CN116002631B - Iridium diselenide photo-thermal conversion nano material and preparation method and application thereof - Google Patents
Iridium diselenide photo-thermal conversion nano material and preparation method and application thereof Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 86
- UUVABROKEMJIHC-UHFFFAOYSA-N bis(selanylidene)iridium Chemical compound [Ir](=[Se])=[Se] UUVABROKEMJIHC-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 150000002503 iridium Chemical class 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 206010028980 Neoplasm Diseases 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003860 storage Methods 0.000 claims abstract description 7
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 39
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 22
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 22
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052741 iridium Inorganic materials 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 19
- 239000011669 selenium Substances 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 16
- 150000003342 selenium Chemical class 0.000 claims description 15
- 235000001014 amino acid Nutrition 0.000 claims description 14
- 150000001413 amino acids Chemical group 0.000 claims description 14
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 14
- 229910052711 selenium Inorganic materials 0.000 claims description 13
- 235000009518 sodium iodide Nutrition 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- -1 tetradodecairidium Chemical compound 0.000 claims description 9
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims description 5
- 239000004471 Glycine Substances 0.000 claims description 4
- 239000003504 photosensitizing agent Substances 0.000 claims description 4
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 3
- FDKWRPBBCBCIGA-UWTATZPHSA-N D-Selenocysteine Natural products [Se]C[C@@H](N)C(O)=O FDKWRPBBCBCIGA-UWTATZPHSA-N 0.000 claims description 3
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 claims description 3
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims description 3
- FFEARJCKVFRZRR-BYPYZUCNSA-N L-methionine Chemical compound CSCC[C@H](N)C(O)=O FFEARJCKVFRZRR-BYPYZUCNSA-N 0.000 claims description 3
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 claims description 3
- 235000004279 alanine Nutrition 0.000 claims description 3
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 125000004989 dicarbonyl group Chemical group 0.000 claims description 3
- HLYTZTFNIRBLNA-LNTINUHCSA-K iridium(3+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ir+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O HLYTZTFNIRBLNA-LNTINUHCSA-K 0.000 claims description 3
- QTRRAHGRSMFAKW-UHFFFAOYSA-N iridium(3+);1-phenylpyrazole Chemical compound [Ir+3].C1=CC=NN1C1=CC=CC=[C-]1.C1=CC=NN1C1=CC=CC=[C-]1.C1=CC=NN1C1=CC=CC=[C-]1 QTRRAHGRSMFAKW-UHFFFAOYSA-N 0.000 claims description 3
- KZLHPYLCKHJIMM-UHFFFAOYSA-K iridium(3+);triacetate Chemical compound [Ir+3].CC([O-])=O.CC([O-])=O.CC([O-])=O KZLHPYLCKHJIMM-UHFFFAOYSA-K 0.000 claims description 3
- HTFVQFACYFEXPR-UHFFFAOYSA-K iridium(3+);tribromide Chemical compound Br[Ir](Br)Br HTFVQFACYFEXPR-UHFFFAOYSA-K 0.000 claims description 3
- SAKXIULONBGRQW-UHFFFAOYSA-K iridium(3+);tribromide;tetrahydrate Chemical compound O.O.O.O.[Br-].[Br-].[Br-].[Ir+3] SAKXIULONBGRQW-UHFFFAOYSA-K 0.000 claims description 3
- YOLNUNVVUJULQZ-UHFFFAOYSA-J iridium;tetrachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Ir] YOLNUNVVUJULQZ-UHFFFAOYSA-J 0.000 claims description 3
- 229930182817 methionine Natural products 0.000 claims description 3
- ZKZBPNGNEQAJSX-UHFFFAOYSA-N selenocysteine Natural products [SeH]CC(N)C(O)=O ZKZBPNGNEQAJSX-UHFFFAOYSA-N 0.000 claims description 3
- 235000016491 selenocysteine Nutrition 0.000 claims description 3
- 229940055619 selenocysteine Drugs 0.000 claims description 3
- VIFHRXBEKXWJKK-UHFFFAOYSA-M sodium;chloride;hexahydrate Chemical compound O.O.O.O.O.O.[Na+].[Cl-] VIFHRXBEKXWJKK-UHFFFAOYSA-M 0.000 claims description 3
- KVDBPOWBLLYZRG-UHFFFAOYSA-J tetrachloroiridium;hydrate Chemical compound O.Cl[Ir](Cl)(Cl)Cl KVDBPOWBLLYZRG-UHFFFAOYSA-J 0.000 claims description 3
- ZRPRRAOCEABMND-UHFFFAOYSA-K trichloroiridium;hydrate;hydrochloride Chemical compound O.Cl.Cl[Ir](Cl)Cl ZRPRRAOCEABMND-UHFFFAOYSA-K 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 125000001554 selenocysteine group Chemical group [H][Se]C([H])([H])C(N([H])[H])C(=O)O* 0.000 claims description 2
- YXZUPOYXZBSGDA-UHFFFAOYSA-H O.Cl[Ir](Cl)(Cl)(Cl)(Cl)Cl.[Na] Chemical compound O.Cl[Ir](Cl)(Cl)(Cl)(Cl)Cl.[Na] YXZUPOYXZBSGDA-UHFFFAOYSA-H 0.000 claims 1
- AHNSTIUMACVREU-UHFFFAOYSA-H [K].Cl[Ir](Cl)(Cl)(Cl)(Cl)Cl Chemical compound [K].Cl[Ir](Cl)(Cl)(Cl)(Cl)Cl AHNSTIUMACVREU-UHFFFAOYSA-H 0.000 claims 1
- HKCXJCNVAGHILG-UHFFFAOYSA-N [N+](=O)([O-])[Ir]([N+](=O)[O-])([N+](=O)[O-])([N+](=O)[O-])([N+](=O)[O-])[N+](=O)[O-].[Na] Chemical compound [N+](=O)([O-])[Ir]([N+](=O)[O-])([N+](=O)[O-])([N+](=O)[O-])([N+](=O)[O-])[N+](=O)[O-].[Na] HKCXJCNVAGHILG-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 12
- 238000001308 synthesis method Methods 0.000 abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 7
- 238000004729 solvothermal method Methods 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 238000007669 thermal treatment Methods 0.000 abstract description 5
- 231100000956 nontoxicity Toxicity 0.000 abstract description 4
- 150000003346 selenoethers Chemical class 0.000 abstract description 4
- 125000003748 selenium group Chemical class *[Se]* 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 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 4
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- DKZXLKGTIOYQTI-UHFFFAOYSA-N [Ir]=[Se] Chemical compound [Ir]=[Se] DKZXLKGTIOYQTI-UHFFFAOYSA-N 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 201000011510 cancer Diseases 0.000 description 2
- 238000002591 computed tomography Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- MJRFDVWKTFJAPF-UHFFFAOYSA-K trichloroiridium;hydrate Chemical compound O.Cl[Ir](Cl)Cl MJRFDVWKTFJAPF-UHFFFAOYSA-K 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- FDKWRPBBCBCIGA-REOHCLBHSA-N (2r)-2-azaniumyl-3-$l^{1}-selanylpropanoate Chemical compound [Se]C[C@H](N)C(O)=O FDKWRPBBCBCIGA-REOHCLBHSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000013056 hazardous product Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910000457 iridium oxide Inorganic materials 0.000 description 1
- MILUBEOXRNEUHS-UHFFFAOYSA-N iridium(3+) Chemical class [Ir+3] MILUBEOXRNEUHS-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical group O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
Abstract
The invention provides an iridium diselenide photo-thermal conversion nano material and a preparation method and application thereof. Adding a surface modifier, a reducing agent and an alcohol solvent into selenium salt and iridium salt in a preset molar ratio, and uniformly mixing to obtain a reaction solution; and transferring the reaction solution into a hydrothermal reaction kettle, and obtaining the iridium diselenide photothermal conversion nano material through hydrothermal reaction. The solvothermal synthesis method used by the invention has the advantages of simple operation, mild experimental conditions, no toxicity of the used chemical reagent, lower cost, stable product morphology, high purity and high repeatability, and is an efficient and controllable synthesis method. The iridium diselenide nano material synthesized by the method has uniform morphology, better absorption in a near infrared region, better dispersibility in water, and great potential in storage devices such as photovoltaic and thermoelectric devices, and in applications such as photo-thermal treatment of cancers. Furthermore, the synthesis method is widely applicable to the preparation of other metal selenides.
Description
Technical Field
The invention relates to the technical field of nanomaterials and photothermal materials, in particular to an iridium diselenide photothermal conversion nanomaterial as well as a preparation method and application thereof.
Background
Iridium, a transition metal element of high atomic number, has unique optical and physical properties, and higher density and X-ray attenuation coefficient. Studies have shown that iridium and its oxide nanomaterials have great potential in multi-modality imaging applications such as tumor therapy-related electronic Computer Tomography (CT), photo Acoustic (PA), and the like. In recent years, various iridium (III) complexes have been shown to have a good therapeutic effect in novel therapies such as Photodynamic (PDT), chemo-dynamic (CDT) and iron death of cancer, and have various advantages such as high stability, long excited state lifetime as photosensitizers. Meanwhile, in the field of photocatalysis, iridium and iridium oxide prove to be oxygen evolution reaction catalysts with high activity in a wide pH range.
However, there are few reports on iridium diselenide, among the only few published iridium diselenide-related documents: zheng Tingting et al, in the document INTERCALATED IRIDIUM DISELENIDE ELECTROCATALYSTS FOR EFFICIENT PH-Universal WATER SPLITTING, mixed Ir and Se powders, heated in a quartz tube at high temperature (1000 ℃ C.) for 30 hours, and then subjected to a lithium intercalation process to synthesize Li-IrSe 2. The synthesis method has the advantages of high reaction temperature, long reaction period and complex process. The literature Ternary Dumbbell Nanowires for Photocatalytic Hydrogen Production discloses a solvothermal method, which is used for successfully preparing IrSe 2 by taking diethyl triamine (DETA) as a solvent, irCl 3 as an Ir source and Se powder as a Se source. However, the solvent DETA is a corrosive hazardous material. So far, in only a few iridium diselenide related documents, the material is applied to the fields of photocatalysis and electrocatalysis, the synthesis method has complex steps and high reaction temperature, and the obtained material has non-uniform morphology and larger size and is not suitable for biological application.
Accordingly, there is a need in the art for improvement.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention aims to provide an iridium diselenide photo-thermal conversion nano material and a preparation method and application thereof, and aims to solve the problems that the iridium diselenide synthesis method in the prior art is complex in steps, high in reaction temperature, uneven in appearance and large in size, and is not suitable for biological application.
The technical scheme of the invention is as follows:
the preparation method of the iridium diselenide photothermal conversion nano material comprises the following steps:
taking selenium salt and iridium salt according to a preset molar ratio of selenium to iridium, and dispersing the selenium salt and the iridium salt in water by ultrasonic to obtain a mixed solution I;
Adding a surface modifier and a reducing agent into the first mixed solution to obtain a second mixed solution;
adding an alcohol solvent into the mixed solution II to obtain a reaction solution;
Reacting the reaction solution at a predetermined reaction temperature for a predetermined time;
after the reaction is finished, the iridium diselenide photothermal conversion nano material is obtained through purification treatment.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the step of preparing the iridium diselenide photothermal conversion nano material, wherein the molar ratio of selenium to iridium is 1:0.01-100.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the following steps of preparing a selenium salt, wherein the selenium salt is selenocyamine dihydrochloride; the iridium salt is selected from one or more of iridium chloride, iridium acetylacetonate, ammonium chloride, sodium chloride hexahydrate, iridium tetrachloride hydrate, iridium trichloride hydrate, iridium chloride hydrate, iridium dicarbonyl acetylacetonate, iridium acetate, iridium bromide, tetradodecairidium, tris (phenylpyrazole) iridium, iridium bromide tetrahydrate, iridium chloride hydrochloride hydrate, sodium hexanitroiridate, potassium hexachloroiridate, sodium hexachloroiridate hydrate and potassium pentachloronitrosyliridium.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the following steps of preparing a surface modifier by using polyvinylpyrrolidone and sodium iodide; the reducing agent is an amino acid.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the steps of (1) (0.1-100) and (0.1-100) of polyvinylpyrrolidone, sodium iodide and amino acid.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the steps of preparing a nano material, wherein the average molecular weight of polyvinylpyrrolidone is 1000-1300000; the amino acid is selected from one or more of glycine, alanine, proline and methionine.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the step of preparing the iridium diselenide photothermal conversion nano material by using an alcohol solvent.
The preparation method of the iridium diselenide photothermal conversion nano material comprises the steps of setting the preset reaction temperature to be 130-230 ℃ and setting the preset time to be 1-30h.
An iridium diselenide photothermal conversion nano material, wherein, the iridium diselenide photothermal conversion nano material is prepared by adopting any one of the preparation methods.
The iridium diselenide photothermal conversion nano material prepared by the preparation method is applied to photovoltaic and thermoelectric storage devices or to preparation of photosensitizers for photothermal treatment of tumors.
The beneficial effects are that: the invention provides an iridium diselenide photo-thermal conversion nano material and a preparation method and application thereof. According to the invention, a certain mass of surface modifier, reducer and alcohol solvent are added into selenium salt and iridium salt in a preset molar ratio, and the mixture is uniformly mixed to obtain a reaction solution; and transferring the reaction solution into a hydrothermal reaction kettle, and obtaining the iridium diselenide photothermal conversion nano material through hydrothermal reaction. The solvothermal synthesis method used by the invention has the advantages of simple operation, mild experimental conditions, no toxicity of the used chemical reagent, low cost, stable product morphology, high purity and high repeatability, and is an efficient and controllable synthesis method. The iridium diselenide nano material synthesized by the method has uniform morphology, better absorption in a near infrared region, better dispersibility in water, and great potential in storage devices such as photovoltaic and thermoelectric devices, and in applications such as photo-thermal treatment of cancers. Furthermore, the synthesis method is widely applicable to the preparation of other metal selenides, such as ZnSe, snSe 2、MoSe2、ReSe2 and the like.
Drawings
Fig. 1 is an SEM schematic diagram of an iridium diselenide nanomaterial according to an embodiment of the present invention.
Fig. 2 is a schematic diagram of STEM-EDS element mapping results of iridium diselenide nanomaterial provided in an embodiment of the present invention.
Fig. 3 is an XPS characterization schematic diagram of an iridium diselenide nanomaterial provided by an embodiment of the present invention.
Fig. 4 is a schematic diagram of an ultraviolet-visible-near infrared absorption spectrum of an iridium diselenide nanomaterial provided by an embodiment of the present invention.
FIG. 5 is a schematic diagram showing the photo-thermal conversion efficiency of the iridium diselenide nanomaterial provided by the embodiment of the invention under irradiation of 808nm laser (0.8W/cm 2).
Detailed Description
The invention provides an iridium diselenide photo-thermal conversion nano material, a preparation method and application thereof, and the invention is further described in detail below in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The embodiment of the invention provides a preparation method of iridium diselenide photothermal conversion nano material, which comprises the following steps:
S100, taking selenium salt and iridium salt according to a preset molar ratio of selenium to iridium, and dispersing the selenium salt and the iridium salt in water by ultrasonic waves to obtain a first mixed solution;
s200, adding a surface modifier and a reducing agent into the first mixed solution to obtain a second mixed solution;
s300, adding an alcohol solvent into the mixed solution II to obtain a reaction solution;
S400, reacting the reaction liquid at a preset reaction temperature for a preset time;
s500, after the reaction is finished, purifying to obtain the iridium diselenide photothermal conversion nano material.
Firstly, weighing selenium salt and iridium salt with certain mass according to a preset molar ratio of selenium to iridium, dispersing the selenium salt and the iridium salt in water by ultrasonic waves, and uniformly mixing to obtain a mixed solution I; then weighing a certain mass of surface modifier and reducer, adding the surface modifier and reducer into the first mixed solution, and uniformly mixing to obtain a second mixed solution; adding a certain volume of alcohol solvent into the mixed solution II, and uniformly mixing to obtain a reaction solution; finally, transferring the reaction solution into a hydrothermal reaction kettle, setting the hydrothermal reaction kettle to a preset reaction temperature, and preserving heat for a preset time to perform a reaction; and after the reaction is finished, cooling the temperature of the hydrothermal reaction kettle to room temperature, and centrifuging and washing to obtain the iridium diselenide photo-thermal conversion nano material.
In some embodiments, the molar ratio of selenium to iridium is from 1:0.01 to 100. If the input amount ratio of Se and Ir sources is changed, the atomic ratio of two elements in the product can be influenced, and the morphology of the product can be further influenced.
In some embodiments, the selenium salt is selenocysteine dihydrochloride; the iridium salt is selected from one or more of iridium chloride, iridium acetylacetonate, ammonium chloride, sodium chloride hexahydrate, iridium tetrachloride hydrate, iridium trichloride hydrate, iridium chloride hydrate, iridium dicarbonyl acetylacetonate, iridium acetate, iridium bromide, tetradodecairidium, tris (phenylpyrazole) iridium, iridium bromide tetrahydrate, iridium chloride hydrochloride hydrate, sodium hexanitroiridate, potassium hexachloroiridate, sodium hexachloroiridate hydrate and potassium pentachloronitrosyliridium.
Specifically, in step S100, a certain mass of selenocyamine dihydrochloride and iridium salt are weighed according to the molar ratio of selenium to iridium of 1:0.01-100, dispersed in water by ultrasonic, and uniformly mixed for later use. If the input amount ratio of Se and Ir sources is changed, the atomic ratio of two elements in the product can be influenced, and the morphology of the product can be further influenced. Wherein the total mass concentration of selenium salt and iridium salt is 5-100mM, preferably 15mM.
In some embodiments, the surface modifying agent is polyvinylpyrrolidone (PVP) and sodium iodide. PVP can be used as a surface stabilizer, growth modifier, nanoparticle dispersant, and reducing agent. The stability is due to the strong repulsive force (steric hindrance) of the hydrophobic carbon chain in PVP in water, so that the mutual aggregation of nano particles can be prevented, and the effect of stabilizing a reaction system is achieved. The PVP hydrophilic pyrrolidone moiety and the hydrophobic alkyl moiety together exhibit amphipathic properties. While sodium iodide is believed to produce iridium selenide nanoparticles of relatively uniform morphology by changing the coordination environment of the metal precursor.
In some embodiments, the reducing agent is an amino acid. The amino acid is reducing and is mainly used for reducing metal precursor.
In some embodiments, the mass ratio of polyvinylpyrrolidone (PVP), sodium iodide, and amino acid is 1 (0.1-100): 0.1-100. The mass ratio has a certain influence on morphology and composition. For example, in the embodiment of the invention, the bead chain-shaped nano-particle iridium diselenide with good dispersibility in water is obtained by adopting polyvinylpyrrolidone, sodium iodide and amino acid in a mass ratio of 1:5:5. Under the same condition, the mass ratio of polyvinylpyrrolidone, sodium iodide and amino acid is changed into 5:5:5 and 0:5:5, and beaded nano particles (with partial large-size products) are obtained after PVP proportion is increased; after no PVP was added, the product became agglomerates with non-uniform morphology.
In some embodiments, the polyvinylpyrrolidone (PVP) has an average molecular weight of 1000 to 1300000; the amino acid is selected from one or more of glycine, alanine, proline and methionine.
Specifically, in step S200, polyvinylpyrrolidone, sodium iodide and amino acid are added into the mixed solution obtained in step S100 according to the mass ratio of 1 (0.1-100): (0.1-100), wherein the total mass concentration of polyvinylpyrrolidone, sodium iodide and amino acid is 0.1-100mg/ml.
In some embodiments, the alcoholic solvent comprises one or both of ethylene glycol, glycerol.
And step S200, taking water as the solvent of the mixed solution, adding a certain volume of glycol or glycerol into the mixed solution, and uniformly mixing to obtain the final reaction solution. Wherein, the volume of the glycol or the glycerol is 1 to 99 percent of that of the water. When different nano materials are synthesized by using a solvothermal method, the ethylene glycol can be used as a solvent, a template agent, a high boiling point solvent, a structure directing agent, a reducing agent and the like, and plays roles in correcting morphology, controlling nucleation, crystallization and the like. For example, in an embodiment of the invention, water: ethylene glycol=2: 1 (volume ratio) to obtain the bead chain-shaped nano-particle iridium diselenide. And under equivalent conditions, increasing (4:1) or decreasing (1:2) water: the volume ratio of the glycol can change the appearance of the obtained product and the appearance is non-uniform.
In some embodiments, in step S400, the predetermined reaction temperature is 130 to 230 ℃ and the predetermined time is 1 to 30 hours.
According to the embodiment of the invention, the nano material is synthesized by a solvothermal method, the reaction solution obtained in the step S300 is transferred into a hydrothermal reaction kettle, the hydrothermal reaction kettle is set to reach the reaction temperature (130-230 ℃), and the reaction kettle is kept for a certain time (1-30 h) to maintain the chemical reaction; and after the reaction is finished, cooling the temperature of the hydrothermal reaction kettle to room temperature, centrifuging, washing, and separating to obtain a hydrothermal product, wherein the product is the synthesized iridium diselenide nano material.
The solvothermal synthesis method used by the invention has the advantages of simple operation, mild experimental conditions, no toxicity of chemical reagents, low cost, stable product morphology, high purity and high repeatability, and is an efficient and controllable synthesis method. Furthermore, the synthesis method is widely applicable to the preparation of other metal selenides, such as ZnSe, snSe 2、MoSe2、ReSe2 and the like.
The embodiment of the invention also provides the iridium diselenide photothermal conversion nano material which is prepared by adopting the preparation method.
The embodiment of the invention also provides application of the iridium diselenide photothermal conversion nano material, which is applied to a photovoltaic and thermoelectric storage device or is applied to preparation of a photosensitizer for photothermal treatment of tumors.
The iridium diselenide nano material synthesized by the invention has uniform morphology, better absorption in a near infrared region, better dispersibility in water and great potential in applications such as photo-thermal treatment of cancers. Moreover, the iridium diselenide nano particles with uniform morphology can also be applied to storage devices such as photovoltaic and thermoelectric devices.
The iridium diselenide photo-thermal conversion nano material, the preparation method and the application thereof are further explained by specific examples.
Example 1
(1) Ultrasonic dispersing iridium chloride (formula IrCl 3, 22.4 mg) and selenocysteine dihydrochloride (formula C 4H14Cl2N2Se2, 18.0 mg) in 10ml of ultrapure water to obtain selenium-iridium mixed aqueous solution;
(2) Adding polyvinylpyrrolidone (molecular formula (C 6H9 NO) n, molecular weight: 360000, 20 mg), glycine (molecular formula NH 2CH2 COOH,100 mg) and sodium iodide (molecular formula NaI,100 mg) into selenium-iridium mixed water solution, and mixing completely by ultrasonic treatment;
(3) Finally, adding 5ml of ethylene glycol (molecular formula C 2H6O2), and uniformly mixing to obtain a final reaction solution;
(4) Transferring the reaction solution into a liner of a reaction kettle, raising the reaction temperature to 220 ℃, keeping the reaction temperature for 16 hours, and naturally cooling to room temperature; after that, the mixture was centrifuged and washed with ultrapure water, and the product was collected. The obtained product is the iridium diselenide nano material.
Example 2
The iridium diselenide nanomaterial obtained in example 1 was subjected to morphological characterization and elemental analysis.
Wherein, fig. 1 shows SEM of iridium diselenide nanomaterial, which is proved to be bead-chain nanoparticle; FIG. 2 shows STEM-EDS element mapping results of iridium diselenide nanomaterial, demonstrating that two elements of Se and Ir in the nanoparticle are uniformly distributed; fig. 3 shows XPS characterization of iridium diselenide nanomaterials: the surface element composition of iridium diselenide is analyzed by X-ray photoelectron spectroscopy (XPS), the existence of two elements of Ir and Se is proved, and the valence states of the two elements are respectively +4 and-2 (shown in the left graph of figure 3); the presence of Ir 4+ was demonstrated by two isolated peaks at 61.5 and 64.5eV, belonging to the Ir 4f 7/2 and Ir 4f 5/2 orbitals, respectively (as in the middle diagram of fig. 3); while peaks of the 3d spectrum of Se belong to the orbitals of Se3d 3/2 (54.8 and 56.1 eV) and Se3d 5/2 (54.1 eV and 55.3 eV) (as right graph of figure 3), which shows that Se exists in the compound in the form of Se 2-, and the nano material is IrSe 2.
Example 3
The iridium diselenide nanomaterial obtained in example 1 was subjected to photothermal conversion efficiency analysis.
The ultraviolet-visible-near infrared absorption spectrum graph of the iridium diselenide nano material is shown in fig. 4, and the ultraviolet-visible-near infrared absorption curve result shows that the iridium diselenide nano material has strong light absorption capacity in the wave band of 700-1000nm, so that the iridium diselenide nano material has certain potential as a photo-thermal reagent and a photo-dynamic reagent for treating cancers in the near infrared wave band. FIG. 5 shows a graph of the photo-thermal conversion efficiency of iridium diselenide nanomaterial under 808nm laser (0.8W/cm 2), which proves that the iridium diselenide nanomaterial has a good near infrared photo-thermal conversion efficiency (32.4%) and is a potential near infrared cancer photo-thermal treatment reagent.
In summary, the invention provides an iridium diselenide photo-thermal conversion nanomaterial and a preparation method and application thereof. According to the invention, a certain mass of surface modifier, reducer and alcohol solvent are added into selenium salt and iridium salt in a preset molar ratio, and the mixture is uniformly mixed to obtain a reaction solution; and transferring the reaction solution into a hydrothermal reaction kettle, and obtaining the iridium diselenide photothermal conversion nano material through hydrothermal reaction. The solvothermal synthesis method used by the invention has the advantages of simple operation, mild experimental conditions, no toxicity of the used chemical reagent, low cost, stable product morphology, high purity and high repeatability, and is an efficient and controllable synthesis method. The iridium diselenide nano material synthesized by the method has uniform morphology, better absorption in a near infrared region, better dispersibility in water, and great potential in storage devices such as photovoltaic and thermoelectric devices, and in applications such as photo-thermal treatment of cancers. Furthermore, the synthesis method is widely applicable to the preparation of other metal selenides, such as ZnSe, snSe 2、MoSe2、ReSe2 and the like.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.
Claims (7)
1. The preparation method of the iridium diselenide photothermal conversion nano material is characterized by comprising the following steps of:
Taking selenium salt and iridium salt according to a preset molar ratio of selenium to iridium, and dispersing the selenium salt and the iridium salt in water by ultrasonic to obtain a mixed solution I; the selenium salt is selenocysteine dihydrochloride; the molar ratio of selenium to iridium is 1:0.01-100;
adding a surface modifier and a reducing agent into the first mixed solution to obtain a second mixed solution; the surface modifier is polyvinylpyrrolidone and sodium iodide; the reducing agent is amino acid; the mass ratio of the polyvinylpyrrolidone to the sodium iodide to the amino acid is 1 (0.1-100);
adding an alcohol solvent into the mixed solution II to obtain a reaction solution;
Reacting the reaction solution at a predetermined reaction temperature for a predetermined time;
after the reaction is finished, the iridium diselenide photothermal conversion nano material is obtained through purification treatment.
2. The method for preparing the iridium diselenide photothermal conversion nanomaterial according to claim 1, wherein the iridium salt is one or more selected from iridium chloride, iridium acetylacetonate, ammonium chloride, sodium chloride hexahydrate, iridium tetrachloride hydrate, iridium trichloride hydrate, iridium chloride acid hydrate, iridium dicarbonyl acetylacetonate, iridium acetate, iridium bromide, tetradodecairidium, tris (phenylpyrazole) iridium, iridium bromide tetrahydrate, iridium chloride hydrochloride hydrate, sodium hexanitroiridium, potassium hexachloroiridium, sodium hexachloroiridium hydrate, and potassium pentachloronitrosyliridium.
3. The method for preparing iridium diselenide photothermal conversion nanomaterial according to claim 1, wherein the average molecular weight of polyvinylpyrrolidone is 1000-1300000; the amino acid is selected from one or more of glycine, alanine, proline and methionine.
4. The method for preparing iridium diselenide photothermal conversion nanomaterial according to claim 1, wherein the alcohol solvent comprises one or two of ethylene glycol and glycerol.
5. The method for preparing iridium diselenide photothermal conversion nanomaterial according to claim 1, wherein the predetermined reaction temperature is 130-230 ℃, and the predetermined time is 1-30h.
6. The iridium diselenide photothermal conversion nanomaterial is characterized in that the iridium diselenide photothermal conversion nanomaterial is prepared by the preparation method according to any one of claims 1 to 5.
7. The application of the iridium diselenide photothermal conversion nano material is characterized in that the iridium diselenide photothermal conversion nano material prepared by the preparation method according to any one of claims 1-5 is applied to photovoltaic and thermoelectric storage devices or is applied to preparation of photosensitizers for photothermal treatment of tumors.
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