CN114293283B - Composite inorganic nanofiber, preparation method thereof and application thereof in photo-thermal conversion film - Google Patents
Composite inorganic nanofiber, preparation method thereof and application thereof in photo-thermal conversion film Download PDFInfo
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 82
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000001354 calcination Methods 0.000 claims abstract description 27
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 24
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 238000009987 spinning Methods 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 8
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 8
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 229960005069 calcium Drugs 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 239000003021 water soluble solvent Substances 0.000 claims description 3
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 claims description 2
- UNMYWSMUMWPJLR-UHFFFAOYSA-L Calcium iodide Chemical compound [Ca+2].[I-].[I-] UNMYWSMUMWPJLR-UHFFFAOYSA-L 0.000 claims description 2
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims description 2
- 229920001661 Chitosan Polymers 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002125 Sokalan® Polymers 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 2
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims description 2
- 229910001622 calcium bromide Inorganic materials 0.000 claims description 2
- 229940059251 calcium bromide Drugs 0.000 claims description 2
- YALMXYPQBUJUME-UHFFFAOYSA-L calcium chlorate Chemical compound [Ca+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O YALMXYPQBUJUME-UHFFFAOYSA-L 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 229960002713 calcium chloride Drugs 0.000 claims description 2
- WGEFECGEFUFIQW-UHFFFAOYSA-L calcium dibromide Chemical compound [Ca+2].[Br-].[Br-] WGEFECGEFUFIQW-UHFFFAOYSA-L 0.000 claims description 2
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 claims description 2
- 239000004227 calcium gluconate Substances 0.000 claims description 2
- 229960004494 calcium gluconate Drugs 0.000 claims description 2
- 235000013927 calcium gluconate Nutrition 0.000 claims description 2
- 229940046413 calcium iodide Drugs 0.000 claims description 2
- 229910001640 calcium iodide Inorganic materials 0.000 claims description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 2
- 159000000007 calcium salts Chemical group 0.000 claims description 2
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 claims description 2
- JXRVKYBCWUJJBP-UHFFFAOYSA-L calcium;hydrogen sulfate Chemical compound [Ca+2].OS([O-])(=O)=O.OS([O-])(=O)=O JXRVKYBCWUJJBP-UHFFFAOYSA-L 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- 150000007522 mineralic acids Chemical class 0.000 claims description 2
- 235000019691 monocalcium phosphate Nutrition 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229960002446 octanoic acid Drugs 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 239000004584 polyacrylic acid Substances 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 claims description 2
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- YAECNLICDQSIKA-UHFFFAOYSA-L calcium;sulfanide Chemical compound [SH-].[SH-].[Ca+2] YAECNLICDQSIKA-UHFFFAOYSA-L 0.000 claims 1
- 239000001384 succinic acid Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 230000004071 biological effect Effects 0.000 abstract description 2
- 238000002074 melt spinning Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 34
- 239000000463 material Substances 0.000 description 13
- 230000000694 effects Effects 0.000 description 11
- 206010028980 Neoplasm Diseases 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 238000001523 electrospinning Methods 0.000 description 4
- YBYGDBANBWOYIF-UHFFFAOYSA-N erbium(3+);trinitrate Chemical compound [Er+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YBYGDBANBWOYIF-UHFFFAOYSA-N 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052691 Erbium Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- JKWVDBMVHDRRLD-UHFFFAOYSA-N 8-bromo-1,2,3,4-tetrahydroisoquinoline;hydrochloride Chemical compound Cl.C1CNCC2=C1C=CC=C2Br JKWVDBMVHDRRLD-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical group [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 108010037362 Extracellular Matrix Proteins Proteins 0.000 description 1
- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- GZTUDAKVGXUNIM-UHFFFAOYSA-K erbium(3+);tribromide Chemical compound Br[Er](Br)Br GZTUDAKVGXUNIM-UHFFFAOYSA-K 0.000 description 1
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 210000002744 extracellular matrix Anatomy 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 239000002502 liposome Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002078 nanoshell Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 150000004032 porphyrins Chemical class 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000008685 targeting Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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Abstract
The invention discloses a composite inorganic nanofiber, a preparation method thereof and application thereof in a photothermal conversion film, wherein the nanofiber contains SiO 2 CaO and MO x Wherein M is selected from long-period metal elements, x>0. The method adopts polymer to assist in electrostatic spinning and is obtained through calcination, compared with high-temperature melt spinning, the method has low temperature requirement and higher biological activity of the obtained fiber, and the nanofiber prepared by the method has good flexibility and high stability, simultaneously has good photo-thermal conversion capability, is simple in preparation process operation, and is suitable for industrial mass production.
Description
Technical Field
The invention belongs to the technical field of tumor photothermal treatment, and particularly relates to a composite inorganic nanofiber, a preparation method thereof and application thereof in a photothermal conversion film.
Background
Photothermal treatment of tumors is an emerging tumor treatment method. Compared with the traditional treatment mode, the photothermal treatment has higher specificity and accurate space-time selectivity, and has excellent effect in tumor treatment. Photothermal therapy is a treatment method that uses a material with high photothermal conversion efficiency, injects it into the inside of a human body, gathers near tumor tissue using a targeting recognition technique, and converts light energy into heat energy under irradiation of an external light source (typically near infrared light) to kill cancer cells. Therefore, the properties of the photothermal conversion material have an important influence on photothermal treatment.
Currently, the photo-thermal conversion materials in the related art mainly include the following four types: (1) carbon materials such as carbon nanotubes and graphene; (2) gold materials such as gold nanorods and gold nanoshells; (3) copper sulfide semiconductor materials; (4) Organic compounds such as porphyrin liposome and high molecular polymer. However, these conventional photothermal conversion materials have some defects, such as very expensive gold materials and carbon materials, poor biocompatibility, etc., and for example, the preparation conditions of these materials are very severe, which increases the production cost and is not beneficial to mass production, and these defects greatly limit the wide application.
Therefore, the development of the photothermal conversion material with low cost, simple preparation and high in vivo biological safety has important significance.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a composite inorganic nanofiber which can be used for photothermal treatment of tumors and has low production cost.
The invention also provides a preparation method of the composite inorganic nanofiber.
The invention also provides application of the composite inorganic nanofiber.
According to one aspect of the present invention, there is provided a composite inorganic nanofiber comprising SiO 2 CaO and MO x Wherein M is selected from long-period metal elements, x>0。
According to a preferred embodiment of the invention, there is at least the following advantageous effect: the nanofiber containing the components of the scheme of the invention has low manufacturing cost, good flexibility, stability, good photothermal conversion capability and excellent biocompatibility, and can be prepared into a nanofiber membrane for photothermal treatment of tumors; meanwhile, the material is nontoxic and degradable, is environment-friendly and has wide application prospect.
In some embodiments of the invention, the M is selected from a transition metal element or a group VA metal element.
In some preferred embodiments of the invention, the M is selected from rare earth elements.
In some preferred embodiments of the invention, the M is selected from at least one of Er, bi, mn, fe, co, ni or Cu. M may be a transition metal element or other metal element, all of which may have similar properties.
In some embodiments of the invention, x is not less than 1.
In some preferred embodiments of the invention, x is not greater than 2.
In some preferred embodiments of the present invention, the diameter of the nanofiber is between 100 and 2000 nm. The diameter is 100-2000 nm, and the fiber can simulate the structure of extracellular matrix in form and structure, and has good biocompatibility.
In some embodiments of the invention, the SiO in the nanofibers 2 CaO and MO x The molar ratio of (0.01-0.99): (0.01-0.5).
In some preferred embodiments of the invention, the SiO in the nanofibers 2 CaO and MO x The molar ratio of (0.5-0.99): (0.01-0.5).
In some more preferred embodiments of the invention, the SiO in the nanofibers 2 CaO and MO x The molar ratio of (2) is 0.84-0.86:0.1-0.14:0.01-0.05.
According to another aspect of the present invention, there is provided a method for preparing a composite inorganic nanofiber, comprising the steps of:
s1, preparing spinning solution: mixing a solution I containing a silicon source, a calcium source, an M source and a catalyst with a solution II containing a polymer to obtain a spinning solution;
s2, electrostatic spinning: carrying out electrostatic spinning on the spinning solution in the step S1 to obtain a fiber felt;
s3, calcining: drying and calcining the fiber felt obtained in the step S2 to obtain the nanofiber;
wherein M is selected from long-period metal elements.
The preparation method according to a preferred embodiment of the present invention has at least the following advantageous effects: the method adopts polymer to assist in electrostatic spinning and is obtained through calcination, compared with high-temperature melt spinning, the method has low temperature requirement and higher biological activity of the obtained fiber, and the nanofiber prepared by the method has good flexibility and high stability, simultaneously has good photo-thermal conversion capability, is simple in preparation process operation, and is suitable for industrial mass production.
In some preferred embodiments of the present invention, the catalyst is selected from at least one of an organic acid or an inorganic acid.
In some more preferred embodiments of the present invention, the catalyst is selected from at least one of formic acid, acetic acid, hydrochloric acid, nitric acid, phosphoric acid, polyphosphoric acid, oxalic acid, propionic acid, butyric acid, caprylic acid, adipic acid, oxalic acid, malonic acid, succinic acid, or maleic acid.
In some embodiments of the invention, the silicon source is a silicon dioxide precursor.
In some preferred embodiments of the invention, the silicon source is selected from silicate esters; more preferably, the silicon source is selected from at least one of ethyl orthosilicate, propyl orthosilicate, tetrabutyl orthosilicate, and ethyl polysilicate.
In some embodiments of the invention, the calcium source is selected from calcium salts.
In some preferred embodiments of the present invention, the calcium source is selected from at least one of calcium dihydrogen phosphate, calcium chloride, calcium bromide, calcium iodide, calcium gluconate, calcium nitrate, calcium bicarbonate, calcium bisulfate, calcium hypochlorite, or calcium chlorate.
In some embodiments of the invention, the M is selected from a transition metal element or a group VA metal element.
In some preferred embodiments of the invention, the M is selected from rare earth elements.
In some preferred embodiments of the invention, the M is selected from at least one of Er, bi or Cu.
In some embodiments of the invention, the M source is selected from erbium salts.
In some preferred embodiments of the invention, the M source is selected from at least one of erbium chloride, erbium nitrate, erbium bromide.
In some embodiments of the invention, the solvent of solution I or solution II is each independently water and/or a water-soluble solvent.
In some embodiments of the invention, the solvent is selected from at least one of water, methanol, ethanol, propanol, ethylene glycol, propylene glycol, ethylene glycol monomethyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, isopropanol, t-butanol, dimethylformamide (DMF), dimethylacetamide, tetrahydrofuran (THF), methylamine, acetic acid, dioxane, acetone, pyridine, or Dimethylsulfoxide (DMSO).
In some embodiments of the invention, the polymer is selected from at least one of chitosan, polyvinyl alcohol, polyvinyl butyral, polyacrylic acid, gelatin, polyethylene oxide, polyvinylpyrrolidone, polyethylene oxide, or polyacrylonitrile.
In some embodiments of the present invention, the mass percentage concentration of the polymer in the solution II is 1% -50%.
In some embodiments of the present invention, the volume ratio of the solution I to the solution II is (0.1-10): 1.
In some preferred embodiments of the invention, the volume ratio of solution I to solution II is about 2:1.
In some embodiments of the present invention, the electrospinning in step S2 is performed by an electrospinning machine comprising the following parameters: the distance of the left and right movement of the sliding table is adjusted to be 5-40 cm; the advancing speed of the electrostatic spinning is 0.1-10 mL/h; the rotation speed of the roller is 50-1000 r/min; the spinning voltage is 5-50 kV, the ambient temperature is 10-40 ℃, and the relative humidity is 10-90%.
In some preferred embodiments of the present invention, the electrospinning in step S2 is performed by an electrospinning machine comprising the following parameters: the distance of the left and right movement of the adjusting sliding table is about 10cm; the advancing speed of electrostatic spinning is 1-2 mL/h; the rotation speed of the roller is 50-80 r/min. The nano fiber prepared by the invention is prepared into an inorganic solution by adopting a sol-gel method, the polymer is used for assisting in electrostatic spinning, and finally the nano fiber is prepared by calcining, and the shape and the size of the fiber can be effectively controlled by controlling the parameters of the spinning solution, the spinning parameters and the calcining parameters.
In some embodiments of the present invention, the temperature of the drying process is 20 to 200 ℃.
In some preferred embodiments of the present invention, the temperature of the drying treatment is 50 to 100 ℃.
In some embodiments of the present invention, the drying time is 2 to 24 hours.
In some preferred embodiments of the present invention, the drying time is 5-10 hours.
In some embodiments of the present invention, the temperature of the calcination treatment is 500 to 1400 ℃.
In some preferred embodiments of the present invention, the temperature of the calcination treatment is 600 to 1000 ℃.
In some embodiments of the invention, the calcination treatment is for 2 to 24 hours.
In some preferred embodiments of the present invention, the calcination treatment is performed for a period of 2 to 8 hours.
In some embodiments of the invention, the calcination is performed at a temperature increase schedule of 1 to 20 ℃/min.
In some preferred embodiments of the invention, the calcination is programmed to heat up at a rate of 10 ℃/min. The nanofiber with better flexibility and stability can be obtained by regulating and controlling the calcination process.
In some embodiments of the invention, the calcination is under an air atmosphere.
According to a further aspect of the present invention, there is provided the use of the above-described nanofibers in the preparation of a photothermal conversion film.
The use according to a preferred embodiment of the invention has at least the following advantages: the scheme of the invention has good photo-thermal effect, so that the invention has good application prospect in the field of photo-thermal conversion, especially in the photo-thermal treatment of tumors.
A photothermal conversion film comprising the above nanofiber.
A tumor photothermal therapeutic agent comprising the above nanofiber.
Drawings
The invention is further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is an SEM image of nanofibers produced in example 1 of the present invention;
FIG. 2 is a physical diagram of nanofibers prepared in example 4 of the present invention;
FIG. 3 is a graph showing the flexibility test effect of the nanofibers prepared in example 1 of the present invention;
FIG. 4 is a thermal image of the temperature change of the nanofibers produced in example 1 of the present invention after irradiation with different light intensities;
FIG. 5 is a graph showing the temperature rise-power relationship of nanofibers produced in example 3 and comparative example 1 of the present invention;
FIG. 6 is a graph showing the results of stability test of nanofibers produced in example 3 of the present invention.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention. The test methods used in the examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
In the description of the present invention, the meaning of a number is one or more, the meaning of a number is two or more, and greater than, less than, exceeding, etc. are understood to exclude the present number, and the meaning of a number is understood to include the present number. The description I, II if provided is for the purpose of distinguishing between technical features and should not be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
In the description of the present invention, the descriptions of the terms "one embodiment," "some embodiments," "illustrative embodiments," "examples," "specific examples," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
In the description of the present invention, the meaning of "about" refers to plus or minus 2%, unless otherwise specified.
Example 1
This example prepared a SiO 2 -CaO-Er 2 O 3 The flexible nanofiber comprises the following specific processes:
1) Preparing a spinning solution: weighing 0.354g of calcium nitrate and 0.088g of erbium (III) nitrate pentahydrate, dissolving in 1.26g of ethyl silicate (the silicon dioxide content is 40%, the mass of silicon dioxide is 1.26g of 0.4/60=0.0084 mol), forming a solution I in a mixed solution of 0.1g of acetic acid, 0.3g of distilled water and 2g of absolute ethyl alcohol, weighing 5g of B-72 polyvinyl butyral, dissolving in 45g of absolute ethyl alcohol solution, and stirring for 2.5 days (all 2-3 days can be carried out) to form a transparent solution II; then the volume ratio of the solution II to the solution I is 2:1, mixing, stirring for 1h to uniformly mix, and driving out bubbles in the solution by means of ultrasound to obtain spinning solution;
2) And (3) electrostatic spinning: loading the prepared spinning solution into an electrostatic spinning device, wherein the propelling speed is 1mL/h, the rotating speed of a roller is 50r/min, the spinning voltage is 15kV, the ambient temperature is 20-25 ℃, the relative humidity is 15-25%, electrostatic spinning is carried out by regulating and controlling the distance between a sliding table and the sliding table to be 7cm, and the SiO after spinning is obtained 2 -CaO-Er 2 O 3 PVB fiber mat;
3) And (3) calcining: siO is made of 2 -CaO-Er 2 O 3 Drying PVB fiber felt in vacuum drying oven at 80deg.C for 6 hr, heating to 800deg.C at 10deg.C/min under air atmosphere, calcining for 2 hr, naturally cooling to room temperature, and taking out to obtain SiO 2 CaO and Er 2 O 3 The molar ratio of 0.84:0.15:0.01.
Example 2
This example prepared a SiO 2 -CaO-Er 2 O 3 The flexible nanofiber comprises the following specific processes:
1) Preparing a spinning solution: weighing 0.59g of calcium nitrate and 0.44g of erbium (III) nitrate pentahydrate, dissolving in 1.05g of ethyl silicate (the silicon dioxide content is 40%, the mass of silicon dioxide is 1.05g of 0.4/60=0.007 mol), forming a solution I in a mixed solution of 0.1g of acetic acid, 0.3g of distilled water and 2g of absolute ethyl alcohol, weighing 5g of B-72 polyvinyl butyral, dissolving in 45g of absolute ethyl alcohol solution, and stirring for 2-3 days to form a transparent solution II; then the volume ratio of the solution II to the solution I is 2:1, mixing, stirring for 1h to uniformly mix, and driving out bubbles in the solution by means of ultrasound to obtain spinning solution;
2) And (3) electrostatic spinning: loading the prepared spinning solution into an electrostatic spinning device, wherein the propelling speed is 1mL/h, the rotating speed of a roller is 50r/min, the spinning voltage is 15kV, the ambient temperature is 20-25 ℃, the relative humidity is 15-25%, electrostatic spinning is carried out by regulating and controlling the distance between a sliding table and the sliding table to be 10cm, and the SiO after spinning is obtained 2 -CaO-Er 2 O 3 PVB fiber mat;
3) And (3) calcining: siO is made of 2 -CaO-Er 2 O 3 Drying PVB fiber felt in vacuum drying oven at 80deg.C for 6 hr, and taking off under air atmosphereHeating to 800 ℃ at a speed of 10 ℃/min, calcining for 2 hours at the temperature, naturally cooling to room temperature, and taking out to obtain SiO 2 CaO and Er 2 O 3 Is 0.70:0.25:0.05 by mole ratio
Example 3
This example prepared a SiO 2 -CaO-Er 2 O 3 A flexible nanofiber which differs from example 1 in that: siO (SiO) 2 CaO and Er 2 O 3 The molar ratio of the spinning solution to the spinning solution is 0.80:0.15:0.05, the propelling speed is 2mL/h, the rotating speed of the roller is 100r/min, the electrostatic spinning is carried out by regulating the distance of a sliding table to be 10cm, the spinning voltage is 20kV, the ambient temperature is 25-30 ℃, and the relative humidity is 30-40%.
Example 4
This example prepared a SiO 2 -CaO-Bi 2 O 3 A flexible nanofiber which differs from example 1 in that: bismuth nitrate is used to replace erbium nitrate in the same amount.
Example 5
This example prepared a SiO 2 CaO-CuO flexible nanofibers, which differ from example 1 in that: copper nitrate is substituted for erbium nitrate in equal amounts.
Example 6
This example prepared a SiO 2 CaO-CuO flexible nanofibers, which differ from example 1 in that: the erbium nitrate is replaced by ferric nitrate in the same amount.
Comparative example 1
This example prepared a SiO 2 CaO nanofibers, which differ from example 1 in that: no erbium source or calcium source is added.
Test examples
This test example tests the properties and performance of nanofibers produced in the above examples and comparative examples. Wherein:
the microstructure of the nanofiber prepared in example 1 was observed by Scanning Electron Microscopy (SEM), and the result is shown in fig. 1. The nanofibers produced in examples 2-6 also had similar microstructures, redundancy was not avoided, and are not shown one by one.
A physical diagram of the nanofiber prepared in example 4 is shown in FIG. 2.
The nanofibers produced in example 1 were tested for flexibility and the results are shown in fig. 3. As can be seen from fig. 3, the nanofiber prepared by the embodiment of the invention has good flexibility. The nanofibers produced in examples 2-6 also have similar flexibility, redundancy is not avoided, and are not shown one by one.
The thermal imaging effect of temperature change after irradiation with different light intensities was tested for the nanofibers prepared in examples 1 to 6, wherein the imaging effect of the nanofibers prepared in example 1 is shown in fig. 4. As can be seen from fig. 4, the heating capacity of the fiber gradually increases with increasing light intensity. Other effects are similar, redundancy is not avoided, not shown here one by one.
The nanofibers prepared in examples 1 to 6 and comparative example 1 were tested for their photothermal heating effect after irradiation with laser light of different powers, and the heating curves of the nanofibers prepared in example 3 and comparative example 1 are shown in fig. 5. As can be seen from fig. 5, the heating capacity of the fiber prepared in example 3 was significantly improved over that of the fiber in comparative example as the laser power and light intensity were increased.
Stability tests were performed on the nanofibers produced in examples 1 to 6. By 2W/cm 2 The nanofiber prepared in example 3 was irradiated with the power of (3), and the effect of temperature rise in three cycles was shown in FIG. 6. From the graph, the temperature rising performance of the nanofiber is hardly changed, so that the nanofiber prepared by the embodiment of the invention has good stability.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of one of ordinary skill in the art without departing from the spirit of the present invention. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.
Claims (23)
1. A preparation method of a composite inorganic nanofiber is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing spinning solution: mixing a solution I containing a silicon source, a calcium source, an M source and a catalyst with a solution II containing a polymer to obtain a spinning solution;
s2, electrostatic spinning: carrying out electrostatic spinning on the spinning solution in the step S1 to obtain a fiber felt;
s3, calcining: drying and calcining the fiber felt obtained in the step S2 to obtain the nanofiber;
wherein the composite inorganic nanofiber contains SiO 2 CaO and MO x The MO is provided with x Is Er 2 O 3 、Bi 2 O 3 Or CuO, wherein the diameter of the nanofiber is 100-2000 nm, the polymer is at least one selected from chitosan, polyvinyl alcohol, polyvinyl butyral, polyacrylic acid, gelatin, polyethylene oxide, polyvinylpyrrolidone, polyethylene oxide or polyacrylonitrile, and the solvent of the solution I or the solution II is water and/or a water-soluble solvent respectively and independently; siO in the nanofiber 2 CaO and MO x The molar ratio of (0.5-0.99): (0.01-0.5); the mass percentage concentration of the polymer in the solution II is 1% -50%; the volume ratio of the solution I to the solution II is (0.1-10): 1; the temperature of the calcination treatment is 500-1400 ℃, and the temperature-raising program of the calcination is to raise the temperature at a speed of 1-20 ℃/min.
2. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the catalyst is selected from at least one of an organic acid or an inorganic acid.
3. The method for preparing the composite inorganic nanofiber according to claim 2, wherein: the catalyst is at least one selected from formic acid, acetic acid, hydrochloric acid, nitric acid, phosphoric acid, polyphosphoric acid, oxalic acid, propionic acid, butyric acid, caprylic acid, adipic acid, oxalic acid, malonic acid, succinic acid or maleic acid.
4. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the silicon source is selected from silicate esters.
5. The method for preparing the composite inorganic nanofiber according to claim 4, wherein: the silicon source is at least one selected from the group consisting of ethyl orthosilicate, propyl orthosilicate, tetrabutyl orthosilicate and ethyl polysilicate.
6. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the calcium source is selected from calcium salts.
7. The method for preparing the composite inorganic nanofiber according to claim 6, wherein: the calcium source is at least one selected from calcium dihydrogen phosphate, calcium chloride, calcium bromide, calcium iodide, calcium gluconate, calcium nitrate, calcium bicarbonate, calcium bisulfate, calcium bisulfide, calcium hypochlorite or calcium chlorate.
8. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the water-soluble solvent is at least one selected from methanol, ethanol, propanol, ethylene glycol, propylene glycol, ethylene glycol monomethyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, isopropanol, tertiary butanol, dimethylformamide, dimethylacetamide, tetrahydrofuran, methylamine, acetic acid, dioxane, acetone, pyridine or dimethyl sulfoxide.
9. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the volume ratio of the solution I to the solution II is 2:1.
10. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the electrostatic spinning in the step S2 is completed through an electrostatic spinning machine, and the electrostatic spinning machine comprises the following parameters: the distance of the left and right movement of the sliding table is adjusted to be 5-40 cm; the advancing speed of the electrostatic spinning is 0.1-10 mL/h; the rotation speed of the roller is 50-1000 r/min; the spinning voltage is 5-50 kV, the ambient temperature is 10-40 ℃, and the relative humidity is 10-90%.
11. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the electrostatic spinning in the step S2 is completed through an electrostatic spinning machine, and the electrostatic spinning machine comprises the following parameters: the distance of the left and right movement of the sliding table is adjusted to be 10cm; the advancing speed of electrostatic spinning is 1-2 mL/h; the rotation speed of the roller is 50-80 r/min.
12. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the temperature of the drying treatment is 20-200 ℃.
13. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the temperature of the drying treatment is 50-100 ℃.
14. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the drying treatment time is 2-24 hours.
15. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the drying treatment time is 5-10 h.
16. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the temperature of the calcination treatment is 600-1000 ℃.
17. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the calcination treatment time is 2-24 hours.
18. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the calcination treatment time is 2-8 hours.
19. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the temperature-rising program of the calcination is to rise at a speed of 10 ℃/min.
20. The method for preparing the composite inorganic nanofiber according to claim 1, wherein: the calcination is under an air atmosphere.
21. A composite inorganic nanofiber produced by the production method according to claim 1.
22. Use of a nanofiber according to claim 21 or a nanofiber obtainable by the method according to any one of claims 1 to 20 in the preparation of a photothermal conversion film.
23. A photothermal conversion film, characterized in that: a nanofiber comprising the nanofiber of claim 21 or made by the method of any one of claims 1 to 20.
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