CN101760171A - Optical resonance composite material in noble metal/titanium dioxide micro-nano structure - Google Patents
Optical resonance composite material in noble metal/titanium dioxide micro-nano structure Download PDFInfo
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Abstract
The invention relates to a composite material in a micro-nano structure and a preparation method thereof, in particular to an optical resonance composite material in a noble metal/titanium dioxide micro-nano structure and a preparation method thereof. The material belongs to a quasi monodisperse floccular micro-nano structure grain with the grain diameter between 300 nm and 3 mum formed by self assembly by nanometer rods with the diameter between 30 and 50 nm and the length between 100 and 500 nm. The material has the main ingredients of titanium dioxide and noble metal of silver or gold, wherein the mol ratio of titanium to silver or gold is 1/0.05 to 0.5. The material has special optical transmission performance in the visible light wave band. The method for preparing the material is a solvent thermosynthesis method, the preparation process is simple, the yield is high, and the grain diameter, the microcosmic appearance, the structure and the performance of the grains can all realize the effective control and regulation. The accompanying drawing shows the scanning electron microscope photos of the composite material in the silver/titanium dioxide micro-nano structure when the mol ratio of the titanium to the sliver is 1/0.25.
Description
Technical field the present invention relates to a kind of micro nano structure matrix material and preparation method thereof, particularly a kind of optical resonance composite material in noble metal/titanium dioxide micro-nano structure and preparation method thereof.
The background technology micro nano structure is meant nanostructure is incorporated in the structural unit of micro-meter scale and a kind of special structural form that forms.In recent years, it is relevant that the magical function of discovering the many biologies of occurring in nature and its surface have micro nano structure, and having super-hydrophobicity and self-cleaning function as lotus leaf surface is also to have nanostructure on the micron mastoid process because of lotus leaf surface; It is to have complicated micro-nano layering fluff structures because of its foot that gecko can freely creep on slick vertical wall and top ceiling; Water skipper can walk as on the ground on the water surface, run, jump, and is to have the bristle of the micro-meter scale of many orientations because of its shank, and has a lot of spiral nanometer grooves on each bristle.These are found to be preparation new function material and device new approaches are provided, and also make preparation and the research of micron and nanometer composite structure material become the focus in many fields simultaneously.The main method that is used to prepare micron and nanometer composite structure at present is a photoetch method, this method technical maturity, can manufacture, but its apparatus expensive, and can not prepare the structure of size less than 100nm.Chemical processes such as template, chemical Vapor deposition process, self-assembly method also are used to prepare the micron and nanometer composite structure material, but the complex process of these methods, the product amount that obtains seldom, and the material that can prepare and structure are more single.
Titanium dioxide (TiO
2) be a kind of very noticeable material, it has wide practical use at emerging fields such as photochemical catalysis, solar cell, gas sensor, high-performance ceramics, and the composite titania material of mixing precious metals such as gold and silver has demonstrated powerful advantage at catalytic field.Research proves that the particle size of titanium dioxide, pattern, crystalline state and surface property all can and be used its performance and produce extremely important influence, and therefore, researchist's expectation can synthesize the particle of the titanium dioxide of various different-shapes and structure.At present, the TiO of multiple patterns such as solid sphere, hollow ball, mesoporous ball, nanotube, nanometer rod
2Particle can synthesize substantially in achieve effective control, still has very big challenge but prepare the precious metal/titanium-dioxide photo resonance composite material with micro nano structure.
Summary of the invention the purpose of this invention is to provide a kind of optical resonance composite material in noble metal/titanium dioxide micro-nano structure and preparation method thereof.This optical resonance composite material in noble metal/titanium dioxide micro-nano structure is that to be about 30-50nm, length by diameter be the monodispersed bobbles shape of a kind of standard particle that the nanometer rod self-assembly of 100-1500nm forms, and this material has special optical transmission performance in visible light wave frequency range.Its preparation method is characterised in that: at first butyl (tetra) titanate and toluene are mixed, stirred 0.5 hour in ice bath; Then the silver nitrate aqueous solution or the tetra chlorauric acid aqueous solution are joined in the mixed solution of butyl (tetra) titanate and toluene; Stir and add titanium tetrachloride aqueous solution, magnetic agitation 1 hour after 0.5 hour more in proportion; Then mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, reactor is put into thermostatic drying chamber reacted 16-48 hour down at 120 ℃, 150 ℃ or 180 ℃.Products therefrom repeatedly washs after-filtration with alcohol, obtains pressed powder through the infrared lamp oven dry; The part pressed powder is put into high temperature resistance furnace, through 200 ℃ of half an hour, 300 ℃ of half an hour, 400 ℃ of one hour, 500 ℃ calcinings of three hours, the silver/titanium dioxide or the gold/titanium dioxide micro-nano structural composite material that can obtain having special optical transmission performance.This preparation technology is simple, the product amount is bigger, and particle grain size, microscopic appearance and structure and performance thereof all can realize effective regulation and control.
Description of drawings
The stereoscan photograph of Fig. 1 silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.05: 1,50wt%TiCl
4)
The stereoscan photograph of Fig. 2 silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.12: 1,50wt%TiCl
4)
The stereoscan photograph of Fig. 3 silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.25: 1,50wt%TiCl
4)
The stereoscan photograph of Fig. 4 silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.37: 1,38wt%TiCl
4)
The stereoscan photograph of Fig. 5 silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.44: 1,25wt%TiCl
4)
The stereoscan photograph of Fig. 6 gold/titanium dioxide micro-nano structural composite material (Au: Ti=0.05: 1,50wt%TiCl
4)
Fig. 7 through the stereoscan photograph of incinerating silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.25: 1,50wt%TiCl
4)
Fig. 8 through the ultimate analysis collection of illustrative plates of incinerating silver/titanium dioxide micro nano structure matrix material (Ag: Ti=0.25: 1,50wt%TiCl
4)
Fig. 9 sample is at the transmission spectrum of visible light wave frequency range
(A) unguyed body particulate solidifies glue No. 107
(B) pure titinium dioxide micro nano structure matrix material is scattered in No. 107 glue
(C) in incinerating silver/titanium dioxide micro nano structure matrix material is scattered in No. 107 glue
Embodiment selects for use analytical pure Silver Nitrate, analytical pure tetra chlorauric acid, chemical pure tetrabutyl titanate, chemical pure titanium tetrachloride, analytical pure dehydrated alcohol, deionized water to make reaction raw materials.Titanium tetrachloride is added drop-wise in the deionized water preparation obtains titanium tetrachloride aqueous solution under condition of ice bath, this aqueous solution is put into refrigerator and cooled hide standby.Butyl (tetra) titanate and toluene are mixed, in ice bath, stirred 0.5 hour; Then the silver nitrate aqueous solution or the tetra chlorauric acid aqueous solution are joined in the mixed solution of butyl (tetra) titanate and toluene; Stir and add titanium tetrachloride aqueous solution, magnetic agitation 1 hour after 0.5 hour more in proportion; Then mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, reactor is put into thermostatic drying chamber reacted 16-48 hour down at 120 ℃, 150 ℃ or 180 ℃.Products therefrom obtains pressed powder with alcohol washing and filtering repeatedly through the infrared lamp oven dry; The part pressed powder is put into high temperature resistance furnace,, can obtain silver/titanium dioxide or gold/titanium dioxide micro-nano structured light resonance composite material through 200 ℃ of half an hour, 300 ℃ of half an hour, 400 ℃ of one hour, 500 ℃ calcinings of three hours.
The performance of implementation procedure of the present invention and material is by embodiment and description of drawings:
Embodiment one:
Titanium tetrachloride is added drop-wise in the deionized water preparation obtains the titanium tetrachloride aqueous solution that massfraction is 50wt% under condition of ice bath, hide standby in refrigerator and cooled this aqueous solution; Getting the 0.2g Silver Nitrate is dissolved in the 1ml deionized water and is mixed with silver nitrate aqueous solution.At first 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The silver nitrate aqueous solution that will prepare all joins in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour again; Add the titanium tetrachloride aqueous solution that the 4ml massfraction is 50wt% then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 150 ℃ of reactions 24 hours.Products therefrom repeatedly washs after-filtration with alcohol, promptly obtains final sample through the infrared lamp oven dry.Gained particulate pattern as shown in Figure 1.
Embodiment two:
Titanium tetrachloride is added drop-wise in the deionized water preparation obtains the titanium tetrachloride aqueous solution that massfraction is 50wt% under condition of ice bath, hide standby in refrigerator and cooled this aqueous solution; Getting the 0.5g Silver Nitrate is dissolved in the 1ml deionized water and is mixed with silver nitrate aqueous solution.At first 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The silver nitrate aqueous solution that will prepare all joins in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour again; Add the titanium tetrachloride aqueous solution that the 4ml massfraction is 50wt% then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 150 ℃ of reactions 24 hours.Products therefrom repeatedly washs after-filtration with alcohol, promptly obtains final sample through the infrared lamp oven dry.Gained particulate pattern as shown in Figure 2.
Embodiment three:
Titanium tetrachloride is added drop-wise in the deionized water preparation obtains the titanium tetrachloride aqueous solution that massfraction is 50wt% under condition of ice bath, hide standby in refrigerator and cooled this aqueous solution; Getting the 1.0g Silver Nitrate is dissolved in the 1ml deionized water and is mixed with silver nitrate aqueous solution.At first 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The silver nitrate aqueous solution that will prepare all joins in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour again; Add the titanium tetrachloride aqueous solution that the 4ml massfraction is 50wt% then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 150 ℃ of reactions 24 hours.Products therefrom repeatedly washs after-filtration with alcohol, promptly obtains final sample through the infrared lamp oven dry.Gained particulate pattern as shown in Figure 3.
Embodiment four:
Titanium tetrachloride is added drop-wise in the deionized water preparation obtains the titanium tetrachloride aqueous solution that massfraction is 38wt% under condition of ice bath, hide standby in refrigerator and cooled this aqueous solution; Getting the 1.0g Silver Nitrate is dissolved in the 1ml deionized water and is mixed with silver nitrate aqueous solution.At first 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The silver nitrate aqueous solution that will prepare all joins in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour again; Add the titanium tetrachloride aqueous solution that the 2ml massfraction is 38wt% then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 150 ℃ of reactions 24 hours.Products therefrom repeatedly washs after-filtration with alcohol, promptly obtains final sample through the infrared lamp oven dry.Gained particulate pattern as shown in Figure 4.
Embodiment five:
Titanium tetrachloride is added drop-wise in the deionized water preparation obtains the titanium tetrachloride aqueous solution that massfraction is 25wt% under condition of ice bath, hide standby in refrigerator and cooled this aqueous solution; Getting the 1.0g Silver Nitrate is dissolved in the 1ml deionized water and is mixed with silver nitrate aqueous solution.At first 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The silver nitrate aqueous solution that will prepare all joins in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour again; Add the titanium tetrachloride aqueous solution that the 2ml massfraction is 25wt% then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 150 ℃ of reactions 24 hours.Products therefrom repeatedly washs after-filtration with alcohol, promptly obtains final sample through the infrared lamp oven dry.Gained particulate pattern as shown in Figure 5.
Embodiment six:
Titanium tetrachloride is added drop-wise in the deionized water preparation obtains the titanium tetrachloride aqueous solution that massfraction is 50wt% under condition of ice bath, hide standby in refrigerator and cooled this aqueous solution; Getting the 0.1g tetra chlorauric acid is dissolved in and is mixed with the tetra chlorauric acid aqueous solution in the 1ml deionized water.At first 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The tetra chlorauric acid aqueous solution that will prepare more all joins in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour; Add the titanium tetrachloride aqueous solution that the 4ml massfraction is 50wt% then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 150 ℃ of reactions 24 hours.Products therefrom repeatedly washs after-filtration with alcohol, promptly obtains final sample through the infrared lamp oven dry.Gained particulate pattern as shown in Figure 6.
Embodiment seven:
Embodiment three prepared samples are put into high temperature resistance furnace, through 200 ℃ of half an hour, 300 ℃ of half an hour, 400 ℃ of one hour, 500 ℃ calcinings of three hours, gained particulate pattern as shown in Figure 7, particulate ultimate analysis figure is as shown in Figure 8.
Embodiment eight:
Embodiment four prepared samples are put into high temperature resistance furnace,, obtain the gray solid particle through 200 ℃ of half an hour, 300 ℃ of half an hour, 400 ℃ of one hour, 500 ℃ calcinings of three hours.
Embodiment nine:
2 milliliters of No. 107 rubbers and 0.05 gram solidifying agent are injected into the glass square box after mixing, after 24 hours the solidified blob of viscose are taken out, this blob of viscose is transparent, at the transmission spectrum of visible light wave frequency range shown in Fig. 9 (A).With 10 milligrams of pure zirconia titanium micro nano structure particles dispersed in 2 milliliters of No. 107 rubbers, add 0.05 gram solidifying agent again, be injected into after mixing and allow its curing in the glass square box, obtained white printing opacity blob of viscose after solidifying in 24 hours, transmission peaks does not appear in this solid gums, its at the transmission spectrum of visible light wave frequency range shown in Fig. 9 (B).The particles dispersed that 10 milligrams of embodiment eight are prepared is in 2 milliliters of No. 107 rubbers, add 0.05 gram solidifying agent again, be injected into after mixing in the glass square box, to solidify blob of viscose after 24 hours takes out, this solid gums transmission peaks occurs at the 510nm place, its at the transmission spectrum of visible light wave frequency range shown in Fig. 9 (C).
Claims (4)
1. optical resonance composite material in noble metal/titanium dioxide micro-nano structure, this material is to be that 30-50nm, length are that a kind of particle diameter that the nanometer rod self-assembly of 100-1500nm forms is accurate single bobbles shape particle that disperses of 200nm-3 μ m by diameter, and its preparation method is the solvent thermal synthesis method.
2. optical resonance composite material in noble metal/titanium dioxide micro-nano structure according to claim 1, the main component that it is characterized in that material is titanium dioxide and precious metal silver or golden, wherein titanium and silver or golden mol ratio are 1: 0.05～0.5.
3. optical resonance composite material in noble metal/titanium dioxide micro-nano structure according to claim 1 is characterized in that special transmission peaks can occurring in the wavelength region of visible light 360nm-800nm.
4. the preparation method of optical resonance composite material in noble metal/titanium dioxide micro-nano structure as claimed in claim 1 is characterized in that preparation process comprises following several steps:
(1) select for use analytical pure Silver Nitrate, analytical pure tetra chlorauric acid, chemical pure tetrabutyl titanate, chemical pure titanium tetrachloride, analytical pure dehydrated alcohol, deionized water to make reaction raw materials;
(2) titanium tetrachloride is added drop-wise in the deionized water preparation under condition of ice bath and obtains the titanium tetrachloride aqueous solution that massfraction is 20～50wt%, hide standby in refrigerator and cooled this aqueous solution; Getting 0.2g～1.5g Silver Nitrate or tetra chlorauric acid is dissolved in the 1ml deionized water and is mixed with silver nitrate aqueous solution;
(3) 4 gram tetrabutyl titanates are joined in 30 milliliters of toluene, in ice bath, stirred 0.5 hour; The Silver Nitrate that will prepare or the tetra chlorauric acid aqueous solution all join in the toluene aqueous solution of tetrabutyl titanate and stirred 0.5 hour again; Add the 4ml titanium tetrachloride aqueous solution then, magnetic agitation 1 hour; At last mixed system being moved into the tetrafluoroethylene is in the stainless steel autoclave of liner, and wherein the volume of reactant is about autoclave volumetrical 80%, and reactor is put into thermostatic drying chamber 120 ℃～180 ℃ scope internal reaction 24 hours; Products therefrom repeatedly washs after-filtration with alcohol, dries through infrared lamp;
(4) sample of oven dry is put into high temperature resistance furnace,, promptly obtain optical resonance composite material in noble metal/titanium dioxide micro-nano structure through 200 ℃ of half an hour, 300 ℃ of half an hour, 400 ℃ of one hour, 500 ℃ calcinings of three hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101884939A (en) * | 2010-08-05 | 2010-11-17 | 黑龙江大学 | Controllable synthesis method of nonmetallic ion-doped nano titanium dioxide by phase separation-hydrolysis solvothermal method |
| CN108383531A (en) * | 2018-05-15 | 2018-08-10 | 西北工业大学 | The MgB of the topological heterogeneous phase doping of illuminator2Base super conductor and preparation method thereof |
| CN109921171A (en) * | 2019-04-03 | 2019-06-21 | 济南鸿泰华丰机械有限公司 | A kind of miniature 5G communication base station antenna |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1210102C (en) * | 2003-09-01 | 2005-07-13 | 武汉理工大学 | High-adsorbability glass beads with photocatalysis function |
| CN100428997C (en) * | 2006-09-06 | 2008-10-29 | 浙江大学 | Method for preparing composite film of silver Nano granule / titanium dioxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101884939A (en) * | 2010-08-05 | 2010-11-17 | 黑龙江大学 | Controllable synthesis method of nonmetallic ion-doped nano titanium dioxide by phase separation-hydrolysis solvothermal method |
| CN101884939B (en) * | 2010-08-05 | 2012-01-25 | 黑龙江大学 | Controllable synthesis method of nonmetallic ion-doped nano titanium dioxide by phase separation-hydrolysis solvothermal method |
| CN108383531A (en) * | 2018-05-15 | 2018-08-10 | 西北工业大学 | The MgB of the topological heterogeneous phase doping of illuminator2Base super conductor and preparation method thereof |
| CN109921171A (en) * | 2019-04-03 | 2019-06-21 | 济南鸿泰华丰机械有限公司 | A kind of miniature 5G communication base station antenna |
| CN109921171B (en) * | 2019-04-03 | 2020-02-18 | 宁波智诚祥科技发展有限公司 | Miniature 5G communication base station antenna |
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