烧结工艺对TA15粉末冶金钛合金组织与性能的影响

采用氢化脱氢TA15钛合金粉末为原料,通过模压成形与真空烧结及进一步热等静压(hot isostatic pressing,HIP)处理,制备TA15钛合金,对烧结合金及其热等静压后的组织形貌与拉伸性能进行分析与测试,研究成形压力及烧结温度对该合金组织与性能的影响。结果表明,随压制压力增大或烧结温度升高,烧结体的抗拉强度和伸长率都提高。热等静压后晶粒趋于球化,抗拉强度提升不明显,伸长率提升较显著。压制压力为700 MPa,烧结温度为1 300℃时,烧结合金的抗拉强度和伸长率都达到最大值,分别为1 050 MPa和2.81%。经HIP处理后合金的抗拉强度最高达到1 170 MPa,最大伸长率为5.6%。     

高纯金属钒粉烧结性能研究

利用电子探针观察高纯金属钒粉粒度和形貌, 使用油压机将高纯金属钒粉压制成坯条, 并采用万能试验机测定钒坯条压溃变形力曲线, 分析钒坯条最优压制压力; 分别通过热压烧结和冷等静压+真空烧结的方法对高纯钒粉进行烧结, 研究烧结工艺对高纯钒粉烧结特性和力学性能的影响。结果表明: 采用冷等静压+真空烧结的方法, 在压制成形过程中, 钒粉压坯密度和相对密度随压力的增加而逐步提高, 压力提高到280 MPa时, 压坯密度和相对密度分别为3.99 g·cm-3和66.94%;经真空烧结后, 坯料密度和相对密度分别为5.28 g·cm-3和88.59%。压制压力由80 MPa提高到200 MPa时, 压溃强度从0.4 MPa增加到6.0 MPa, 增大趋势较为明显; 压制压力提高到280 MPa时, 压溃强度增加到7.4 MPa, 增大趋势变缓。经热压烧结坯料的相对密度比冷等静压+真空烧结坯料的相对密度高, 280MPa压力下热压烧结坯料密度和相对密度分别达到5.51g·cm-3和92.91%。     

素坯制备工艺对反应烧结碳化硅结构与性能的影响

本文以酚醛树脂为粘结剂,采用粉末冶金方法制备碳化硅素坯,研究碳化硅素坯制备工艺对反应烧结碳化硅材料显微结构和性能的影响.结果表明:反应烧结碳化硅材料的抗弯强度和密度随碳化硅颗粒粒径的增大而减小,随素坯成形压力的增大呈现先增大后减小的趋势.密度和硬度随碳化硅素坯中碳密度的下降而减小.碳化硅颗粒粒径为W7时,酚醛树脂加入量为12％,碳加入量为13％和成形压力为120MPa为碳化硅素坯制备的最优参数组合,此时反应烧结碳化硅材料的抗弯强度、密度和HRA分别为330MPa、2.987 g/cm3和95.     

FeAl金属间化合物粉末注射成形工艺研究

通过机械合金化制备Fe-48at%Al金属间化合物粉末,分别按照33%、40%和50%的粉末装载量(体积分数)进行注射成形,成形坯经溶剂脱脂和热脱脂以及1 200℃真空烧结,得到FeAl金属间化合物.重点研究粉末装载量对喂料混炼、注射成形温度及压力、脱脂率及烧结组织和力学性能的影响.结果表明,机械合金化FeAl粉末由于具有不规则形状和层片结构,其注射成形喂料流动性较差;在使用高粉末装载量时应提高注射温度和压力,且溶剂脱脂率较低(7 h后为94.3%),需进一步延长脱脂时间;FeAl金属间化合物烧结试样的相对密度和抗弯强度均随粉末装载量增大而提高,当粉末装载最为50%,注射温度和注射压力分别为154℃和4.0 MPa时,材料的相对密度为92%,抗弯强度达587 MPa.     

原始粉BET,CIP压力与烧结温度对ITO靶材微观结构及结瘤情况的影响

以不同比表面积(BET)气化In_2O_3和SnO_2粉(In_2O_3/SnO_2=9:1)为原料,使用模压辅助冷等静压(CIP)成型的方法制备出铟锡氧化物(ITO)坯体,又在不同温度条件下烧结制得ITO靶材。研究了原始粉BET,CIP压力与烧结温度对靶材微观结构及结瘤的影响,结果表明:BET更大的A配方粉末烧结活性更高,在较低的烧结温度即可致密,而微观结构致密性的提高有利于防止靶材结瘤;当CIP压力由285 MPa提高至400 MPa,坯体各方向收缩率明显增加,且相对密度由64.90%提高至70.23%,CIP压力继续提高至500 MPa,坯体密度不再继续增加,稳定在70%左右;在1540℃常压氧气氛烧结20 h后,CIP压力为285 MPa和400 MPa的靶材相对密度均超过99.8%,晶粒尺寸均在4～10μm,但前者含少量尺寸在2μm以下的微孔,而后者微观致密性更好、晶内小微粒尺寸更大,且溅射后未出现结瘤;在1575℃常压氧气氛烧结20 h后,CIP压力为285 MPa和400 MPa的靶材相对密度均超过99.8%,均未出现微孔缺陷,但靶材晶粒尺寸均偏大,范围大致在4～17μm,其中400 MPa靶材出现了更多数量的异常大晶粒;当CIP压力均为400 MPa时,1575℃烧结靶材结瘤偏多,而1540℃烧结靶材未出现结瘤。     

氧化铌阴极微观结构对电脱氧制备铌的影响

采用电脱氧法,以Nb2O5烧结片为阴极,石墨棒为阳极,在CaCl2-NaCl混合熔盐中制备金属铌.分别研究了压制压力、烧结温度对阴极片微观结构和电脱氧反应及其产物的影响.实验结果表明,烧结温度和压制压力对Nb2O5烧结片的晶粒尺寸、孔隙度和孔隙尺寸具有明显的影响,从而影响到电脱氧的反应速率和效果.晶粒细、孔隙度高和连通性好的烧结氧化铌阴极能够提高电脱氧的反应速率和效果.研究表明,12MPa压制成型后经1 200℃烧结的阴极片,电脱氧效果最佳.     

氧化锆微注射成形工艺参数

采用微注射成形工艺制备3Y-TZP陶瓷材料,借助正交实验法,以烧结后试样的抗弯强度作为目标值,研究注射温度、注射速度、塑化压力及保压速度等工艺参数的影响。检测烧结试样的维氏硬度、断裂韧性等力学性能以及收缩率、晶粒大小和相对密度,并且分别使用X射线衍射、扫描电镜及能谱仪分析和观察烧结后的显微组织、晶粒形态及成分分布。最后通过变异数分析,找出最佳注射工艺参数,进行实验验证。结果显示:在160℃注射温度、200 mm/s注射速度、12 MPa塑化压力及20 mm/s保压速度下进行氧化锆粉末的微注射成形,烧结试样具有最佳综合性能:抗弯强度为1 003 MPa,硬度1300 HV,相对密度为98.8%,断裂韧性为4 MPa-m1/2,烧结收缩率为24%,平均晶粒尺寸约0.45 um,所得组织为四方晶(t-ZrO2)及单斜晶(m-ZrO2)2种构成相。     

ITER用高性能轧制W板制备及其组织性能研究

以纯度为99.95%的钨粉为原料,在200 MPa压力下冷等静压成形,2 300℃于H2气氛中进行烧结制得钨烧结坯。钨烧结坯在1 250~1 500℃于H2气氛中经过4道次轧制制得接近理论密度的钨板。通过金相、维氏硬度和高温拉伸强度分析了轧制过程和退火过程中钨板组织和性能的变化规律。通过电子背散射衍射(EBSD)分析了退火过程中钨板织构的衍变。结果表明:轧制过程中钨板的密度、维氏硬度和高温抗拉强度随材料变形量的升高而增大,经过4道次轧制钨板的密度可接近理论密度,维氏硬度和高温抗拉强度分别为HV450和540 MPa;轧制态的钨板晶粒组织有明显沿RD方向拉长,1 350℃退火时,形变织构明显减弱,晶粒取向分布趋于随机。通过统计面积分数分析得到1 350℃钨板晶粒再结晶组织比例占65.8%。     

难熔金属注射成形的研究

采用金属粉末注射成形技术成功制得了形状复杂的纯钨和纯钼零件。粉末注射成形工艺为：粉末装载量为52%,注射温度为165℃,注射压力为65 MPa,溶剂脱脂＋热脱脂两步脱脂法,经2300℃氢气气氛烧结,钨烧结样品的密度可达18.26 g.cm^-3,相对密度为94.61%;经1900℃氢气气氛烧结,钼烧结样品的密度为9.7 g.cm^-3,相对密度达95.09%,制品尺寸精度控制在±0.3%以内。同时,通过实验对比研究了掺加少量的稀土氧化物（La2O3,Y2O3）对注射成形钨和钼制品性能的影响。实验结果表明：稀土元素氧化物的添加,提高了注射成形钨和钼制品烧结后的密度,明显细化了烧结后样品的晶粒,稀土氧化物作为第二相粒子弥散分布于晶界处,提高了注射成形钨和钼制品的强度。     

冷压烧结法制备碳纤维增强铜基复合材料的研究

以碳纤维和Cu粉为原材料,采用冷压烧结法制备了碳纤维增强铜基复合材料,研究了压制压力、烧结温度和烧结时间对复合材料性能的影响。结果表明:随着压力的增加,冷成形压坯的密度和压溃强度均先快速提高,而后缓慢增长,较合理的压制压力为238~286 MPa;碳纤维增强铜基复合材料的密度和强度都随着烧结温度的增大而快速提高,但在800℃以上,密度基本不变,强度开始下降;提高烧结温度可提高复合材料的抗摩擦性能,当烧结温度超过750℃时,摩擦性能基本保持不变;碳纤维增强铜基复合材料的密度、强度和抗摩擦性能都随着烧结时间的延长而提高,但是提高速度越来越慢,当烧结时间超过40 min后,这些性能基本不再随时间变化。     

Ni对热变形Nd-Fe-B磁体磁性能及力学性能的影响

为提高热压结合热变形工艺制备的各向异性Nd-Fe-B磁体的力学性能,向磁体中掺杂高熔点、弱磁性金属元素Ni,研究Ni含量对磁体的磁性能、力学性能以及微观结构的影响。掺杂Ni的质量分数在0~5%之间时,Nd-Fe-B复合磁体的抗弯强度先增大后减小,2%Ni含量的Nd-Fe-B复合磁体具有最高平均抗弯强度212 MPa,其最大磁能积保持在40 MGOe以上。从磁体断口形貌上看,Ni会在孔洞附近富集,强化增韧晶界相,从而提高晶界相的裂纹扩展阻力,使抗弯强度提高。     

烧结钕铁硼的微观结构研究

利用扫描电镜观察了35AH、N35、N50和33SH四个牌号不同尺寸长方体形的烧结Nd-Fe-B磁体的微观结构。从晶粒的大小、形状、分布和晶界状况等方面比较了高性能与普通性能烧结Nd-Fe-B磁体微观结构的异同。高性能磁体的微观结构更接近于理想状态，即主相晶粒细小，分布均匀，形状规则，有适量的呈薄层状分布的富钕相将主相晶粒包裹。     

烧结Nd-Fe-B磁体的温度稳定性缺陷分析

采用SEM、EDAX及粒度分析手段,研究了烧结Nd-Fe-B磁体开路磁通不可逆损失(hirr)异常偏高的原因。结果表明,磁体显微组织中晶粒尺寸分布不均匀及存在少量粗大晶粒,是导致其温度稳定性缺陷的主要因素,表现为少数产品hirr异常偏高。在磁体工业生产过程中,改进原料的铸锭和制粉技术,避免出现粗大粉末颗粒,减少极细粉末颗粒的数量,保证磁体显微组织精细均匀,是制备温度稳定性高的烧结Nd-Fe-B磁体的基本措施。     

烧结Nd-Fe-B磁体晶界扩散TbH2高温稳定性及其机理

采用涂敷方式,在烧结钕铁硼表面均匀涂敷TbH₂粉末,经过不同的扩散温度处理,制备出晶界扩散磁体。研究了晶界扩散TbH₂对烧结Nd-Fe-B磁体常温磁性能及高温稳定性的影响,并分析了磁体矫顽力提升的机理。常温磁性能研究表明,扩散磁体经过890 ℃+490 ℃工艺处理后性能达到最优,矫顽力从1 383 kA/m提升到1 988 kA/m。高温磁性能结果显示,扩散磁体200 ℃的矫顽力温度系数|β|比原始磁体降低0.032%/℃,磁通不可损失hirr比原始磁体降低21.47%,扩散TbH₂明显提高了烧结Nd-Fe-B磁体的热稳定性。分析得出,晶界扩散TbH₂磁体矫顽力提升的机理是Nd₂Fe₁₄B晶粒外延层形成了（Tb, Nd）₂Fe₁₄B核壳结构,提高了磁晶各向异性场;同时改善了磁体的微观组织结构,有效地隔绝了晶粒之间的磁交换耦合作用。      

Nd-Fe-B磁体烧结致密化过程的研究

定量描述了Nd-Fe-B磁体的烧结致密化过程, 分析了有效稀土含量、合金粉末粒度与烧结致密化过程的关系, 讨论了Nd-Fe-B磁体烧结过程的致密化机制. Nd-Fe-B磁体烧结致密化过程可分为3个阶段, 即致密化过程迅速进行阶段、缓慢进行阶段、相对稳定阶段;随着烧结温度的上升, 第一阶段表现得更为突出, 第二阶段对应的烧结时间区段大大缩短. 有效稀土含量的提高、合金粉末粒度的减小显著促进Nd-Fe-B磁体烧结致密化过程. 主相颗粒重排以及主相颗粒长大与形状适位性变化是Nd-Fe-B磁体烧结过程的两类主要致密化机制, 而且后者对于Nd-Fe-B烧结磁体实现完全致密化起着决定性的作用.     

生坯密度对烧结 Nd-Fe-B 磁体结构与性能的影响

结合国内烧结Nd-Fe-B磁体工业生产过程，研究了压制成型时生坯密度变化对烧结Nd—Fe—B磁体致密化程度、显微组织、取向度与磁性能的影响。试验结果表明，生坯密度的提高可促进烧结致密化过程，抑制烧结过程晶粒的不均匀长大，提高取向度，改善磁性能。     

Effects of Pr-Cu-Ti intergranular addition on microstructure and magnetic properties of heavy-rare-earth-free Nd-Fe-B sintered magnets

By intergranular addition of Pr-Cu-Ti alloy powders in the Nd-Fe-B sintered magnets with the normal B component, we propose an approach to the optimization of grain boundary and local Nd-Fe-B composition system. The coercivity is enhanced from 1.42 to 1.86 T, while further addition leads to a reduction in remanence and coercivity. The analyses of phase composition reveal that Ti mainly exists in the form of metallic Ti alloy, and part of Ti combines with B to form the TiB₂ phase after the liquid phase sintering process. This process results in a consumption of B in the local Nd-Fe-B composition system and a change of the grain boundary component, which contributes to the formation process of the RE₆(Fe,M)₁₄ phase after the annealing process. Therefore, with the modification of grain boundary and composition system, the intergranular addition of Pr-Cu-Ti induces the generation of continuous thin grain boundary phases. It promotes the intergrain exchange decoupling, increasing the coercivity in the annealed magnet. While the excess addition results in the segregation of TiB₂, as well as the precipitation of TiB₂ into the Nd-Fe-B phase, which leads to structural defects. Thus, the further effort for the addition alloy with Ti to reduce the deterioration of the microstructure will lead to further improvement in magnetic properties.     

Study on Fabrication Process of Anisotropic Injection Bonded Nd-Fe-B Magnets

This study is on the injection molding process for the fabricating anisotropic Nd-Fe-B bonded magnets. The effects of powder loading, particle size of the magnetic powder, polymer binder and the fabricating process on the magnetic and the mechanical properties of anisotropic Nd-Fe-B magnets were investigated. The proper powder loading, particle size and binder are 60%(vol%), 75–106 μm and PA 1010, respectively. The optimum condition for good magnetic properties of anisotropic injection bonded Nd-Fe-B magnets is mixing the binder and the chemicals in the temperature between 205–215 °C, injection temperature of 265 °C, the injection pressure of 5–6 MPa, the press time of 5 second, and molding temperature of 80 °C. The magnetic properties of anisotropic bonded Nd-Fe-B magnets made in above conditions from d-HDDR powder were: B_r=0.72 T, _iH_c=983 kA/m, (BH)_max=75 kJ/m^c.     

Improvement of coercivity and thermal stability of Nd-Fe-B sintered magnets by intergranular addition of Tb80Fe20 alloy

To improve the coercivity and temperature stability of Nd-Fe-B sintered magnets for high-temperature applications, the eutectic Tb₈₀Fe₂₀ (wt%) alloy powders were added into the Nd-Fe-B sintered magnets by intergranular method to enhance the coercivity (H_cj) and thermal stability. The microstructure, magnetic properties and thermal stability of the Nd-Fe-B magnets with different Tb₈₀Fe₂₀ contents were studied. The experimental results demonstrate that the coercivity (H_cj) of the sintered Nd-Fe-B magnet is significantly enhanced from 14.12 to 27.78 kOe, and the remanence (B_r) decreases not obviously by introducing 4 wt% Tb₈₀Fe₂₀ alloy. Meanwhile, the reversible temperature coefficients of coercivity (β) and remanence (α) of the Nd-Fe-B magnets are increased from ?0.5634%/℃ to ?0.4506%/℃ and ?0.1276%/℃ to ?0.1199%/℃ at 20–170 ℃, respectively. The Curie temperature (T_C) of the Nd-Fe-B magnet is slightly enhanced with the increase of Tb₈₀Fe₂₀ content. Moreover, the irreversible flux magnetic loss (h_irr) is obviously reduced as Tb₈₀Fe₂₀ addition increases. Further analysis of the microstructure reveals that a modified microstructure, i.e. clear and continuous RE-rich grain boundary layer, is acquired in the sintered magnets by introducing Tb₈₀Fe₂₀ alloy. The associated mechanisms on improved coercivity and thermal stability were comprehensively researched.     

Improvement of microstructure and coercivity for Nd-Fe-B sintered magnets by boundary introducing low melting point alloys

Different from the grain boundary diffusion process(GBDP),which is suitable for modifying thin magnet,a green-pressing agents permeation process(GAPP) that uses low melting point alloys was applied to the Nd-Fe-B green compact with a thickness over 15 mm to reconstruct the boundary microstructure of a sintered Nd-Fe-B magnet.The coercivity increases from 12.3 kOe for the sample free of Pr_(80)Al_(20) to16.8 kOe for the sample with 2 wt% Pr_(80)Al_(20).By further increasing the Pr_(80)Al_(20) content to 3 wt%,the coercivity increases slightly,but the remanence and H_k/H_(cj) deteriorate obviously.The optimal comprehensive properties of H_(cj)=16.8 kOe,B_r=13.4 kG and H_k/H_(cj)=0.975 are obtained at 2 wt% Pr_(80)Al_(20),since matrix phase grains are separated by relatively continuous thin grain boundary layers,which weaken the magnetic coupling between adjacent grains.The coercivities of the samples from the GAPP that use2 wt% Pr_(80)Al_(20),Pr_(70)Al_(30) and Pr_(60)Tb_(20)Al_(20) alloys,respectively,can be enhanced to a large extent.However,the coercivity of the magnet reconstructed with Pr_(80)Al_(20) is lower than that of the sample with Pr_(60)Tb_(20)Al_(20) but is higher than that of the sample reconstructed with Pr_(70)Cu_(30) alloy.Moreover,the coercivity of the sample from the GAPP using 2 wt% Pr_(80)Al_(20) is much higher than that of the sample from the GBDP,which is due to a nearly uniform boundary microstructure from the surface to the interior of the thick magnet from the GAPP,thus providing new insights into the fabrication of thick and bulky permanent magnets with high coercivity.