硼热还原法制备LaB_6粉末

研究了采用硼热还原法制备LaB6 粉末的反应合成工艺 .La2 O3-B系反应热力学分析表明 ,气体分压对LaB6 的形成有重要影响 ,减小气体分压可以明显降低LaB6 的合成温度 ;结合DTA测定结果 ,确定了制备LaB6 粉末的合成温度 .同时 ,对不同温度和保温时间条件下所生成的LaB6 粉末的相组成、颗粒尺寸与形貌以及纯度进行了测试分析 ,实验结果表明 ,La2 O3-B系制备LaB6 粉末的优化工艺是真空度133Pa ,192 3K保温 6h ,所合成的LaB6 粉末平均粒径为 6 μm ,纯度达 99.2 % ,颗粒形态比较规整 ,多数呈近似团块状 .     

硼热还原法制备LaB6粉末

研究了采用硼热还原法制备LaB6粉末的反应合成工艺,La2O3-B系反应热力学分析表明,气体分压对LaB6的形成有重要影响,减小气体分压可以明显降低LaB6的合成温度,结合DTA测定结果,确定了制备LaB6粉末的合成温度,同时,对不同温度的和保温时间条件下所生成的LaB6粉末的相组成、颗粒尺寸与形貌以及纯度进行了测试分析,实验结果表明,La2O3-B系制备LaB6粉末的优化工艺是真空度133Pa,1923K保温6h,所合成的LaB6粉末平均粒径为6um,纯度达99.2%,颗粒形态比较规整,多数呈氨似团块状。     

葡萄糖为碳源合成AlN-Al2O3复合粉末及其反应机理

以葡萄糖(C6H12O6·H2O)和氢氧化铝(Al(OH)3)为起始原料,利用碳热还原法在氮气(N2)气氛下合成AlN-Al2O3复合粉末.研究了反应温度对AlN-Al2O3复合粉末的物相组成和显微形貌的影响,并探讨了AlN-Al2O3复合粉末的合成反应机理.采用X-射线衍射仪(XRD)、激光粒度分析仪(LPSA)、扫描电镜(SEM)等手段对产物进行表征.结果表明:AlN-Al2O3复合粉末适宜的合成条件为在1500℃保温2h.在1500℃下合成的AlN-Al2O3复合粉末主要有少量的片状颗粒和大量的近似球状颗粒所构成,大部分粒径在100～500nm之间的颗粒发生聚集或堆积形成0.5～1.5μm的大颗粒.在碳热还原反应过程中,Al(OH)3原料分解生成的Al2O3首先生成金属铝蒸汽和Al2O气体氧化物,然后进一步氮化生成AlN.     

TiB2-SiC复合粉末的碳热还原法合成及其表征

以TiO2、B4C、炭黑和硅溶胶为原料,采用碳热还原法合成了TiB2 -SiC超细复合粉末.对碳热还原反应过程进行了热力学分析和计算,采用XRD和SEM等研究了反应温度对合成TiB2-SiC复合粉末的物相组成和显微形貌的影响,并对合成的TiB2-SiC复合粉末的氧化性能进行了探讨.结果表明:TiB2-SiC复合粉末合成的适宜条件为在1600℃保温1h.在反应过程中,TiB2先于SiC形成,所合成的复合粉末由球状、片状、短棒状颗粒以及晶须等多样化结构组成.TiB2-SiC复合粉末的氧化过程中,首先是TiB2优先与氧发生反应生成TiO2和B2O3,然后是SiC与氧反应生成SiO2和CO,氧化产物中没有发现低熔点B2O3的存在.     

尿素对前驱物及氮化铝粉末粒度形貌的影响

以硝酸铝 [Al(NO3) 3·9H2 O]、葡萄糖 [C6 H1 2 O6 ·H2 O]为原料 ,利用碳热还原法制备氮化铝粉末 ,研究了尿素对前驱物及其氮化反应产物的组成和显微形貌的影响。研究发现 :尿素不仅可以影响前驱物的组成和显微形貌 ,还对氮化反应产物的显微形貌有重要影响。在溶液里添加尿素后 ,它与硝酸铝发生了低温燃烧合成反应 ,生成了比表面积高的泡沫状前驱物 ,该过程中碳燃烧损失较大。在没有添加尿素的溶液中 ,没有燃烧反应发生 ,碳的损失小 ,生成的前驱物团聚现象严重 ,比表面积低。两种前驱物的氮化反应产物保留了各自前驱物的形貌特征 ,对于不添加尿素合成的前驱物 ,在其氮化反应后所生成的氮化铝粉末板结严重 ;而添加尿素合成的前驱物的氮化反应产物是由球形颗粒组成的软团聚体。利用XRD ,SEM等分析方法对粉末进行了表征     

小粒径BaMgAl_(10)O_(17):Eu~(2+)荧光粉的合成机理

使用化学沉淀法制备细粒径、分散性好的圆饼状α-Al2O3粉体,并以此为原料,通过高温固相法制备粒径细小、颗粒形貌规则的高性能BaMgAl10O17:Eu2+(BAM)荧光粉,重点研究合成过程中的物相转变及颗粒生长等过程。结果表明:氧化铝原料颗粒对最终BAM荧光粉的颗粒形貌和粒径起到重要作用,经过1500℃煅烧2h后生成的BAM仍基本维持原α-Al2O3颗粒的圆饼状外形,颗粒粒径仍为2.5μm左右且分散性良好。高温固相法制备BAM荧光粉的过程中,1000℃时,首先在α-Al2O3颗粒表面反应形成一层BaAl2O4相,当温度继续升高,MgO参与反应,通过BaAl2O4层进行传质过程,并最后完全转变为BaMgAl10O17相。发光性能测试表明:使用自制氧化铝制备的BAM荧光粉具有良好的发光特性,其发射光谱峰的强度和半峰宽与使用商用氧化铝原料所制得的荧光粉的相当。     

碳热还原法合成B4C及B4C／TiB2复合粉末的研究

以工业硼酸、碳黑及TiO2为原料，经碳热还原法于1650～1800℃合成了纯B4C及TiB2含量分别为10～20vol%的B4C/TiB2复合粉末，同时确定了原料B/C摩尔比，进行了热力学分析并探讨了球磨工艺、TiB2的生成对粉末合成的影响。结果表明：原料及产物的B／C摩尔比分别为4．4和3．98～4．03，产物纯度均大于99wt％；湿法球磨可迅速消除粉末的团聚现象，降低原始粉末的粒度，TiB2颗粒较均匀分散于B4C中，呈近圆片状，TiB2的生成有助于降低B4C／TiB2的合成温度，由1800℃降至1650℃，并改善了B4C的颗粒形状，由无定形态变为近球形及条状。     

熔盐法合成钨酸锌纳米晶及花朵状氧化锌

采用熔盐法成功制备出了钨酸锌(ZnWO4)纳米晶.用XRD、SEM分别对产物的相组成、粒度、显微结构等进行了表征.结果表明:以Na2WO4·2H2O、Zn(NO3)2·6H2O为原料,NaNO3-LiNO3为熔盐,分别在200～400℃保温12h均能合成纯相的ZnWO4粉体;当温度达到500℃时生成花朵状的ZnO片状粉体;ZnWO4颗粒的形貌与煅烧温度和保温时间有密切关系,随温度升高,颗粒形貌的演变过程为:当温度为200℃时生成纳米颗粒;升高温度至300℃时,生成棒状纳米晶体;继续升高温度到400℃时,形成了块状的微米晶体.随着保温时间的延长,颗粒形貌的演变过程为:由纳米颗粒转变为棒状纳米晶体.     

镍基Al2O3-TiB2金属陶瓷粉末机械合金化机制研究

本文研究了添加不同质量分数的Ni对机械合金化合成Al2O3-TiB2金属陶瓷粉末的影响.应用X射线衍射仪、扫描电镜对球磨不同时间后的产物进行了物相和颗粒形貌的分析.结果表明:不含Ni粉的Al、TiO2和B2O3的混合粉末,在机械合金化12 h后,按照化学方程式10Al+ 3TiO2+ 3B2O3=5Al2O3+ 3TiB2发生固相反应,获得Al2O3、TiB2复相组织;当加入Ni粉后Al、TiO2和B2O3的混合粉末,由于在机械球磨过程中,Ni优先与Al形成中间相NiAl,NiAl比Al更容易与TiO2及B2O3发生反应,按照化学方程式10NiAl+ 3TiO2+ 3B2O3=5Al2O3+ 3TiB2+10Ni发生固相反应,获得Al2O3、TiB2复相组织;使得机械合金化时间随着Ni粉加入量的增大而减小,当添加质量分数为5％、10％、15％、20％、25％和30％的Ni粉后,分别在机械合金化12 h、10 h、8h、8h、6h和4h后,得到Al2O3、TiB2复相组织.     

用于分离和回收锌的氯化物熔融工艺

采用燃烧合成二硼化镁粉末的制备方法。该方法是将原料粉装入混料机内经混合后，再装入燃烧合成器中抽真空和充氩保护并进行燃烧合成反应，然后再取出生成产物进行漂洗，其特征在于原料B2O3和Mg粉的配入质量分别是B2O3粉为29％～42％，Mg粉为58％～71％，原料粉的平均粒径≤30μm，燃烧合成是经点火引燃反应原料发生高温合成反应，然后将反应产物于酸性液中漂洗后，     

超声法制备低温态偏硼酸钡纳米粉体及其表征

以Ba(OH)2.8H2O和硼酸为原料,采用超声法合成了偏硼酸钡(β-BaB2O4)纳米粉体。该方法的特点是在反应体系中添加双氧水和表面活性剂PEG-400,并采用超声合成的方法,同时避免了颗粒的硬团聚和软团聚现象。FT-IR分析证明初始产物为BaB2O4.H2O2。TG-DTA-DTG分析证明BaB2O4.H2O2在553℃左右发生分解反应,失去结晶双氧水。XRD分析表明,β-BaB2O4的空间群分别为R3c(161)和C2/c(15)。TEM形貌观察表明,产品粒子均匀,分散性较好,平均粒径小于70 nm。还对双氧水的作用、滴加速度、非晶态转化为晶态的温度和超声波与表面活性剂的影响作了初步探讨。     

Synthesis of Calcium Hexaboride Powder via the Reaction of Calcium Carbonate with Boron Carbide and Carbon

The synthesis of calcium hexaboride (CaB₆) powder via the reaction of calcium carbonate (CaCO₃) with boron carbide (B₄C) and carbon has been investigated systematically in the present study. The influences of heating temperature and holding time on the reaction products have been studied using X-ray diffractometry, and the morphologies of CaB₆ obtained at various temperatures and holding times have been investigated via scanning electron microscopy. The interaction in the CaCO₃–B₄C–carbon system by which CaB₆ is formed is a solid-phase process that passes through the transition phases Ca₃B₂O₆ and CaB₂C₂. The optimal conditions for CaB₆ synthesis are a holding time of 2.5 h at a temperature of 1673 K, under vacuum (a pressure of 10⁻² Pa). CaB₆ powder has the same morphology as B₄C, and the properties and the shape of CaB₆ powders can be improved by choosing good-quality raw materials.     

Reaction mechanism and size control of CaB6 micron powder synthesized by the boroncarbide method

Reaction synthesis mechanism of Calcium hexaboride (CaB₆) powder was investigated by using CaCO₃-B₄C-C system. Micron-scale CaCO₃ and B₄C powders were used as main raw materials. The synthesized powder was determined by X-ray diffraction, showing no left reactants if enough CaCO₃ was added to compensate the evaporation of calcium atoms at high temperature. The powder morphology was observed through SEM. The synthesized CaB₆ powder formed hard agglomerates which consisted of cubic CaB₆ crystallites when the reaction completely finished. Reaction process was illustrated indicating it was a solid-state reaction occurred from B₄C surface to the centre. The dry high-energy ball milling was used to investigate the influence of ball-milling time on the shape and size of powder particles. The particle granularity was measured by laser size analysis method. It is obvious that the particles were refined greatly after ball milling for 8 h. However, the CaB₆ powder could not been refined markedly after 16 h. Finally, optimized parameters for size controlling were given in this paper.     

添加B2O3对Y掺杂BaZrO3烧结性及电导率的影响

研究了加入不同量氧化硼（B2O3）对 Y 掺杂 BaZrO3（BaY0.1Zr0.9O2.95）质子导体烧结性及电导率的影响。研究表明：加入适量 B2O3（质量分数为0.5%～0.75%）可以使 Y 掺杂 BaZrO3的烧结温度降低到 1500 ℃,保温时间缩短到 4～6h,相对密度可达 95%左右,远大于不加 B2O3试样的。与未掺入 B2O3的 Y 掺杂 BaZrO3试样相比,该体系材料的电导率没有明显降低。过量 B2O3（1.0%）的加入将使其以第二相形式存在于烧结体中,从而降低材料的电导率。     

Low‐Temperature Synthesis of Calcium Hexaboride Powder via Transient Boron Carbide Formation

Calcium hexaboride (CaB₆) powder was synthesized by carbothermal reduction using a low‐temperature synthesis method for boron carbide (B₄C) powder. A B₄C precursor consisting of boron oxide (B₂O₃) and carbon components was prepared from a condensed boric acid (H₃BO₃)‐poly(vinyl alcohol) (PVA) product by thermal decomposition in air, which was then mixed with calcium carbonate (CaCO₃) powder. CaB₆ was formed via the transient formation of calcium borate (Ca₃B₂O₆) and B₄C, which were in close contact owing to the finely dispersed B₂O₃/carbon structure of the B₄C precursor. CaB₆ powder with fine particles was synthesized by heat treatment at 1400°C for 10 h in an Ar flow.     

Preparations of lanthanum hexaboride (LaB6) and cerium hexaboride (CeB6)

Due to strong anti-poisoning ability, good emission stability, high emission current density, lanthanum hexaboride (LaB₆) and cerium hexaboride (CeB₆) have been maturely applied in electron emission emitter. In this paper, a new manufacturing method for LaB₆ (or CeB₆) powder was proposed by using La₂O₃ (or CeO₂), B₄C, and Al as raw materials. After high-temperature reaction in the range of 1673–1773 K and the following alkaline leaching at 90°C, LaB₆ or CeB₆ powder with particle size of about 10 μm was obtained. Furthermore, by Al metal flux method, the obtained powder was used to manufacture single crystal block with size of several millimeters.     

钛酸钡制备新方法研究

用ＢａＣｌ２．２Ｈ２Ｏ和Ｈ２ＴｉＯ３作反应物,（ＮＨ４）２ＣＯ３作沉淀共沉淀法制备钛酸钡。研究了（Ｎ４）２ＣＯ３和ＢａＣｌ２．２Ｈ２ｏ及ＢａＣｌ２．２Ｈ２Ｏ和Ｈ２ＴｉＯ３的配比、反应温度和时间、煅烧温度和时间、液固比对产品质量的影响。     

Synthesis,densification, microstructure,and mechanical properties of samarium hexaboride ceramic

Samarium hexaboride (SmB₆) powders were synthesized by boro/carbothermal reduction of Sm₂O₃ with B₄C. Nominally pure SmB₆ powder had a mean particle size of about 400 nm and an oxygen content of 0.12 wt%. SmBO₃ formed as an intermediate phase during the synthesis. The synthesized powder was hot pressed at 1950°C to produce SmB₆ ceramics with relative densities >99.6% and a mean grain size of 4.4 μm. Vickers’ hardness was 20.1 ± 0.7 GPa. Young's modulus measured by bending and ultrasonic methods was 271 and 244 GPa, respectively. The flexure strength was 253 ± 79 MPa and fracture toughness was 2.1 ± 0.1 MPa m^1/2. These are the first reported results of the microstructure and bulk mechanical behavior of SmB₆ ceramics.     

超细CuCr_2O_4粉体的制备及表征

以Cu(NO32)·3H2O、Cr(NO3)2·9H2O和柠檬酸为原料,采用柠檬酸配位法合成了超细CuCr2O4催化剂,用XRD、SEM对产物进行了表征,用DTA研究了CuCr2O4对高氯酸铵(AP)热分解性能的影响,测量了加入CuCr2O4后CMDB推进剂的燃速。结果表明,在最佳合成条件下(即nCu∶nCr=1∶2,温度700℃)可制得纯四方尖晶石型CuCr2O4。加入超细CuCr2O4后,AP的高温分解温度提前至339.6℃,CMDB推进剂在6MPa下的燃速从35.84mm/s提高到61.00mm/s,压强指数从0.62降低到0.14。