陶瓷注射成型混料工艺及坯体产生缺陷研究

采用保形性较好的聚苯乙烯粘结剂体系和ZrO2-3%Y2O3(摩尔分数)粉末混合制备喂料。研究了加料顺序对喂料性能的影响,通过研究混料时间对喂料均匀性的影响确定合适的混料时间,分析了注射成型和脱脂过程产生缺陷的成因。结果表明,当先混合ZrO2粉末、聚苯乙烯(PS)与油,再加入硬脂酸(SA)和邻苯二甲酸二丁酯(DBP)时,所制备的喂料更均匀、性能更好;混料时间为63min时,喂料均匀。     

超细316L不锈钢粉末注射成形的脱脂工艺

采用溶剂脱脂和热脱脂相结合的方法,研究了超细316L不锈钢粉末注射成形坯的脱脂工艺。注重考察了升温速度和保温时间对不锈钢注射坯的热脱脂工艺的影响。研究表明注射成形坯经正己烷溶剂脱脂后,石蜡组元全部被脱除。其它组元在后续的热脱脂中被去除,确定了优化的升温速度和保温时间,试样没有出现缺陷,并缩短了脱脂周期,该周期大约为10小时。     

陶瓷粉末微注射成形脱脂与烧结机理相关研究

分析了粉末微注射成形亚微米级结构广阔的应用前景,以及亚微米尺度下脱脂和烧结理论研究的重要意义。综述了不同脱脂阶段的微观结构特征,亚微米尺度对不同阶段粘结剂的脱出机制,以及建立包含微结构比表面积的脱脂时间/速率数学模型的研究现状,讨论了获得脱脂过程中保形控制原理,亚微米阵列致密化过程中物质的迁移机制及晶粒长大的主要驱动力,以及坯体几何尺寸对不同烧结阶段物质扩散机制影响规律的关键作用,论述了明确陶瓷亚微米级结构力学特性的重要性。提出了亚微米级结构的脱脂和烧结机理今后的重点研究方向。     

Ti(C,N)基金属陶瓷注射成形脱脂技术研究

使用传统蜡基粘结剂和改进型蜡基粘结剂分别研究了Ti(C,N)基金属陶瓷粉末注射成形,热脱脂和溶剂脱脂 热脱脂工艺过程,其中包括根据粘结剂TGA制定并优化热脱脂的工艺曲线、不同的溶剂和温度对溶剂脱脂的影响、后续热脱脂工艺路线的确定.结果表明:使用改进型蜡基粘结剂的2#试样热脱脂工艺简单、周期短并易于控制;2#溶剂脱脂率明显高于使用传统蜡基粘结剂的1#试样;经过溶剂脱脂 热脱脂,1#试样脱脂率达到93%,2#试样脱脂率达到96%以上;1#烧结试样的抗弯强度为700 MPa左右,2#则达到1300 MPa,从烧结样品抗弯断口和显微组织的SEM图片得到了验证.Ti(C,N)基金属陶瓷注射成形采用改进型蜡基粘结剂比传统蜡基粘结剂脱脂效果好、力学性能高,改进型蜡基粘结剂更适合Ti(C,N)基金属陶瓷注射成形.     

新型陶瓷注射成形喂料催化脱脂过程的研究

陶瓷注射成形是一种受到日益广泛关注的技术 ,但其中脱脂一步传统采用的热脱脂技术脱脂速度慢 ,效率较低。本研究采用以聚甲醛为主要粘结剂制备了可快速脱脂的新型陶瓷注射成形喂料体系 ,并进行催化脱脂工艺的研究 ,记录了该过程中样品失重的情况 ,分析了脱脂阶段不同特征及其原因 ,指出催化脱脂过程速度的控制因素是气态催化剂和气体产物扩散过程。通过脱脂前后样品表面及截断面的扫描电镜分析 ,直观反映了脱脂前后样品微观形貌上的差异及特点。观察了脱脂过程不同时刻样品外围与中心区域的微观形貌 ,证明了脱脂过程是由外围逐渐向内部扩散的 ;记录了经注射成形的试样烧结前后的密度变化     

新型陶瓷注射成形喂料催化脱脂过程的研究

陶瓷注射成形是一种受到日益广泛关注的技术，但其中脱脂一步传统采用的热脱脂技术脱脂速度慢，效率较低，本研究采用以聚甲醛为主要粘结剂制备了可快速脱脂的新型陶瓷注射成形喂料体系，并进行催化脱脂工艺的研究，记录了该过程中样品失重的情况，分析了脱脂阶段不同特征及其原因，指出催化脱脂过程速度的控制因素是气态催化剂和气体产物扩散过程，通过脱脂前后样品表面及截断面的扫描电镜分析，直观反映了脱脂前后样品微观形貌上的差异及特点，观察了脱脂过程不同时刻样品外围与中心区域的微观形貌，证明了脱脂过程是由外围逐渐向内部扩散的；记录了经注射成形的试样烧结前后的密度变化。     

水溶性粘接剂氧化锆粉末注射成形喂料的研究

采用聚乙二醇(PEG)为水溶脱脂粘接剂,聚甲醛(POM)/聚乙烯醇缩丁醛(PVB)为保型粘接剂,混炼制备水溶性粘接剂氧化锆粉末注射成形喂料;通过傅里叶红外光谱和旋转流变测试研究硬脂酸改性氧化锆对注射成形喂料的性能影响,并通过喂料流变行为、注射生坯脱脂率、生坯弯曲强度以及生坯脱脂前后断面形貌扫描电镜分析、烧结体的X射线衍射、硬度及密度表征,研究粘接剂组分配比和喂料粉末装载量对喂料性能的影响.结果表明:硬脂酸可以成功对氧化锆粉末进行改性,并可以明显降低注射成形喂料的黏度;当粉末装载量达到52%(体积分数),粘接剂各组分配比w(PEG)∶w(POM)∶w(PVB)=6∶2∶2时,喂料具有较好的流动性且粉末分散良好,生坯中粘接剂形成网状结构赋予生坯较高的弯曲强度,4 h后水脱脂率超过80%,水脱脂后生坯形成细小且连续脱脂通道;生坯经水脱脂、1 450℃烧结2 h后,烧结体晶型主要由四方相组成,平均晶粒尺寸1μm,密度6.01 g/cm~3,平均维氏硬度达到1 147 HV,与模压成型烧结氧化锆性能相当.     

钛合金粉末注射成形热脱脂工艺的研究

采用粉末注射成形方法制备了钛合金坯体,然后利用溶剂脱脂方法脱除坯体中可溶性粘结剂.在热脱脂速率为2.0℃/min、最高脱脂温度600℃、保温时间为1h和真空脱脂气氛条件下脱除坯体中剩余粘结剂,坯体中残余碳氧含量分别0.092%(质量分数)和0.28%,低于国外报道的PIM钛合金脱脂坯中残余碳氧含量.XRD结果表明,脱脂坯中只存在α相,没有TiC,Ti3Al,TiO和TiN等杂质相存在.N2气氛下脱脂,脱脂坯中残余碳含量较低,但氧含量较高.     

Ti-Mo吸气材料注射成形脱脂工艺的研究

采用粉末注射成形技术制备Ti-Mo合金吸气材料。研究了脱脂工艺对坯体质量、微观结构及其元件性能的影响。讨论了化学脱脂中的溶剂、温度、时间对坯体脱脂率的影响,较优的脱脂溶剂为三氯乙烯,在脱脂温度为50℃、脱脂时间为6h条件下,脱脂率达71.55%;通过DTA/TG曲线对热脱脂工艺进行了优化,确定了热脱脂工艺参数为室温-120℃,升温速率10℃/min;120~230℃,升温速率5℃/min;230~500℃,升温速率2℃/min,保温60 min;再经过800℃烧结工艺,制备出性能优异的Ti-Mo吸气剂元件,吸气性能特征为S10=738.5 mL/s,Q120=995.6Pa·mL。     

增塑挤压成形钨基合金棒材溶剂-热二步脱脂工艺研究

大长径比钨基合金棒材制备的关键是成形、脱脂和后续的烧结控制.基于增塑挤压成形的研究,对Ф24 mm钨基合金挤压棒坯的快速无缺陷脱脂,即溶剂-热二步脱脂工艺进行了研究.结果表明:在溶剂脱脂温度为45℃,脱脂12 h后,Ф24 mm钨基合金棒材一次脱脂率达45%;在溶剂脱指过程中增加干燥阶段,脱脂率可达70%以上;在真空气氛下对脱脂棒材进行后续热脱脂,坯体保形性好,且在12 h内,脱脂可以全部完成.采用溶剂-热二步脱脂工艺可以实现Ф24 mm钨基合金挤压棒材的快速无缺陷脱脂.     

金属注射成形蜡基粘结剂的研究

本文研究了综合蜡基和油基粘结剂优点的改进型蜡基粘结剂体系 ,其组成为PP PW 植物油 SA 改性剂。改进型蜡基粘结剂分阶段热解 ,各组元间有较强的相互作用 ,相容性较好。该粘结剂和金属粉末具有较好的混合均匀性 ,改性剂的加入提高了粉末装载量。喂料是一种假塑性流体 ,非牛顿指数n较大 ,粘流活化能ΔEη 较低 ,具有良好的注射填充性。改进型蜡基粘结剂既可热脱脂 ,又可溶剂脱脂 ,溶剂脱脂速度快、维形能力好。     

Influence of the Compacts Homogeneity on the Incidence of Cracks during Thermal Debinding in Ceramic Injection Molding

During thermal debinding in ceramic injection molding, the inhomogeneity of green body is a key origin of cracks. In this study, the impact of low molecular weight binders on the homogeneity of the green body was investigated. Incidence of cracks during thermal debinding indicated that the volume ratio of wax to stearic acid should be out of high viscosity and incompletely wetting region. In these two formulation regions,typical inhomogeneous microstructures were observed. By mercury intrusion method, it was shown that pore size distribution of the debinded compacts was determined by thermal degradation of low molecular weight binders. A particle-rich region model was established to predict the nucleation of cracks caused by solid loading fluctuation. The criterion of cracks nucleation was that local capillary force from solid loading fluctuation was larger than the suction force from the surroundings.     

Thermal, Solvent, and Vacuum Debinding Mechanisms of PIM Compacts

The mechanisms of thermal, solvent, and vacuum debinding processes for powder injection molded (PIM) compacts were investigated. Mercury intrusion porosimetry (MIP) and scanning electron microscope (SEM) observations on PIM specimens showed that fine interconnected pores were developed in the early stages of debinding in all three processes. These pores were formed as a result of the decomposition of low temperature binders such as paraffin wax during thermal debinding or arise from the extraction of soluble binder components in solvent debinding. In the later stages of thermal and vacuum debinding, decomposed gases could be trapped in the center region and build up a pressure causing cracking or blistering defects. The solvent debinding process could alleviate these problems, but the penetration of solvent into the binder could still cause cracking or distortion due to swelling of the binder.

It was found that the pore structure evolution was influenced by the heating rate, temperature, pore size, and the amount of existing porosity. From the observed microstructure and mercury porosimetry data, debinding mechanisms were derived and the defects which were frequently seen during debinding were explained with these mechanisms.     

新型金属注射成形催化脱脂型粘结剂的催化快速分解研究

催化脱脂是目前MIM技术领域新的发展方向,研究了新型金属注射成型催化脱脂型粘结剂的催化快速分解,研究结果表明,该催化脱脂型粘结剂在以HNO3为催化剂进行催化脱脂时,注射成形坯经3－4h催化脱脂后,脱脂坯内部已形成大量的连通孔道,脱脂时间,脱脂温度以及 不同粘结剂组成影响催化脱脂效果。     

Production of injection moulded 316L stainless steels reinforced with TiC(N) particles

Abstract

Metal matrix composites, based on 316L stainless steel and reinforced with TiC and TiCN particles, were manufactured following a powder injection moulding route: mixing, preparation of feedstock, moulding, debinding and sintering. The 316L stainless steel and carbide powders were dry mixed and moulded with wax based binder. The critical powder loading for injection moulding was 62·5 vol.-% for all samples. Binder debinding was performed by solvent and thermal method. After debinding, the samples were sintered at 1250 and 1385°C for 1 h in pure H₂. Metallographic studies were conducted to extend densification and the corresponding microstructural changes. The sintered samples were characterised by measuring tensile strength, hardness and wear behaviour. Wear loss was determined for all samples after wear tests. All powder, fracture surfaces of moulded and sintered samples, and worn surfaces of all the samples, were examined using scanning electron microscope. The sintered density of injection moulded 316L stainless steel samples, reinforced and unreinforced, increases with increasing sintering temperature. The addition of TiC and TiCN improves the hardness and wear resistance with increasing sintering temperature.     

Structure and thermal conductivity of powder injection molded AlN ceramic

AlN powders doped with Y₂O₃ (5 wt.%) were compacted by employing powder injection molding (PIM) technique. The binder consisted of paraffin wax (PW, 60 wt.%), polypropylene (PP, 35 wt.%) and stearic acid (SA, 5 wt.%). The feedstock was prepared with a solid loading of 62 vol.%. The binder was removed through debinding process in two steps, solvent debinding followed by thermal debinding. At last, the debound samples were sintered in flowing nitrogen gas at atmospheric pressure. The result reveals that thermal debinding atmosphere has significant effect on the thermal conductivity and structure of AlN ceramics. The thermal conductivity of injection molded AlN ceramics thermal debound in flowing nitrogen gas is 231 W m^?1 K^?1.     

Fabrication of ceramic composites consisting of powders with different specific gravity by the slip-casting technique

For composites, it is of great importance to fabricate well-dispersed green compacts, in order to improve their mechanical properties and reliability. In the present study, the slip-casting technique was applied to the fabrication of ZrO2-WC-Al2O3 composites. The specific gravity of each composition in this material was very different, that is, 6.07 for ZrO2, 15.6 for WC and 3.94 for Al2O3. The compositions in the green compacts were afraid to separate from each other owing to the difference in their specific gravities, leading to heterogeneity in the microstructure. The relative density of the obtained compacts was approximately 60%. WC and Al2O3 were well-dispersed in the ZrO2 matrix. The separation and/or heterogeneity due to difference could not be recognized by energy-dispersive X-ray analysis. The slip-casting technique was found to be applicable to the fabrication of ceramic composites consisting of raw powders with different specific gravities. This revised version was published online in November 2006 with corrections to the Cover Date.     

Debinding and sintering defects from particle orientation in ceramic injection moulding

The causes of the defects in injection-moulded ceramic bars during debinding and sintering were investigated using density and shrinkage measurements in combination with macroscopic observation. Differential shrinkage during sintering is the main cause of post-debinding defects. Particle shape, mould geometry and gate position have a large effect on this differential shrinkage, while the volumetric shrinkage is almost constant and the influences of moulding conditions are relatively small. Particles with plate-like morphology orientate during moulding and contribute markedly to defect formation during debinding and sintering.     

Effects of debinding parameters on powder injection molded Ti-6Al-4V/HA composite parts

Titanium alloy-hydroxyapatite(Ti-6Al-4V/HA) composite powders produced by a ceramic slurry were mixed with a multi-component binder system in the powder injection molding process. The binder system comprises mainly of natural wax, fatty acid wax, stearic acid, poly-oxialkyen-etherand olefln-hydrocarbons. After molding, the binder system was removed by conventional thermal debinding. The effects of heating rate and gas flow rate on the quality of the debound part in terms of defects, mass of binder removed and residual carbon level were discussed. A slow heating rate (20° C/h) at the beginning stage of the debinding step and a higher gas flow rate (250 cm³ /min) were required for the production of defect-freeparts with minimal carbon level.