水溶性交联聚合物微球的制备及性能

采用反相微乳液聚合制备水溶性交联聚合物微球。交联比为0 1%、0 5%、1 0%时,微球平均粒径分别为74 9、151 8、214 9nm。水化时间由0增至144h时,微球平均粒径由106 7nm增大到189 5nm。盐质量分数由0增至0 5%时,微球平均粒径由202 7nm减小到93 5nm。微孔滤膜封堵性能随水化时间无明显变化,随盐质量分数的增加而明显降低。岩心封堵实验表明,交联聚合物微球对气测渗透率为3 058μm2的岩心的流动阻力可达120kPa。     

化学还原法制备Ag-TiO2光催化抗菌材料的研究

选用平均粒径分别为30nm和8μm的二氧化钛为原料,利用化学还原法制得银质量分数为0. 7% ~5%的Ag-TiO2光催化抗菌材料,采用抑菌圈试验对其抗菌性能进行研究,通过光催化降解亚甲基蓝实验研究了二氧化钛载银前后光催化活性的改变。结果表明,负载1% (质量分数)银的平均粒径为30nm的二氧化钛经250℃热处理后具有良好的抗菌性,其催化活性没有改变。     

纳米TiO_2-Pt修饰电极上甲醇的电催化氧化研究

用电化学法合成前驱体Ti(OEt)4,经直接水解法制备纳米TiO2膜,通过直接在纳米TiO2膜上电沉积Pt微粒得到纳米TiO2 Pt复合催化电极。扫描电子显微镜(SEM)和X射线衍射(XRD)分析结果表明,纳米TiO2的晶形为锐钛矿型,粒径约30nm,电沉积纳米Pt粒子(平均粒径约60nm)均匀地分散在纳米TiO2膜表面。循环伏安和计时电位测试表明,纳米TiO2 Pt修饰电极对甲醇的电氧化具有高催化活性和稳定性,Pt载量为0 68mg/cm2时,室温下甲醇氧化电流达到190mA/cm2,是纯Pt电极上的7 6倍。     

冷藏运输用Al_2O_3-H_2O纳米流体蓄冷相变时间分析

利用恒温浴槽分别对质量分数为5%,Al2O3粒径分别为10,20,50,100,500 nm和粒径为10 nm,质量分数分别为5%,10%,12%,15%,20%的两组Al2O3-H2O纳米流体进行冻结,分析了纳米流体和去离子水在冻结过程中的温度变化,讨论了Al2O3粒径和浓度对冻结过程的影响。结果表明,在去离子水基液中加入Al2O3纳米颗粒,减少了凝固相变时间,且当质量分数为5%时,相变时间随粒径增大而增加,粒径为10 nm时,相变时间最短;当粒径为10 nm,质量分数小于10%或大于12%时,相变时间均随质量分数的增大而增加,但质量分数为12%时,相变时间最短。相对于冰作为蓄冷材料,纳米蓄冷材料可节省蓄冷时间,有效提高能源利用效率。     

改良单质硅水解法制备硅溶胶的工艺研究

采用改良单质硅水解法工艺,经胶核制备和胶粒生长步骤制备硅溶胶.通过正交试验发现,对硅溶胶胶核平均粒径和硅粉转化率的综合影响因素大小顺序为硅粉加入量＞水玻璃加入量＞反应温度＞反应时间.最优胶核制备条件为:硅粉加入量80 g;水玻璃加入量30 mL;反应温度90 ℃;反应时间6 h.此时得到的硅溶胶胶核粒径:7～9 nm,硅粉转化率:63%～66%,SiO2质量分数:16%～20%,Na2O质量分数:0.5%.经多次胶粒生长,可制得平均粒径20 nm、40 nm、60 nm、80 nm的硅溶胶产品.     

BaMoO4：Eu^3＋红色荧光粉的制备及发光性质

采用柠檬酸溶胶-凝胶法制备了BaMoO4：Eu^3＋红色荧光粉,差热（DSC）和X射线衍射（XRD）研究结果表明,经过700℃高温烧结后可得到BaMoO4纯物相。粒度分析结果表明,经700℃烧结后样品的粒径约为200nm,随着烧结温度的升高,产物的粒径明显增大,当烧结温度为800℃时,样品的粒径约为500 nm。分别以392 nm的近紫外光和462 nm的可见光激发样品,BaMoO4：Eu^3＋荧光粉发红光,对应于Eu3＋的4f-4f跃迁,其中以615nm附近的5D0→7F2电偶极跃迁发光最强,当Eu3＋的掺杂浓度约为25 mol%时,在616 nm处的发光强度最大。荧光粉在392 nm和462 nm的吸收分别与紫外光和蓝光LED芯片相匹配。因此,BaMoO4：Eu^3＋荧光粉是一种可能应用在白光LED上的红色荧光材料。     

机械化学法制备ZrO_2∶Eu~(3+)纳米晶及其发光特性

以ZrOCl2·8H2O、EuCl3·6H2O和NaOH为原料,采用机械化学法制备ZrO2∶Eu3+发光粉体。采用透射电镜、X射线衍射仪和荧光光谱仪对其微观形貌、物相和发光特征进行表征。结果表明:ZrO2∶Eu3+发光粉体为分散均匀,粒径约为10nm的纳米晶。主晶相为t-ZrO2,随着煅烧温度的升高,出现少量m-ZrO2。发射光谱为Eu3+在604nm和595nm处的特征发射,分别对应5D0→7F2和5D0→7F1跃迁。m-ZrO2出现导致ZrO2∶Eu3+对称性的下降,在610nm处出现发射峰。Eu3+掺杂量为8mol%时达到最大发光强度。     

BaMoO_4:Eu~(3+)红色荧光粉的制备及发光性质

采用柠檬酸溶胶-凝胶法制备了BaMoO4:Eu3+红色荧光粉,差热(DSC) 和X射线衍射(XRD)研究结果表明,经过700 ℃高温烧结后可得到BaMoO4纯物相.粒度分析结果表明,经700 ℃烧结后样品的粒径约为 200 nm,随着烧结温度的升高,产物的粒径明显增大,当烧结温度为800 ℃时,样品的粒径约为 500 nm.分别以392 nm 的近紫外光和 462 nm 的可见光激发样品,BaMoO4:Eu3+荧光粉发红光,对应于Eu3+的4f-4f跃迁,其中以615 nm附近的5D0→7F2电偶极跃迁发光最强,当Eu3+的掺杂浓度约为25 mol %时,在616 nm处的发光强度最大.荧光粉在392 nm和462 nm的吸收分别与紫外光和蓝光LED芯片相匹配.因此,BaMoO4:Eu3+荧光粉是一种可能应用在白光LED上的红色荧光材料.     

低温制备金红石型纳米TiO2粉体

利用TiCl4低温水解法,添加TiO2溶胶制备了纳米TiO2粉体.用X射线衍射、透射电子显微镜和激光粒度仪研究了制备的纳米TiO2粉体的晶型、形貌、晶粒尺寸及粒径分布.结果表明:所得纳米TiO2粉体原始沉淀为金红石型,其粒径为10 nm左右的棒状粒子,经500℃煅烧2h,获得结晶完整、球形、粒径分布很窄的纳米TiO2粉体,其平均粒径为34 nm,粒径分布范围为20～50 nm.     

溶胶-凝胶法制备SrAl_2O_4∶Eu~(2+),Dy~(3+)纳米发光材料

采用溶胶 -凝胶法在低温、还原气氛下制备了SrAl2 O4∶Eu2 ,Dy3 纳米长余辉光致发光材料。XRD分析表明 ,当焙烧温度为 80 0～130 0℃时 ,所合成的样品为SrAl2 O4单斜晶系晶体结构 ,晶格常数为 :a =0 .8442 4nm ,b=0 .882 2nm ,c =0 .5 160 7nm。 110 0℃以上观察到样品长余辉发光。激发光谱与发射光谱分析表明 :发射光谱是峰值位于 5 2 3nm的宽带谱 ,激发光谱是峰值在 2 40 ,330 ,378,42 5nm的连续宽带谱。样品在自然光照射后持续发出明亮的绿光。样品的合成温度从 110 0℃增加到 130 0℃ ,样品的颗粒尺寸不断增大。TEM和电子衍射分析表明 ,110 0℃烧结 4h的SrAl2 O4∶Eu2 ,Dy3 纳米粉末为结晶相 ,粒径为 30～ 40nm。     

均相沉淀法制备纳米Al2O3先驱体

以分析纯硫酸铝铵和碳酸氢铵为原料，采用均相沉淀法制备纳米Al23先驱体。结果表明，溶液的混合方式，超声振动，陈化时间对粉体的尺寸和形貌有很大的影响。采用先缓慢滴加，然后喷雾混合的方式可获得平均粒径为10mm的NH4Al(OH)2CO3粉体，并对粉体进行了扫描电镜（SEM），透射电镜（TEM），比表面积（BET），X射线衍射（XRD），红外光谱分析（IR），热重／差热（TG／DTA）等表征。     

A novel thermal decomposition method for the synthesis of ZnO nanoparticles from low concentration ZnSO4 solutions

In this research work, ZnO nanoparticles were prepared by direct thermal decomposition method with Zn₄(SO₄)(OH)₆·0.5 H₂O as a precursor. The precursor was calcinated in air for 1 h at 825 °C. Samples were characterized by X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), infrared spectrum (IR), and scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The XRD, EDS, and IR results indicated that the ZnO nanoparticles were pure. The average crystallite and particle size of the ZnO nanoparticles were estimated to be 87 nm and 92 nm by XRD and TEM, respectively. The SEM and TEM images showed that the ZnO nanoparticles were of spherical shape. The simplicity of the present method suggests its potential application at industrial scale as a cheap and convenient way to produce pure ZnO nanoparticles from low concentration ZnSO₄ solutions.     

室温固相合成掺杂ZnO纳米粉体制备ZnO压敏电阻

以金属离子盐和草酸为原料,采用室温固相化学反应合成掺杂ZnO前驱物,根据DSC-TG分析结果,将其在450℃热分解2 h,得到掺杂ZnO粉体,并用此粉体制备了片式ZnO压敏电阻。借助XRD、TEM、BET等检测手段对粉体产物的物相、形貌、粒度等进行了表征。研究了烧结温度对ZnO压敏电阻电性能的影响。结果表明,所制备的粉体为平均粒径24 nm左右、颗粒呈球状、分散性好的纤锌矿结构掺杂ZnO。在1 080℃烧结时,ZnO压敏电阻的综合电性能达到最佳,电位梯度为791.64 V/mm,非线性系数为24.36,漏电流为43μA。     

旋转填料床气液反应制备超细氧化锌工艺研究

以氨气和硝酸锌为原料,在旋转填料床中通过气液反应制备前驱体氢氧化锌.经煅烧后可得超细氧化锌粒子,经XRD和FEM检测得到其粒径为20-80nm。重点研究旋转填料床转速、原料浓度、氨气分率、气液比等对前驱体氢氧化锌粒径的影响,选择洗涤条件及优化煅烧温度和时间.确定了旋转填料床气液反应制备超细氧化锌的最佳工艺条件。     

利用铅锌废渣制备纳米ZnO的试验研究

以铅锌废渣为锌源,通过浸取、除杂、蒸发、干燥和焙烧等步骤制备纳米ZnO.ZnO前驱体的X射线衍射(XRD)、红外光谱分析(IR)、热重(TGA)和差热分析(DSC)分析表明:ZnO 前驱体是无定型碱式碳酸锌(Zn5 (CO3)2(OH)6),加热过程中它先分解成ZnO和Zn(OH)2,然后Zn(OH)2进一步分解成ZnO.焙烧产物的XRD、扫描电镜(SEM)和粒度分析显示:在400 ℃的温度下下焙烧时,ZnO前驱体分解产物是红锌矿(ZnO)和Ashoverite (Zn(OH)2);在500 ℃和600 ℃焙烧时,前驱体完全转化为红锌矿,其形貌不规则,但是前驱体在500 ℃焙烧时,产物ZnO的粒径较小,主要分布在80~150 nm,在600 ℃焙烧时,产物的颗粒团聚严重.     

Formation and Morphology of Zn(2)Ti(3)O(8) Powders Using Hydrothermal Process without Dispersant Agent or Mineralizer

Synthesis of Zn(2)Ti(3)O(8) powders for attenuating UVA using TiCl(4), Zn(NO(3))(2)·6H(2)O and NH(4)OH as precursor materials by hydrothermal process has been investigated. The X-ray diffractometry (XRD) results show the phases of ZnO, anatase TiO(2) and Zn(2)Ti(3)O(8) coexisted when the zinc titanate powders were calcined at 600 °C for 1 h. When calcined at 900 °C for 1 h, the XRD results reveal the existence of ZnO, Zn(2)TiO(4), rutile TiO(2) and ZnTiO(3). Scanning electron microscope (SEM) observations show extensive large agglomeration in the samples. Transmission electron microscope (TEM) and electron diffraction (ED) examination results indicate that ZnTiO(3) crystallites formed with a size of about 5 nm on the matrix of plate-like ZnO when calcined at 700 °C for 1 h. The calcination samples have acceptable absorbance at a wavelength of 400 nm, indicating that the zinc titanate precursor powders calcined at 700 °C for 1 h can be used as an UVA-attenuating agent.     

PREPARATION OF ZINC OXIDE NANOPARTICLE VIA UNIFORM PRECIPITATION METHOD AND ITS SURFACE MODIFICATION BY METHACRYLOXYPROPYLTRIMETHOXYSILANE

Zinc oxide nanoparticles were prepared by uniform precipitation using urea hydrolysis. The ZnO precursor was slowly deposited from aqueous solution. Anionic surfactant was added into solution to block ZnO crystal growth and its agglomeration. Then ZnO nanoparticles were synthesized by the calcination of the precursor at high temperature. Transmission electron microscope (TEM) observation and particle size analyzer demonstrated that the ZnO nanoparticle exhibited nearly spheric shape with 10-40 nm particle size. The surface of the ZnO nanoparticle was modified by methacryloxypropyltrimethoxysilane (MPS). FT-IR (Fourier transform-infrared spectrophotometry) and XPS (X-ray photoelectron spectrophotometry) revealed that MPS was grafted onto the zinc oxide nanoparticle. XRD (X-ray diffraction) showed that the ZnO nanoparticle was a hexagonal crystal with a perfect crystalline structure, and its crystalline morphology was not altered through surface modification. The activation index (AI) of the modified ZnO nanoparticle was measured. It was found that the surface of the ZnO nanoparticle was changed from hydrophilicity into hydrophobicity via surface modification, implying the enhancement of its compatibility with organic polymers. FE-SEM (field scanning electron microscopy) showed that the modified ZnO nanoparticles were homogeneously dispersed in PVC matrices. Consequently, ZnO nanoparticles were integrated with PVC matrices by the grafting organic molecule.     

氧化锌纳米粒子的制备

以ＺｎＳＯ_４· ７Ｈ_２ Ｏ为原料,添加 ＮａＯＨ溶液和 ＮＨ_４ ＨＣＯ_３粉末,制备出晶粒细小的碱式碳酸盐前驱体。８０℃干燥后,分别在３００、４００、５００℃焙烧１ｈ,制备出氧化锌ＺｎＯ纳米粒子。经ＸＲＤ和ＴＥＭ检测,粒径为１０、１４、２０ｎｍ。由于采用了对盐渍化的凝胶状前驱体先焙烧,然后用蒸馏水浸洗除去硫酸钠的方法,氧化锌纳米粒子粒径细小而均匀。     

纳米ZnO的制备及其光催化降解酸性红B

以Zn（acac）2·H2O为单源前驱体,用水热法成功地制备了纳米ZnO,利用X-射线衍射、扫描电子显微镜、透射电子显微镜等手段对样品进行了表征。对自制的纳米ZnO进行了光催化活性研究,结果表明：纳米ZnO对200～380nm波长范围的光和在可见光范围内都有较强的吸收作用。利用纳米ZnO作为光催化剂对有机染料溶液进行了降解实验,发现在太阳光照射3h后,对酸性红B的降解率可达到100%。     

PREPARATION OF ZINC OXIDE NANOPARTICLE VIA UNIFORM PRECIPITATION METHOD AND ITS SURFACE MODIFICATION BY METHACRYLOXYPROPYLTRIMETHOXYSILANE

Zinc oxide nanoparticles were prepared by uniform precipitation using urea hydrolysis. The ZnO precursor was slowly deposited from aqueous solution. Anionic surfactant was added into solution to block ZnO crystal growth and its agglomeration. Then ZnO nanoparticles were synthesized by the calcination of the precursor at high temperature. Transmission electron microscope (TEM) observation and particle size analyzer demonstrated that the ZnO nanoparticle exhibited nearly spheric shape with 10–40 nm particle size. The surface of the ZnO nanoparticle was modified by methacryloxypropyltrimethoxysilane (MPS). FT-IR (Fourier transform-infrared spectrophotometry) and XPS (X-ray photoelectron spectrophotometry) revealed that MPS was grafted onto the zinc oxide nanoparticle. XRD (X-ray diffraction) showed that the ZnO nanoparticle was a hexagonal crystal with a perfect crystalline structure, and its crystalline morphology was not altered through surface modification. The activation index (AI) of the modified ZnO nanoparticle was measured. It was found that the surface of the ZnO nanoparticle was changed from hydrophilicity into hydrophobicity via surface modification, implying the enhancement of its compatibility with organic polymers. FE-SEM (field scanning electron microscopy) showed that the modified ZnO nanoparticles were homogeneously dispersed in PVC matrices. Consequently, ZnO nanoparticles were integrated with PVC matrices by the grafting organic molecule.