BaFe_（12）O_（19）/PU复合微球的制备及改性研究
|
摘要
本论文针对现有磁性微球存在的磁性物质含量低、粒度不均一、表面缺乏活性功能基团、生物相容性差等缺点,选择钡铁氧体粒子和聚氨酯(PU)为研究对象,制备出了一种结合了BaFe_(12)O_(19)的X光显影性和PU高分子的高弹性、优良的生物相容性等优点的BaFe_(12)O_(19)/PU磁性复合微球,并对合成微球进行了表面改性,获得了表面氨基化、高磁性物质含量、粒度均一的磁性复合微球。研究了微米、纳米BaFe_(12)O_(19)磁性粒子的合成及表面改性,优化了复合微球的制备工艺,对微球的理化性能进行了表征,对改性微球吸附性能进行了初步探讨。
确定了复合微球中磁性组分的制备工艺:采用自燃烧法合成BaFe_(12)O_(19)微粒,粒子为片状结构,平均粒径约1μm;以适量乙二醇和聚乙烯醇混合溶液为新助剂,采用柠檬酸盐溶胶凝胶法,利用快速升温和预烧热处理工艺,合成了球形BaFe_(12)O_(19)纳米粒子,粒子粒径为30-50 nm。微米、纳米BaFe_(12)O_(19)粒子均有较大的饱和磁化强度。
讨论了磁性粒子种类、搅拌速度等对微球包覆率、磁性能、形貌等的影响。本研究结合扫描电子显微镜(SEM)观察了微球的表面和内部形貌,红外光谱仪(IR)表征了微球的化学结构,热重分析仪分析了微球磁性无机物的含量即包覆率,振动样品磁强计(VSM)分析了微球的磁性能,紫外吸收光谱分析了微球的吸附量。结果表明:纳米BaFe_(12)O_(19)/PU磁性复合微球的包覆率20.06%要高于微米BaFe_(12)O_(19)/PU磁性复合微球的包覆率14.02%,粒子越小,磁性越强,包覆率越大;磁性复合微球在一定的粒径范围内,磁性物质的包覆量随着粒径的增大而增大,采用中速搅拌合成微球磁性物质含较高、粒度均一、球形度好;Nano-BaFe_(12)O_(19)/PU复合微球的饱和磁化强度(7.50emu/g)高于Micro-BaFe_(12)O_(19)/PU复合微球的饱和磁化强度(6.33 emu/g);微球经表面改性后成功接枝上了活性功能基团-NH_2,吸附实验研究表明,每1g微球吸附95 mg的卵磷脂,微球单位质量的吸附量较大,吸附率ω=72.24%,达到了良好的吸附效果。
At present,magnetic microspheres have many defects,such as low content of magnetic substance,broad distribution of particles size,lack of active functional groups on surface,bad biocompatibility and so on.In this study,Ba-ferrite particles and PU were chosen to prepare BaFe_(12)O_(19)/PU magnetic composite microspheres combining with X-ray radioparency and high magnetic response of BaFe_(12)O_(19) and excellent elasitisity,good biocompability of PU polymer.After surface modification, the microspheres obtained aminated surface,high magnetic contents and narrow size-distribution.The paper focused on preparation and surface modification of micro- and nano- BaFe_(12)O_(19) particles,the optimal technological conditions for preparation,physic-chemical properties and adsorptive Capacities of the composite microspheres.
An appropriate preparation technology for magnetic composite microspheres was established.BaFe_(12)O_(19) powder with flake structure and 1μm of average size was prepared by self-combustion method.Spherical nano-BaFe_(12)O_(19) particles were synthesized by using citrate sol-gel method combined with rapid warming and pre-heat treatment process,glycol and PVA were utilized as auxiliaries.The average size of nano-BaFe_(12)O_(19) particles was 30-50 nm.Both of micro-BaFe_(12)O_(19) and nano-BaFe_(12)O_(19) had high saturation magnetization.
In this paper,the influence of magnetic particles' size and stirring rate on the coating rate,magnetic properties and structure of microspheres were studied.The sutructure of microsphere was observed by SEM.The chemical constitution of microsphere was tested by FT-IR.The content of magnetic inorganic and magnetic properties of microspheres were analyzed by TG and VSM respectively.The adsorption quantity of microspheres was investigated by UV absorption spectra.The results showed that the coating rate of nano-BaFe_(12)O_(19)/PU magnetic composite microspheres was more than that of micro-BaFe_(12)O_(19)/PU ones.The magnetic properties and coating rate of microspheres increased with its particle size decreasing.When the size of magnetic particles kept in some range,coating rate of microspheres increased with its average size increasing.Magnetic microspheres had high purity,narrow particle size distribution and perfect sphere when medium stirring rate was adopted.Compared with micro-BaFe_(12)O_(19)/PU,nano-BaFe_(12)O_(19)/PU microspheres had high saturation magnetization.After surface modification,-NH_2 was grafted on the surface of microspheres.From adsoption experimet,we found that per gram microsphere could adsorb 95 mg lecithin,and the adsoption rate was 72.24%.
确定了复合微球中磁性组分的制备工艺:采用自燃烧法合成BaFe_(12)O_(19)微粒,粒子为片状结构,平均粒径约1μm;以适量乙二醇和聚乙烯醇混合溶液为新助剂,采用柠檬酸盐溶胶凝胶法,利用快速升温和预烧热处理工艺,合成了球形BaFe_(12)O_(19)纳米粒子,粒子粒径为30-50 nm。微米、纳米BaFe_(12)O_(19)粒子均有较大的饱和磁化强度。
讨论了磁性粒子种类、搅拌速度等对微球包覆率、磁性能、形貌等的影响。本研究结合扫描电子显微镜(SEM)观察了微球的表面和内部形貌,红外光谱仪(IR)表征了微球的化学结构,热重分析仪分析了微球磁性无机物的含量即包覆率,振动样品磁强计(VSM)分析了微球的磁性能,紫外吸收光谱分析了微球的吸附量。结果表明:纳米BaFe_(12)O_(19)/PU磁性复合微球的包覆率20.06%要高于微米BaFe_(12)O_(19)/PU磁性复合微球的包覆率14.02%,粒子越小,磁性越强,包覆率越大;磁性复合微球在一定的粒径范围内,磁性物质的包覆量随着粒径的增大而增大,采用中速搅拌合成微球磁性物质含较高、粒度均一、球形度好;Nano-BaFe_(12)O_(19)/PU复合微球的饱和磁化强度(7.50emu/g)高于Micro-BaFe_(12)O_(19)/PU复合微球的饱和磁化强度(6.33 emu/g);微球经表面改性后成功接枝上了活性功能基团-NH_2,吸附实验研究表明,每1g微球吸附95 mg的卵磷脂,微球单位质量的吸附量较大,吸附率ω=72.24%,达到了良好的吸附效果。
At present,magnetic microspheres have many defects,such as low content of magnetic substance,broad distribution of particles size,lack of active functional groups on surface,bad biocompatibility and so on.In this study,Ba-ferrite particles and PU were chosen to prepare BaFe_(12)O_(19)/PU magnetic composite microspheres combining with X-ray radioparency and high magnetic response of BaFe_(12)O_(19) and excellent elasitisity,good biocompability of PU polymer.After surface modification, the microspheres obtained aminated surface,high magnetic contents and narrow size-distribution.The paper focused on preparation and surface modification of micro- and nano- BaFe_(12)O_(19) particles,the optimal technological conditions for preparation,physic-chemical properties and adsorptive Capacities of the composite microspheres.
An appropriate preparation technology for magnetic composite microspheres was established.BaFe_(12)O_(19) powder with flake structure and 1μm of average size was prepared by self-combustion method.Spherical nano-BaFe_(12)O_(19) particles were synthesized by using citrate sol-gel method combined with rapid warming and pre-heat treatment process,glycol and PVA were utilized as auxiliaries.The average size of nano-BaFe_(12)O_(19) particles was 30-50 nm.Both of micro-BaFe_(12)O_(19) and nano-BaFe_(12)O_(19) had high saturation magnetization.
In this paper,the influence of magnetic particles' size and stirring rate on the coating rate,magnetic properties and structure of microspheres were studied.The sutructure of microsphere was observed by SEM.The chemical constitution of microsphere was tested by FT-IR.The content of magnetic inorganic and magnetic properties of microspheres were analyzed by TG and VSM respectively.The adsorption quantity of microspheres was investigated by UV absorption spectra.The results showed that the coating rate of nano-BaFe_(12)O_(19)/PU magnetic composite microspheres was more than that of micro-BaFe_(12)O_(19)/PU ones.The magnetic properties and coating rate of microspheres increased with its particle size decreasing.When the size of magnetic particles kept in some range,coating rate of microspheres increased with its average size increasing.Magnetic microspheres had high purity,narrow particle size distribution and perfect sphere when medium stirring rate was adopted.Compared with micro-BaFe_(12)O_(19)/PU,nano-BaFe_(12)O_(19)/PU microspheres had high saturation magnetization.After surface modification,-NH_2 was grafted on the surface of microspheres.From adsoption experimet,we found that per gram microsphere could adsorb 95 mg lecithin,and the adsoption rate was 72.24%.
引文
[1]刘吉平,郝向阳.纳米科学与技术.北京:科学出版社,2005
[2]Meldrum F C,Heywood B R,Mann S.Magnetoferritin:in vitro synthesis of a novel magnetic protein.Science,1992,257(2):522-523
[3]Murray C B,Sun S,Doyle H.Conformational Behavior of Giant DNA through Binding with Ag+and Metallization.Mater Res Soc Bull,2001,26(1):985-991
[4]吕慧丹,刘峥,刘勇平.磁性高分子微球的制备及生物医学应用.化工新型材料,2004,32(3):10-13
[5]马秀玲,黄丽梅,郑思宁.磁性微球的制备及研究进展.广州化学,2003,28(3):58-64
[6]魏衍超,杨连生.超顺磁性葡聚糖氧化铁纳米颗粒的制备及其作为基因载体的可行性研究.磁性材料及器件,1999,30(6):18-21
[7]T Bahar S,S Celibi,J Appl Polym.Immobilization of gluocoamylase on magnetic poly(styrene) particles.Science,1999,72(1):69-73
[8]丁小斌,孙宗华.磁性高分子微球的制备和应用研究进展.化学通报,1997,(1):1-5
[9]贺枰.高Fe3O_4含量单分散的P(St/AA)纳米复合微球的制备及生物应用研究:[硕士学位论文].上海:上海交通大学化学化工学院,2007
[10]Guang Ming Qiu.Incorporation of Iron Oxide Nanoparticles and Quantum Dots into Silica Microspheres.Biomacromolecules,2005,6(1):1041-1047
[11]Guang Ming Qiu.α-amylase immobilized by Fe_3O_4/poly(styrene-co-maleic anhydride)magnetic composite microspheres:preparation and characterizationJournal of Applied Polymer.Science,2005,95(2):328-335
[12]X L Xu,G riedman,K D Humfeld,et al.Facile Synthesis and Characterization of Cobalt Ferrite Nanocrystals via a Simple Reduction-Oxidation Route.Chem Mater,2002,14(3):1249-1256
[13]P C Wang,W Y Chiu,C F Lee,et al.A novel approach to hollow superparamagnetic magnetite/polystyrene nanocomposite microspheres via interfacial polymerization.J Polym Science A:Polym Chem,2004,42(1):5695-5705
[14]Liliana P Ramirez,Katharina Landfester.Effects of Crosslinking Methods on Structure and Properties of Cellulose/PVA Hydrogels.Macromol Chem phys,2003,204(1):22-31
[15]Weiming Zheng,Feng Gao,Hongchen Gu.Investigation of Interactions Between Dendrimer-coated Magnetite Nanoparticles and Bovine Serum Albumin.Journal of Magnetic Materials,2005,293(1):252-258
[16]Z L Liu,Z H Ding,K L Yao.Characterization and application of Fe_3O_4/SiO_2 nanocomposites.Journal of Magnetic and Magnetic Materials,2003,265(5):98-102
[17]Denkbas,EmirBaki:Kilieay,Ebur:Birtikseven,Cengiz:OUZtkr,Eylem.Mangetic chitosan microspheres:Preparation and characterization.Reaetive&Functional Polymers,2002,50(3):225-232
[18]Rembaum,A.Dreyer,W.J.Immunomierospheres:reagent for cell labeling and separation.Seience,1980,208(1):364-68
[19]王胜林,朱以华,吴秋芳等.微悬浮聚合法合成聚苯乙烯磁性微球.华东理工大学学报,2001,27(4):364-367
[20]万惠文,张强,宋宏涛等.聚合物磁性粒子的制备.武汉工业大学学报,1999,21(1):22-24
[21]蒋中华,张津辉.生物分子固定化技术及应用.北京:化学工业出版社,1998
[22]任广智,李振华,何炳林.磁性壳聚糖微球用于酶的固定化研究.离子交换与吸附,2001,17(3):224-229.
[23]邹耀邦,王璐,刘波.聚乙二醇(PEG)的活化及其在药物释放和反应载体中的应用.世界科技研究与发展,2003,25(2):63-68.
[24]Whitesides,G.M.,Kazlauskas,R.J.and Jesephson,L.Magnetic separation in biotechnology.Trends Biotechnol,1983,1(15):144-148
[25]DekkerRFM,APPL.Biosynthesis and Biodegradation of Wood Components.Biochem.Biotech,1989,22(1):486-470
[26]徐修生.高性能铁氧体磁性材料的研制.金属矿山,2000,(7):26-27
[27]张密云,周铭,辛艳凤等.柠檬法合成SrFe_(12)O_(19)超微粉末.硅酸盐学报,1996,24(6):685-689
[28]王志良,王步云.钡铁氧体磁记录材料发展概况.信息记录材料,2003,4(4):49-53
[29]Jenike A W.Storage and flow of solids.Utah.Eng.Exp.Stn.Bull.,1964,21(2):159-165
[30]DUAN Hong-Zhen,LI Feng-Sheng,LI Qiao-Ling.Cailiao Kexue Yu Gongcheng(Journal of Materials Science&Engineering),2007,25(2):179-183
[31]都有为.铁氧体.南京:江苏科学技术出版社,1995
[32]Kloubek J.J.Cell.Preparation and magnetic properties of different morphology nano-SrFe_(12)O_(19) particles prepared by sol-gel method.Science,1994,163(2):10-18
[33]周志刚.铁氧体磁性材料.北京:科学出版社,1981
[34]李荫远,李国栋.铁氧体物理学.北京:科学出版社,1978
[35]贡长生,张克立.新功能材料.北京:化学工业出版社,2001
[36]黄健,戴红莲,邵海成等.自燃烧法制备钡铁氧体微粉.国外建材科技,2005,26(4):8-10
[37]Lin CH,ShinZW.Hydrothermal processing to produce magnetic particulates.IEEE Trans Magn,1990,26(1):15-17
[38]谢丹阳,高发明.M-型钡铁氧体的制备与表征.兵器材料科学与工程,2004,27(1):6-9
[39]龙春泉,刘颖,余智勇.共沉淀法制备钡铁氧体.过程工程学报,2004,4(5):435-437
[40]卓长平,张雄,李敏.sol-gel法制备之纳米钡铁氧体微波性能的研究.电子元件与材料,2005,24(5):15-16
[41]ZENG Aixiang,XIONG Weihao.Structure and Properties of BaFe_(12)O_(19) Coated Fly Ash -Cenospheres by Sol-Gel Process.Wuhan University of Technology-Mater.Science.,2006,21(3):130-131
[42]王艳丽,黄英,闫梨等.柠檬酸溶胶-凝胶法制备钡铁氧体.硅酸盐通报,2006,25(4):84-88
[43]沈国柱,徐政,李轶.纳米级M型铁氧体的溶胶-凝胶法制备和形貌控制.材料科学与工程学报,2005,23(5):522-523
[44]谢晶曦.红外光谱在有机化学和约物化学中的应用.北京:科学出版社,1990
[45]赵文俞,张清杰,李鹏等.柠檬酸法合成SrFe_(12)O_(19)磁铅石型铁氧体的晶化过程研究.硅酸盐学报,2003,31(1):21-30
[46]郭方方,徐劲峰,徐政等.六角晶系钡铁氧体纳米晶微波吸收剂的晶化特性研究.材料科学与工程学报,2004,22(6):872-874
[47]Zhong W,Ding W.P,Zhang N,Hong J.M,Yan Q.J.Key step in synthesis of ultrafine BaFe_(12)O_(19) by sol-gel technique.Journal of magnetic Materials,1997,168(1):196-200
[48]任平,官建国,王琦等.热处理温度对M型BaFe_(12)O_(19)铁氧体空心微球结构和静磁特性的影响.硅酸盐学报,2005,33(1):70-72
[49]Yue Z X,Zhou J,Li L,et al.Synthesis of nano crystalline NiCuZn ferrite powders by sol-gel auto-combustion method.Journal of Magnetism and Magnetic Materials,2000,208(1):55-60
[50]司新文,刘建中,杨正等.钡铁氧体超微磁粉颗粒的表面磁特性.化工治金,1997,18(3):197-201
[51]Hultman,T.,Bergh,S.,Moks,T.and Uhlen,M.Bidirectional solid-phase sequencing of in vitro-amplified plasmid DNA.Bio/Techniques,1991,10(4):84-93
[52]陈龙武,任煜,甘礼华等.无机粉体的表面改性技术.实验室研究与探索,2003,6(22):45-46
[53]刘峥.Fe_3O_4微粒表面有机改性及其应用研究.化工技术与开发,2004,3(33):12-15
[54]郭云亮,张涑戎,李立平.偶联剂的种类和特点及应用.橡胶工业,2003,11(50):692-697
[55]赵虹.含氧化合物的红外光谱特征.光谱学与光谱分析,2001,21(4):506-507
[56]黄英,王艳丽,闫梨等.热处理条件对纳米钡铁氧体磁性能的影响.西北工业大学学报,2007,25(6):875-879
[57]Bodker,F.Morup,S.Linderoth,S.Phys.Investigation of the Growth Mechanism of Iron Oxide Nanoparticles via a Seed-Mediated Method and Its Cytotoxicity Studies.Rev Lett,1994,72(2):282-285
[58]M.Respaud,J.M.Broto,M.oiran,et al.Dynamical properties of non-interacting Co nanoparticles.Phys.Rev.B,1998,57(5):2925-2935
[59]M.Jamet,V.Dupuis,P.M(?)linon,et al.Structure and magnetism of well defined cobalt nanoparticles embedded in a niobium matrix.Phys.Rev.B,2000,62(1):493-497
[60]傅明源,孙酣经.聚氨酯弹性体及其应用.北京:化学工业出版社,2006
[61]周超.聚氨酯磁性复合微球的制备及表征:[硕士学位论文].武汉:武汉理工大学材料学院,2007
[62]Christina Freij-Larsson,Patric Jannasch,BengtWesslen.Polyurethane SurfacesModified by Amphilic Poly-mers:effects on Protein Adsorption.Biomaterial,2000,21(1):307-315
[63]Archambault J G,Brash J L.Protein Resistant Polyure-thane Surfaces by Chemical Grafting of PEO:amino-ter-minated PEO as Grafting Reagent.Colloids and Sur-faces B:Biointerfaces,2004,39(2):9-16
[64]Mehlika Pulat,Dogan Babayigit.Surface Modification of PU Membranes by Graft Copolymerization with Acrylam-ide and Itaconic Acid Monomers.Polymer Testing,2001,20(1):209-216
[65]Archambault JG,Brash JL.Protein Repellent Polyurethane-urea Surfaces by Chemical Grafting of Hydroxyl-termi-nated Poly(ethylene oxide):effects of Protein Size and Charge.Colloids and Surfaces B:Biointerfaces,2004(3):111-120
[66]Matzumoto Koichi.Yu Shi.Studies on the Constituents and Bioactivity of Crocus sativus.Dictamnus angustifolius and the Synthesis of Phenanthraquinones,1983,36(10):46-52
[67]Kullenbery F W.Preferential degradation of noncholine phosphatides in soybean lecithin by thermalization.Journal of the American Oil Chemists' Society,1994,71(2):1195-1199
[68]凌关庭.大豆磷脂、蛋黄磷脂及其系列化精制品.中国食品添加剂,1999,45(3):67-77
[69]宋国安.大豆卵磷脂的开发及应用前景.中国油脂,2001,26(4):33-35
[70]庞玉珍,王玉静.速溶奶粉中卵磷脂含量的测定.中国乳品工业,1998,26(3):46-47
[71]陈卫涛,张德权,张柏林等.紫外分光光度法测定保健品中卵磷脂的含量.中国粮油学报,2006,21(3):190-191
[72]王强华等.卵磷脂的红外光谱和紫外光谱研究.南京师大学报,1994,17(2):51-53
[73]赵振国,陈小慧,顾惕人.砗胶自溶液中吸附胆固醇和卵磷脂.应用化学,1987,4(5):65-68
[2]Meldrum F C,Heywood B R,Mann S.Magnetoferritin:in vitro synthesis of a novel magnetic protein.Science,1992,257(2):522-523
[3]Murray C B,Sun S,Doyle H.Conformational Behavior of Giant DNA through Binding with Ag+and Metallization.Mater Res Soc Bull,2001,26(1):985-991
[4]吕慧丹,刘峥,刘勇平.磁性高分子微球的制备及生物医学应用.化工新型材料,2004,32(3):10-13
[5]马秀玲,黄丽梅,郑思宁.磁性微球的制备及研究进展.广州化学,2003,28(3):58-64
[6]魏衍超,杨连生.超顺磁性葡聚糖氧化铁纳米颗粒的制备及其作为基因载体的可行性研究.磁性材料及器件,1999,30(6):18-21
[7]T Bahar S,S Celibi,J Appl Polym.Immobilization of gluocoamylase on magnetic poly(styrene) particles.Science,1999,72(1):69-73
[8]丁小斌,孙宗华.磁性高分子微球的制备和应用研究进展.化学通报,1997,(1):1-5
[9]贺枰.高Fe3O_4含量单分散的P(St/AA)纳米复合微球的制备及生物应用研究:[硕士学位论文].上海:上海交通大学化学化工学院,2007
[10]Guang Ming Qiu.Incorporation of Iron Oxide Nanoparticles and Quantum Dots into Silica Microspheres.Biomacromolecules,2005,6(1):1041-1047
[11]Guang Ming Qiu.α-amylase immobilized by Fe_3O_4/poly(styrene-co-maleic anhydride)magnetic composite microspheres:preparation and characterizationJournal of Applied Polymer.Science,2005,95(2):328-335
[12]X L Xu,G riedman,K D Humfeld,et al.Facile Synthesis and Characterization of Cobalt Ferrite Nanocrystals via a Simple Reduction-Oxidation Route.Chem Mater,2002,14(3):1249-1256
[13]P C Wang,W Y Chiu,C F Lee,et al.A novel approach to hollow superparamagnetic magnetite/polystyrene nanocomposite microspheres via interfacial polymerization.J Polym Science A:Polym Chem,2004,42(1):5695-5705
[14]Liliana P Ramirez,Katharina Landfester.Effects of Crosslinking Methods on Structure and Properties of Cellulose/PVA Hydrogels.Macromol Chem phys,2003,204(1):22-31
[15]Weiming Zheng,Feng Gao,Hongchen Gu.Investigation of Interactions Between Dendrimer-coated Magnetite Nanoparticles and Bovine Serum Albumin.Journal of Magnetic Materials,2005,293(1):252-258
[16]Z L Liu,Z H Ding,K L Yao.Characterization and application of Fe_3O_4/SiO_2 nanocomposites.Journal of Magnetic and Magnetic Materials,2003,265(5):98-102
[17]Denkbas,EmirBaki:Kilieay,Ebur:Birtikseven,Cengiz:OUZtkr,Eylem.Mangetic chitosan microspheres:Preparation and characterization.Reaetive&Functional Polymers,2002,50(3):225-232
[18]Rembaum,A.Dreyer,W.J.Immunomierospheres:reagent for cell labeling and separation.Seience,1980,208(1):364-68
[19]王胜林,朱以华,吴秋芳等.微悬浮聚合法合成聚苯乙烯磁性微球.华东理工大学学报,2001,27(4):364-367
[20]万惠文,张强,宋宏涛等.聚合物磁性粒子的制备.武汉工业大学学报,1999,21(1):22-24
[21]蒋中华,张津辉.生物分子固定化技术及应用.北京:化学工业出版社,1998
[22]任广智,李振华,何炳林.磁性壳聚糖微球用于酶的固定化研究.离子交换与吸附,2001,17(3):224-229.
[23]邹耀邦,王璐,刘波.聚乙二醇(PEG)的活化及其在药物释放和反应载体中的应用.世界科技研究与发展,2003,25(2):63-68.
[24]Whitesides,G.M.,Kazlauskas,R.J.and Jesephson,L.Magnetic separation in biotechnology.Trends Biotechnol,1983,1(15):144-148
[25]DekkerRFM,APPL.Biosynthesis and Biodegradation of Wood Components.Biochem.Biotech,1989,22(1):486-470
[26]徐修生.高性能铁氧体磁性材料的研制.金属矿山,2000,(7):26-27
[27]张密云,周铭,辛艳凤等.柠檬法合成SrFe_(12)O_(19)超微粉末.硅酸盐学报,1996,24(6):685-689
[28]王志良,王步云.钡铁氧体磁记录材料发展概况.信息记录材料,2003,4(4):49-53
[29]Jenike A W.Storage and flow of solids.Utah.Eng.Exp.Stn.Bull.,1964,21(2):159-165
[30]DUAN Hong-Zhen,LI Feng-Sheng,LI Qiao-Ling.Cailiao Kexue Yu Gongcheng(Journal of Materials Science&Engineering),2007,25(2):179-183
[31]都有为.铁氧体.南京:江苏科学技术出版社,1995
[32]Kloubek J.J.Cell.Preparation and magnetic properties of different morphology nano-SrFe_(12)O_(19) particles prepared by sol-gel method.Science,1994,163(2):10-18
[33]周志刚.铁氧体磁性材料.北京:科学出版社,1981
[34]李荫远,李国栋.铁氧体物理学.北京:科学出版社,1978
[35]贡长生,张克立.新功能材料.北京:化学工业出版社,2001
[36]黄健,戴红莲,邵海成等.自燃烧法制备钡铁氧体微粉.国外建材科技,2005,26(4):8-10
[37]Lin CH,ShinZW.Hydrothermal processing to produce magnetic particulates.IEEE Trans Magn,1990,26(1):15-17
[38]谢丹阳,高发明.M-型钡铁氧体的制备与表征.兵器材料科学与工程,2004,27(1):6-9
[39]龙春泉,刘颖,余智勇.共沉淀法制备钡铁氧体.过程工程学报,2004,4(5):435-437
[40]卓长平,张雄,李敏.sol-gel法制备之纳米钡铁氧体微波性能的研究.电子元件与材料,2005,24(5):15-16
[41]ZENG Aixiang,XIONG Weihao.Structure and Properties of BaFe_(12)O_(19) Coated Fly Ash -Cenospheres by Sol-Gel Process.Wuhan University of Technology-Mater.Science.,2006,21(3):130-131
[42]王艳丽,黄英,闫梨等.柠檬酸溶胶-凝胶法制备钡铁氧体.硅酸盐通报,2006,25(4):84-88
[43]沈国柱,徐政,李轶.纳米级M型铁氧体的溶胶-凝胶法制备和形貌控制.材料科学与工程学报,2005,23(5):522-523
[44]谢晶曦.红外光谱在有机化学和约物化学中的应用.北京:科学出版社,1990
[45]赵文俞,张清杰,李鹏等.柠檬酸法合成SrFe_(12)O_(19)磁铅石型铁氧体的晶化过程研究.硅酸盐学报,2003,31(1):21-30
[46]郭方方,徐劲峰,徐政等.六角晶系钡铁氧体纳米晶微波吸收剂的晶化特性研究.材料科学与工程学报,2004,22(6):872-874
[47]Zhong W,Ding W.P,Zhang N,Hong J.M,Yan Q.J.Key step in synthesis of ultrafine BaFe_(12)O_(19) by sol-gel technique.Journal of magnetic Materials,1997,168(1):196-200
[48]任平,官建国,王琦等.热处理温度对M型BaFe_(12)O_(19)铁氧体空心微球结构和静磁特性的影响.硅酸盐学报,2005,33(1):70-72
[49]Yue Z X,Zhou J,Li L,et al.Synthesis of nano crystalline NiCuZn ferrite powders by sol-gel auto-combustion method.Journal of Magnetism and Magnetic Materials,2000,208(1):55-60
[50]司新文,刘建中,杨正等.钡铁氧体超微磁粉颗粒的表面磁特性.化工治金,1997,18(3):197-201
[51]Hultman,T.,Bergh,S.,Moks,T.and Uhlen,M.Bidirectional solid-phase sequencing of in vitro-amplified plasmid DNA.Bio/Techniques,1991,10(4):84-93
[52]陈龙武,任煜,甘礼华等.无机粉体的表面改性技术.实验室研究与探索,2003,6(22):45-46
[53]刘峥.Fe_3O_4微粒表面有机改性及其应用研究.化工技术与开发,2004,3(33):12-15
[54]郭云亮,张涑戎,李立平.偶联剂的种类和特点及应用.橡胶工业,2003,11(50):692-697
[55]赵虹.含氧化合物的红外光谱特征.光谱学与光谱分析,2001,21(4):506-507
[56]黄英,王艳丽,闫梨等.热处理条件对纳米钡铁氧体磁性能的影响.西北工业大学学报,2007,25(6):875-879
[57]Bodker,F.Morup,S.Linderoth,S.Phys.Investigation of the Growth Mechanism of Iron Oxide Nanoparticles via a Seed-Mediated Method and Its Cytotoxicity Studies.Rev Lett,1994,72(2):282-285
[58]M.Respaud,J.M.Broto,M.oiran,et al.Dynamical properties of non-interacting Co nanoparticles.Phys.Rev.B,1998,57(5):2925-2935
[59]M.Jamet,V.Dupuis,P.M(?)linon,et al.Structure and magnetism of well defined cobalt nanoparticles embedded in a niobium matrix.Phys.Rev.B,2000,62(1):493-497
[60]傅明源,孙酣经.聚氨酯弹性体及其应用.北京:化学工业出版社,2006
[61]周超.聚氨酯磁性复合微球的制备及表征:[硕士学位论文].武汉:武汉理工大学材料学院,2007
[62]Christina Freij-Larsson,Patric Jannasch,BengtWesslen.Polyurethane SurfacesModified by Amphilic Poly-mers:effects on Protein Adsorption.Biomaterial,2000,21(1):307-315
[63]Archambault J G,Brash J L.Protein Resistant Polyure-thane Surfaces by Chemical Grafting of PEO:amino-ter-minated PEO as Grafting Reagent.Colloids and Sur-faces B:Biointerfaces,2004,39(2):9-16
[64]Mehlika Pulat,Dogan Babayigit.Surface Modification of PU Membranes by Graft Copolymerization with Acrylam-ide and Itaconic Acid Monomers.Polymer Testing,2001,20(1):209-216
[65]Archambault JG,Brash JL.Protein Repellent Polyurethane-urea Surfaces by Chemical Grafting of Hydroxyl-termi-nated Poly(ethylene oxide):effects of Protein Size and Charge.Colloids and Surfaces B:Biointerfaces,2004(3):111-120
[66]Matzumoto Koichi.Yu Shi.Studies on the Constituents and Bioactivity of Crocus sativus.Dictamnus angustifolius and the Synthesis of Phenanthraquinones,1983,36(10):46-52
[67]Kullenbery F W.Preferential degradation of noncholine phosphatides in soybean lecithin by thermalization.Journal of the American Oil Chemists' Society,1994,71(2):1195-1199
[68]凌关庭.大豆磷脂、蛋黄磷脂及其系列化精制品.中国食品添加剂,1999,45(3):67-77
[69]宋国安.大豆卵磷脂的开发及应用前景.中国油脂,2001,26(4):33-35
[70]庞玉珍,王玉静.速溶奶粉中卵磷脂含量的测定.中国乳品工业,1998,26(3):46-47
[71]陈卫涛,张德权,张柏林等.紫外分光光度法测定保健品中卵磷脂的含量.中国粮油学报,2006,21(3):190-191
[72]王强华等.卵磷脂的红外光谱和紫外光谱研究.南京师大学报,1994,17(2):51-53
[73]赵振国,陈小慧,顾惕人.砗胶自溶液中吸附胆固醇和卵磷脂.应用化学,1987,4(5):65-68