CN105056849A - Hollow sphere adopting metal oxide/Pt/C three-layer nano structure and preparation method of hollow sphere - Google Patents
Hollow sphere adopting metal oxide/Pt/C three-layer nano structure and preparation method of hollow sphere Download PDFInfo
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- CN105056849A CN105056849A CN201510412672.8A CN201510412672A CN105056849A CN 105056849 A CN105056849 A CN 105056849A CN 201510412672 A CN201510412672 A CN 201510412672A CN 105056849 A CN105056849 A CN 105056849A
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Abstract
The invention discloses a hollow sphere adopting a metal oxide/Pt/C three-layer nano structure. A spherical shell of the hollow sphere sequentially comprises a metal oxide layer, a Pt layer and an amorphous carbon layer from inside to outside. A template adsorption method is used, a hollow metal oxide sphere is prepared firstly, Pt particles are prepared on the surface of metal oxide with an impregnation method, finally, the surface of the hollow metal oxide sphere coated with the Pt particles is coated with amorphous carbon through hydro-thermal treatment, and then the hollow sphere adopting the metal oxide/Pt/C three-layer nano structure is prepared. The prepared hollow sphere with the metal oxide/Pt/C three-layer nano structure has a regular core-shell structure, the thickness is adjustable, and the specific surface area is larger than 200 m <2>/g. A method is simple, the cost is lower, industrial production can be easily realized, and the hollow sphere can be well applied to fields such as photocatalytic decomposition of water for hydrogen production, gas sensing, super capacitors, lithium ion batteries and the like.
Description
Technical field
The present invention relates to a kind of nano-hollow ball and preparation method thereof, particularly relate to a kind of metal oxide/Pt/C tri-layers of nanostructured hollow ball and preparation method thereof.
Background technology
Photocatalytic hydrogen production by water decomposition is the preferred approach of solar energy chemical conversion, because Hydrogen Energy has the incomparable advantage of other energy such as clean, safe, efficient as secondary energy sources.Climate change, fuel cell technology and the environmental problem become increasingly conspicuous have promoted the generation of " hydrogen economy ", replace or partly replace the direction that existing energy supply will become mankind's effort with hydrogen.At present, fossil fuel hydrogen manufacturing is industrial main path, and the whole world has the hydrogen of more than 95% to be manufactured by fossil fuel.Although the existing technical maturity of fossil resource hydrogen manufacturing, production cost is also lower, but resource-constrained and non-renewable, while acquisition hydrogen, in air, discharge a large amount of GHG carbon dioxide, will the two fold problem of shortage of resources and environment deterioration be faced with fossil resource hydrogen manufacturing.In the long run, this does not meet the needs of sustainable development.Therefore, utilize regenerative resource hydrogen manufacturing from non-fossil fuel, comprise biological hydrogen production, solar energy photocatalytic decomposing hydrogen-production and renewable energy power generation water electrolysis hydrogen production, it is one of effective way solving national energy security and environmental problem, wherein utilize solar energy photocatalytic hydrogen production by water decomposition, cause the extensive attention of countries in the world in recent years.
In semi-conducting material photocatalysis system, the effective separation realizing photo-generate electron-hole be by photocatalytic applications in the energy and environmental problem must through approach.Common single compound photochemical catalyst is metal oxide or sulfide semiconductor material.As TiO
2, WO
3deng.They have all had in photocatalysis field applies very widely.But they also have the imperfect part of intrinsic, single semi-conducting material is because internal flaw and intrinsic compound, make photo-generate electron-hole after generation, have the photo-generate electron-hole directly and surface pairings compound inner at semiconductor close to 90%, instead of with water and pollutant effect.Which results in the waste of most photo-generate electron-hole, greatly limit the utilization to solar energy.Therefore, impel being separated of light induced electron and hole, suppress its compound, thus improve quantum efficiency, to make full use of solar energy, the stability improving photochemical catalyst is the key problem of modern photocatalysis field.At present, the modification technology of the semiconductor light-catalysts having several conventional, mainly comprises the compound etc. of noble metal decorated, doped transition metal ions and semiconductor light-catalyst.Noble metal decorated have photocatalysis efficiency high, increase the concern absorption of visible ray being generally subject to people.
In addition, metal oxide and amorphous carbon combine, and can not only increase the absorption to visible ray, and can effective metastatic electron, the separation that favourable photo-generate electron-hole is right, thus the photocatalysis efficiency of raising composite.
To sum up, if we can design the composite construction of metal-oxide semiconductor (MOS)/noble metal/amorphous carbon, the photocatalysis efficiency of material is inherently improved.
Summary of the invention
The object of this invention is to provide that a kind of specific area is large, the simple metal oxide/Pt/C of preparation technology tri-layers of nanostructured hollow ball and preparation method thereof.
Metal oxide/Pt/C of the present invention tri-layers of nanostructured hollow ball, it is characterized in that the structure of this hollow ball is from inside to outside followed successively by metal oxide layer, noble metal platinum (Pt) stratum granulosum and agraphitic carbon (C) layer, metal oxide layer and Pt stratum granulosum form hetero-junctions, metal oxide layer thickness is between 7 ~ 50 nanometers, the particle diameter of platinum grain is in 5 ~ 8 nanometers, the thickness of amorphous carbon layer is in 10 ~ 15 nanometers, and hollow ball diameter is 100 ~ 600 nanometers.
In technique scheme, described metal oxide is selected from the oxide of Al, B, Bi, Ba, Ca, Co, Cr, Ce, Cu, La, Ni, Fe, Zn, Sn, Rh, W, Nb, Ta, Ti, V, Hf, Mn, In, Li, Ge, Se, Zr, Mg, Ga or Si.
Prepare the method for above-mentioned metal oxide/Pt/C tri-layers of nanostructured hollow ball, comprise the steps:
1) adsorbent solution is configured: be dissolved in solvent by metal oxide salt, be configured to the metal oxide salting liquid that concentration of metal ions is 0.01 ~ 1M, described slaine is selected from the acetate of Al, B, Bi, Ba, Ca, Co, Cr, Ce, Cu, La, Ni, Fe, Zn, Sn, Rh, W, Ta, Ti, V, Hf, Mn, In, Li, Ge, Se, Zr, Mg, Ga, Si, chlorate, nitrate, sulfate or ester salt, and described solvent is deionized water, ethanol, formamide or ethylene glycol;
2) adsorbing metal ions: spherical template surface with carboxyl and hydroxyl immerses in the adsorbent solution of step 1), spherical template content is made to be 1g/L ~ 10g/L, ultrasonic spherical template is fully disperseed, centrifugal or suction filtration after stirring and adsorbing 4 ~ 48h, obtain the spherical template after absorption, be placed in 60 ~ 100 DEG C, dry 6 ~ 48h; Described spherical template is carbon ball, PS ball or SiO
2ball;
3) remove template: by step 2) in dried carbon ball or PS ball heat treatment 3 ~ 60h at 300 ~ 800 DEG C remove carbon ball template or PS ball template obtains metallic oxide hollow sphere; Or by step 2) in dried SiO
2ball is at 300 ~ 800 DEG C after heat treatment 3 ~ 60h, then at 60 ~ 100 DEG C, immerse concentration be keep 0.5 ~ 24h in the NaOH solution of 1 ~ 20M, removes SiO
2ball template obtains metallic oxide hollow sphere;
4) platinum grain is added: it is in the platinum acid chloride solution of 0.05 ~ 1mg/mL that the 10 ~ 100mg metallic oxide hollow sphere obtained in step 3) is joined 10 ~ 50mL platinum concentration, by dry for the water evaporation in solution at 60 ~ 100 DEG C, by the sample that obtains under atmosphere of hydrogen at 200 ~ 300 DEG C of heat treatment 2 ~ 6h, obtain metal oxide/Pt nano-hollow sphere structured;
5) agraphitic carbon is added: it is in the D/W of 0.1 ~ 1M that the metal oxide of the 10 ~ 60mg obtained in step 4)/Pt nano-hollow ball is joined 30 ~ 50mL concentration, ultrasonic 10 ~ 60min is placed in water heating kettle, 6 ~ 8h is reacted at 150 ~ 180 DEG C, after being cooled to room temperature, centrifugal, cleaning and at 60 ~ 100 DEG C, dry 6 ~ 48h, obtains metal oxide/Pt/C tri-layers of nanostructured hollow ball.
In the present invention, described surface has the preparation method of the spherical template of carboxyl and hydroxyl can with reference to Sun, X.; Li, Y.,
angewandteChemieInternationalEdition 2004, 43(29), 3827-3831, Lou, X.W.; Archer, L.A.; Yang, Z.,
advancedMaterials 2008, 20(21), 3987-4019 and Wang, D.; Hisatomi, T.; Takata, T.; Pan, C.; Katayama, M.; Kubota, J.; Domen, K.,
angewandteChemieInternationalEdition 2013, 52(43), 11252-11256.
In the present invention, utilize rich surface to contain the spherical template of anionic group, prepare metallic oxide hollow sphere; Metal forming particle is formed on metal-oxide semiconductor (MOS) hollow ball surface by infusion process; One deck agraphitic carbon is formed on the surface of hollow ball again by hydro-thermal method.
Beneficial effect of the present invention is: metal oxide/Pt/C of the present invention tri-layers of nanostructured hollow ball, and the structure of hollow ball is from inside to outside followed successively by metal oxide, noble metal platinum (Pt) particle and agraphitic carbon (C).Metal oxide layer and Pt stratum granulosum form hetero-junctions, and amorphous carbon layer is electron transfer layer, plays the effect of protective layer simultaneously, and shell thickness can regulate and control, and adopt this structure can well realize the separation of electron hole, and the specific area of this structure are greater than 200m
2/ g.Method of the present invention is simple, cost is lower, is beneficial to suitability for industrialized production, in photocatalytic hydrogen production by water decomposition, gas sensing, ultracapacitor and lithium ion battery etc., has good application.
Accompanying drawing explanation
Fig. 1 is TiO
2the SEM diffraction picture of/Pt/C tri-layers of nanostructured hollow ball.
Fig. 2 is TiO
2the N of/Pt/C tri-layers of nanostructured hollow ball
2adsorption-desorption curve.
Fig. 3 is TiO
2the photocatalysis performance comparison diagram of/Pt/C tri-layers of nanostructured hollow ball.
Detailed description of the invention
Embodiment 1
TiO
2/ Pt/C nano-hollow ball:
(1) 0.34g butyl titanate is placed in 100mL ethanol and dissolves, and obtains 0.01M titanium ion solution, in this adsorbent solution, then add the SiO that 0.1g surface has carboxyl and hydroxyl
2ball template, ultrasonicly makes spherical template fully disperse, centrifugal after stirring and adsorbing 4h, obtains the spherical template after absorption, is placed in 60 DEG C, dry 6h;
(2) by the sample that obtains in step (1) in air at 300 DEG C after heat treatment 60h, then at 60 DEG C, immerse concentration be keep 0.5h in the NaOH solution of 1M, removes SiO
2ball template obtains titanium oxide hollow ball housing;
(3) by step 2) in the 10mgTiO that obtains
2the concentration that hollow ball joins 10mL noble metal platinum is in the platinum acid chloride solution of 0.05mg/mL, by dry for the water evaporation in solution at 60 DEG C, collects sample.By the sample that obtains in atmosphere of hydrogen at 200 DEG C heat treatment 2h, can TiO be obtained
2/ Pt is nano-hollow sphere structured.
(4) TiO of 10mg will obtained in step 3)
2it is in the D/W of 0.1M that/Pt nano-hollow ball joins 30mL concentration, and ultrasonic 10min is placed in water heating kettle, at 150 DEG C, react 6h, after being cooled to room temperature, centrifugal, cleaning and at 60 DEG C, dry 6h, can obtain TiO
2/ Pt/C is nano-hollow sphere structured.
The TiO that this example is obtained
2/ Pt/C nano-hollow sphere structured SEM figure as shown in Figure 1, N
2as shown in Figure 2, photocatalysis performance is illustrated in figure 3 adsorption-desorption curve.As shown in Figure 1, TiO
2/ Pt/C is nano-hollow sphere structured is that nano-hollow is spherical, and diameter is between 100 ~ 600nm; As shown in Figure 2, TiO
2the nano-hollow sphere structured specific area of/Pt/C is higher than 200m
2/ g; As shown in Figure 3, TiO
2/ Pt/C is nano-hollow sphere structured has good photocatalysis performance.
Embodiment 2
Bi
2o
3/ Pt/C nano-hollow ball:
(1) 24g five water bismuth nitrate is placed in 50mL ethylene glycol and dissolves, obtain the bismuth ion solution of 1M, then in this adsorbent solution, add the carbon ball template that 0.5g surface has carboxyl and hydroxyl, ultrasonic spherical template is fully disperseed, centrifugal after stirring and adsorbing 48h, obtain the spherical template after absorption, be placed in 100 DEG C, dry 48h;
(2) sample obtained in step (1) is obtained Bi after heat treatment 20h in air at 500 DEG C
2o
3hollow ball housing;
(3) by step 2) in the 100mgBi that obtains
2o
3the concentration that hollow ball joins 50mL noble metal platinum is in the platinum acid chloride solution of 1mg/mL, by dry for the water evaporation in solution at 100 DEG C, collects sample.By the sample that obtains in atmosphere of hydrogen at 300 DEG C heat treatment 6h, can Bi be obtained
2o
3/ Pt is nano-hollow sphere structured.
(4) Bi of 60mg will obtained in step 3)
2o
3it is in the D/W of 1M that/Pt nano-hollow ball joins 50mL concentration, and ultrasonic 60min is placed in water heating kettle, at 180 DEG C, react 8h, after being cooled to room temperature, centrifugal, cleaning and at 100 DEG C, dry 48h, can obtain Bi
2o
3/ Pt/C is nano-hollow sphere structured.
Embodiment 3
CeO
2/ Pt/C nano-hollow ball:
(1) 21.7g six water cerous nitrate is placed in 100mL ethanol and dissolves, obtain the bismuth ion solution of 0.5M, then in this adsorbent solution, add the PS ball template that 0.8g surface has carboxyl and hydroxyl, ultrasonic spherical template is fully disperseed, centrifugal after stirring and adsorbing 12h, obtain the spherical template after absorption, be placed in 80 DEG C, dry 24h;
(2) sample obtained in step (1) is obtained CeO after heat treatment 3h in air at 800 DEG C
2hollow ball housing;
(3) by step 2) in the 50mgCeO that obtains
2the concentration that hollow ball joins 30mL noble metal platinum is in the platinum acid chloride solution of 0.5mg/mL, by dry for the water evaporation in solution at 80 DEG C, collects sample.By the sample that obtains in atmosphere of hydrogen at 250 DEG C heat treatment 4h, can CeO be obtained
2/ Pt is nano-hollow sphere structured.
(4) CeO of 40mg will obtained in step 3)
2it is in the D/W of 0.5M that/Pt nano-hollow ball joins 40mL concentration, and ultrasonic 40min is placed in water heating kettle, at 170 DEG C, react 7h, after being cooled to room temperature, centrifugal, cleaning and at 80 DEG C, dry 18h, can obtain CeO
2/ Pt/C is nano-hollow sphere structured.
Embodiment 4
ZrO
2/ Pt/C nano-hollow ball:
(1) 4.29g five water zirconium nitrate is placed in 100mL ethanol and dissolves, obtain the bismuth ion solution of 0.1M, then in this adsorbent solution, add the carbon ball template that 0.3g surface has carboxyl and hydroxyl, ultrasonic spherical template is fully disperseed, centrifugal after stirring and adsorbing 24h, obtain the spherical template after absorption, be placed in 70 DEG C, dry 12h;
(2) sample obtained in step (1) is obtained ZrO after heat treatment 30h in air at 600 DEG C
2hollow ball housing;
(3) by step 2) in the 70mgZrO that obtains
2the concentration that hollow ball joins 40mL noble metal platinum is in the platinum acid chloride solution of 0.1mg/mL, by dry for the water evaporation in solution at 70 DEG C, collects sample.By the sample that obtains in atmosphere of hydrogen at 280 DEG C heat treatment 5h, can ZrO be obtained
2/ Pt is nano-hollow sphere structured.
(4) ZrO of 50mg will obtained in step 3)
2it is in the D/W of 0.7M that/Pt nano-hollow ball joins 35mL concentration, and ultrasonic 30min is placed in water heating kettle, at 160 DEG C, react 8h, after being cooled to room temperature, centrifugal, cleaning and at 70 DEG C, dry 24h, can obtain ZrO
2/ Pt/C is nano-hollow sphere structured.
Embodiment 5
Ga
2o
3/ Pt/C nano-hollow ball:
(1) 7.65g anhydrous nitric acid gallium is placed in 100mL formamide and dissolves, obtain the bismuth ion solution of 0.3M, then in this adsorbent solution, add the carbon ball template that 0.7g surface has carboxyl and hydroxyl, ultrasonic spherical template is fully disperseed, centrifugal after stirring and adsorbing 12h, obtain the spherical template after absorption, be placed in 65 DEG C, dry 24h;
(2) sample obtained in step (1) is obtained Ga after heat treatment 12h in air at 400 DEG C
2o
3hollow ball housing;
(3) by step 2) in the 20mgGa that obtains
2o
3the concentration that hollow ball joins 20mL noble metal platinum is in the platinum acid chloride solution of 0.8mg/mL, by dry for the water evaporation in solution at 90 DEG C, collects sample.By the sample that obtains in atmosphere of hydrogen at 230 DEG C heat treatment 3h, can Ga be obtained
2o
3/ Pt is nano-hollow sphere structured.
(4) Ga of 20mg will obtained in step 3)
2o
3it is in the D/W of 0.6M that/Pt nano-hollow ball joins 30mL concentration, and ultrasonic 20min is placed in water heating kettle, at 180 DEG C, react 6h, after being cooled to room temperature, centrifugal, cleaning and at 80 DEG C, dry 12h, can obtain Ga
2o
3/ Pt/C is nano-hollow sphere structured.
Claims (4)
1. metal oxide/Pt/C tri-layers of nanostructured hollow ball, it is characterized in that, the spherical shell of this hollow ball is from inside to outside followed successively by metal oxide layer, Pt stratum granulosum and amorphous carbon layer, metal oxide layer and Pt stratum granulosum form hetero-junctions, the thickness of metal oxide layer is 7 ~ 50 nanometers, in Pt stratum granulosum, the particle diameter of Pt particle is 5 ~ 8 nanometers, and the thickness of amorphous carbon layer is 10 ~ 15 nanometers, and the diameter of described hollow ball is 100 ~ 600 nanometers.
2. metal oxide/Pt/C according to claim 1 tri-layers of nanostructured hollow ball, it is characterized in that, described metal oxide is selected from the oxide of Al, B, Bi, Ba, Ca, Co, Cr, Ce, Cu, La, Ni, Fe, Zn, Sn, Rh, W, Nb, Ta, Ti, V, Hf, Mn, In, Li, Ge, Se, Zr, Mg, Ga or Si.
3. prepare the preparation method of metal oxide/Pt/C as claimed in claim 1 tri-layers of nanostructured hollow ball, it is characterized in that, comprise the steps:
1) adsorbent solution is configured: be dissolved in solvent by metal oxide salt, be configured to the metal oxide salting liquid that concentration of metal ions is 0.01 ~ 1M, described slaine is selected from the acetate of Al, B, Bi, Ba, Ca, Co, Cr, Ce, Cu, La, Ni, Fe, Zn, Sn, Rh, W, Ta, Ti, V, Hf, Mn, In, Li, Ge, Se, Zr, Mg, Ga, Si, chlorate, nitrate, sulfate or ester salt, and described solvent is deionized water, ethanol, formamide or ethylene glycol;
2) adsorbing metal ions: spherical template surface with carboxyl and hydroxyl immerses in the adsorbent solution of step 1), spherical template content is made to be 1g/L ~ 10g/L, ultrasonic spherical template is fully disperseed, centrifugal or suction filtration after stirring and adsorbing 4 ~ 48h, obtain the spherical template after absorption, be placed in 60 ~ 100 DEG C, dry 6 ~ 48h; Described spherical template is carbon ball, PS ball or SiO
2ball;
3) remove template: by step 2) in dried carbon ball or PS ball heat treatment 3 ~ 60h at 300 ~ 800 DEG C remove carbon ball template or PS ball template obtains metallic oxide hollow sphere; Or by step 2) in dried SiO
2ball is at 300 ~ 800 DEG C after heat treatment 3 ~ 60h, then at 60 ~ 100 DEG C, immerse concentration be keep 0.5 ~ 24h in the NaOH solution of 1 ~ 20M, removes SiO
2ball template obtains metallic oxide hollow sphere;
4) platinum grain is added: it is in the platinum acid chloride solution of 0.05 ~ 1mg/mL that the 10 ~ 100mg metallic oxide hollow sphere obtained in step 3) is joined 10 ~ 50mL platinum concentration, by dry for the water evaporation in solution at 60 ~ 100 DEG C, by the sample that obtains under atmosphere of hydrogen at 200 ~ 300 DEG C of heat treatment 2 ~ 6h, obtain metal oxide/Pt nano-hollow sphere structured;
5) agraphitic carbon is added: it is in the D/W of 0.1 ~ 1M that the metal oxide of the 10 ~ 60mg obtained in step 4)/Pt nano-hollow ball is joined 30 ~ 50mL concentration, ultrasonic 10 ~ 60min is placed in water heating kettle, 6 ~ 8h is reacted at 150 ~ 180 DEG C, after being cooled to room temperature, centrifugal, cleaning and at 60 ~ 100 DEG C, dry 6 ~ 48h, obtains metal oxide/Pt/C tri-layers of nanostructured hollow ball.
4. a purposes for metal oxide/Pt/C as claimed in claim 1 tri-layers of nanostructured hollow ball, it is characterized in that, this nano-hollow ball can be used for photocatalytic hydrogen production by water decomposition, light degradation, gas sensing, ultracapacitor or lithium ion battery.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109301222A (en) * | 2018-10-12 | 2019-02-01 | 台州学院 | A kind of NiO/Pt nanometer combined electrode material and preparation method thereof |
| CN110165201A (en) * | 2019-07-08 | 2019-08-23 | 广西师范大学 | A kind of preparation method of Si@Cu hollow core-shell composite material |
| CN110267909A (en) * | 2017-02-02 | 2019-09-20 | 本田技研工业株式会社 | Core shell |
| CN110743539A (en) * | 2019-09-29 | 2020-02-04 | 济南大学 | Method for preparing carbon platinum hollow spheres by using haematococcus pluvialis as reduction template agent |
| CN111036198A (en) * | 2018-10-12 | 2020-04-21 | 中国石油化工股份有限公司 | Double-shell core-shell structure metal catalyst and preparation method thereof |
| WO2021072638A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Mgo/au@aulno2 heterogeneous photocatalytic material and preparation method therefor |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110267909A (en) * | 2017-02-02 | 2019-09-20 | 本田技研工业株式会社 | Core shell |
| CN110267909B (en) * | 2017-02-02 | 2022-04-29 | 本田技研工业株式会社 | Core shell |
| CN109301222A (en) * | 2018-10-12 | 2019-02-01 | 台州学院 | A kind of NiO/Pt nanometer combined electrode material and preparation method thereof |
| CN111036198A (en) * | 2018-10-12 | 2020-04-21 | 中国石油化工股份有限公司 | Double-shell core-shell structure metal catalyst and preparation method thereof |
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| CN110165201A (en) * | 2019-07-08 | 2019-08-23 | 广西师范大学 | A kind of preparation method of Si@Cu hollow core-shell composite material |
| CN110743539A (en) * | 2019-09-29 | 2020-02-04 | 济南大学 | Method for preparing carbon platinum hollow spheres by using haematococcus pluvialis as reduction template agent |
| WO2021072638A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Mgo/au@aulno2 heterogeneous photocatalytic material and preparation method therefor |
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Application publication date: 20151118 |