The Effect of Sintering on the Properties of Ultrafine

研究了一种化学气相沉积(CVD)制备超细铼粉的新方法,即以NH4ReO7为原料,通过将其分解为Re2O7后气相输运至还原区,经氢气还原生成超细铼粉。对不同还原温度下制备的超细铼粉样品,采用XRD、SEM、激光粒度分析进行表征,实验揭示了烧结作用对晶粒尺寸、形貌、表面状态及粒度等粉末性能的影响规律。结果表明,随还原温度升高,烧结作用增强,制备的超细铼粉晶粒尺寸增大,具有更好的球形度,表面趋于光洁,平均粒径增大。     

球形钴粉的制备及其在超细晶粒硬质合金中的应用

以碳酸钻为原料,采用氢气还原法在带式无舟皿连续还原炉中制备超细球形钻粉。考察还原温度和还原时间对钻粉粒度的影响。结果表明,在420～460℃还原180min左右,可以制备费氏粒度为0．9μm左右的超细球形钻粉。采用二氧化碳气体钝化处理技术降低了钻粉的氧含量。采用制备的钻粉为超细晶粒硬质合金的粘结剂,用低压烧结工艺制备出钻相高度分散、晶粒均匀的超细晶粒YG10硬质合金。其晶粒度为0．4μm,矫顽磁力达38．0kA／m,硬度大于93．0HRA,抗弯强度高于3700MPa。     

采用CVD法还原挥发性铼的氧化物制备超细铼粉(英文)

研究了一种以高铼酸铵为原料,采用化学气相沉积(CVD)制备超细铼粉的新方法。通过控制氧分压,使得NH4ReO7分解为具有挥发性的ReO4、Re2O7,再采用载气将其输运至还原区,经氢气还原生成超细铼粉。热力学计算表明,在NH4ReO7分解过程中,控制氧分压高于101.248Pa时,Re2O7将不会分解为低价氧化物,DSCTGA分析结果也证实了这一点。采用该方法制备的铼粉,粒度为100~800nm,D50为308nm,比表面积为4.37m2/g,氧含量为0.45%。     

湿化学法制备W-TiC复合粉体及其SPS烧结行为

采用湿化学法制备W-TiC复合粉体,然后采用放电等离子体烧结(SPS)技术制备超细晶W-TiC复合材料,并对其复合粉体形貌和烧结复合材料组织结构进行研究。结果表明,对原始TiC粉进行活化预处理,使TiC粉表面获得均匀分布的缺陷,提高TiC粉表面的的亲水性,通过化学还原获得第二相TiC颗粒,且均匀弥散分布于W基体晶界和晶粒内。采用SPS烧结技术获得的超细晶W-TiC复合材料晶粒尺寸为400 nm,致密度为95%,维氏显微硬度值HV0.2达到1280。     

超细硬质合金中晶粒非均匀长大机理

采用市售的粒度为0.8μm的WC粉末和粒度为1.6μm的Co粉制备了WC-10%Co超细硬质合金,通过金相显微镜﹑扫描电子显微镜观察了不同烧结温度下制备的试样WC晶粒形貌,对超细晶粒硬质合金非均匀长大现象及机理进行了研究。结果表明:粉末湿磨后的粗大颗粒在烧结过程中起晶核作用,是引起晶粒非均匀长大的关键因素。固相烧结时,烧结体中细小颗粒受到张力的作用发生旋转,当其取向与邻近的大颗粒取向一致时,形成共格界面,以粗大晶粒为核心以并合的方式非均匀长大;液相烧结时,细小晶粒溶解并优先地在大晶粒的某些低能量晶面如(0001)和(1010)面析出,引起晶粒异常长大。本研究中,当烧结温度达到1 410℃时,WC晶粒可异常长大为接近20μm的粗大晶粒。     

纳米及超细复合粉添加对超粗晶硬质合金晶粒长大的影响及机制

在粗颗粒WC/Co混合粉末中分别添加平均粒径为100、250、400nm的WC-8Co复合粉,经球磨混合压坯后在不同温度进行Ar气保护烧结。针对烧结块体的形貌、晶粒尺寸及其分布进行了研究,并分析了复合粉添加对不同烧结阶段WC晶粒长大的影响机理。研究发现,在WC/Co混合粉中加入纳米和亚微米复合粉末均可制备得到超粗晶硬质合金,且添加纳米复合粉烧结的试样平均晶粒尺寸达到9.3μm。烧结初期,纳米和亚微米复合粉通过增加混合粉末的表面能而有效促进WC晶粒长大;当达到液相烧结温度时,添加纳米复合粉的烧结块体中,由于小晶粒具有更大的溶解驱动力,促使小晶粒溶解并在周围大晶粒表面析出,进一步增大烧结块体的晶粒尺寸;添加亚微米复合粉的块体中,小晶粒WC呈集中分布,使其溶解驱动力较小,且析出主要发生在周围细小晶粒之间,达到溶解析出动态平衡,从而使烧结块体的平均晶粒尺寸增长缓慢。     

两步烧结对超细晶WC-4%Co硬质合金微观组织及性能的影响

采用瞬时烧结法确定了超细晶WC-4%Co硬质合金在烧结过程中矫顽磁力突变温度,据此设计了该合金两步烧结工艺曲线。采用传统烧结方法和两步烧结方法制备超细晶WC-4%Co合金,研究了两步烧结方法对超细硬质合金的微观组织、力学性能和切削性能的影响规律。结果表明:超细晶WC-4%Co合金矫顽磁力突变的温度点在1 450℃以上。采用传统烧结方法制备的超细晶WC-4%Co合金中WC晶粒的三维形貌为多台阶层状结构,WC晶粒尺寸分布范围宽;两步烧结方法制备的WC-4%Co合金中WC的晶粒三维形貌发育为单层和三棱柱混合结构,WC晶粒尺寸分布范围窄。由于细颗粒WC溶解-析出行为的充分进行,两步烧结方法制备的合金硬度略微下降,断裂韧性有较大幅度提高。铣削试验结果表明:两步烧结制备的超细晶WC-4%Co合金木工铣刀的的抗崩刃性能及铣削寿命高于传统方法烧结的合金产品。     

自贡厂研制成超细WC粉和超细硬质合金牌号

自贡硬质合金厂承担了作为“八五”国家级重点开发项目之一超细WC粉及4个超细硬质合金牌号的研制。该厂的科技人员与中南工大粉冶所紧密合作，在研制过程中解决了两大难题。一是制粉问题，采用一种较为特殊的，称之谓“气相还原──—碳化法”，即以高纯鹤的化合物为原料，添加少量Cr、V等为抑制剂，能工业生产BET平均粒度＜0．15μm，小角度X射线散射测定＜0．1μm，粒度分布窄的超细WC粉。与此同时还研制成超细Co粉，平均粒度（朋T）＜0.4μmm；二是解决了利用上还超细WC粉和钴粉配制的超细合金在烧结过程中的晶粒长大问题。该厂研…     

预处理工艺对放电等离子烧结超细晶WC-Co硬质合金组织和性能的影响

采用不同粒度的WC粉与超细Co粉混合得到初始粉末,利用直接放电等离子烧结(SPS)技术和一种包括真空预处理和SPS烧结的新制备方法,研制超细晶WC-Co硬质合金块体.结果表明,两种不同粒度匹配的混合粉末经真空预处理后SPS烧结得到的试样较直接SPS烧结试样的硬度稍有降低,但断裂韧性得到提高,尤其是抗拉强度得到显著提高.对试样显微组织和性能分析表明,混合粉末的真空预处理工艺对SPS烧结WC-Co硬质合金具有重要作用:去除混合粉末吸附气体,消除Co池,同时保证WC晶粒不发生明显长大.     

原位合成复合粉制备超细WC-Co硬质合金

以偏钨酸铵、可溶钴盐、可溶碳源为原料,经喷雾转化、煅烧、低温还原碳化制备超细晶WC-Co复合粉;采用同样成分配比及工艺,在煅烧后增加短时球磨工艺,制备出另一种超细晶WC-Co复合粉;分别以2种复合粉为原料,用放电等离子直接烧结制备超细WC-Co硬质合金。采用SEM、XRD、钴磁仪、矫顽磁力计、维氏硬度计等对复合粉形貌、合金显微组织与性能进行表征分析。结果表明,未短时球磨的粉末呈现出球形结构,WC颗粒被Co相粘结在一起,可观察到烧结颈并有异常长大晶粒,经过短时球磨工序制备的粉末为分散颗粒,2种粉末中Co相同时以fcc与hcp的结构存在,粉末WC晶粒尺寸约为0.26μm;未短时球磨的粉末制备的合金存在少量孔隙,致密度较低,有异常长大晶粒。短时球磨能有效提高粉末颗粒的分散性,减少烧结体中的显微组织缺陷,制备的合金综合性能得到提高。     

Optimization of the synthesis conditions of LiCoO2 for lithium secondary battery by ultrasonic spray pyrolysis process

LiCoO₂ powders for lithium secondary battery were successfully prepared by the ultrasonic spray pyrolysis process. In this work, the statistical experimental design method was used to compare the characteristics (particle size, standard deviation, surface area, tab density) of the LiCoO₂ particles according to the four parameters (synthesis temperature, sintering temperature, sintering time, sintering heating rate). The optimal synthesis conditions for the synthesis of LiCoO₂ particles in ultrasonic spray pyrolysis process were to be obtained. The above-mentioned optimal conditions were used to prepare the particles with particle size 4.7 μm (standard deviation: ±1.3%) and the experimental results were in a good agreement with simulated values. The oxide powders were characterized by scanning electron microscopy, X-ray diffraction and electrochemical method including charge–discharge cycling. The characteristics as a cathode for lithium ion battery depended on the sintering temperature and sintering time. Consequently, LiCoO₂ powders made by the ultrasonic spray pyrolysis process displayed a good electrochemical performance and the experimental design method was well applied.     

纳米CeO2的醇水法制备及其对GaAs晶片的抛光性能

在醇水体系中以HMT为缓释沉淀剂制备了纳米CeO2粉体,并用TEM、SAD、XRD对其进行了表征,将制备的不同粒径纳米CeO2粉体配制成抛光液,对GaAs晶片进行了化学机械抛光。研究了醇的引入及煅烧温度对粉体性能的影响,并就纳米CeO2磨料尺寸对GaAs晶片抛光后表面粗糙度的影响机理进行了探讨。结果表明:醇水体系中制备的纳米CeO2颗粒较水溶液中制备的颗粒粒径小,且分散性好;随着煅烧温度的升高,颗粒逐渐增大,不同尺寸的纳米颗粒具有不同的抛光效果;随着磨料粒径的增大,表面粗糙度值也随之升高。     

Microstructure and properties of liquid-phase sintered tungsten heavy alloys by using ultra-fine tungsten powders

The microstructure and properties of liquid-phase sintered 93W-4.9Ni-2.1Fe tungsten heavy alloys using ultra-fine tungsten powders (medium particle size of 700 nm) and original tungsten powders (medium particle size of 3um) were investigated respectively. Commercial tungsten powders (original tungsten powders) were mechanically milled in a high-energy attritor mill for 35 h. Ultra-fine tungsten powders and commercial Ni, Fe powders were consolidated into green compacts by using CIP method and liquid-phase sintering at 1465℃ for 30 rain in the dissociated ammonia atmosphere. Liquid-phase sintered tungsten heavy alloys using ultra-fine tungsten powders exhibit full densification (above 99% in relative density) and higher strength and elongation compared with conventional liquidphase sintered alloys using original tungsten powders due to lower sintering temperature at 1465℃ and short sintering time. The mechanical properties of sintered tungsten heavy alloy are found to be mainly dependent on the particles size of raw tungsten powders and liquid-phase sintering temperature.     

Modeling of the beam transportation behavior in selective laser transmission sintering the translucent core–shell composite powder

In the paper, selective laser transmission sintering the 2%PF/silica sand core–shell composite powders was studied based on a developed optical model by using a Zemax optical design program. The construction of the powder bed was made by the particle stacking model with the composite particle assumed as a three-component optical system. It showed that simulation results agreed well with the experimental data. A focus point after the first layer particle was produced by the translucent spherical lens of particles and then laser beam was quickly diverged by subsequent particles along the beam transportation path. The occurrence of the vaporization at the focus point had little effect on the whole properties of the sintered sample because of its relatively small size. Since no melting pool was produced in the sintering process owing to the thin polymer binder, the rearrangement of the powder bed was not remarkable which led to a constant porosity of the powder bed before and after laser sintering. Laser transmission sintering of core–shell composite powders was basically “contaction” sintering, where particles near to each other as well as within the beam transportation path had an opportunity to sinter together.     

Sintering of a nano-crystalline tungsten heavy alloy powder

A nano-crystalline Tungsten heavy alloy powder was obtained by mechanical alloying of elemental powders in a jar mill with a high ball to powder ratio. The chemical composition of the primary powder was 93 W-4.9Ni-2.1Fe (wt%). The mechanically alloyed powder had 22 nm sized tungsten crystallites distributed in an amorphous nickel base phase. Mechanical alloying reduced particle size of powders and also yielded to more uniform particles size distribution. Sintering behavior and microstructural development of that powder were studied and compared with a conventionally mixed powder. Mechanically stored energy and better distribution of primary elements in Nano-crystalline powder had decreased motivation energy of sintering and that powders showed more densification at relatively lower sintering temperatures. Sintering at low temperatures can depress grain growth during sintering and provide desirable properties. A transient intermetallic phase was formed in the nano-crystalline powder during sintering that has not been seen in conventionally mixed powders.     

微波法制备纳米TiO2粉末

以海绵钛为原料,源溶液经微波辐射,生成水合二氧化钛溶胶,加入少量无水乙醇,在１００℃以下,常压烘干,制备出纳米ＴｉＯ２粉末。ＸＲＤ分析纳米ＴｉＯ２粉末的晶体结构为锐钛矿型;ＴＥＭ显示,纳米颗粒的形貌为球形,粒径在６０ｎｍ～１００ｎｍ之间,粒度分布均匀;试样在水中分散的Ｚｅｔａ电位值为＋４８．７ｍＶ,分散性好。此种方法,原料成本低,工艺简单易行,粒度容易控制。     

单分散近球形和片状金粉的制备及表征

以HAuCl4·4H2O为前驱体,抗坏血酸(VC)为还原剂,线性聚乙烯亚胺(L-PEI)为表面活性剂在水相中制备了单分散的近球形和片状金粉.采用SEM、XRD和激光粒度分析仪对金粉的形貌、粒径、结晶和分散性进行了测试和表征.研究了还原剂和金前驱体的摩尔比、L-PEI浓度、温度及反应溶液的pH对近球形和片状金粉的形貌和粒径大小的影响.给出了制备微米级近球形和片状金粉的反应条件,同时也提出了近球形和片状金粉的成核和晶核生长的可能解释.     

选择性激光烧结法制备SiC颗粒预制体

介绍了一种新的制备颗粒预制体的方法,即采用选择性激光烧结(SLS)法制备SiC颗粒预制体。结果表明,用表面已预处理的SiC与粘结剂混合粉料作为SLS用粉,在一定的激光烧结工艺条件下,可将其烧结成SiC颗粒均匀分散的预制体;并可通过控制烧结粉末的配比获得不同孔隙率的SiC颗粒预制体。