment of (001) texture in YVO4. The transmittance, however, is not determined onlyby one microstructural factor of the (001) texture, but also affected by other microstructuralfactors of the grain size and porosity [28,29]. Both samples exhibit the similar porosity, as shownin Fig. 8(c), (d), the larger grain size, however, in the random YVO4 sample (3.67 µm) wouldincrease the birefringent scattering loss at the grain boundaries, and may thus also cause thereduction in transmittance of the random sample. These results suggest that the (001) texturedstructure of YVO4 ceramics, is sufficiently effective in suppressing the birefringent scattering atthe grain boundaries, and hence, effectively contributed to enhance the transmittance of YVO4.Research Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16984Fig. 8. SEM images of (001) textured-YVO4 ceramics fabricated at (a) 1100 °C, (b) 1200 °C,(c) 1300 °C, and (d) the SEM image of random YVO4 fabricated at 1300 °C, with a constantdwelling time of 10 min and a heating rate of 100 °C/min.Fig. 9. Distribution of misorientation angle in random and textured YVO4. The ideal lineof MacKenzie is also presented.Research Article Vol. 33, No. 8 / 21 Apr 2025 / Optics Express 16985Fig. 10. Transmittance efficiencies of the (001) textured- and the random YVO4 ceramicsfabricated at 1300 °C with a constant dwelling time of 10 min and a heating rate of100 °C/min.4. ConclusionsA well-dispersed and highly stable slurry with 15 vol% YVO4 was achieved by a colloidaltechnique using 1 wt% A6114 as dispersant at the slurry pH> 9. The (001) textured YVO4 wassuccessfully formed by controlling the crystalline orientation through the strong magnetic fieldalignment processing during the slip casting. As the SPS sintering temperature increased from1100 to 1300 °C, grain size and density increased, and the orientation of the sample improved aswell. For the optimum SPS processing at T = 1300 °C for dwelling time of 10 min and heatingrate of 100 °C /min, the (001) textured-YVO4 exhibits much higher transmission efficiency atthe whole wavelength range than that of the non-textured random YVO4 sample, indicating thatcontrolling the microstructure using a textured structure method is a suitable way to enhancethe transmittance of YVO4 ceramics. It is expected that this method can be easily applied andorientation can be achieved even when Nd is doped into YVO4.Funding. Innovative Science and Technology Initiative for Security (JPJ004596).Acknowledgments. Part of this work was financially supported by Innovative Science and Technology Initiativefor Security, Grant Number JPJ004596, ATLA, Japan.Disclosures. The authors declare no conflicts of interest.Data availability. 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