CN108704642A - A kind of dumbbell shaped gold nano bipyramid-titanic oxide nano compound material and preparation method thereof - Google Patents
A kind of dumbbell shaped gold nano bipyramid-titanic oxide nano compound material and preparation method thereof Download PDFInfo
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- CN108704642A CN108704642A CN201810667962.0A CN201810667962A CN108704642A CN 108704642 A CN108704642 A CN 108704642A CN 201810667962 A CN201810667962 A CN 201810667962A CN 108704642 A CN108704642 A CN 108704642A
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000010931 gold Substances 0.000 title claims abstract description 100
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 98
- 239000000463 material Substances 0.000 title claims abstract description 37
- 150000001875 compounds Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims description 16
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 4
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 12
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 8
- 238000000862 absorption spectrum Methods 0.000 abstract description 3
- 239000002114 nanocomposite Substances 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 206010037660 Pyrexia Diseases 0.000 abstract description 2
- 229910010062 TiCl3 Inorganic materials 0.000 abstract description 2
- 230000004888 barrier function Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 71
- 239000003643 water by type Substances 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 6
- 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 5
- 238000004140 cleaning Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 4
- 239000002159 nanocrystal Substances 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- IVNOJHSSOXLLSM-UHFFFAOYSA-N 2-pyran-2-ylidenepyran-3-carboximidamide Chemical compound NC(=N)C1=CC=COC1=C1OC=CC=C1 IVNOJHSSOXLLSM-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910001258 titanium gold Inorganic materials 0.000 description 2
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 241000209094 Oryza Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- HRHBQGBPZWNGHV-UHFFFAOYSA-N azane;bromomethane Chemical compound N.BrC HRHBQGBPZWNGHV-UHFFFAOYSA-N 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000002659 cell therapy Methods 0.000 description 1
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical class CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 1
- 229960002163 hydrogen peroxide Drugs 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect 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
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 238000007704 wet chemistry method Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
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- H—ELECTRICITY
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- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a kind of dumbbell shaped gold nano bipyramid/titanic oxide nano compound materials and preparation method thereof, belong to technical field of material chemistry.The method that the present invention uses wet-chemical, passes through TiCl3Hydrolysis generates TiO at the both ends of gold nano bipyramid2, obtain the structure of dumbbell shaped.The present invention is compound with titanium dioxide by gold nano bipyramid, widens the absorption spectrum of titanium oxide to visible light and near-infrared region, while improving the separation of charge of metal fever electronics to greatest extent.Structure relative to nucleocapsid shape, this dumbbell shaped is spatially separating structure, so that golden bipyramid middle section is exposed, under the irradiation of visible light and near infrared light, the SPR thermoelectrons of generation cross over the Schottky barrier formed with titanium dioxide, it is transferred on titanium dioxide, is effectively isolated from gold nano bipyramid, leave positive charge directly can occur oxidation reaction in golden biconic surface and electron donor.The nanocomposite of dumbbell shaped can effectively enhance thermionic generation and light-catalysed performance.
Description
Technical field
The invention belongs to technical field of material chemistry.Specifically disclose a kind of dumbbell shaped gold nano bipyramid/titanium dioxide composite wood
Material and preparation method thereof, which has wide application in photocatalysis, the fields such as solar cell and photo-thermal therapy
Foreground.
Background technology
Gold nano-crystal is caught due to being widely used in solar energy with unique physical chemistry and plasma characteristics
It obtains, biotechnology, medical diagnosis on disease and nanometer medicine and other fields.In gold nanocrystals, this elongated gold nanocrystals of similar gold stick
Because of its synthetic method maturation, the advantages such as plasma wavelength is adjustable are widely used in various research fields.
Other than gold nanorods, gold nano bipyramid is another with adjustable longitudinal plasma resonance wavelength
（LSPR）Slender type gold nanocrystals (Adv. Funct. Mater. 2016,26,341).There are two the bottom of at for gold nano bipyramid
The pentagonal prism composition that portion connects together, there are two sharp vertex, gold nano bipyramid is more more stable than golden stick.With gold nanorods phase
Seemingly, gold nano bipyramid also there are two it is corresponding with electronic direction along longitudinal direction with lateral surface plasma body resonant vibration peak and
LSPR wavelength can systematically regulate and control.Relative to gold nanorods, gold nano bipyramid has more pointed end and narrower pattern
And Size Distribution, therefore the Extinction Cross of gold nano bipyramid and local electric-field enhancing are stronger than gold nanorods very much.Therefore Jenner
Rice bipyramid is sensing, the advantage with bigger in the application in fields such as biomedical and plasma enhancing spectrum.
Nano-titanium dioxide is a kind of semi-conducting material of N-shaped, cheap and nontoxic with its excellent photocatalytic activity
The advantages that harmless, is widely used.But there is also some shortcomingss, such as light absorption for titanium dioxide optical catalyst
Wave-length coverage is relatively narrow, and for absorbing wavelength mostly in ultra-violet (UV) band, the utilization rate of solar energy is low；And the recombination rate of carrier is higher, amount
Sub- transfer efficiency is relatively low.
Invention content
Present invention aims at a kind of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material of offer and its preparation sides
Method, to overcome some shortcomings existing in the prior art.
The specific preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material of the present invention is as follows：
（1）The seed law prepares gold nano bipyramid, and seed is added, and synthesizing has the gold nano at different longitudinal plasma resonance peaks double
Cone, detailed process are as follows：By 0.1 ~ 0.4mL seeds according to prior art preparation gold nano bipyramid original solution, centrifugation is dispersed in
Gold nano bipyramid solution is obtained in 10mL ultra-pure waters.After golden bipyramid solution and cetyl trimethylammonium bromide solution mixing,
Obtain mixed solution；A concentration of 0.3-1.5mmol/L of cetyl trimethylammonium bromide solution, preferably 0.3-1 mmol/L,
The volume ratio of golden bipyramid solution and cetyl trimethylammonium bromide solution is 1 ︰ 3；
（2）Titanium trichloride solution (being purchased from Aladdin, 15-20 wt%, hydrochloric 30 wt%, similarly hereinafter) is dispersed in ultra-pure water,
The sodium bicarbonate solution that 0.9 ~ 1mol/L is added adjusts pH=2 ~ 3, obtains the hydrolyzate of titanium, titanium trichloride solution and ultra-pure water
Volume ratio is 1 ︰ 25；
（3）By step（1）Obtained mixed liquor is added to step（2）It is reacted in the solution of gained, reacts 30 ~ 120min, it will be molten
Liquid centrifuges, and removes supernatant, obtained solid is dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, by obtained solid
Again it is scattered in 5mL ultra-pure waters and preserves.
The present invention uses wet chemistry method, passes through TiCl3Hydrolysis, is prepared for dumbbell shaped gold nano bipyramid/nano titania
Structure.The compound is made of titanium oxide and gold nano bipyramid, and two tops of gold nano bipyramid are by coated by titanium dioxide, centre
Partially due to not being wrapped by and being exposed, the structure of dumbbell shaped is showed.After titanium oxide and gold nano bipyramid are compound, light absorption
The range of spectrum is extended to visible and near infrared region by ultra-violet (UV) band, and the utilization rate of sunlight improves.Gold nano bipyramid generates SPR thermoelectricity
Subflow is to titanium oxide so that leave positive charge on golden bipyramid, due to be exposed gold nano bipyramid can directly in reaction environment
Molecule contacts occur oxidation reaction, improve electronics and the separation rate in hole, and then improve reaction rate.
The present invention demonstrates the variation at composite material plasmon absorption peak by uv-visible absorption spectra, together
When the nano composite structure that demonstrates also by transmission electron microscope there is dumbbell structure, while have good dispersibility and
Homogeneity.
The structure of gold nano bipyramid and the compound obtained dumbbell shaped of titanium dioxide is widened the absorption of titanium dioxide by the present invention
Spectrum improves the separation of charge of metal fever electronics to greatest extent to visible light and near-infrared region.Relative to nucleocapsid shape
Structure, this dumbbell shaped is spatially separating structure so that golden bipyramid middle section is exposed, under the irradiation of visible light,
The SPR thermoelectrons of generation cross over the Schottky barrier formed with titanium oxide, are transferred on titanium oxide, effectively from gold nano bipyramid
In isolate, leave positive charge directly can occur oxidation reaction in golden biconic surface and electron acceptor.Dumbbell shaped it is nano combined
Material can effectively enhance thermionic generation and light-catalysed performance.Therefore need to synthesize it is such a can be by golden bipyramid and oxygen
Change titanium to combine, and the novel photocatalysis nanostructure that gold nano bipyramid part can be exposed.
Description of the drawings
Fig. 1 is that 0.4mL seeds, 0.2mL seeds, 0.1mL seeds are added in embodiment to obtain the Jenner of different LSPR
The ultraviolet-visible spectrum of rice bipyramid；
Fig. 2 is the transmission electron microscope picture of gold nano bipyramid in embodiment；
Fig. 3 is the transmission electron microscope picture of dumbbell shaped gold nano bipyramid/nano titania composite construction made from embodiment 1 to 5；
Fig. 4 is the ultraviolet-visible light of gold nano bipyramid and gold nano bipyramid/titanic oxide nano compound material in embodiment 1
Spectrum.
Specific implementation mode
Embodiment of the present invention is described in detail below.
Embodiment 1
A kind of preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, includes the following steps：
（1）The preparation of gold nano bipyramid seed：By the citric acid three sodium solution of 0.25mL 0.01mol/L, 0.125mL
After the chlorauric acid solution of 0.01mol/L is added sequentially in the ultra-pure water of 9.625mL, it is uniformly mixed and obtains mixed solution.Then
The sodium borohydride solution of the 0.15mL 0.01mol/L newly matched is added in mixed liquor, is quickly stirred, solution is become from yellow
Light red, static 2 hours of room temperature, you can obtain seed solution.
（2）The growth of gold nano bipyramid：By the chlorauric acid solution of 2mL 0.01mol/L, the nitric acid of 0.4mL 0.01mol/L
The ascorbic acid solution of silver-colored solution, the hydrochloric acid solution of 0.8mL 1mol/L, 0.32mL 0.1mol/L is added sequentially to 40mL
In the cetyl trimethylammonium bromide solution of 0.1mol/L, it is uniformly mixed and obtains growth solution.It is molten that seed is added thereto again
Liquid stirs 10 seconds mixings, is placed at room temperature for a night.
（3）The purifying of gold nano bipyramid：Solution 7000rpm is centrifuged 15 minutes, supernatant is removed, precipitation is dispersed in again
Then 8mL 0.01mol/L AgNO3 are added in the hexadecyltrimethylammonium chloride solution of 20mL 0.08mol/L thereto,
0.32mL 0.1mol/L AA, mixing, solution are positioned over the concussion 4 hours of 60 DEG C of shaking table and react.Solution 5000rpm is centrifuged after reaction
15 minutes, supernatant is removed, precipitation is dispersed in again in the cetyl trimethylammonium bromide solution of 30mL 0.04mol/L, room temperature
4 hours are stood, gold nano bipyramid contracted payment nanometer rods are sunken to tube bottom.Supernatant is cleared, the ten of precipitation dispersion 10mL 0.002mol/L
In six alkyl trimethyl ammonium bromide solution, 0.8mL ammonia spirits are then added（30 wt%）With 0.4mL hydrogenperoxide steam generators（6
wt%）, it is stored at room temperature 4 hours after mixing.Solution 5000rpm centrifuges 15min, removes supernatant, and precipitation is scattered in 10mL again
It is preserved in solution in 0.1mol/L cetyl trimethylammonium bromide solutions, the original solution as gold nano bipyramid.
（4）The seed of 0.4mL is added, from ultraviolet-visible collection of illustrative plates 1 it is found that the peaks LSPR of the gold nano bipyramid of synthesis are
746nm；After ten minutes by gold nano bipyramid original solution 7000rpm centrifugations, remove supernatant, precipitation is dispersed in 10mL ultra-pure waters
Obtain gold nano bipyramid solution；By 0.5mL gold nano bipyramid solution and 0.5mM 1.5mL cetyl trimethylammonium bromide solutions
Mixed solution is obtained after mixing；
（5）0.2mL titanium trichloride solutions are dispersed in 5mL ultra-pure waters, are slowly stirred, by the carbonic acid of 0.93 mol/L of 1.2mL
It is 2.5 that hydrogen sodium solution, which is added dropwise and adjusts pH, obtains the hydrolyzate of titanium trichloride；
（6）By step（1）Obtained mixed liquor is added to step（2）60min is reacted at room temperature in the solution of gained, by solution
5000rpm centrifuge 8min, remove supernatant, precipitation with absolute ethyl alcohol eccentric cleaning twice after, be scattered in 5mL ultra-pure waters, obtain
Dumbbell shaped gold nano bipyramid/titanic oxide nano compound material；
（7）It is compound to gold nano bipyramid and gold nano bipyramid/nano titania using Tecnai G2 20 using transmission electron microscope
Material is characterized, and as shown in Fig. 2,3a, the composite material that the present embodiment known to comparison obtains is dumbbell structure, titanium dioxide
The both ends of gold nano bipyramid are coated on, middle section is completely exposed.The ultraviolet spectrometer of Hitachi U-4100 is to gold nano bipyramid（I.e.
AuBPs in Fig. 4）And gold nano bipyramid/titanic oxide nano compound material（AuBPs/TiO i.e. in figure2）It is characterized such as
Shown in Fig. 4, since coated by titanium dioxide is at golden bipyramid both ends, so that the dielectric constant around golden bipyramid is changed, cause to obtain
Composite material the peaks LSPR occur red shift, illustrate titanium dioxide with gold bipyramid contact it is preferable.
Embodiment 2
A kind of preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, includes the following steps：
（1）The seed law prepares gold nano bipyramid（Method is the same as embodiment 1）, the seed of 0.4mL is added, it is total to synthesize longitudinal plasma
Shake the gold nano bipyramid that peak is 746nm；After ten minutes by gold nano bipyramid original solution 7000rpm centrifugations, remove supernatant, precipitate
It is dispersed in 10mL ultra-pure waters and obtains gold nano bipyramid solution；By 0.5mL gold bipyramid solution and 0.3 mM 1.5mL hexadecanes
Mixed solution is obtained after base trimethylammonium bromide solution mixing；
（2）0.2mL titanium trichloride solutions are dispersed in 5 mL ultra-pure waters, are slowly stirred, by the carbon of 0.93 mol/L of 1.2mL
It is 2.5 that sour hydrogen sodium solution, which is added dropwise and adjusts pH, obtains the hydrolyzate of titanium trichloride；
（3）By step（1）Obtained mixed liquor is added to step（2）60min is reacted at room temperature in the solution of gained, by solution
5000rpm centrifuge 8min, remove supernatant, precipitation with absolute ethyl alcohol eccentric cleaning twice after, be scattered in again in 5mL ultra-pure waters i.e.
Dumbbell shaped gold nano bipyramid/titanic oxide nano compound material can be obtained；
（4）Gold nano bipyramid/titanic oxide nano compound material is characterized using Tecnai G2 20 using transmission electron microscope,
As shown in Figure 3b, the composite material obtained is dumbbell shaped, and pattern is similar to Example 1.
Embodiment 3
A kind of preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, includes the following steps：
（1）The seed law prepares gold nano bipyramid（Method is the same as embodiment 1）, the seed of 0.4mL is added, it is total to synthesize longitudinal plasma
Shake the gold nano bipyramid that peak is 746nm；After ten minutes by gold nano bipyramid original solution 7000rpm centrifugations, remove supernatant, precipitate
It is dispersed in 10mL ultra-pure waters and obtains gold nano bipyramid solution；By 0.5mL gold bipyramid solution and 0.8mM 1.5mL cetyls
Mixed solution is obtained after trimethylammonium bromide solution mixing；
（2）0.2mL titanium trichloride solutions are dispersed in 4 mL ultra-pure waters, are slowly stirred, by the carbon of 0.93 mol/L of 1.2mL
It is 2.5 that sour hydrogen sodium solution, which is added dropwise and adjusts pH, obtains the hydrolyzate of titanium trichloride；
（3）By step（1）Obtained mixed liquor is added to step（2）60min is reacted at room temperature in the solution of gained, by solution
5000rpm centrifuge 8min, remove supernatant, precipitation with ethyl alcohol eccentric cleaning twice after, being scattered in again in 5mL ultra-pure waters can obtain
To dumbbell shaped gold nano bipyramid/titanic oxide nano compound material；
（4）Gold nano bipyramid/titanic oxide nano compound material is characterized using Tecnai G2 20 using transmission electron microscope,
As shown in Figure 3c, the composite material obtained is dumbbell shaped, and pattern is similar to Example 1.
Embodiment 4
A kind of preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, includes the following steps：
（1）The seed law prepares gold nano bipyramid（Method is the same as embodiment 1）, the seed of 0.2mL is added, it can from ultraviolet-visible collection of illustrative plates 1
Know, the peaks LSPR of the gold nano bipyramid of synthesis are 800nm；After ten minutes by gold nano bipyramid original solution 7000rpm centrifugations, remove
Supernatant, precipitation, which is dispersed in 10mL ultra-pure waters, obtains gold nano bipyramid solution；By 0.5mL gold bipyramid solution and 0.5 mM
Mixed solution is obtained after 1.5mL cetyl trimethylammonium bromide solution mixings；
（2）By 0.2mL titanium trichloride solutions (17.1 wt%, hydrochloric 20-30 wt%）It is dispersed in 4 mL ultra-pure waters, slowly stirs
It mixes, it is 2.5 that the sodium bicarbonate solution of 0.93 mol/L of 0.9mL, which is added dropwise, and adjusts pH, obtains the hydrolyzate of titanium trichloride；
（3）By step（1）Obtained mixed liquor is added to step（2）60min is reacted at room temperature in the solution of gained, by solution
5000rpm centrifuge 8min, remove supernatant, precipitation with ethyl alcohol eccentric cleaning twice after, being scattered in again in 5mL ultra-pure waters can obtain
To dumbbell shaped gold nano bipyramid/titanic oxide nano compound material.
（4）Gold nano bipyramid/titanic oxide nano compound material is carried out using Tecnai G2 20 using transmission electron microscope
Characterization, as shown in Figure 3d, obtained composite material are dumbbell shaped, and pattern is similar to Example 1.
Embodiment 5
A kind of preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, includes the following steps：
（1）The seed law prepares gold nano bipyramid, and the seed of 0.1mL is added, from ultraviolet-visible collection of illustrative plates 1 it is found that the gold nano of synthesis
The peaks LSPR of bipyramid are 850nm；After ten minutes by gold nano bipyramid original solution 7000rpm centrifugations, remove supernatant, precipitation dispersion
Gold nano bipyramid solution is obtained in 10mL ultra-pure waters；By 0.5mL gold bipyramid solution and 0.5 mM 1.5mL cetyls three
Mixed solution is obtained after methyl bromide ammonium salt solution mixing；
（2）0.2mL titanium trichloride solutions are dispersed in 5 mL ultra-pure waters, are slowly stirred, by the carbon of 0.93 mol/L of 1.2mL
It is 2.5 that sour hydrogen sodium solution, which is added dropwise and adjusts pH, obtains the hydrolyzate of titanium trichloride；
（3）By step（1）Obtained mixed liquor is added to step（2）60min is reacted at room temperature in the solution of gained, by solution
5000rpm centrifuge 8min, remove supernatant, precipitation with ethyl alcohol eccentric cleaning twice after, being scattered in again in 5mL ultra-pure waters can obtain
To dumbbell shaped gold nano bipyramid/titanic oxide nano compound material.
（4）Gold nano bipyramid/titanic oxide nano compound material that Tecnai G2 20 are obtained is used using transmission electron microscope
It is characterized, as shown in Figure 3 e, obtained composite material is dumbbell shaped, and pattern is similar to Example 1.
The ultraviolet spectrometer of Hitachi U-4100 is compound to gold nano bipyramid/nano titania obtained of embodiment 2 ~ 5
Material is characterized, and obtained ultraviolet variation tendency is also the same, and red shift all occurs.
There are two resonance absorbing peaks in visible and near infrared region for nanocomposite prepared by the present invention（Specifically such as Fig. 4 institutes
Show）, there are wider absorption spectrum ranges, compensate for deficiency of the titanium dioxide in visible absorption so that the profit of sunlight
It is improved with rate, therefore can be used as the materials'use of solar cell.It is exposed among gold nano bipyramid in composite material so that
Golden bipyramid can be combined with reactant, and redox reaction is promoted to occur simultaneously in material surface.The material is controlled in photocatalysis, photo-thermal
It treats, the fields such as solar cell and photoelectric sensing have broad application prospects.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material, which is characterized in that including as follows
Step：
（1）The seed law prepares gold nano bipyramid：Seed is added, synthesizing has the gold nano at different longitudinal plasma resonance peaks double
Cone；
（2）Titanium source is dispersed in ultra-pure water, it is 2 ~ 3 to adjust pH, obtains the hydrolyzate of titanium；
（3）By step（1）Obtained mixed liquor is added to step（2）It is reacted in the solution of gained, reacts 30min-120min, from
The heart, removes supernatant, and obtained solid is to receive dumbbell shaped gold nano bipyramid/titanic oxide nano compound material.
2. the preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material according to claim 1, feature
It is, the step（1）Detailed process it is as follows：0.1 ~ 0.4mL seeds are added, gold nano bipyramid original solution is made, centrifuge, it will
Precipitation, which is dispersed in ultra-pure water, obtains golden bipyramid solution, by golden bipyramid solution and cetyl trimethylammonium bromide solution mixing
Afterwards, the gold nano bipyramid solution with different longitudinal plasma resonance peaks is obtained.
3. the preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material according to claim 2, feature
It is, a concentration of 0.3 ~ 1.5mmol/L of the cetyl trimethylammonium bromide solution, the volume of ultra-pure water is 10mL, gold
The volume ratio of bipyramid solution and cetyl trimethylammonium bromide solution is 1 ︰ 3.
4. the preparation method of dumbbell shaped gold nano bipyramid/titanic oxide nano compound material according to claim 1, feature
It is, step（2）Middle titanium source is the titanium trichloride solution of a concentration of 15 ~ 20wt%, the volume ratio of titanium trichloride solution and ultra-pure water
For 1 ︰ 25, pH, a concentration of 0.9 ~ 1mol/L of sodium bicarbonate solution are adjusted using sodium bicarbonate solution.
5. dumbbell shaped gold nano bipyramid/nano titania composite wood made from any preparation method of Claims 1-4
Material.
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| CN110061223A (en) * | 2019-05-06 | 2019-07-26 | 合肥工业大学 | A method of lithium titanate, which is prepared, based on nearly Chemical Equilibria Systems coats nickelic tertiary cathode material |
| CN110350108A (en) * | 2019-07-25 | 2019-10-18 | 京东方科技集团股份有限公司 | Luminescent device and preparation method thereof, display panel, gold-galactic nucleus shell nanocone preparation method |
| CN110455770A (en) * | 2019-08-12 | 2019-11-15 | 深圳市人民医院 | A kind of surface enhanced Raman scattering substrate and its preparation method and application |
| CN112113925A (en) * | 2020-09-28 | 2020-12-22 | 重庆大学 | Au NDC @ Ag NRs probe and preparation method and application thereof |
| CN112570727A (en) * | 2020-11-26 | 2021-03-30 | 四川大学 | Bipyramid gold nanoparticle and preparation method thereof |
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| CN110061223A (en) * | 2019-05-06 | 2019-07-26 | 合肥工业大学 | A method of lithium titanate, which is prepared, based on nearly Chemical Equilibria Systems coats nickelic tertiary cathode material |
| CN110061223B (en) * | 2019-05-06 | 2020-10-23 | 合肥工业大学 | Method for preparing lithium titanate-coated high-nickel ternary cathode material based on near-chemical equilibrium system |
| CN110350108A (en) * | 2019-07-25 | 2019-10-18 | 京东方科技集团股份有限公司 | Luminescent device and preparation method thereof, display panel, gold-galactic nucleus shell nanocone preparation method |
| CN110455770A (en) * | 2019-08-12 | 2019-11-15 | 深圳市人民医院 | A kind of surface enhanced Raman scattering substrate and its preparation method and application |
| CN112113925A (en) * | 2020-09-28 | 2020-12-22 | 重庆大学 | Au NDC @ Ag NRs probe and preparation method and application thereof |
| CN112570727A (en) * | 2020-11-26 | 2021-03-30 | 四川大学 | Bipyramid gold nanoparticle and preparation method thereof |
| CN115400753A (en) * | 2022-08-10 | 2022-11-29 | 武汉理工大学 | Preparation method of gold-silver core-shell nanometer bipyramid-cerium dioxide composite material |
| CN115400753B (en) * | 2022-08-10 | 2024-03-26 | 武汉理工大学 | Preparation method of gold-silver core-shell nano bipyramid-cerium dioxide composite material |
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