Spark plasma sintering of silicon nitride using nanocomposite particles

The spark plasma sintering (SPS) of silicon nitride (Si₃N₄) was investigated using nanocomposite particles composed of submicron-size α-Si₃N₄ and nano-size sintering aids of 5 wt% Y₂O₃ and 2 wt% MgO prepared through a mechanical treatment. As a result of the SPS, Si₃N₄ ceramics with a higher density were obtained using the nanocomposite particles compared with a powder mixture prepared using conventional wet ball-milling. The shrinkage curve of the powder compact prepared using the mechanical treatment was also different from that prepared using the ball-milling, because the formation of the secondary phase identified by the X-ray diffraction (XRD) method and liquid phase was influenced by the presence of the sintering aids in the powder compact. Scanning electron microscopy (SEM) observations showed that elongated grain structure in the Si₃N₄ ceramics with the nanocomposite particles was more developed than that using the powder mixture and ball-milling because of the enhancement of the densification and α-β phase transformation. The fracture toughness was improved by the development of the microstructure using the nanocomposite particles as the raw material. Consequently, it was shown that the powder design of the Si₃N₄ and sintering aids is important to fabricate denser Si₃N₄ ceramics with better mechanical properties using SPS.     

Bio-inspired structured boron carbide-boron nitride composite by reactive spark plasma sintering

Nature creates composite materials with complex hierarchical structures that possess impressive mechanical properties enhancement capabilities. An approach to improve mechanical properties of conventional composites is to mimic the biological material structured ‘hard’ core and ‘soft’ matrix system. This would allow the efficient transfer of load stress, dissipation of energy and resistance to cracking in the composite. In the current study, reactive spark plasma sintering (SPS) of boron carbide B₄C was carried out in a nitrogen N₂ gas environment. The process created a unique core-shell structured material with the potential to form a high impact-resistant composite. Transmission electron microscopy observation of nitrided-B₄C revealed the encapsulation of B₄C grains by nano-layers of hexagonal-boron nitride (h-BN). The effect of the h-BN contents on hardness were measured using micro- and nano-indentation. Commercially available h-BN was also mechanically mixed and sintered with B₄C to compare the effectiveness of nitrided B₄C. Results have shown that nitrided B₄C has a higher hardness value and the optimum content of h-BN from nitridation was 0.4%wt with the highest nano-indentation hardness of 56.7 GPa. The high hardness was attributed to the h-BN matrix situated between the B₄C grain boundaries which provided a transitional region for effective redistribution of the stress in the material.     

Fabrication of silicon nitride nanoceramics—Powder preparation and sintering: A review

Fine-grained silicon nitride ceramics were investigated mainly for their high-strain-rate plasticity. The preparation and densification of fine silicon nitride powder were reviewed. Commercial sub-micrometer powder was used as raw powder in the “as-received” state and then used after being ground and undergoing classification operation. Chemical vapor deposition and plasma processes were used for fabricating nanopowder because a further reduction in grain size caused by grinding had limitations. More recently, nanopowder has also been obtained by high-energy milling. This process in principle is the same as conventional planetary milling. For densification, primarily hot pressing was performed, although a similar process known as spark plasma sintering (SPS) has also recently been used. One of the advantages of SPS is its high heating rate. The high heating rate is advantageous because it reduces sintering time, achieving densification without grain growth. We prepared silicon nitride nanopowder by high-energy milling and then obtained nanoceramics by densifying the nanopowder by SPS.     

氮化硅晶须对反应烧结氮化硅多孔陶瓷介电性能的影响

以硅粉和氮化硅晶须为原料,通过添加30%(质量分数)成孔剂球形颗粒,以聚乙烯醇作粘结剂,采用干压成型工艺,反应烧结制备了多孔氮化硅陶瓷,分析对比了氮化硅晶须对反应烧结氮化硅多孔陶瓷介电性能的影响.实验结果表明,随着氮化硅晶须加入量的升高,氮化硅多孔陶瓷的介电常数和介电损耗都升高,介电性能恶化.     

放电等离子烧结制备高导热SiC_P/Al电子封装材料

为了满足电子封装材料越来越高的性能要求,采用放电等离子烧结(SPS)工艺制备了SiCP/Al复合材料。研究了烧结温度和保温时间等工艺条件对SiCP/Al复合材料组织形貌和性能的影响。结果表明:采用SPS烧结,温度为700℃、保温时间为5 min时,所制备的70 vol%SiCP/Al复合材料热导率达到195.5 W(m.K)-1,与传统15%W-Cu合金相当,是Kovar合金的10倍,但密度小,仅为3.0 g.cm-3;其热膨胀系数为6.8×10-6K-1,与基板材料热膨胀系数接近;抗弯强度为410 MPa,抗拉强度为190 MPa,达到了电子封装材料对热学性能和力学性能的要求。     

放电等离子烧结(SPS)YAG陶瓷的初步研究

研究了采用放电等离子烧结(Spark Plasma Sintering SPS),利用高纯的氧化钇和氧化铝,在1500～1700℃,真空度优于10Pa,反应快速合成YAG陶瓷,但试样的致密度不高,而低气孔率是制备透明陶瓷的关键,实验表明,TEOS的掺加和粉料粒度的减小对烧结试样致密度的提高有一定的作用.     

Microstructure and thermal conductivity of spark plasma sintering AlN ceramics

Abstract

Dense aluminium nitride ceramics were prepared by spark plasma sintering at a lower sintering temperature of 1700°C with Y₂O₃, Sm₂O₃ and Dy₂O₃ as sintering additives respectively. The effects of three kinds of sintering additives on the phase composition, microstructure and thermal conductivity of AlN ceramics were investigated. The results showed that those sintering additives not only facilitated the densification via the liquid phase sintering mechanism, but also improved thermal conductivity by decreasing oxygen impurity. Sm₂O₃ could effectively improve thermal conductivity of AlN ceramics compared with Y₂O₃ and Dy₂O₃. Observation by scanning electron microscopy showed that AlN ceramics prepared by spark plasma sintering method manifested quite homogeneous microstructures, but AlN grain sizes and shapes and location of secondary phases varied with the sintering additives. The thermal conductivity of AlN ceramics was mainly affected by the additives through their effects on the growth of AlN grain and the location of secondary phases.     

放电等离子烧结技术制备 Ti合金表面 HA活性涂层

采用放电等离子烧结(SPS)技术，低温、快速地在Ti合金表面制备HA活性涂层。研究了涂层成分和厚度对涂层与基体结合强度的影响，观察了断口形貌。结果表明：随着涂层厚度的减小，结合强度提高；梯度涂层能提高涂层与基体的结合强度；特别是经钝化处理后烧结的试样，涂层与基体的结合强度显著提高，最高达到了64MPa，超过目前使用的生物涂层种植体材料的指标。     

氮化铝一维纳米结构制备方法和物性研究的最新进展

全面总结了近年来氮化铝一维纳米结构的各种制备方法及物理性能等研究的最新进展,并提出了有待进一步深入研究的一些发展方向。     

Investigation of Ti coatings on cubic boron nitride (cBN) grits by discharge treatment in spark plasma sintering system

The Ti coatings on cubic boron nitride (cBN) grits were prepared by discharge treatment on a mixture of Ti powders and cBN grits in spark plasma sintering system. The uniform and full coatings with a thickness of ～1.2 μm were prepared at 850 °C for 60 min, which were constituted with TiB₂, TiN, and Ti phases. The compressive fracture strength and toughness impact of the Ti-coated cBN grits were 11.6% and 7.4% higher than the cases of the pristine ones, respectively. With the aid of Ti coatings, the interface bonding strength between cBN grits and Fe-based matrix was improved by 335 MPa in the Fe-based matrix/cBN composites.     

放电等离子烧结Ti-Al系金属间化合物

用机械合金化法(MA)制备了Ti-45% Al纳米晶合金粉末,并对其进行放电等离子烧结(SPS),烧结时间仅为5min.用D-maxIIA型X射线衍射仪、JEM-2000EX型透射电子显微镜对粉末和烧结块体的微观组织及机械性能进行了研究.研究表明:Ti和Al的粉末随着球磨时间的延长,粉末有明显的细化趋势,球磨5h即有非晶产生,球磨20h后得到接近完全非晶相;采用SPS烧结技术,在1200℃下能够制备出较高硬度的TiAl金属间化合物块体材料.     

放电等离子烧结（SPS）制备DyB6多晶块体材料

以微米硼粉和采用氢直流电弧法制备出Dx纳米粉末为原料,利用放电等离子烧结（SPS）技术制备了DyB6多晶块体材料,并分析了烧结温度对样品微观结构及性能的影响。实验结果表明当烧结压力为60MPa,烧结温度为1275℃时,可得到单相DyB6。烧结工艺为1425℃,60MPa所制备样品的密度、维氏硬度和抗弯强度分别为5.191g/cm3、23.32GPa和112.8MPa,当阴极温度为1933K时的发射电流密度为3.6A/cm2。     

大气中烧结多孔氮化硅的相变和氧化机理研究

以α—Si3N4为原料，分别以Y2O3-Al2O3和MgO-Al2O3-SiO2两个体系作为烧结助剂，在大气中对氮化硅坯体在1400～1550℃进行烧结。研究了烧结温度、烧结助剂体系对氮化硅的氧化程度、氧化产物的影响。结果表明，以MgO-Al2O3-SiO2作烧结助剂有利于α-Si3N4转变为β-Si3N4，且该烧结助剂体系的的抗氧化能力也明显优于Y2O3-Al2O3体系。氮化硅在不同温度烧结时形成的氧化产物不同。     

Properties of reaction bonded silicon nitride obtained from slip cast preforms

Fabrication of silicon preforms of high green density (>1·2 g/cm³) by slip casting of silicon (in aqueous medium) has been studied. The nitridation product consists of 59–85% α-Si₃N₄, 7–22%β-Si₃N₄ and 7–23% Si₂N₂O phase. The amounts of un-nitrided silicon were negligible. The microstructure is either granular or consists of needle-like grains (α-Si₃N₄) and whiskers deposited in the large pores. MOR values of the specimens are almost constant up to 1000°C or 1400°C or show slight increase up to 1000°C or 1200°C. In some cases a little dip around 1200°C, then a sharp increase in MOR up to 1400°C was observed.K _ic values are almost constant up to 1000°C, and thereafter increase sharply. Pore size distribution, existence of Si₂N₂O phase and oxidation of RBSN at high temperatures have been considered for the explanation of the observed behaviour.     

放电等离子烧结新型NdFeB永磁材料工艺研究

采用放电等离子烧结技术制备了新型NdFeB磁体，研究了烧结工艺和热处理工艺对磁体的磁特性、尺寸精度及致密度的影响。同时利用B-H回线仪、扫描电子显微镜对其磁特性、显微组织结构进行了分析测试。结果表明，这种新型的烧结NdFeB磁体具有独特的显微组织结构，主相NdFe14B晶粒细小、尺寸均匀，富钕相弥散分布在主相边界上。获得最佳工艺条件下制备的磁体的磁特性为：最大磁能积(BHmax)240kJ／m^3，内禀矫顽力(Hci)1160kA／m，磁体的密度达到7．58g／cm^3，接近材料的理论密度，同时磁体的尺寸精度达到20μm。     

聚碳硅烷氮化热解法制备Si3N4纤维

将PCS电子束交联丝在氨气氛中氮化热解、脱碳氨化,继在氮气氛中高温热引发缩合/转氨基反应,生成硅氮烷并最终形成氮化硅(Si3N4)纤维。所制备的Si3N4纤维白色透明,横截面和表面均光滑致密,无明显缺陷和孔洞。还研究了氮化热解的反应机理以及热解工艺对氮化硅(Si3N4)纤维结构和性能的影响。红外光谱和元素分析的结果显示,氮化热解脱碳彻底,Si3N4纤维C含量<1%;烧结温度提高,N含量随之增加,O含量则先增后减;烧结温度不超过1500℃,纤维为无定型。力学性能结果分析表明,随热解温度的提高,纤维力学性能先提后降,1300℃时达到最大值。氮化热解过程是采用NH3进行脱碳氨化,并在N2气氛下高温热引发缩合/转氨基反应产生硅氮烷并最终形成Si3N4的过程。     

Effect of NH3 flow rate on growth, structure and luminescence of amorphous silicon nitride films by electron cyclotron resonance plasma

In this paper, hydrogenated amorphous silicon nitride (a-SiN_x:H) films have been deposited using an electron cyclotron resonance chemical vapor deposition system. The effect of NH₃ flow rate R on the deposition rate, structure and luminescence were studied using various techniques such as optical emission spectroscopy, Fourier Transform Infrared absorption (FTIR), X-ray photoelectron spectroscopy (XPS) and fluoro-spectroscopy, respectively. Optical emission behavior of SiH₄ + NH₃ plasma shows that atomic Si radical concentration determines the film deposition rate. Structural transition of a-SiN_x film from Si-rich one to near-stoichiometric/N-rich one with R was revealed by FTIR and the two phase separation of a-Si and a-Si₃N₄ was also convinced in Si-rich SiN_x films by XPS. Either photo- or electroluminescence for all the SiN_x films with R > 3 sccm shows a strong light emission in visible light wavelength range. As R < 6 sccm, recombination of electrons and holes in a-Si quantum dots is the main mechanism of photo/electroluminescence for Si-rich SiN_x films, however, for photoluminescence, gap states' luminescence is also in competition; as R > 6 sccm, light emission of the SiN_x film originates from defect states in its band gap.     

Effect of sintering temperature on optical properties and microstructure of translucent zirconia prepared by high-pressure spark plasma sintering

Aiming to characterize the effect of sintering temperature on transparency of zirconia, we have evaluated the optical properties and microstructure of translucent cubic zirconia prepared by high-pressure spark plasma sintering (SPS) at 1000–1200 ^○C. Color centers (oxygen vacancies with trapped electrons) and residual pores were primary defects in the samples. In SPS samples, the total forward transmittance and in-line transmittance are mainly affected by color centers with a limited contribution from residual pores; in contrast, the changes in reflectance are only related to the porosity. The amounts of color centers and residual pores increase with sintering temperature that reduces the total forward and in-line transmittance of the as-sintered zirconia. Annealing in oxidizing atmosphere improves the total forward and in-line transmittance. During the annealing, the concentration of color centers decreases but the porosity increases.     

Effect of sintering temperature on optical properties and microstructure of translucent zirconia prepared by high-pressure spark plasma sintering

Abstract

Aiming to characterize the effect of sintering temperature on transparency of zirconia, we have evaluated the optical properties and microstructure of translucent cubic zirconia prepared by high-pressure spark plasma sintering (SPS) at 1000–1200 ^○C. Color centers (oxygen vacancies with trapped electrons) and residual pores were primary defects in the samples. In SPS samples, the total forward transmittance and in-line transmittance are mainly affected by color centers with a limited contribution from residual pores; in contrast, the changes in reflectance are only related to the porosity. The amounts of color centers and residual pores increase with sintering temperature that reduces the total forward and in-line transmittance of the as-sintered zirconia. Annealing in oxidizing atmosphere improves the total forward and in-line transmittance. During the annealing, the concentration of color centers decreases but the porosity increases.