Ti-B-C-N粉末烧结的微观组织及其性能

以Ti-B-C-N四元相陶瓷粉末为实验材料,采用真空热压烧结和放电等离子烧结(SPS)工艺对其进行烧结,真空热压烧结和放电等离子烧结温度分别为1900℃和1450℃,烧结压力分别为20 MPa和40 MPa,保温时间分别为1h和3min。使用X射线衍射仪分析试样物相组成,扫描电子显微镜观察试样表面微观形貌和断口形貌,并测试了烧结试样的硬度和抗弯强度。结果表明:真空热压烧结和放电等离子烧结块体的主要生成相为TiB2相和TiCN相,相对密度分别为97.40%和93.06%,热压烧结试样致密度高,颗粒尺寸大,放电等离子烧结试样孔隙较多,晶粒尺寸小;抗弯强度分别为259.98 MPa和335.17 MPa;弹性模量分别为89.11GPa和162.92GPa;洛氏硬度分别为78.8和84.9;放电等离子烧结试样表现出较好的力学性能。     

Li7La3Zr2O12固态电解质的制备及表征研究

固态电解质作为全固态电池的关键材料备受关注,而石榴石结构固态电解质因其高电导率成为了研究热点.通过低成本的高温固相和静压两步法制备的四方相石榴石材料Li7La3Zr2O12(LLZO),采用X射线衍射对不同烧结时间得到的样品进行物相分析,利用电化学工作站交流阻抗法测试材料的离子电导率.结果表明:烧结6 h的样品衍射峰尖锐,结晶度良好,空间点阵群属于I41/acd,为纯四方相结构,离子电导率相对较高,为5.96×10-8S/cm.     

氧化锆流延基片的烧结温度及其性能研究

比较了3种不同的烧结温度对氧化锆流延基片性能的影响。结果表明,随着烧结温度的升高,基片的收缩率和相对密度增加、硬度增加、气孔率减小、晶粒和气孔的平均尺寸均有所增加。在1500℃保温3h可以获得较高的致密度（相对密度97．8％）和合适的晶粒尺寸,试样在1073K时离子电导率为1．187×10^-2S·cm^-1,烧结体物相主要为四方相。     

Mg掺杂对CuRh2-2xMg2xO4陶瓷热电性能的影响

采用固相烧结和放电等离子烧结(SPS)法制备CuRh_(2-2x)Mg_(2x)O_4样品,研究不同Mg含量对CuRh_(2-2x)Mg_(2x)O_4热电材料物相组成,晶粒尺寸和热电性能的影响.通过对样品进行XRD,断口形貌SEM,热导率及Seebeck-电阻率进行测试分析,检测结果表明:Mg掺杂后CuRh_(2-2x)Mg_(2x)O_4X射线衍射峰的峰位较CuRh_2O_4标准PDF卡片整体偏移,晶格常数减小;掺杂后的样品晶粒尺寸减小,Mg的掺入使CuRh_2O_4的热导率下降,并且掺杂量越多,热导率越小;Mg掺杂改善了CuRh_2O_4的电学性能,提高了样品的电导率.当Mg掺杂量x=0.25时,试样CuRh_(1.5)Mg_(0.5)O_4的ZT值取得最大值,在900℃下达到了0.182 28.     

高岭土掺杂NASICON固体电解质及全固态电池性能

针对LiTi2(PO4)3基固态电解质电导率低的问题,采用浙江三门高岭土矿作为主要原料,以高温固相法制备铝、镁、硅共掺杂钠超离子导体(NASICON)型快离子导体Li1+2x+2yAlxMgyTi2-x-ySixP3-xO12.研究掺杂比例、温度对固态电解质离子电导率的影响.结果表明,组成为Li1.8Al0.1Mg0.3Ti1.6Si0.1P2.9O12固体电解质在423 K时有最高离子电导率7.86×10-4 S·cm-1.以该组成固态电解质为基片,喷雾热解原位制备Al/ Li1+xV3O8/ Li1.8Al0.1Mg0.3Ti1.6Si0.1 P2.9O12 /C全固态电池并在1.8～3.9 V电压区间进行50次充放电测试.该电池具有较好的稳定性及循环容量保持能力.30次循环以后放电容量基本稳定在190～205 mAh·g-1之间,充放电效率大于90%.     

热压合成Ti_4AlN_3及其物理性能研究

以摩尔比为Ti ◇Al ◇TiN=1 1.2 2.7的混合粉为原料,采用真空热压烧结工艺在1400℃保温2 h成功合成了高纯Ti4AlN3块体材料,Ti4AlN3烧结试样结晶良好,晶粒发育完善,内部较为均匀致密,相对密度达到98.5%,具有较高的抗弯强度（384 MPa）、抗压强度（523 MPa）和断裂韧性（6.5（MPa.m1/2））,较低的维氏硬度（2.9 GPa）和抗破坏能力,具备良好的机械加工性能。Ti4AlN3常温电导率和热导率分别为4.6×105（Ω-1.m-1）和12（W.m-1.K-1）,其热导率在25～600℃范围呈上升趋势;25～1100℃的线膨胀系数为9.0×10-6K-1,良好的导热性能和高温热稳定性使其可以应用于高温领域。     

不同振荡热压烧结温度下90W-10Cu难熔合金组织和性能的研究

高压电触头材料用90W-10Cu难熔合金由于高熔点和高比重差异,在高温长时间的粉末冶金过程中存在致密化困难和晶粒异常长大而影响其性能。新型振荡热压烧结（Hot oscillatory pressure, HOP）技术在常规热压烧结基础上用一定频率的循环振荡单轴压力代替静单轴压力,可快速促进陶瓷等材料的致密化。因此,为了研究振荡热压烧结对90W-10Cu难熔合金的低温烧结效果,本文将振荡热压烧结技术应用到90W-10Cu（质量分数）难熔合金的制备中,研究了烧结温度（1000-1300 ℃）对其微观组织、致密度、晶粒尺寸、硬度及电导率性能的影响。研究结果发现振荡热压烧结90W-10Cu合金由W相基体和Cu相粘结相组成。随着烧结温度的升高,90W-10Cu难熔合金的致密度逐渐增大,在烧结温度最高为1300 ℃时,其致密度最高可达到99.35%,同等温度下均高于热压烧结样品的致密度;而晶粒尺寸仅为4.97 μm左右,没有异常长大,达到了细化晶粒的效果;同时其W晶粒邻接度逐渐减低,合金的微观组织均匀性得到优化和改善;维氏硬度和电导率分别达到225.78 HV30和27.88% IACS,高于同等温度甚至高100 ℃时的热压烧结体,性能得到显著提升,达到了低温烧结效果。结果表明振荡热压烧结能够有效地促进90W-10Cu难熔合金的致密化,降低烧结温度和抑制晶粒生长,显著优化其微观组织均匀性,有利于在较低温度下获得高致密度、晶粒细小、高硬度和高电导率的90W-10Cu难熔合金材料。     

碱土掺杂硅酸镧电解质材料的制备与性能

采用尿素-硝酸盐燃烧法在600～800℃下制备了较高纯度无杂质相的碱土掺杂磷灰石型La9.33Mx(SiO4)6O2+δ(M为Sr,Ca,Mg)电解质.通过X射线衍射、扫描电镜和交流阻抗测试,对样品的晶体结构、表面微观形貌及电导性能进行了研究.结果表明,燃烧合成的电解质粉体La9.33(SiO4)6O2(LSO)具有p63/m磷灰石型晶体结构;LSO烧结体的微观形貌随x值的不同而出现了细微变化;LSO烧结体具有良好的电阻可逆性和稳定性.适当的掺杂量能有效提高LSO的离子电导率,最佳掺杂浓度为0.2.相同掺杂量下,三种碱土金属阳离子掺杂对电导性能也有一定的影响,随着离子半径的增大,掺杂效果越来越好.     

高温固相法制备Li7La3Zr2O12固态电解质及其性能研究

全固态电池的固态电解质因其优秀的安全性能、较宽的电化学窗口以及良好的化学稳定性得到广泛研究,但固态电解质的离子电导率与传统液态电解质相比还是偏低.为了提高固态电解质的离子电导率,采用高温固相法和高速球磨工艺制备石榴石型固态电解质Li_7La_3Zr_2O_(12)(LLZO),根据冷等静压在不同烧结温度制备得到LLZO固态电解质片,利用X射线衍射(XRD)、扫描电子显微镜(SEM)对固态电解质LLZO的物相、微观结构进行表征,采用电化学工作站测试阻抗,再计算离子电导率.结果表明:烧结温度为1 000℃制备得到的样品,衍射峰清晰且尖锐,颗粒尺寸为3～5μm,结晶度良好,为纯的立方相LLZO结构,在室温下测得的离子电导率较高,为8.6×10~(-6) S/cm.     

过渡元素掺杂固体电解质的制备及电性能

为了解决固体氧化物电解质在中温范围（500 ℃～800 ℃）工作电导效果不佳的问题,采用燃烧合成方法以氧化镧及过渡离子氧化物为原料,制备了过渡金属元素掺杂的硅酸镧体系电解质材料. 用X-射线衍射图谱、扫描电子显微镜以及红外光谱对所得电解质进行了物相和显微结构分析. 研究表明,掺杂离子对电解质的物相结构及形貌影响很小,但是通过引入适量过渡掺杂离子,能够有效提高电解质的电导率. 当掺杂量摩尔比x=1.0时,锌掺杂后硅酸镧电解质具有最高的离子电导率,在500 ℃时的电导率可达2.106×10-2 S/cm. 相比于未掺杂电解质在500 ℃电导率为1.71×10-3 S/cm有了显著提升. 元素铜的掺入对电解质的致密度有促进作用,压片和二次烧结后电解质的密度达94.1%. 同时通过交流阻抗测试分析证实镍在硅位掺杂会降低电解质的电导率.     

Comparative study of β-Si3N4 powders prepared by SHS sintered by spark plasma sintering and hot pressing

β-Si3N4 powders prepared by self-propagating high-temperature synthesis (SHS) with additions of Y2O3 and Al2O3 were sintered by spark plasma sintering (SPS). The densification, microstructure, and mechanical properties of Si3N4 ceramics prepared using this method were compared with those obtained by hot pressing process. Well densified Si3N4 ceramics with finer and homogeneous microstructure and better mechanical properties were obtained in the case of the SPS technique at 200℃ lower than that of hot pressing. The microhardness is 15.72 GPa, the bending strength is 716.46 MPa, and the fracture toughness is 7.03 MPa.m1/2.     

不同铅气氛对PMSZT压电陶瓷机电性能的影响

采用固相烧结法制备了三元系压电陶瓷Pb0.98Sr0.02（Mn1/3Sb2/3）x（Zr0.5Ti0.5）1-xO3（0%〈x〈0.1）（PMSZT）,研究了铅气氛和非铅气氛保护条件烧结对其相结构、微观结构、介电性能以及压电性能的影响．实验结果表明：在烧结温度1100-1300℃范围内,铅气氛保护烧结的试样其综合性能优于非铅气氛保护烧结的试样．铅气氛保护条件下于1200℃得到最佳性能：εr=1717、d33=301、Kp=0．55、tanδ=0．42％、Qm=1453．     

碳化铬-镍铬涂层对几种陶瓷的滑动摩擦磨损

在ＭＭ－２００块－环接触磨损试验机上，测定了等离子喷涂碳化铬－镍铬涂层对烧结Ａｌ２Ｏ３、热压烧结Ｓｉ３Ｎ４、ＳｉＣ和等离子喷涂ＴｉＯ２涂层等四种陶瓷材料在干摩擦条件下的滑动摩擦系数和磨损量；利用ＳＥＭ、ＥＤＡＸ和ＸＲＤ等技术，观察和分析了摩擦副材料在磨损后的形貌、物质转移和物相转变；讨论了摩擦副材料的显微结构和某些物理性能、机械性能对碳化铬－镍铬涂层摩擦磨损行为的影响，结果表明：涂层与不同陶瓷对磨，不仅其磨损量相差很大，而且其摩擦磨损机理也不相同，摩擦磨损过程中对磨材料向涂层表面的转移，有利于提高涂层的耐磨能力。配对陶瓷的显微颗粒尺寸和弹性模量愈小，导热系数愈高，则与碳化铬－镍铬涂层的配对性能愈好。     

Na_(0.5)K_(0.5)NbO_3织构化陶瓷制备与表征

采用凝固法制备出各向异性的片状钛酸钡作为模板,利用模板晶粒生长(TGG)法制备出Na0.5K0.5NbO3(NKN)织构化陶瓷.研究了NKN织构化陶瓷的工艺、组织和性能.研究结果表明,钛酸钡可以作为NKN陶瓷的模板,在陶瓷烧结过程中诱导NKN晶粒的生长,模板的取向决定了NKN陶瓷晶粒取向,随着烧结温度的升高陶瓷的压电性能(d33)达到69 pC/N,在合理的烧结工艺下得到了取向比较明显的织构化陶瓷.     

Comparative study of β-Si3N4 powders prepared by SHS sintered by spark plasma sintering and hot pressing

β-Si3N4 powders prepared by self-propagating high-temperature synthesis (SHS) with additions of Y2O3 and Al2O3 were sintered by spark plasma sintering (SPS). The densification, microstructure, and mechanical properties of Si3N4 ceramics prepared using this method were compared with those obtained by hot pressing process. Well densified Si3N4 ceramics with finer and homo- geneous microstructure and better mechanical properties were obtained in the case of the SPS technique at 200°C lower than that of hot pressing. The microhardness is 15.72 GPa, the bending strength is 716.46 MPa, and the fracture toughness is 7.03 MPa?m1/2.     

Effect of SiO2 addition on the dielectric properties and microstructure of BaTiO3-based ceramics in reducing sintering

The effect of SiO2 doping on the sintering behavior,microstructure,and dielectric properties of BaTiO3-based ceramics has been investigated.Silica was added to the BaTiO3-based powder prepared by the solid state method with 0.075mo1%,0.15mo1%,and 0.3mo1%,respectively.The SiO2-doped BaTiO3-based ceramic with high density and uniform grain size were obtained,which were sintered in reducing atmosphere.A scanning electron microscope,X-ray diffraction,and LCR meter were used to determine the microstructure as well as the dielectric properties.SiO2 can form a liquid phase belonging to the ternary system of BaO-TiO2-SiO2,leading to the formation of BaTiO3 ceramics with high density at a lower sintering temperature.The SiO2-doped BaTiO3-based ce-ramics can be sintered to a theoretical density higher than 95% at 1220℃ with a soaking time of 2 h.The dielectric constants of the sample with 0.15mo1% SiO2 addition sintered at 1220℃ is about 9000.Doping with a small amount of silica can improve the sinter-ing and dielectric properties of BaTiO3-based ceramics.     

Sol-gel法制备CaSiO3基LTCC陶瓷

采用溶胶凝胶法(Sol-gel)制备了CaSiO3基低温共烧陶瓷,在800℃、825℃、850℃、875℃下烧结,并对烧结样品进行了热重-差热分析、X射线扫描分析、扫描电子显微镜形貌分析.测试了在烧结温度为800℃、825℃、850℃、875℃下各样品的烧结密度和介电性能.结果表明Sol-gel 法制备的CaSiO3基...     

Atomic force microscope study of WC-10Co cemented carbide sintered from nanocrystalline composite powders

In order to compare the spark plasma sintedng （SPS） process plus hot isostatic press （HIP） with vacuum sintedng plus HIP, an investigation was carried out on the topography, microstructure and gain size distribution of nanocrystalline WC-10Co composite powder and the sintered specimens prepared by SPS plus HIP and by vacuum sintering plus HIP by means of atomic force microscopy （AFM）. The mechanical properties of the sintered specimens were also investigated. It is very easy to find cobalt lakes in the specimen prepared by vacuum sintering plus HIP process. But the microstructure of the specimen prepared by SPS plus HIP is more homogeneous, and the grain size is smaller than that prepared by vacuum sintering plus HIP. The WC-10Co ultrafine cemented carbide consolidated by SPS plus HIP can reach a relative density of 99.4%, and the transverse rupture strength （TRS） is higher than 3540 MPa, the Rockwell A hardness （HRA） is higher than 92.8, the average grain size is smaller than 300 nm, and the WC-10Co ultrafine cemented carbide with excellent properties is achieved. The specimen prepared by SPS with HIP has better properties and microstructure than that prepared by vacuum sintering with HIP.     

Dielectric properties of Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ceramics by impedance spectroscopic method

Various lead-free ceramics have been investigated in search for new high-temperature dielectrics. In particular, Bi₄Ti₃O₁₂ is a type of ferroelectric ceramics, which is supposed to replace leadcontaining ceramics for its outstanding dielectric properties in the near future. Ferroelectric ceramics of Bi₄Ti₃O₁₂ made by conventional mixed oxide route have been studied by impedance spectroscopy in a wide range of temperature. X-ray diffraction patterns show that Bi₄Ti₃O₁₂ ceramics are a single-phase of ferroelectric Bi-layered perovskite structure whether it is calcined at 800 °C or after sintering production. This study focused on the effect of the grain size on the electric properties of BIT ceramics. The BIT ceramics with different grain sizes were prepared at different sintering temperatures. Grain becomes coarser with the sintering temperature increasing by 50 °C, relative permittivity and dielectric loss also change a lot. When sintered at 1 100 °C, r values peak can reach 205.40 at a frequency of 100 kHz, the minimum dielectric losses of four different frequencies make no difference, all close to 0.027. The values of E _a range from 0.52 to 0.68 eV. The dielectric properties of the sample sintered at 1 100 °C are relatively better than those of the other samples by analyzing the relationship of the grain, the internal stresses, the homogeneity and the dielectric properties. SEM can better explain the results of the dielectric spectrum at different sintering temperatures. The results show that Bi₄Ti₃O₁₂ ceramics are a kind of dielectrics. Thus, Bi₄Ti₃O₁₂ can be used in high-temperature capacitors and microwave ceramics.     

High toughness alumina ceramics with elongated grains developed from seeds

Alumina ceramics have been used in a wide variety of engineering fields because of their excellent mechanical and electric properties as well as relatively low cost of manufacture. Now such alumina ceramics with flexural strength as high as 700—1000 MPa and Weibole mode of 40 have been prepared by using pure and ultra-fine powder[1,2]. However, the fracture toughness of the materials is very low, typically around 3 MPa·m1/2. Therefore, much effort has been made on the improvement of fractu…