CN107118563A - 一种纳米线/聚合物/纳米颗粒夹心复合材料的制备方法 - Google Patents
一种纳米线/聚合物/纳米颗粒夹心复合材料的制备方法 Download PDFInfo
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- CN107118563A CN107118563A CN201710429729.4A CN201710429729A CN107118563A CN 107118563 A CN107118563 A CN 107118563A CN 201710429729 A CN201710429729 A CN 201710429729A CN 107118563 A CN107118563 A CN 107118563A
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- 239000002070 nanowire Substances 0.000 title claims abstract description 96
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 74
- 239000002131 composite material Substances 0.000 title claims abstract description 68
- 229920000642 polymer Polymers 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 24
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000011065 in-situ storage Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000002604 ultrasonography Methods 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 46
- 229920002627 poly(phosphazenes) Polymers 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 31
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 14
- 150000003839 salts Chemical class 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 9
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 241000209094 Oryza Species 0.000 claims description 5
- 235000007164 Oryza sativa Nutrition 0.000 claims description 5
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 235000009566 rice Nutrition 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- -1 Phosphine nitrile Chemical class 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000002082 metal nanoparticle Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- ITHPEWAHFNDNIO-UHFFFAOYSA-N triphosphane Chemical compound PPP ITHPEWAHFNDNIO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 235000013339 cereals Nutrition 0.000 claims description 3
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical group C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 claims description 3
- 235000012149 noodles Nutrition 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims 4
- 229910052802 copper Inorganic materials 0.000 claims 2
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- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 239000002798 polar solvent Substances 0.000 claims 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
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- 239000011787 zinc oxide Substances 0.000 description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 20
- 239000000243 solution Substances 0.000 description 16
- 239000010949 copper Substances 0.000 description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 9
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- 230000009102 absorption Effects 0.000 description 7
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- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 235000011083 sodium citrates Nutrition 0.000 description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical class [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 2
- 235000013904 zinc acetate Nutrition 0.000 description 2
- 244000131522 Citrus pyriformis Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052603 melanterite Inorganic materials 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Substances [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000472 sulfonyl group Chemical group *S(*)(=O)=O 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G79/00—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule
- C08G79/02—Macromolecular compounds obtained by reactions forming a linkage containing atoms other than silicon, sulfur, nitrogen, oxygen, and carbon with or without the latter elements in the main chain of the macromolecule a linkage containing phosphorus
- C08G79/025—Polyphosphazenes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
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Abstract
本发明公开了一种纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，涉及纳米复合材料技术领域。本发明先合成出不同功能的纳米线；再将其超声分散在特定溶剂中，并以纳米线作为模板，加入聚合物单体，超声聚合反应一定时间，经简单后处理后即可得到原位生成的纳米线/聚合物功能材料；然后再将纳米线/聚合物功能材料作为模板，利用聚合物表面的活性基团，在该模板上原位生成功能性金属或金属氧化物纳米颗粒，得到纳米线/聚合物/纳米颗粒夹心复合材料。本工艺过程简单，成本低，产率高，具有一定的普适性，制得的纳米线/聚合物/纳米颗粒夹心复合材料结构可控、功能可调，在多功能复合材料领域有着广泛的应用前景。
Description
技术领域
本发明涉及纳米复合材料技术领域，尤其涉及一种多功能纳米材料的制备方法。
背景技术
一维纳米材料具有奇异的化学、物理效应，如：独特的电学、磁学、光学、热学、力学和催化性能等，因而，在光电子器件、吸波材料、光电催化、生物医学等众多领域有着广泛的应用前景。其中，金属或金属氧化物纳米线的合成方法简单、工艺成熟、易于生产，且不同的金属或金属氧化物纳米线具有不同的功能。如Cu，Pt等纳米线具有良好的催化性能，可以直接催化有机反应；Zn及ZnO纳米线具有良好的光电力学性能，在光电器件、压电材料、生物传感等领域具有广泛应用前景；Fe、Co，Ni等及其氧化物纳米线具有良好的电磁性能和生物相容性，在吸波材料、磁存储及生物医学领域有着广泛应用；Au，Ag等贵金属纳米线具有良好的导电性、催化性、生物相容性，可用作人工器脏、光电材料、催化材料等。
聚(环三膦腈-co-4,4’-二羟基二苯砜)(简称PZS)是一类新型有机无机杂化高分子，分子链中含有氮、磷、硫、氧等杂原子，具有优异的光热稳定性及生物相容性等，易于在纳米线表面通过单体原位聚合得到。此外，聚膦腈比表面积大，易于吸附无机纳米晶，继而在表面原位生长出纳米粒子。
本方法旨在利用聚膦腈独特的结构和化学合成特性，将纳米线、纳米粒子、聚合物的优异性能结合在一起，合成出带有多重功能的纳米复合材料。例如，铁纳米线/聚膦腈/氧化锌纳米粒子同时具有磁性、光催化性以及聚合物的化学活性；铂纳米线/聚膦腈/银纳米粒子同时具有化学催化性、导电性以及聚合物的化学活性。本方法首先在超声中以纳米线为模板，在纳米线表面原位聚合聚膦腈单体得到纳米线/聚膦腈纳米复合材料，然后在聚膦腈表面原位生长出纳米粒子，得到纳米线/聚膦腈/纳米颗粒夹心复合材料。本方法的优势在于：(1)合成的纳米线/聚膦腈/纳米颗粒夹心复合材料既具有纳米线的优异性能，又具有聚膦腈材料的优异特性，同时还具有纳米粒子的优异性能，是一种具有多重功能的纳米复合材料。(2)合成的纳米线/聚膦腈/纳米颗粒夹心复合材料结构可控，功能可控。聚合物和纳米粒子的包覆层厚度均可通过调节纳米线、聚膦腈、纳米粒子的比例进行调控。(3)工艺简单，条件温和，设备要求低，易于加工生产。
发明内容
本发明的目的是针对现有技术的不足而提供一种纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特点是先利用现有技术合成出金属或金属氧化物纳米线，再在超声中，以纳米线为模板，原位聚合生成金属或金属氧化物/聚膦腈复合纳米线材料；然后利用聚膦腈的表面性质，在金属或金属氧化物/聚膦腈复合纳米线表面原位生成金属或金属氧化物纳米粒子，从而得到纳米线/聚合物/纳米颗粒夹心复合材料。
该制备方法加工工艺简单，设备要求低，易于加工生产，制备出的纳米线/聚合物/纳米颗粒夹心复合材料兼具纳米线、聚合物、纳米颗粒的多种性能，是一种多功能型纳米复合材料，性能优异，应用前景广阔。
本发明一种纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，按照下述步骤进行：
(1)称取一定质量的纳米线，将其超声分散在一定量溶剂中，依次加入一定量六氯环三膦腈、4,4’-二羟基二苯砜、三乙胺，在一定反应条件下进行原位聚合；经后处理后，得到纳米线/聚膦腈复合材料。
(2)称取一定质量的纳米线/聚膦腈复合材料，加入溶剂、金属盐、一定反应条件下在聚合物表面原位生成金属或金属氧化物纳米粒子。经后处理后，得到纳米线/聚膦腈/纳米颗粒夹心复合材料。
其中步骤(1)所述的纳米线可以是金属纳米线，如Au，Ag，Pt，Si，Fe，Co，Ni，Zn等纳米线，也可以是金属氧化物纳米线，如ZnO，Fe3O4，SiO2，TiO2等金属氧化物纳米线。
其中步骤(1)所述的纳米线/聚膦腈复合材料的制备过程中：超声功率为100～240W，超声频率为80kHz，温度为0-80℃，溶剂可以是甲醇、四氢呋喃、乙醇、乙腈、丙酮等极性溶剂。
其中步骤(1)所述的纳米线/聚膦腈复合材料的制备过程中：纳米线、六氯环三膦腈和4,4’-二羟基二苯砜的质量比为0.1-1：1：1-3，纳米线的浓度为0.5-5g/L，三乙胺的浓度为0.05～0.1g/L。
其中步骤(2)所述的纳米线/聚膦腈/金属或金属氧化物纳米粒子夹心复合材料的制备过程中生成金属纳米颗粒的反应条件通常为：溶剂为水、温度为25-200℃，气氛可以是氮气、氩气等，金属盐为对应金属的硫酸盐、盐酸盐、磷酸盐、醋酸盐等，还原剂为NaBH4、柠檬酸钠等。纳米线/聚膦腈复合材料的浓度为0.5-5g/L，金属盐的浓度为0.05-0.5g/L。
其中步骤(2)所述的纳米线/聚膦腈/金属或金属氧化物纳米粒子夹心复合材料的制备过程中生成金属氧化物纳米颗粒的反应条件通常为：溶剂为水、温度为25-200℃，气氛可以是氮气、氩气等，金属盐为对应金属的硫酸盐、盐酸盐、磷酸盐、醋酸盐等。纳米线/聚膦腈复合材料的浓度为0.5-5g/L，金属盐的浓度为0.05-0.5g/L。
其中所述的聚合物为聚(环三膦腈-co-4,4’-二羟基二苯砜)。
其中所述的纳米颗粒可以是金属纳米颗粒，如Au，Ag，Pt，Si，Fe，Co，Ni，Zn等纳米颗粒，也可以是金属氧化物纳米颗粒，如ZnO，Fe3O4，SiO2，TiO2等金属氧化物纳米颗粒。
本发明与现有技术相比具有以下显著优点：
(1)利用聚膦腈的结构特点和合成特性，在纳米线表面原位生成聚膦腈，继而在聚膦腈表面原位生成纳米粒子，得到纳米线/聚合物/纳米颗粒夹心复合材料，聚合过程简单，工艺条件温和。
(2)得到的纳米线/聚合物/纳米颗粒夹心复合材料结构可控、功能可控。
(3)工艺简单、设备要求低，成本低廉，易于实现规模化生产。
(4)应用本发明合成出的纳米线/聚合物/纳米颗粒夹心复合材料具有多重功能，涉及光、电、磁、催化等多领域，应用范围广，具有良好的应用前景和经济效益。
附图说明：
图1是实施例1所得的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的傅里叶变换红外光谱图；
图2是实施例1所得的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的热重图；
图3是实施例1所得的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的透射电镜照片；
图4是本发明纳米线/聚合物/纳米颗粒夹心复合材料的制备路径图。
具体实施方式
实施例1Ag纳米线/PZS/ZnO纳米粒子的制备
在100ml圆底烧瓶中加入0.05g银纳米线，0.01g六氯环三膦腈和0.025g4,4’-二羟基二苯酚，随后倒入50ml无水四氢呋喃和50ml无水乙醇混合溶剂。超声分散加入5ml三乙胺，该溶液在室温下超声反应10h(50w)，然后将溶液以8000r/min的转速离心。分别用去离子水和四氢呋喃洗，放入真空干燥箱50℃，干燥24h，得到Ag纳米线/PZS复合材料。
在三口瓶中加入0.05g Ag/PZS,超声后加入0.5g醋酸锌，125ml一缩二乙二醇、5ml水组成的溶液，超声半小时后置于175℃油浴中磁力搅拌1.5h。静置一段时间后将反应液离心，沉淀物用去离子水和95％乙醇各洗3次，然后在50℃下真空干燥24h，即得Ag纳米线/PZS/ZnO纳米粒子夹心复合材料。合成得到的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料可用于光电催化领域。
图1是实施例1所得的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的傅里叶变换红外光谱图。(a)图为Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的IR图，(b)图为Ag纳米线/PZS的IR图，(c)图为纯PZS的IR图。(a)图中1596cm-1和1500cm-1谱带是苯环中碳碳双键的共振吸收，1200cm-1和1300cm-1谱带是砜基的共振吸收，1200cm-1谱带是P＝N键的共振吸收，940cm-1谱带是P－O－Ar键的共振吸收。波谱分析表明其结构为聚膦腈的结构。银和氧化锌为无机物，在红外中的特征吸收峰很弱，被聚膦腈的特征吸收峰所掩盖。但是通过(a)、(b)、(c)图对比可知，Ag纳米线/PZS/ZnO纳米粒子夹心复合材料具备所有聚膦腈的特征吸收峰，Ag/PZS/ZnO相对Ag/PZS而言，Ag/PZS相对于PZS而言，部分特征吸收峰发生了不同程度地蓝移，说明Ag、ZnO与聚合物之间存在一定的相互作用，Ag、ZnO对聚合物有一定影响。
图2是实施例1所得的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的热重图。
图3是实施例1所得的Ag纳米线/PZS/ZnO纳米粒子夹心复合材料的透射电镜照片。里层(黑色衬底的纳米线)为Ag纳米线，中间层纳米线表面(灰色部分)为包覆的PZS聚合物，最外层黑色衬底的纳米粒子为ZnO纳米粒子。
图4是本发明纳米线/聚合物/纳米颗粒夹心复合材料的制备路径图。
实施例2
Cu纳米线/PZS/Ag纳米粒子的制备
在100ml圆底烧瓶中加入0.01g铜纳米线，0.1g六氯环三膦腈和0.1g4,4’-二羟基二苯酚，随后倒入10ml无水四氢呋喃和10ml无水乙醇混合溶剂。超声分散加入1ml三乙胺，该溶液在室温下超声反应10h(50w)，然后将溶液以8000r/min的转速离心。分别用去离子水和四氢呋喃洗，放入真空干燥箱50℃，干燥24h，得到Cu纳米线/PZS复合材料。
0.05g Cu纳米线/PZS复合材料,100mlH2O，0.005g AgNO3,室温150w超声30min。25ml50mmol柠檬酸钠和0.01wt％NaBH4逐滴加入。室温反应30min。离心，水洗、乙醇各洗3次，真空干燥24h，得到Cu纳米线/PZS/Ag纳米粒子夹心复合材料。合成得到的Cu纳米线/PZS/Ag纳米粒子夹心复合材料可用于电催化领域。
实施例3
Cu纳米线/PZS/Ag纳米粒子的制备
在100ml圆底烧瓶中加入0.1g铜纳米线，0.1g六氯环三膦腈和0.3g4,4’-二羟基二苯酚，随后倒入10ml无水四氢呋喃和10ml无水乙醇混合溶剂。超声分散加入2ml三乙胺，该溶液在室温下超声反应10h(50w)，然后将溶液以8000r/min的转速离心。分别用去离子水和四氢呋喃洗，放入真空干燥箱50℃，干燥24h，得到Cu纳米线/PZS复合材料。
0.5g Cu纳米线/PZS复合材料,100mlH2O，0.05g AgNO3,室温150w超声30min。25ml50mmol柠檬酸钠和0.01wt％NaBH4逐滴加入。室温反应30min。离心，水洗、乙醇各洗3次，真空干燥24h，得到Cu纳米线/PZS/Ag纳米粒子夹心复合材料。
实施例4
Ag纳米线/PZS/Fe3O4纳米粒子的制备
在100ml圆底烧瓶中加入0.05g银纳米线，0.01g六氯环三膦腈和0.025g4,4’-二羟基二苯酚，随后倒入50ml无水四氢呋喃和50ml无水乙醇混合溶剂。超声分散加入5ml三乙胺，该溶液在室温下超声反应10h(50w)，然后将溶液以8000r/min的转速离心。分别用去离子水和四氢呋喃洗，放入真空干燥箱50℃，干燥24h，得到Ag纳米线/PZS复合材料。
在三口瓶中加入0.0500g Ag/PZS，0.15g无水FeCl3，0.15g FeSO4·7H2O，50ml去离子水，在150W下超声分散，通氮气。滴加15ml KOH 0.02g/mL水溶液，滴加完毕后再超声反应3h。静置一段时间后将反应液离心，沉淀物用去离子水和95％乙醇各洗3次，然后在50℃下真空干燥24h，得到Ag纳米线/PZS/Fe3O4纳米粒子夹心复合材料。
实施例5
Fe纳米线/PZS/Ag纳米粒子的制备
在100ml圆底烧瓶中加入0.05g铁纳米线，0.01g六氯环三膦腈和0.025g4,4’-二羟基二苯酚，随后倒入50ml无水四氢呋喃和50ml无水乙醇混合溶剂。超声分散加入5ml三乙胺，该溶液在室温下超声反应10h(50w)，然后将溶液以8000r/min的转速离心。分别用去离子水和四氢呋喃洗，放入真空干燥箱50℃，干燥24h，得到Fe纳米线/PZS复合材料。
0.05g Fe纳米线/PZS复合材料,100mlH2O，0.0034g AgNO3,室温150w超声30min。25ml50mmol柠檬酸钠和0.01％wt％NaBH4逐滴加入。室温反应30min。离心，水洗、乙醇各洗3次，真空干燥24h，得到Cu纳米线/PZS/Ag纳米粒子夹心复合材料。
实施例6
Pt纳米线/PZS/ZnO纳米粒子的制备
在100ml圆底烧瓶中加入0.05gPt纳米线，0.01g六氯环三膦腈和0.025g4,4’-二羟基二苯酚，随后倒入50ml无水四氢呋喃和50ml无水乙醇混合溶剂。超声分散加入5ml三乙胺，该溶液在室温下超声反应10h(50w)，然后将溶液以8000r/min的转速离心。分别用去离子水和四氢呋喃洗，放入真空干燥箱50℃，干燥24h，得到Pt纳米线/PZS复合材料。
在三口瓶中加入0.05g Pt纳米线/PZS,超声后加入0.5g醋酸锌，125ml一缩二乙二醇、5ml水组成的溶液，超声半小时后置于175℃油浴中磁力搅拌1.5h。静置一段时间后将反应液离心，沉淀物用去离子水和95％乙醇各洗3次，然后在50℃下真空干燥24h，即得Pt纳米线/PZS/ZnO纳米粒子夹心复合材料。
Claims (7)
1.一种纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于按以下步骤进行：
（1）称取一定质量的纳米线，将其超声分散在一定量溶剂中，依次加入一定量六氯环三膦腈、4,4’-二羟基二苯砜、三乙胺，在一定反应条件下进行原位聚合；经后处理后，得到纳米线/聚膦腈复合材料；
（2）称取一定质量的纳米线/聚膦腈复合材料，加入溶剂、金属盐、一定反应条件下在聚合物表面原位生成金属或金属氧化物纳米粒子；经后处理后，得到纳米线/聚膦腈/纳米颗粒夹心复合材料。
2.根据权利要求1所述的纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于所述的聚合物为聚（环三膦腈-co-4,4’-二羟基二苯砜）。
3.根据权利要求1所述的纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于其中步骤（1）所述的纳米线可以是金属纳米线，如Au，Ag，Cu，Pt，Si，Fe，Co，Ni，Zn等纳米线，也可以是金属氧化物纳米线，如ZnO，Fe3O4，CuO，SiO2，TiO2等金属氧化物纳米线。
4.根据权利要求1所述的纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于其中步骤（2）所述的纳米颗粒可以是金属纳米颗粒，如Au，Ag，Cu，Pt，Si，Fe，Co，Ni，Zn等纳米颗粒，也可以是金属氧化物纳米颗粒，如ZnO，Fe3O4，CuO，SiO2，TiO2等金属氧化物纳米颗粒。
5.根据权利要求1所述的纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于步骤（1）所述的纳米线/聚膦腈复合材料的制备过程中：超声功率为100～240 W，超声频率为80 kHz，温度为0-80℃，溶剂可以是甲醇、四氢呋喃、乙醇、乙腈、丙酮等极性溶剂；
纳米线、六氯环三膦腈和4,4’-二羟基二苯砜的质量比为0.1-1：1：1-3，纳米线的浓度为0.5-5g/L，三乙胺的浓度为0.05～0.1g/L。
6.根据权利要求1所述的纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于步骤（2）所述的纳米线/聚膦腈/金属或金属氧化物纳米粒子夹心复合材料的制备过程中生成金属纳米颗粒的反应条件通常为：溶剂为水、温度为25-200℃，气氛可以是氮气、氩气等，金属盐为对应金属的硫酸盐、盐酸盐、磷酸盐、醋酸盐等，还原剂为NaBH4、柠檬酸钠等；纳米线/聚膦腈复合材料的浓度为0.5-5 g/L，金属盐的浓度为0.05-0.5 g/L。
7.根据权利要求1所述的纳米线/聚合物/纳米颗粒夹心复合材料的制备方法，其特征在于步骤（2）所述的纳米线/聚膦腈/金属或金属氧化物纳米粒子夹心复合材料的制备过程中生成金属氧化物纳米颗粒的反应条件通常为：溶剂为水、温度为25-200℃，气氛可以是氮气、氩气等，金属盐为对应金属的硫酸盐、盐酸盐、磷酸盐、醋酸盐等；纳米线/聚膦腈复合材料的浓度为0.5-5 g/L，金属盐的浓度为0.05-0.5 g/L。
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