With the development of terahertz frequency band, the size of the slow wave structure, which plays key roles in realizing effective interaction between electron beams and terahertz signals, has decreased by an order of magnitude from mm to hundreds of μm scale. How to produce the high aspect ratio and fine-structure in such a small μm-scale structure has become a key factor that largely restricts the performance of terahertz devices. With the help of fully utilizing the excellent tolerance of UV-LIGA technology (Ultraviolet Lithography, Galvano forming, Abforming), the influence of intrinsic material properties of copper substrates (including oxygen content, grain size and distribution) on the surface polishing accuracy and slow wave microstructure processing accuracy are firstly investigated. The results indicate that low oxygen content and fine-grained substrates are beneficial for achieving high surface quality and precision of photolithography processing channels, which can satisfy the precision design requirements of 0.34 THz or even higher frequency terahertz slow wave structures.
The effects of cryogenic treatment (CT) and tempering-cryogenic treatment (TCT) on the microstructure and properties of coarse-grained WC–10Co cemented carbides with different carbon contents were researched. The binder phase, WC mean grain sizes, W solubility in the binder, relative magnetic saturation, densities, hardness, wear resistance and second phase precipitation of cemented carbides with different heat treatments were discussed. The results show that there are significant changes of microstructure and properties in the samples with CT and TCT, especially due to the precipitation of metastable nanoparticles W_xCo_yC_z in the binder during the heat treatments of CT and TCT. With the simultaneous combination of microstructure and nanoparticle-reinforced binder, a dramatically improved combination of hardness and wear resistance of the samples after TCT has been achieved.
Impurities and their distributions in osmium targets for M-type cathodes affect the coating quality on porous tungsten and cathode emission performance.Glow discharge mass spectrometry(GDMS) and X-ray photoelectron spectroscopy(XPS) were used to analyze the impurity contents and distributions in the osmium target.The chemical states of impurity elements were analyzed and characterized.The total amount of metallic impurity in the target was lower than 0.01 wt%.
High quality osmium targets are the key influence in improving the emission performance, lifetime and reliability of M-type cathodes. In this experiment, oxidative distillation was used to prepare osmium powder with a purity greater than 99.99%. The effect of hydrogen sintering and hot pressing sintering processes on the densities and grain size of the targets was investigated. The results show that the oxidation distillation process can effectively separate Os from Si, Fe, Ni, Zn and other impurity elements, and the purity of osmium powder prepared by multiple oxidation distillation was not less than 99.99%. Both hydrogen sintering and hot pressing sintering processes can be used to obtain osmium targets with a density of not less than 95%. However, the sintering temperature and time used in the hot pressing sintering process under pressure assistance are significantly lower than those of hydrogen sintering, which is more conducive to inhibiting grain growth during the high densification sintering process. By optimizing the parameters of the hot pressing sintering process, the sintering temperature of 1500°C and the holding time of 1.5h resulted in an osmium target with a density of 99.11% and a grain size of ≤12. XPS analysis of the highly dense fine crystalline osmium targets prepared by hot pressing sintering showed that the C and O mass fractions on the surface of the targets were 0.85% and 4.43% respectively, and the C and O contents gradually decreased with increasing etching depth. The above highly dense and fine crystalline osmium targets can be used in the M-type cathode standard coating process to obtain high purity, dense and strong bonded osmium films.
采用电感耦合等离子体质谱仪(ICP-MS)、室温拉伸及电子背散射衍射(EBSD)分析等手段研究了轧制态钨窄带在800℃、900℃退火时显微组织、织构及力学性能的变化.结果表明,轧制态钨窄带样品具有精细的纤维层状结构,层宽约0.5μm;包含α织构和γ织构,以α织构为主,最强织构{111}<110>占比35.7%;使其抗拉强度达到2062 MPa,延伸率为5%,综合力学性能优异.经退火后,平均纤维层宽增加到1μm及以上,最强织构类型不变,且占比增至42.1%;5°以下低角度晶界占比微增,说明了900℃退火时仅发生了少量的回复过程;退火后强度有所降低而塑性未能改善,预示着钨窄带的退火应以低温短时的消除应力处理为宜;退火后钨窄带的强度保持及强塑性匹配,对其绕制成型性及服役可靠性至关重要.
The W–4.9Ni–2.1Fe–xDy2O3 heavy alloy was fabricated by high-energy ball milling and spark plasma sintering (SPS) technique, and the microstructure, mechanical and friction behavior and anti-corrosion ability were investigated by scanning electron microscope (SEM), Rockwell hardness tester, X-ray diffraction (XRD), reciprocating friction and wear tester, electrochemical station, etc. The results show that the trace Dy2O3 particles, which mainly distributes in the W–M (tungsten-matrix) interface and the tungsten matrix phase, can dramatically decrease the tungsten grain size and the amount of O and P impurities aggregating in the interface, promote the γ-(Ni, Fe) bonding phase and tungsten particles uniform distribution, and increase the relative density, hardness, and wear and corrosion resistance properties. But the excessive Dy2O3 addition can make the inhibition effect weaken, resulting in the decrease in the comprehensive performances of the alloy. So, the amount of Dy2O3 should be appropriate. When the adding amount of Dy2O3 particles is 0.7 wt%, the comprehensive performances of the heavy alloy are the best.
This paper first reviewed the pore design requirements of porous tungsten matrix materials (PTMM). Secondly, the preparations of PTMM as the main line were introduced, including the process of tungsten powder pretreatment and forming, tungsten compact sintering, copper infiltration and removal, porous tungsten HIP and cryogenic machining. Finally, the test methods of properties of PTMM were summarized. Tungsten powders plasma spheroidization, tungsten compact extrusion and injection moulding are a future development trend for the dispenser cathodes matrix. Porous tungsten capsule-free HIP contributes to high-reliability and long-life of dispenser cathodes. Porous tungsten cryogenic machining, an advanced sustainable process, is capable of short process manufacturing for porous tungsten matrix of dispenser cathodes.
Al0.7Sb2Te3 ternary target was prepared by vacuum synthesis and sintering-HIP using mixed powder of Al, Sb and Se in an atomic ratio of 0.7:2:3 as raw material. Target properties were characterized by XRD, FESEM, EDS and XPS, and the state of Al in the ternary target was researched primarily by XPS. The results show that with aluminum doping, the lattice constant of main phase Sb2Te3 changes, and the aluminum dispersoids can coexist together with Al0.1Sb2Te3 matrix, which confirms the effect of aluminum doping on target organization structure; with the increase of the etching depth from 0 to 405.9 nm, the aluminum's valence is gradually transferred from the compound state of Al2O3 to simple substance state, and the area depth of aluminum dominated by Al2O3 is about 90 nm; XPS analysis with the etching depth of 405.9 nm shows the aluminum of Al0.1Sb2Te3 matrix influences target structure by effective formation of AlSb.
研究了不同后续热等静压工艺对镀铜钼粉制取的MoCu30合金性能的影响.研究发现,表面镀铜钼粉所制得MoCu30合金在1130℃温度下、压力100 MPa条件下进行2h后续热等静压处理后,提高了合金的综合性能:其中铜相随着钼骨架受力而发生变形、流动,促进了组织中铜相的均匀分布以及孔洞的减少,使合金的致密度达到99.7%,接近全致密;高温处理时铜晶粒长大,晶界数量减少,这样降低了晶界与孔洞缺陷对声子的散射作用,从而增强了MoCu30合金的声子导热机制,提高了合金的热导率;相对于未经后续热等静压处理的MoCu30合金,合金热等静压处理后铜相分布更加均匀,合金受力时塑性较好的铜相优先发生变形,同时减少了孔洞等裂纹源,使得合金的25℃拉伸及压缩屈服强度略有提高,分别达到451,543 MPa,而合金的400℃拉伸及压缩屈服强度也有所增加,分别达到349,372 MPa.
Al-Sb-Te相变薄膜与CMOS兼容性高,热稳定性佳,所以能很好满足相变存储器高温稳定工作的需求.以原子比Al∶Sb∶Te=0.7∶2.0∶3.0的混合粉为原料,采用真空合成法与烧结-热等静压制备Al-Sb-Te合成粉及用于溅射沉积Al0.7 Sb2Te3薄膜的三元靶材,通过X射线衍射仪(XRD),场发射扫描电镜(FESEM)及金相显微镜(OM)、能谱仪(EDS)分别表征粉体物相、靶材显微组织及元素分布等.结果 表明:Al0.7Sb2Te3合成粉的主相为Sb2Te3相,且与Sb2Te3二元合金粉相比,Al原子的掺杂使Sb2Te3主相的品格常数与晶胞体积均减小,具体表现为:品格常数a,c从Sb2Te3二元合金粉的0.4267,3.0443 nm减小到Al0.7Sb2Te3合成粉的0.4258,3.0423 nm,且晶胞体积减小0.486%;再用Al0.7 Sb2Te3合成粉为原料,制备出的三元靶材相对密度达到99.5%,且其平面与截面显微组织基本一致,均形成明显的Al0.1Sb2Te3基体相与单质Al弥散相两相组成,基体相与弥散相结合紧密,界面处存在宽度2~3 μm的过渡区域.所制备的近全致密两相Al0.7Sb2Te3合金靶材,有望改进磁控溅射法制备Al-Sb-Te系列薄膜的工艺和效果.
The crystallographic orientation and microstructure of the 0.5 mm thick cold-rolled annealed molybdenum sheets for vacuum electron devices were analysed by electron back-scattered diffraction (EBSD) and metallography, and the correlation with mechanical performance was discussed. The results show that the molybdenum sheets with excellent processability have some characteristics: grain orientation distribution which is relatively weaker and more diffused, mainly consists of alpha-fiber and gamma-fiber texture. In the a-fiber texture, rotation cubic {001}< 110 > is the maximum component, and an amount of {112}< 110 > exists. Observed microstructures are mostly flat cloud-flake grains arrayed orderly along rolling direction and paralleled to rolling surface. Relatively less high-angle boundaries with theta > 50 degrees are detected. Therefore, the Mo sheets show higher yield ratio and elongation, and weaker elongation anisotropy in RD, TD, and 45 degrees-RD directions, i.e. excellent strength and toughness matching.
以原子比Al:Sb:Te=0.7:2:3的混和粉为原料,采用真空合成法与烧结-热等静压制备Al 0.7 Sb 2 Te 3 三元靶材,通过XRD、FESEM、EDS、XPS等手段表征其性能,且重点采用XPS研究Al在Al 0.7 Sb 2 Te 3 三元靶材的存在状态。结果表明:Al掺杂后,靶材主相Sb 2 Te 3 的晶格常数变化,且单质Al弥散相与Al 0.1 Sb 2 Te 3 基体相共存,表明掺杂对靶材的组织结构确有影响;刻蚀深度从0 nm增加至405.9 nm,Al价态从以Al 2 O 3 的化合态为主逐渐过渡至以单质态为主,且Al以Al 2 O 3 形态为主的区域深度约90 nm;刻蚀深度为405.9 nm的XPS分析表明,Al 0.1 Sb 2 Te 3 中的Al通过有效化合形成AlSb影响着靶材的组织结构。
本文通过开展周期性校准,评定不确定度,在积累了一定数据基础上,采用最大似然估计法,分析并优化了我司电子天平的校准周期.对保障测量结果的准确可靠性,同时降低校准的经济成本和时间成本有重要实践意义.
According to the failure mechanism of the cathode used in space travelling wave tubes,the developments of cathode material were illustrated and factors limiting the long-lifetime of cathodes were analyzed.Effects of particle characteristics and porous performance of the substrate on evaporation rate of active material penetrating into the substrate were discussed.The work function of M-cathode would change continuously in working process because of the influence of elemental alloying on surface,barium supplying in channels and surface coverage.It was suggested that narrow size distributed powders with regular shapes and mean grain size of 4 μtm were helpful for improving porous property and reducing percentage of close pores.Mixing cathode substrate with noble metal Os or Ir,or covering cathode surface with Os or Ir film,could effectively slow down the alloying speed,reduce the evaporation,keep low work function,and so improve cathodes lifetime.
采用直接氮化法对铝粉进行氮化,分别研究了添加剂、反应温度、保温时间对合成产物的影响。运用扫描电镜(SEM)、X射线衍射物相分析(XRD)、X射线荧光光谱分析(XRF)对合成产物进行了表征,研究结果表明:提高反应温度、延长保温时间可以有效促进铝粉转化为氮化铝,提高合成产物的氮含量。同时提高反应温度可以促进添加剂的挥发,减小杂质元素的残留量。在1000℃下保温3 h后,对多孔疏松的合成产物进行球磨24 h处理,最终可以得到氮含量大于32%,Cl的残余含量低于0.3%,K的残余含量低于0.1%,平均粒度小于2μm氮化铝粉末。同时在多孔疏松状合成产物表面观察到了氮化铝晶须的存在,这说明铝粉直接氮化法也可以制备出氮化铝晶须。
Os–Ir–Al alloy was fabricated by powder metallurgy technique. IrAl and OsIr interalloys were synthesized to reduce the Al evaporation and ensure the composition of the ternary alloy. Analysis on microstructures shows that each component is distributed homogeneously, and the green density reaches 94.9 %. Ba–W cathodes with Os–Ir–Al alloy magnetic sputtered on the tips are prepared and directly current density tests are carried out on these cathodes. It is found that at 1,050 °C, the average zero field emission density of the cathode reaches up to 20 A·cm−2. The improvements of cathodic current density and stability may indicate the prosperous application of Os–Ir–Al alloy on cathode.
High purity CuInSe 2 material was prepared. Purification process including molten salt refining-electrolysis refining-zone purification and vacuum distillation-zone purification was used to eliminate impurities from raw material In and Se, and In with purity of 99.9999% and Se with purity of 99.9995% were obtained respectively. Intermediate compounds consisted of single phase CuSe and In 2Se 3 structure, with both purities higher than 99.999% were synthesized by multi-chamber vacuum grads fabrication process. Breaking, milling the intermediate compounds properly, pressing and sintering at proper parameters, then uniform CuInSe 2 with purity up to 99.999% was prepared. The alloy mainly consisted of single CuInSe 2 phase, analyzing by XRD testing.
Diamond composites with diamond volume fraction up lo 80 % is prepared by high temperature and high pressure( HTHP) sintering method. Factors including particle size, sintering temperature and sintering time are investigated to illustrate the influence on romposition. interfacial state and thermal conductivity of the composites. The results indicates that a high thermal conductivity value of 639 W · m -1 · K -1 could he achieved when diamond particle diameter is 80 μm .A critical diameter value is determined by the volume fraction of diamond,and the thermal conductivity of the composite increases with the particle diameter increasing and then lends to decrease when it reaches tin-critical value: An optimal match of sintering temperature and sintering time is beneficial for a good cohesion at the interface and good thermal conductivity of the composites.
Ongoing trends of miniaturization of electronic devices have made diamond composite an open and challenging area for researchers.Research status and development of diamond composites for thermal management are illustrated and factors relating to thermal conductivity are analyzed.According to thermal conductivity models and experimental study,the heat conduction mechanisms across the metal-diamond interface are discussed,and conclusions that effectively conductive passages with high strength and low thermal resistance interfaces in the composites are helpful for excellent properties is deduced.Therefore,diamond thermal management materials are promising in electronic industry application.
This paper introduces the performance and function of Cu、In、Ga、Se,discusses the preparation method of selenode targets.The experiment shows that after the technology such as synthesis of gradient by vacuum and hot-pressed sintering,the purity and density of selenode targets using in absorbing layer of GIGS thin film solar cell were over 99.999% and 99.1% respectively.The process with simple equipment and easy operation is suitable to industrial production.