预加SiC粉的碳热还原法制备SiC-B_4C复合陶瓷粉

为了改善制备SiC-B_4C复合陶瓷的传统工艺流程(B_4C与SiC机械混合后烧结),提高B_4C与SiC在微观尺度上结合的均匀性和紧密性,使其更有利于烧结致密化,从而进一步提高复合陶瓷的综合性能,在碳热还原法制备B_4C的配料中分别添加占总质量1%、2%、3%、4%、5%的SiC粉,干混均匀,再加入5%(w)的水搅拌均匀,然后采用油压千斤顶以20 MPa压力模压成型为15 mm×10 mm的样坯,在80℃干燥10 h后,在1 800℃空气气氛中频感应炉中烧结50 min,最后进行XRD分析和SEM观察。结果表明:采用在碳热还原法制备B_4C的配料中预加SiC粉的方法,成功制备了B_4C分布均匀、SiC与B_4C结合紧密的SiC-B_4C复合陶瓷粉。随着SiC添加量的增多,B_4C衍射峰强度明显增强,B_4C晶粒形貌变得更加规则,且晶粒尺寸有所增大,表明SiC添加量增多促进了B_4C的生成及其晶粒的生长。     

不同种类碳源对SiC-B4C超细复合粉体合成的影响

选择不同种类的碳源(炭黑和淀粉)、硅溶胶和硼酸为原料,采用碳热还原法在氩气气氛下合成SiC-B4C复合粉体.对比研究了不同碳源对SiC-B4C超细复合粉体的质量失重率、物相组成、粒度大小及分布等方面的影响.结果表明:以炭黑为碳源合成SiC-B4C复合粉体的适宜条件为在1550℃下保温2h.而以淀粉为碳源合成SiC-B4...     

自蔓延合成Al4SiC4和B4C及其在含碳耐火材料中的应用

以金属铝粉、硅粉、炭黑或石墨为原料,采用自蔓延化学炉法制备了Al4SiC4粉体,并将其添加到以板状刚玉、电熔刚玉、氧化铝微粉和石墨为主要原料的铝碳材料中,经混合、150 MPa冷等静压成型后于1100℃保温5h氮气保护烧成,研究其对铝碳材料的物理性能、抗氧化性能和抗水化性能的影响;以B203、金属Mg、炭黑和超细石墨为主要原料,采用自蔓延镁热还原法制备了B4C粉体,并将自蔓延产物添加到以电熔镁砂和超细石墨为主要原料的低碳镁碳砖中,经混合、200 MPa干压成型后于1600℃5h埋炭烧成,研究其对镁碳材料的物理性能、抗氧化性能的影响.结果表明:1)以Al、Si、炭黑或石墨为原料可以合成纯度高、不合Al4C3相的Al4SiC4粉体;添加7％ Al4SiC4粉体的铝碳材料具有良好的常温和高温性能,具有良好的抗氧化性和抗水化性能.2)以B2O3、Mg和炭黑为原料可以合成晶粒细小、活性较高的B4C粉体;添加B4C复合粉体的低碳镁碳砖具有良好的常温性能和热态强度,其抗氧化性能优于添加市售B4C和金属Al粉的试样.     

Fe_2O_3对天然原料合成Al_4SiC_4/Al_4O_4C复合耐火材料的影响(英文)

以焦宝石、活性炭和铝粉为原料并添加Fe2O3后制备了Al4SiC4/Al4O4C复合耐火材料。利用化学分析、X射线衍射和扫描电镜研究了Fe2O3对所制备复合材料的物相组成和显微结构的影响。结果表明:在烧结过程中,从1400℃开始,Fe2O3转变为低熔点物相Fe3Si,产生液相促进Al4SiC4成核、细化晶粒,同时包裹Al4SiC4。此外,未添加Fe2O3的样品中生成的Al4O4C短纤维,Fe2O3的加入使得Al4O4C相变为细小的晶粒。     

超细炭素原料对Al2O3-ZrO2-C材料性能及微孔结构的影响

研究比较了粒度＜25 nm的炭黑A、粒度＜50 nm的炭黑B及粒度＜0.147 mm的鳞片石墨3种炭素原料对铝锆碳滑板材料的性能及微孔结构的影响,并采用扫描电镜观察材料中原位生成SiC晶须的显微结构变化.结果表明由于炭黑A和炭黑B的粒度细,它们在烧结过程中与硅粉更容易发生反应原位生成SiC晶须;SiC晶须发育良好,填充气孔,使试样中直径d＜1μm的微孔数量大大增加,同时提高了试样的强度.因此,添加炭黑A、炭黑B的试样的性能优于添加鳞片石墨的,而以添加炭黑A的最好.     

保温温度对固相烧结SiC/B4C复合陶瓷力学性能及微观形貌影响

以碳化硅、碳化硼微粉为原料,酚醛树脂为粘结剂,用固相烧结法制备了高温性能优异的SiC/B4C复合陶瓷,研究了保温温度对SiC/B4C复合陶瓷力学性能及微观形貌的影响.研究结果表明:2150℃保温45min可制备出相对密度高达96.60％且综合性能优异的SiC/B4C复合陶瓷,其维氏硬度为26.5GPa,断裂韧性为4.04MPa·m1/2,抗弯强度为345MPa;B4C晶粒周围被SiC呈板状结构包裹,少量B2O3存在于晶界处;当温度高于2150℃时,出现整体排列的片层状SiC,SiC由6H-SiC向4H-SiC转变.     

专利信息

一种碳化铝铬陶瓷粉体的常压合成方法;一种含铌的SiC陶瓷先驱体的制备方法;一种用于导电坩埚的多元复相陶瓷材料及其制备方法;一种硼化物-碳化硅-碳化硼三元陶瓷基复合材料及其制备方法;压电陶瓷坯膜的制备方法     

固相反应合成Al4SiC4材料

采用粒度14μm的磨料级碳化硅,粒度10 μm的工业级金属铝粉和粒度5 μm的工业级炭黑粉为原料,按SiCAlC质量比为225919配料制成试样,在氩气保护下,分别在1200℃8 h、1600℃2 h和1650℃2 h烧成,研究了通过固相反应合成Al4SiC4材料的条件和动力学过程.通过X射线衍射仪进行物相分析,扫描电子显微镜和透射电子显微镜的形貌分析以及能谱分析确定成分.结果表明反应体系在1200℃以下,铝和炭黑反应首先生成中间相Al4C3;从1200℃开始通过SiC+Al4C3=Al4SiC4固相反应生成Al4SiC4;当合成温度达到1650℃时,获得Al4SiC4材料;制备的Al4SiC4材料的颗粒均匀,尺寸在几百纳米到几微米之间.     

锆英石碳热还原合成ZrB_2—SiC复合粉体

以锆英石、氧化硼、活性炭为原料,采用碳热还原合成工艺制备了ZrB2—SiC复合粉体,并对合成过程进行了热力学分析。考察了反应温度及原料配比对碳热还原合成ZrB2—SiC复合粉体的物相的组成、含量和显微结构的影响。结果表明:提高反应温度有利于ZrB2—SiC复合粉体的合成,适当过量氧化硼及活性炭有利于ZrB2—SiC复合粉体的合成。合成ZrB2—SiC复合粉体的最优参数为:当ZrSiO4、B2O3和C的摩尔比为1∶2∶12,在1 773K保温3h,可得到几乎纯相的ZrB2—SiC复合粉体。     

B4C-部分石墨化炭黑复合粉体的合成及其抗氧化性

分别以64.7%的硼粉 35.3%的炭黑或55%的硼粉 45%的炭黑为试样组成,分别在真空和非真空条件下,采用自蔓延燃烧法于1400℃保温10~20min进行了B4C-部分石墨化炭黑复合粉体的合成研究。采用XRD、SEM及电子探针等方法对合成粉体的物相及形貌进行了分析;以差热法(TG-DSC)研究了合成粉体的氧化特性。结果表明:炭黑和硼粉加入量(w)分别为45%和55%时,经自蔓延燃烧反应后可以得到粒度均匀的碳化硼(B4C)粉体,且碳黑已部分石墨化。与工业B4C相比,复合粉体中的B4C具有更好的保护碳不被氧化的特性。     

In Situ Polysilane-Derived Silicon Carbide Particulates Dispersed in Silicon Nitride Composite

A dense (97% of theoretical density) Si₃N₄—SiC composite containing 10 wt%β-SiC was prepared by introducing a SiC phase by the pyrolysis of a polymeric SiC precursor. The composite material was produced by mixing an alkyl/aryl-substituted polysilane with Si₃N₄ powder and, by subsequently forming green compacts, pyrolyzing the polymeric species, and finally sintering the sample. Synthesis and characterization of the polymeric compound was described. Its transformation reactions to SiC and the characterization of the ceramic residue were also studied. High ceramic yields were obtained by curing the as-synthesized polysilane at 500°C in an Ar atmosphere. The heat treatment had no effect on the good solubility of the polymeric precursor in organic solvents. This was important for processes such as infiltration, sealing, and coating and for the mixing of the polymer with powders for the preparation of homogeneous composite ceramics. The dense microstructure of the pyrolyzed and sintered Si₃N₄ powder–polysilane mixture exhibited reduced grain growth of the Si₃N₄ particles and a very homogeneous distribution of the in situ-formed β-SiC phase.     

Improved thermal shock stability and oxidation resistance of low-carbon MgO–C refractories with introduction of SiC whiskers

This research focuses on the utilization of SiC whiskers synthesized from rice husk powders in low-carbon magnesia–carbon (MgO–C) refractories, and attempts to reduce the flake graphite content in refractories by adding synthesized SiC whiskers. The effect of the addition amount of SiC whiskers on the microstructure, mechanical properties, thermal shock stability and oxidation resistance of MgO–C refractories with different graphite content was studied. The results indicated that the introduction of SiC whiskers facilitated the generation and growth of ceramic phases in MgO–C refractories. By adding 1 wt% SiC whiskers, the graphite content could be reasonably reduced (from 5 wt% to 4 wt%), and the strength, thermal shock stability and oxidation resistance of refractories were enhanced by the synergistic effect of the introduced SiC whiskers and the generated ceramic phases, the CMOR, CCS, residual CCS, and oxidation resistance were increased by 44, 6, 12 and 27% respectively.     

Effects of SiC content on thermal shock behavior and elastic modulus of cordierite–mullite composites

Cordierite (Mg₂Al₄Si₅O₁₈) is a commercially available ceramic with low fracture toughness that hampers its broad industrial applications. Although several studies have reported the mechanical improvement of cordierite using various reinforcements, modulating its mechanical and thermal shock characteristics is not explored precisely. In the present research, we investigated the manufacturing of cordierite–mullite ceramics and the role of SiC on their thermomechanical properties. The in-situ formed mullite particles were obtained by mixing andalusite-talc-alumina and addition of SiC. It was found that thermal shock behavior and elastic moduli are dependent on SiC content and retained porosity. Furthermore, the addition of SiC to cordierite-based ceramics could enhance the thermal shock resistance via proper activation of the crack bridging mechanism in the matrix of the prepared composite.     

Fe2O3对天然原料合成Al4SiC4/Al4O4C复合耐火材料的影响（英文）

以焦宝石、活性炭和铝粉为原料并添加Fe2O3后制备了Al4SiC4/Al4O4C复合耐火材料。利用化学分析、X射线衍射和扫描电镜研究了Fe2O3对所制备复合材料的物相组成和显微结构的影响。结果表明：在烧结过程中,从1400℃开始,Fe2O3转变为低熔点物相Fe3Si,产生液相促进Al4SiC4成核、细化晶粒,同时包裹Al4SiC4。此外,未添加Fe2O3的样品中生成的Al4O4C短纤维,Fe2O3的加入使得Al4O4C相变为细小的晶粒。

Abstract：

Al4SiC4/Al4O4C composite refractory was synthesized by using flint clay,activated carbon and aluminum powders as the raw materials and Fe2O3 as the additive. The effects of Fe2O3 on the phase composition and microstructure of Al4SiC4/Al4O4C composite refractory were investigated by chemical analysis,X-ray diffraction and scanning electron microscopy. The results show that Fe2O3 transforms into a low melting point phase of Fe3Si above 1 400 ℃,which leads to generate liquid phase and promote the nu-cleation and grain refinement of Al4SiC4 phase. Fe3Si also could coat Al4SiC4 grains. Moreover,the morphology of Al4O4C in Al4SiC4/Al4O4C composite refractory without addition of Fe2O3 is short fibrous-like structure,but changes into fine granules structure after adding Fe2O3.     

In-situ formation of BN layers by nitriding boron powders in BN/Si3N4-based composite ceramics

Boron nitride/silicon nitride (BN/Si₃N₄) composite ceramics were fabricated via the in-situ nitridation of boron (B) and silicon (Si) powders in forming gas (95%N₂/5%H₂) at 1390?°C. The effect of the B content on the phase composition, microstructure, density/porosity, machinability as well as mechanical properties of nitridized BN/Si₃N₄ composite ceramics was investigated. The addition of B slightly increased the nitridation degree of the Si and B powders mixture, and improved the ratio of the β-Si₃N₄ phase significantly at low B contents. B powders may have acted as a nucleating agent to promote the formation of β-Si₃N₄ crystals. A core-shell Si₃N₄/BN structure was revealed by the TEM technique, and the number of BN layers increased with the increase of the B content. The in-situ BN formed by the nitridation of B played a similar role with the BN directly added in enhancing the machinability of the BN/Si₃N₄ composite ceramics. The method of the in-situ nitridation of B is also effective to prepare SiC fiber-reforced BN/Si₃N₄ ceramic matrix composites.     

Reactive Hot Pressing of ZrB2–SiC Composites

A ZrB₂–SiC composite was prepared from a mixture of zirconium, silicon, and B₄C via reactive hot pressing. The three-point bending strength was 506 ± 43 MPa, and the fracture toughness was 4.0 MPa·m^1/2. The microstructure of the composite was observed via scanning electron microscopy; the in-situ -formed ZrB₂ and SiC were found in agglomerates with a size that was in the particle-size ranges of the zirconium and silicon starting powders, respectively. A model of the microstructure formation mechanism of the composite was proposed, to explain the features of the phase distributions. It is considered that, in the reactive hot-pressing process, the B and C atoms in B₄C will diffuse into the Zr and Si sites and form ZrB₂ and SiC in situ , respectively. Because the diffusion of Zr and Si atoms is slow, the microstructure (phase distributions) of the obtained composite shows the features of the zirconium and silicon starting powders.     

Influence of SiAlON addition on the microstructure development of hot-pressed ZrB2–SiC composites

The impact of SiAlON on densification behavior and microstructure of the ZrB₂-SiC composite was investigated. ZrB₂, SiC, and SiAlON were used as the initial materials to produce ZrB₂-SiC composite by hot pressing at 1900 °C. A fully dense composite was obtained having ~99.9% relative density. High-resolution X-ray diffraction (HRXRD) assessment verified the in-situ formation of ZrC, and the presence of residual carbon, SiAlON, and ZrB₂ and SiC phases in the as-sintered ceramic. Furthermore, the thermodynamic calculations confirmed the results attained by HRXRD. In addition, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were utilized for the microstructural investigation. SEM fractographs indicated the impact of SiAlON on the hindering of grain growth and the formation of flaky phases (graphitized carbon or solidified liquid phase) at the grain boundaries. TEM studies revealed the presence of a transparent glassy phase at the particle interfaces. A significant impact of liquid phase sintering was also affirmed in the clean interfaces.     

B4C/SiCw陶瓷喷砂嘴的制备及其冲蚀磨损机理研究

采用热压烧结工艺制备了B4C/SiCw陶瓷喷砂嘴,研究了SiC晶须的含量对B4C/SiCw陶瓷材料性能的影响.以SiC和Al2O3磨料对B4C/SiCw陶瓷喷砂嘴进行冲蚀磨损试验,研究不同磨料对B4C/SiCw陶瓷喷砂嘴冲蚀磨损的影响,分析了其冲蚀磨损机理.结果表明:B4C/SiCw陶瓷喷砂嘴的冲蚀磨损机理主要表现为脆性断裂和磨料粒子对喷嘴的切入所造成的微观切削作用.磨料的硬度和粒度对陶瓷喷嘴的磨损有重要的影响,磨料的硬度和粒度越大,陶瓷喷嘴的磨损速度加快.     

Fabrication of Machinable Silicon Carbide-Boron Nitride Ceramic Nanocomposites

SiC/BN nanocomposite powders with the microstructure of micrometer-sized SiC particles coated with nanometer-sized BN particles were prepared via a chemical reaction, which used a mixture of boric acid (H₃BO₃) and urea (CO(NH₂)₂) as reactants coated on the surface of the SiC particles to react under a nitrogen-gas atmosphere. The results of XRD, TEM, and SAED studies showed that the coating layer (BN) was composed mostly of amorphous and nanometer-sized BN particles at the reaction temperature of 850°C. When the nanocomposite powders were hot-pressed at 1850°C, machinable SiC/BN ceramic nanocomposites with fine grain size and homogeneous microstructure were fabricated. The composite that contained 20 wt% BN exhibited high strength (the three-point bending strength was 588.4 ± 26.8 MPa) and excellent machinability.     

c—SiC—B4C复合材料的制备及其抗氧化性能研究

以生石油焦为炭质原料,向其中掺入定量SiC、B4CN瓷相,以改质煤焦油沥青作为粘结剂,通过模压制备出C—SiC—B4C复合材料。通过XRD、SEM、DTA—TG、EDS等分析方法研究了SiC、B4CNJ瓷相对C—SiC—B4C复合材料结构和性能的影响。研究表明,C—SiC—B4C复合材料的高温抗氧化性与氧化温度、各陶瓷相含量、本身气孔率等有关。掺入的Sic、B4C能够在一定程度上降低炭材料的气孔率,同时,高温条件下陶瓷相形成硼硅酸玻璃覆盖炭基体表面,减少材料表面活性区域数量,提高炭材料的表观活化能。