Effect of Al_2O_3-SiC Composite Powder on Properties of Al_2O_3-SiC一C Bricks

Al2O3- SiC- C specimens were prepared using white fused corundum( 3- 1,≤1 and ≤0. 044 mm),Al2O3- SiC composite powders( d50≤5 μm),α-Al2O3micropowder( d50= 1. 2 μm),SiC powder( ≤0. 044mm),flake graphite( ≤0. 088 mm),Si powder( d50= 42. 8 μm) and B4C powder( d50≤10 μm) as main starting materials,and thermosetting phenolic resin as binder. 4%,8%,12% and 16%( in mass,the same hereinafter) of Al2O3- SiC composite powders substituted the same quantity of α-Al2O3micropowder + SiC powder.Effects of composite powder additions on apparent porosity,bulk density,cold modulus of rupture,cold crushing strength,hot modulus of rupture( 1 400 ℃),therma shock resistance( 1 100 ℃,water quenching) and oxidation resistance( 1 000 and 1 500 ℃) of Al2O3- SiC- C specimens after 180 ℃ curing,1 000 ℃ 3 h carbon-embedded firing and 1 500 ℃ 3 h carbon-embedded firing,respectively,were researched. The results indicate that:( 1) with the increase of Al2O3- SiC composite powder,cold strengths of the cured specimens decline,those of the specimens fired at 1 000 ℃ change a little,and those of the specimens fired at 1 500 ℃ change a little except for an obvious improvement of cold crushing strength;( 2) with the increase of Al2O3- SiC composite powder,hot modulus of rupture at 1 400 ℃ decreasesand thermal shock resistance enhances significantly;( 3) when Al2O3- SiC composite powder addition is4%,the oxidation resistance at 1 500 ℃ is the best,and the reason may be the composite powder is finer and more active,which is beneficial to form dense mullite protective layer to retard the O2diffusion into the specimens.     

esearch and Application of Burned Microporous High Alumian—Graphite（Al／C） Brick in Blast Furnace

This paper inroduces the research background,technology,product property and application of burned microporous high alumina-graphite brick (Al2O3-C brick) used in blast furnace,The difference of property between Al2O3-C brick and other blast furnace refractories is discussed .The results of simulative tests show that ,Al2O3-C brick has good alkali resistance,slag resistance,thermal shock resistance,oxidation resistance,high thermal conductivity,low permeability and low solubility in molten iron,The brick with micropores of average radius less than 1μm has been successively applied to fourteen blast furnaces, the lining life of the brick is almost as long as that of Si3N4 bonded SiC brick Al2O3-C brick will be widely used in lower stack ,belly,bosh and hearth in the future.     

Influences of Al and Si Powders on Microstructure and Hot Mechanical Properties of Al2O3-C Slide Plates

The basic formulation of Al2O3- C slide plates was65%( in mass,the same hereinafter) white fused corundum particles,25% white fused corundum fines,6% active α-Al2O3 micropowder,4% carbon black and flake graphite, and additional 4% phenolic resin.Based on this formulation,3% Al powder,3% Si powder,and 3% Al + 3% Si powder were used to substitute equivalent white corundum fines to improve the hot mechanical properties of Al2O3- C slide plates. The specimens with dimensions of 140 mm × 25 mm × 25 mm were pressed at 150 MPa,dried at 200 ℃ for 24 h,and hot treated at 1 400 ℃ for 3 h in carbon embedded condition. Then hot modulus of rupture and thermal shock resistance of the specimens were tested and the phase compositions and microstructure were analyzed. The results show that specimen with 3% Al powder has the higher hot modulus of rupture but lower residual modulus of rupture after thermal shock than the specimen with3% Si powder; the specimen with 3% Al + 3% Si powders exhibits the highest hot modulus of rupture and the best thermal shock resistance; the change of mechanical property is closely related with the in-situ formed nonoxides: AlN in the form of bars is formed in specimens with Al powder; fibrous SiC whiskers are formed in specimens with Si powder; in the specimens with both Al and Sipowders,besides AlN and SiC whiskers,hexagonal tabular SiAlON is in-situ synthesized,which interlocks with each other.     

Properties and Microstructure Evolution of Al_2O_3-Si Material Fired in Different Atmospheres

Al2O3- Si composite specimens were prepared using fused corundum,ultra-fine α-Al2O3and Si powder as starting materials and resin as binder. Effects of sintering atmospheres on properties,phase composition and microstructure of specimens after firing at 1 500 ℃ were investigated. The results show that:( 1) after firing in oxidizing or weak oxidizing atmosphere,there is some Si in the specimens and some glass phases containing mullite form on specimen surface,the density and strength at room temperature are relatively high,but hot modulus of rupture and thermal shock resistance are relatively poor;( 2) after firing in weak reducing or reducing atmosphere,Si reacts completely with CO or N2forming whisker-like SiC,granular Si2N2O or O'-SiAlON,and the thermo-mechanical properties of specimens are enhanced;( 3) after firing in nitrogen atmosphere,Si reacts completely with N2,CO or C forming whisker-like SiC and columnar β-SiAlON crystals,the hot modulus of rupture and thermal shock resistance of specimens are enhanced noticeably.     

Investigation on The Properties of Fe-Si3N4 Bonded SiC Composite

The mechanical properties of pressureless sintering Fe-Si3N4 bonded SiC and Si3N4 bonded SiC with same manufacture process have been compared in this paper.The oxidizing mechanism of Fe-Si3 N4 bonded SiC ceramic matrix composite has been investigated especially through TG-DSC (thermo gravimetric analysis-differential scanning calorimeter) experiment. During oxidation procedure the main reaction is the oxidation of SiC and Si3 N4, SiO2 which form protecting film to prevent further oxidizing. And residual iron in the samples become Fe2O3 and Fe3O4, the oxidation kinetics at 1100 - 1300℃ of Fe-Si3N4 bonded SiC has been studied especially. The weight gain per unit area at initial stage changes according to beeline rule, in the middle according to conic, and in the last oxidation period follows parabola rule,     

Effect of processing parameters on in situ screen printing-assisted synthesis and electrical properties of Ti3SiC2-based structures

This work reports on the development of pastes containing Ti,TiC,Si,and C elementary powders for in situ synthesis of Ti3SiC2 via screen printing.Four paste compositions were manufactured using two powder mixtures(Ti/Si/C and Ti/TiC/Si/C)with different stoichiometry.The pastes were screen printed onto Al2O3 substrates and sintered at 1400℃in argon varying the dwell time from 1 to 5 h.The printed pastes containing TiC and excess of Si exhibited the lowest surface roughness and after 5 h sintering comprised of Ti3SiC2 as the majority phase.The electrical conductivity of this sample was found to range from 4.63×10⁴to 2.57×10⁵S·m^-1in a temperature range of 25-400℃.     

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.     

Thermodynamic Properties of Non-Oxide Composite Refractories

For initiative application of non-oxides in refractories, it is essential to study thermodynamic properties of non-oxides. The stability and stable order of non-ox- ides under oxidized atmosphere are analyzed firstly and then a new process, “converse reaction sintering”, is proposed. The results of study on oxidation mechanism of silicon and aluminum nitrides indicate that the gaseous suboxides can be produced observably when the oxygen partial pressure is lower than “conversion oxygen partial pressure”. The suboxides can be deposited near the surface of composite to become a compact layer. This causes the material possessing a performance of “self-impedient oxidation”. Metal Si and Al are the better additives for increasing the density and width of compact layer and increasing the ability of anti-oxidation and anti-corrosion. The study on Si3 N4-Al2O3, Si3N4-MgO, Si3 N4-SiC systems is also enumerated as examples in the paper. The experimental results show that the converse reaction sintering is able to make high performance composites and metal Si and Al not only can promote the sintering but also increase the density and width of compact layer.     

Thermo-mechanical Properties of In-situ Formed Al_2O_3-SiC-SiAION Composites

Al_2O_3-SiC-SiAlON composite specimens have been prepared using fused alumina,ultra fine α-Al_2O_3,Si and Al powders as starting materials and liquid phenol formaldehyde resin as binder and firing at 1 500 ℃ for3 h in carbon embedded condition. Thermo-mechanical properties of Cr_2O_3-Al_2O_3-Zr O2 composites have been studied. The results show:( 1) Cr_2O_3-Al_2O_3-Zr O2 composites can be prepared and sintered at 1 500 ℃ under carbon embedded condition. When Si / Al ratio is 8 /0and 7 /1, the prepared composite is Al_2O_3-SiC-O'-Si Al ON; when Si / Al ratio is 5/3 and 3 /5,the prepared composite is Al_2O_3- SiC-β-Si Al ON.( 2) The composites possess high temperature strength properties.Hot modulus of rupture at 1 400 ℃ is 10- 30 MPa.They are in elastic range up to 1 000 ℃,after which plastic deformation is observed; even at 1 400 ℃,amount of deformation is relatively low.( 3) The composites possess good thermal shock resistance,their residual strength ratio( ΔT = 1 100 ℃) is 65%- 80%.( 4) The marked improvement in thermo-mechanical properties of Cr_2O_3-Al_2O_3-Zr O2 composites may be attributed to the in-situ formation of Si C,Si Al ON and Al N,the fibrous Si C,columnar Si Al ON and tabular-like Al N fill in the corundum skeleton structure creating strengthening and toughening effects.     

Oxidation Behaviour of Si3N4 Materials in Air and Nitrogen Atmosphere

Si3N4 powder and hot-pressed Si3N4 ceramics added with Al2O3 are used for investigate their oxidation behvior in air and nitrogen atmosphere(with oxygen partial pressure PO2=1-10Pa),The oxidation products of Si3N4 are examined by chemical analysi,X-ray diffraction (XRD) and XPS method,Also, thermodynamic calculation is made to analyze oxidation behavior of Si3N4.The results show that only passive oxidation will occur when Si3N4 is oxidized in air at high temperature,whereas in N2 at high temperature,the active oxidation is dominant in spite of the existence of a little passive oxidation.     

Si粉氮化法合成Si3N4-SiC材料

以SiC、Si粉和Al2O3微粉为主要原料,羧甲基纤维素(CMC)为临时结合剂,采用氮化反应烧结法合成了Si3N4-SiC材料,主要研究了Si粉的粒度(≤0.074、≤0.044 mm)和加入量(质量分数分别为15%、17%、19%、21%)、烧成温度(分别为1 380、1 400、1 420、1 430、1 440、1 460和1 480℃)、Al2O3微粉添加量(质量分数分别为0、1%、2%、3%、4%,取代相应量的SiC粉)对Si3N4-SiC材料的显气孔率、体积密度、常温耐压强度、常温抗折强度、高温抗折强度及Si3N4含量的影响。结果表明:1)采用粒度较细Si粉的试样具有较高的致密度、常温强度、高温抗折强度和Si3N4含量;随着Si粉加入量的增加,试样的致密度略有增大但变化不大,常温强度和Si3N4含量逐渐增大,而高温抗折强度先增大后减小;2)适当提高烧成温度会明显改善Si3N4-SiC材料的高温抗折强度,但当温度超过1 440℃反而略有下降;3)添加Al2O3微粉对烧后试样的致密度、常温强度和高温抗折强度有益。综合来看,Si粉的适宜添加量(质量分数)为17%,较适宜的烧成温度为1 420～1 440℃,Al2O3微粉的适宜添加质量分数为2%。     

纳米NiO掺杂Carbores'P对Al2O3-C耐火材料力学性能的影响

为提高低碳铝碳耐火材料的力学性能,以≤1 mm的棕刚玉、Si粉和Carbores’P为原料,外加纳米NiO为催化剂,制备Al2O3-C基质试样,利用XRD、SEM、激光拉曼光谱研究纳米NiO对Carbores’P炭化产物的影响。以棕刚玉(粒度为5~3、3-1、≤1 mm)、电熔白刚玉粉、Si粉、鳞片石墨、Carbores’P、纳米NiO为原料制备低碳Al2O3-C试样,研究纳米NiO掺杂Carbore’P对试样力学性能的影响。结果表明:1400℃埋碳热处理后,添加纳米NiO能提高基质的石墨化度,促进碳纳米管和SiC晶须的生成;正是由于它们的生成,提高了Al2O3-C试样的致密度、常温强度和断裂前的位移量,使试样韧性增强。     

化学激励燃烧合成SiC超细粉末的工艺和机理研究

研究了利用聚四氟乙烯（-C2F4-）n作活化剂时Si/C混合粉末在氮气中的燃烧行为，结果表明：少量聚四氟乙烯的加入就可有效激励Si-C弱放热反应，使之以燃烧合成方式生成SiC，氮气参与反应时可进一步提高燃烧反应温度，并且首先以气相-晶体机制生成Si3N4，然后在反应前沿分解为SiC，调整工艺参数可获得亚微米级SiC粉末，综合X射线衍射、差热/热量分析及扫描电镜观察，提出了Si-C-N-(-C2F4-）n体系中的燃烧反应机制，并从热力学角度对实验结果进行了讨论。     

不同原料体系对无压烧结合成Ti3SiC2的影响及其腐蚀行为

通过液相磁力搅拌混合原料粉末,压片后无压烧结合成了三元Ti3SiC2,研究不同原料配比Ti/Si/C,Ti/SiC/C/和TiC/Si/Ti对合成Ti3SiC2的影响,同时为了比较,在相同条件下加入少量Al或Sn,研究其对Ti3SiC2的合成过程及最终产物的影响,并探讨Ti3SiC2的合成机理.结果表明:3Ti/1.2Si/2C/0.1Al在1400 ℃无压烧结合成了较高纯度的Ti3SiC2,Al粉的加入可以降低混合粉末的起始反应温度,有利于三元层状化合物Ti3SiC2的合成和纯度的提高,其合成机制为,在铝粉形成的熔池中,经形核钛和硅反应生成钛硅金属间化合物,钛与石墨反应生成碳化钛,随后扩散,长大,随着温度的升高,反应生成三元层状Ti3SiC2.而以TiC或SiC为Ti或Si源制备的Ti3SiC2含杂质较多,不适用于无压烧结合成Ti3SiC2.合成的Ti3SiC2在HF溶液中经200 ℃溶剂热反应后,产物主要为两种不同晶型的SiC和AlF3立方体,且随着反应时间的延长,AlF3的含量增加,结晶更完善.     

氮化硅铁在Al2O3-C体系中的高温行为

为了研究高温条件下Al2O3-C体系中氮化硅铁的状态,以闪速燃烧合成氮化硅铁、炭黑、刚玉粉为原料,将试样在高温炉中分别加热至1 450、1 500、1 600℃保温5 h,急速水冷后,对其进行XRD和显微结构分析。结果表明:1 450℃烧后试样的物相包含β-Si3N4、α-Si3N4、α-Al2O3和Fe3Si;1 500℃烧后试样的物相为β-Si3N4、SiC、α-Al2O3和Fe3Si;1 600℃烧后试样中Si3N4大部分转变为SiC,其他物相未发生变化。在升温过程中,氮化硅逐渐转化为碳化硅,材料结构致密。     

Mechanical Behavior and Electromagnetic Interference Shielding Properties of C/SiC–Ti3Si(Al)C2

In this paper, a low‐temperature densification process of Al–Si alloy infiltration was developed to fabricate C/SiC–Ti₃Si(Al)C₂, and then the microstructure, mechanical, and electromagnetic interference (EMI) shielding properties were studied compared with those of C/SiC–Ti₃SiC₂ and C/SiC–Si. The interbundle matrix of C/SiC–Ti₃Si(Al)C₂ is mainly composed of Ti₃Si(Al)C₂, which can bring various microdeformation mechanisms, high damage tolerance, and electrical conductivity, leading to the high effective volume fraction of loading fibers and electrical conductivity of C/SiC–Ti₃Si(Al)C₂. Therefore, C/SiC–Ti₃Si(Al)C₂ shows excellent bending strength of 556 MPa, fracture toughness 21.6 MPa·m^1/2, and EMI shielding effectiveness of 43.9 dB over the frequency of 8.2–12.4 GHz. Compared with C/SiC–Si and C/SiC–Ti₃SiC₂, both the improvement of mechanical properties and EMI shielding effectiveness can be obtained by the introduction of Ti₃Si(Al)C₂ into C/SiC, revealing great potential as structural and functional materials.     

Pressure‐less joining of C/SiC and SiC/SiC by a MoSi2/Si composite

A MoSi₂/Si composite obtained in situ by reaction of silicon and molybdenum at 1450°C in Ar flow is proposed as pressure‐less joining material for C/SiC and SiC/SiC composites. A new “Mo‐wrap” technique was developed to form the joining material and to control silicon infiltration in porous composites. MoSi₂/Si composite joining material infiltration inside coated and uncoated C/SiC and SiC/SiC composites, as well as its microstructure and interfacial reactions were studied. Preliminary mechanical strength of joints was tested at room temperature and after aging at service temperatures, resulting in interlaminar failure of the composites in most cases.     

添加物对MgO-ZrO2-C材料性能的影响

研究了Al和Si添加物对镁锆炭砖碳化烧成后膨胀性能的影响及机理。结果表明 :Al和Si在高温下氧化成Al2 O3和SiO2 ,继而与CaZrO3或用于稳定氧化锆的稳定剂反应 ,生成铝酸钙、MA、C2 S和M2 S,另外 ,C2 S和ZrO2 还发生了晶型转变。这一系列反应使试样产生很大的体积膨胀 ,从而破坏了制品结构。因此 ,与镁炭砖不同 ,Al和Si不但不能增强镁锆炭砖 ,而且使其结构破坏和耐侵蚀性降低。     

Microstructure and mechanical properties of SiC-SiC joints joined by spark plasma sintering

The development of reliable joining technology is of great importance for the full use of SiC. Ti₃SiC₂, which is used as a filler material for SiC joining, can meet the demands of neutron environment applications and can alleviate residual stress during the joining process. In this work, SiC was joined using different powders (Ti₃SiC₂ and 3Ti/1.2Si/2C/0.2Al) as filler materials and spark plasma sintering (SPS). The influence of the joining temperature on the flexural strength of the SiC joints at room temperature and at high temperatures was investigated. Based on X-ray diffraction and scanning electron microscopy analyses, SiC joints with 3Ti/1.2Si/2C/0.2Al powder as the filler material possess high flexural strengths of 133 MPa and 119 MPa at room temperature and at 1200 °C, respectively. The superior flexural strength of the SiC joint at 1200 °C is attributed to the phase transformation of TiO₂ from anatase to rutile.