固相反应法制备透明多晶YAG陶瓷

采用高纯α-Al2O3和Y2O3作为原料并由固相反应法合成了钇铝石榴石(yttrium aluminum garnet,YAG)透明多晶陶瓷.α-Al2O3和Y2O3的摩尔比为5∶3,并添加0.5%(质量分数)正硅酸乙脂为烧结助剂的混合粉体经球磨后,在1 400℃空气中煅烧,经成形并在1 750℃真空烧结4h制备得到透明YAG陶瓷.1 850℃真空烧结4h的YAG陶瓷晶粒粗大,晶界宽化,晶界处有共晶相YAlO3相和α-Al2O3相存在.     

Y_2O_3添加方式对Al_2O_3陶瓷烧结过程中的物相变化影响

采用非均匀沉淀法和机械球磨法2种方法添加Y2O3获得Al2O3陶瓷,通过研究烧结过程中Al2O3陶瓷的物相变化,对比了2种添加方法的优劣。结果表明:对于非均匀沉淀法制备的Al2O3复合粉体来说,烧结过程中开始生成钇铝石榴石(YAG)相的温度约为1 400℃,低于机械球磨法添加Y2O3烧结过程中YAG的生成温度;YAG的生成量大于机械球磨法;加入较少量的Y2O3(0.05%,质量分数)即可检测到Y3+在Al2O3晶格中的固溶态。扫描电子显微镜照片和面扫结果显示烧结过程中生成的YAG位于Al2O3晶界处。     

Y_2O_3-Al_2O_3粉体固相反应制备Y-Al-O体系陶瓷的对比研究

研究了摩尔比n(Y2O3):n(Al2O3)分别为2:1、1:1和3:5的粉体在不同温度发生的相变及其高温烧结的陶瓷。Y2O3-Al2O3粉体经球磨后在1750℃真空烧结制备陶瓷。用差热-热重、X射线衍射及扫描电子显微镜表征制备的Y2O3-Al2O3材料。结果表明:在低于800℃时,Y2O3-Al2O3之间未发生反应;在1000℃煅烧后,出现Y4Al2O9(YAM)相;1200℃煅烧后,出现YAlO3(YAP)相和钇铝石榴石(yttrium aluminumgarnet,YAG)相。n(Y2O3):n(Al2O3)=3:5粉体在1400℃煅烧后生成YAG纯相。n(Y2O3):n(Al2O3)=2:1、3:5粉体烧结的陶瓷的物相分别为YAM相和YAG相,其相对体积密度分别为97.8%和99.95%,n(Y2O3):n(Al2O3)=1:1粉体烧结陶瓷的物相为多相共存,3种配比制备陶瓷断口的形貌差别较大。     

均相法和共沉淀法制备Nd：YAG透明陶瓷的对比研究

以Al(NO3)3·9H2O、Y2O3、Nd2O3、尿素和NH4HCO3为主要原料,分别采用均相法和共沉淀法制备了Nd:YAG纳米粉体和透明陶瓷。对比研究了两种方法的粉体的制备工艺,物相,形貌和陶瓷的透过率、形貌。结果发现,均相法制备的前驱体疏松,1200℃煅烧时先形成YAP相,后形成纯相粉体。共沉淀法制备的前驱体较硬,1000℃锻烧直接形成纯相粉体。最后,两种方法制备的陶瓷素坯经真空烧结、处理后,在1064 nm的透过率达80%。共沉淀法条件温和,易于得到纯相YAG,更适合于工业化开发。     

固相反应法制备YAG透明陶瓷

研究了固相反应法制备钇铝石榴石(yttrium aluminum garnet，YAG)透明陶瓷的工艺。采用高纯Y2O3和Al2O3超徽粉为原料，在1300℃煅烧2h，制备出YAG粉末。YAG相生成温度比常规温度大约低200℃。加入0．5％(质量分数)正硅酸乙醑烧结助剂后，YAG坯体在1700℃真空烧结5h，得到了高透光的YAG陶瓷，其在可见光区最大透光率为63％，在红外光区的透光率接近70％。YAG陶瓷具有均匀的微观结构，晶粒尺寸大约为10～30μm。     

共沉淀法合成钇铝石榴石纳米粉体及透明陶瓷的制备

以硝酸铝[Al(NO3)3·H2O]和硝酸钇[Y(NO3)3·6H2O]为原料、以碳酸氢铵[NH4HCO3]为沉淀剂,硫酸铵[(NH4)2SO4]为分散剂,用共沉淀法合成钇铝石榴石(yttrium aluminum garnet,YAG)纳米粉体.用X射线衍射仪、红外光谱仪、热分析仪和场发射扫描电镜等测试手段对YAG前驱体和煅烧后的粉体进行表征.结果表明:前驱体经过1 000℃煅烧5h后已完全转变成纯立方相YAG,所得的粉体分散性好、无团聚、形状近似球形、平均颗粒尺寸约为100 nm.以该YAG粉体为原料,正硅酸乙酯[Si(OC2H5)4,TEOS]为添加剂,用真空烧结技术在1 700～1 800℃煅烧20h制备YAG透明陶瓷.YAG陶瓷样品的平均晶粒尺寸为10 μm,存在少量气孔相和杂质相.为了提高YAG陶瓷的透过率,需要进一步优化陶瓷的制备工艺.     

溶胶-凝胶法制备巨介电常数材料CaCu3Ti4O12

通过溶胶-凝胶法制备CaCu3Ti4O12干凝胶,再经700～900℃,6～10h预烧和950～1 100℃,16～20h烧结,成功制备了CaCu3Ti4O12粉体和CaCu3Ti4O12巨介电常数陶瓷材料.用X射线衍射、扫描电镜分别确定了样品的结晶性能和形貌.用阻抗分析仪在10～106Hz范围内测试了陶瓷样品的介电性能.结果表明:粉体的结晶性能与煅烧温度有关,陶瓷介电性能与其晶粒大小有关.相对于传统固相反应合成法制备的粉体和陶瓷,粉体的预烧和陶瓷的烧结温度都有明显降低,烧成温度至少降低100℃.在800℃预烧的CaCu3Ti4O12粉体并在1 100℃温度下烧结制备的陶瓷,其介电常数可达194753.     

高能球磨法制备La0.2Y1.8O3纳米粉体及透明陶瓷

以Y2O3为基质材料,掺杂不同含量的La3+,采用高能球磨法制备出性能良好的La0.2Y1.8O3纳米粉.对不同球磨时间后的粉体进行了X射线衍射、透射电镜和比表面积等分析.结果表明:La3+完全固溶于Y2O3的立方晶格中,La0.2Y1.8O3粉体大小均匀,近似球形,且随着球磨时间延长,其颗粒逐渐变小,晶格畸变增加;900℃煅烧2h的粉末尺寸约40～60 nm左右.1650℃真空烧结3h后,得到了La0.2Y1.8O3透明陶瓷.     

钛酸铝固溶体陶瓷的制备与性能

用工业级原料采用固相反应法合成了钛酸铝固溶体[Al2(1-0.2)Mg0.2Ti1 0.2O5].研究了氧化镁(MgO)在钛酸铝(Al2TiO5)结构中的固溶对粉体合成的影响,通过测量Al2(1-0.2)Mg0.2Ti1 0.2O5陶瓷的体密度、热膨胀系数和抗弯强度,进一步研究了其烧结行为、热膨胀行为和机械性能.结果表明:由于MgO的固溶,在相对较低的温度(1 300℃)煅烧便合成纯相Al2(1-0.2)Mg0.2Ti1 0.2O5粉体,并且具有良好的烧结活性.用1 380℃合成的粉体,经1 450℃保温4h烧结的Al2(1-0.2)Mg0.2Ti1 0.2O5陶瓷,不仅具有低膨胀特性,而且有足够高的抗弯强度.     

薄水铝石粒度对煅烧形成α-Al2O3粉体的影响

研究了薄水铝石粒度对其煅烧形成α-Al2O3粉体的影响.先用水热法制备出均匀分散的纳米、亚微米及几个微米的薄水铝石前驱体,用x射线衍射仪和电子显微镜分析了薄水铝石在不同温度煅烧所得产物的相结构及形貌.结果表明,粒度30～100 nm的薄水铝石在1200℃煅烧1 h转变为α-Al2O3,为蠕虫状的烧结颗粒;粒度0.4～0.6 μm的薄水铝石在1 250℃煅烧1 h可转变为α-Al2O3,颗粒尺寸变化不大,仍在0.4～0.6 μm范围内;粒度1 μm左右的薄水铝石在1350℃下煅烧2 h尚不能完全转变为α相,并已出现明显烧结.因此,以水热法制备的亚微米级薄水铝石晶体作为前驱体,经直接煅烧可以制备出分散性较好的亚微米级α-Al2O3粉体.     

高能球磨对Pr_6O_(11)和Y_2O_3掺杂ZnO压敏电阻微观结构和电学性能的影响

利用高能球磨法制备Pr6O11、Y2O3掺杂ZnO压敏电阻,并对球磨时间对微观结构、物相组成及电学性能的影响进行了研究和分析。高能球磨有利于微观组织的均匀化和晶粒的细化,从而提高了电学性能。当球磨时间从0到10 h时,烧结后的ZnO晶粒尺寸变化从8.7到4.0μm,坯体烧结密度变化从5.40到5.62 g/cm3。最佳的制备工艺为球磨时间为7.5 h,烧结温度为1100℃,其对应的电学性能分别为:电位梯度(V1mA)是542 V/mm,漏电流(IL)是2.88μA,非线性系数(α)是47。     

若干激光基质材料的晶纤生长及荧光性能

制备了以ZrO_2,Gd_2O_2,LiNbO_3或YAG为基质,具有不同掺杂离子的12个单晶纤维试样,还测量了这些试样的化学成份及荧光光谱。     

激光强化电刷镀n-Al2O3/Ni复合镀层残余应力研究

利用Nd3+:YAG激光器对电刷镀过程进行强化,在45钢上制备了n-Al2O3/Ni复合镀层。采用X射线衍射法测定了镀层的轴向残余应力及其随镀层厚度变化情况。结果表明,镀层厚度从10μm增加到200μm,激光强化电刷复合镀层的轴向残余应力由压应力逐渐转变为拉应力。当激光功率为600W时,厚度为200μm的镀层的残余应力为103MPa,比普通电刷镀层降低约255MPa。分析了激光对n-Al2O3/Ni电刷复合镀层轴向残余应力的影响机理。     

The effects of ball milling time on the rheological,optical, and microstructural properties of YAG transparent ceramics

Stable slurries dispersed mixture of commercial Al₂O₃ and Y₂O₃ powders, ammonium poly meta acrylate (Dolapix CE64) as the dispersant, and tetraethyl orthosilicate (TEOS) as the sintering aid were prepared by ball milling process. The effects of the milling time on the fabrication of transparent polycrystalline yttrium aluminum garnet (YAG) ceramics were investigated by slip casting and vacuum sintering. The results showed that the best milling time for the deagglomeration of the powder mixture was 16 hours and the slurry prepared during this time showed a near-Newtonian behavior due to the better deagglomeration and lower viscosity. X-ray patterns also showed that all samples were pure YAG phase. The results also revealed that the sample prepared by 16 hours ball milling time suspensions exhibited higher relative green and final density, as well as the maximum transmittance at 1064 nm (≈ 77%). These samples had a more uniform microstructure too.     

高能球磨法制备亚微米TATB炸药

高能球磨法是对敏感炸药进行安全细化的有效方法,本文采用高能球磨法对TATB炸药进行微纳化,研究了微纳过程中影响TATB细化效果的因素,包括表面活性剂、水料比、球磨温度、转速和球磨时间;总结了高能球磨法制备超细TATB的操作技巧,如球磨罐的安装、装料量的控制、磨腔内物料降温和磨球上物料的冲洗。上述研究和总结为安全高效利用高能球磨机制备超细炸药进行了有益尝试与探索,优化条件下得到了亚微米级超细TATB炸药。     

Fe- and Eu-doped TiO2 Photocatalytical Materials Prepared by High Energy Ball Milling

TiO₂ nanopowders, doped with Fe³⁺ and Eu³⁺ were obtained by high-energy ball milling and their physical properties were investigated as a function of the doping content and ball milling time. A noticeable red shift and high photoactivity in the degradation and catalytic oxidation reactions of styrene and phenol were found for all doped specimens.     

Effect of milling method and time on the properties and electrochemical performance of LiFePO4/C composites prepared by ball milling and thermal treatment

Effects of ball milling way and time on the phase formation, particulate morphology, carbon content, and consequent electrode performance of LiFePO₄/C composite, prepared by high-energy ball milling of Li₂CO₃, NH₄H₂PO₄, FeC₂O₄ raw materials with citric acid as organic carbon source followed by thermal treatment, were investigated. Three ball milling ways and five different milling durations varied from 0 to 8 h were compared. LiFePO₄/C composites could be obtained from all synthesis processes. TEM examinations demonstrated LiFePO₄/C from ball milling in acetone resulted in sphere shape grains with a size of ∼60 nm, similar size was observed for LiFePO₄/C from dry ball milling but in a more irregular shape. The ball milling in benzene resulted in a much larger size of ∼250 nm. The LiFePO₄/C composites prepared from dry ball milling and ball milling in acetone showed much better electrochemical performance than that from ball milling in benzene. SEM examinations and BET measurements demonstrated that the high-energy ball milling effectively reduced the grain size. A ball milling for 4 h resulted in the best electrochemical performance, likely due to the proper amount of carbon and proper carbon structure were created.     

High-efficiency mechanochemical synthesis of Strontium carbonate nanopowder from Celestite

In this study, the conversion of Celestite to SrCO₃ was studied by wet mechanochemical synthesis in a high-energy ball mill and treatment with Na₂CO₃. For this purpose, solid strontium carbonate and soluble Na₂SO₄ were obtained after wet milling of Celestite powder and sodium carbonate. The solid phase was washed with water at room temperature by filter pressing. X-Ray diffraction patterns showed that the SrCO₃ nanopowder was synthesized and conversion boosted with increasing the milling time up to 8 hours Also, Rietveld refinement analysis was used to calculate the fraction of SrCO₃ as well as structural properties of synthesized samples. It was found that initial Celestite could be converted to strontium carbonate with a purity more than 98% using high-energy milling without simultaneous heating. The optimum milling time was determined as 4 hours resulting in formation of nanopowders with an average particle size around 90 nm. Field Emission Scanning Electron Microscopy (FE-SEM), clearly showed the nanoscale structure of the synthesized powders.     

MnO2对自蔓延高温合成陶瓷复合钢管陶瓷层结构和性能的影响

采用MnO2作为添加剂自蔓延高温合成法制备了具有Al2O3和FeAl2O4陶瓷层的复合钢管,研究其对陶瓷层和过渡层的结构和性能的影响.结果表明:添加了MnO2后,陶瓷层表面晶粒排布更加致密,陶瓷层的内表面为层叠状的Al2O3细晶和少量的FeAl2O4;过渡层为Al2O3和混入的FeAl2O4外,还含有SiO2和MnO2,过渡层出现了向钢基体中渗透的网状结构.MnO2的加入并未改变复合钢管Al2O3和FeAl2O4陶瓷层的物相.加入4%(质量分数)MnO2的复合管的抗压度强度和陶瓷层的抗剪强度分别达到416 MPa和19.2 MPa,比未添加MnO2的样品分别提高了18.2%和12.3%     

New Strategies for Preparing NanoSized Silicon Nitride Ceramics

We report the preparation of nanosized silicon nitride (Si₃N₄) ceramics via high-energy mechanical milling and subsequent spark plasma sintering. A starting powder mixture consisting of ultrafine β-Si₃N₄ and sintering additives of 5-mol% Y₂O₃ and 2-mol% Al₂O₃ was prepared by high-energy mechanical milling. After milling, the powder mixture was mostly transformed into a non-equilibrium amorphous phase containing a large quantity of well-dispersed nanocrystalline β-Si₃N₄ particles. This powder precursor was then consolidated by spark plasma sintering at a temperature as low as 1600°C for 5 min at a heating rate of 300°C/min. The fully densified sample consisted of homogeneous nano-Si₃N₄ grains with an average diameter of about 70 nm, which led to noticeable high-temperature ductility and elevated hardness.