CN106268846B - A kind of crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure hollow ball and preparation method thereof - Google Patents
A kind of crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure hollow ball and preparation method thereof Download PDFInfo
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- CN106268846B CN106268846B CN201510298469.2A CN201510298469A CN106268846B CN 106268846 B CN106268846 B CN 106268846B CN 201510298469 A CN201510298469 A CN 201510298469A CN 106268846 B CN106268846 B CN 106268846B
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- 239000013078 crystal Substances 0.000 title claims abstract description 43
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 18
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 8
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000001179 sorption measurement Methods 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 46
- 229910052799 carbon Inorganic materials 0.000 claims description 46
- 239000003463 adsorbent Substances 0.000 claims description 30
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 235000013842 nitrous oxide Nutrition 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 229910021592 Copper(II) chloride Inorganic materials 0.000 claims description 5
- 229910004537 TaCl5 Inorganic materials 0.000 claims description 5
- 239000004065 semiconductor Substances 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical group 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention discloses a kind of crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure hollow ball, spherical shell are amorphous Ta2O5, crystal Cu is distributed in spherical shell surface2O nano particles, crystal Cu2O nano particles and amorphous Ta2O5Form crystal/amorphous contact；The hollow ball of the present invention is prepared using template adsorption method.The hollow ball of the present invention is eliminated due to the contact of its unique crystal/amorphous in crystal/crystal hetero-junctions intrinsic crystal lattice mismatch and electronic mismatch so that the photo-generate electron-hole separative efficiency of nano heterojunction is close to 100%.The hollow ball large specific surface area of the present invention, heterojunction thickness is small, and preparation method is simple, cost is relatively low, is conducive to the application of industrialization.
Description
Technical field
The present invention relates to a kind of nano-heterogeneous structure hollow ball and preparation method thereof more particularly to a kind of crystal Cu2O/ is non-
Brilliant Ta2O5Nano-heterogeneous structure hollow ball and preparation method thereof.
Background technology
Along with the development of world civilization, the energy of human needs' consumption is more and more, and corresponding, the ring of discharge
Border pollutant is also more and more.Due to the resource of the earth be it is limited, thus energy and environment problem oneself must as contemporary development
The huge challenge that must be faced.In recent years, the severe situation increasingly to warm in face of traditional energy increasingly imbalance of supply and demand, global climate,
Countries in the world increase the dynamics of the development and utilization to new technology of energy and green technology one after another.Solar energy resources potentiality are big, ring
Low, sustainable use is polluted in border, is the important energy source for being conducive to harmony between man and nature development.And Photocatalitic Technique of Semiconductor is because of it
Can reaction directly be driven using solar energy, have important application prospect in the energy and environmental area.It is urged in semi-conducting material light
In change system, realize that efficiently separating for photo-generate electron-hole is in the necessary approach of energy and environmental problem by photocatalytic applications.
Common single compound photochemical catalyst is metal oxide or sulfide semiconductor material.Such as TiO2、WO3Deng,（Nowotny,
J., Energy & Environmental Science 2008, 1 (5), 565-572. Xi, G.; Ouyang, S.;
Li, P.; Ye, J.; Ma, Q.; Su, N.; Bai, H.; Wang, C., Angewandte Chemie
International Edition 2012, 51 (10), 2395-2399.）They all have very wide in photocatalysis field
General application.But they also have an intrinsic imperfect part, and single semi-conducting material is because of internal flaw and intrinsic compound
Reason so that photo-generate electron-hole after generation, has the photo-generate electron-hole close to 90% directly inside semiconductor and surface is matched
To compound rather than act on water and pollutant.Which results in the waste of most of photo-generate electron-hole, the days of one's doom
The utilization to solar energy is made.Therefore, promote the separation in light induced electron and hole, inhibit its compound, so as to improve quantum efficiency,
To make full use of solar energy, the stability for improving photochemical catalyst is the key problem of modern photocatalysis field.At present, semiconductor
Photochemical catalyst it is compound（Tong, H.; Ouyang, S.; Bi, Y.; Umezawa, N.; Oshikiri, M.; Ye,
J., Advanced Materials 2012, 24 (2), 229-251.）, particularly heterojunction material is by the extensive of people
Concern.Hetero-junctions is usually combined by two different semi-conducting materials by heteroepitaxial growth, and being generated because it is internal can
With the built in field that electron hole is promoted to detach, so there is unique physicochemical property on photo-generate electron-hole separation is promoted.
Due to nanometer size effect so that the diffusion length of electron hole greatly reduces, so the heterojunction semiconductor of nanoscale compares phase
The bulk semiconductor hetero-junctions answered has more obvious photoelectric properties advantage.Prepare and study Nano semiconductor hetero-junctions material
Material, explores its application, is one of research frontier of international nano material in recent years, has very big challenge and important
Scientific meaning.
However modern nano heterojunction is compound still extremely serious, is by having the not isomorphous this is mainly due to hetero-junctions
What two kinds of materials of body structure were formed, the interface of two kinds of materials certainly exists lattice mismatch and electronic mismatch, these mismatch meetings
Cause photo-generated carrier in the violent compound of heterojunction interface and then reduce the photocatalysis efficiency of nano heterojunction.
Invention content
The purpose of the present invention is to provide a kind of high crystal Cu of photo-generate electron-hole separative efficiency2O/ amorphous Ta2O5Nanometer
Heterojunction structure hollow ball and preparation method thereof eliminates the interface mismatch and electricity of hetero-junctions to realize using crystal/amorphous contact
Sub- mismatch.
The crystal Cu of the present invention2O/ amorphous Ta2O5Nano-heterogeneous structure hollow ball, spherical shell are amorphous Ta2O5, spherical shell surface
Crystal Cu is distributed with2O nano particles, crystal Cu2O nano particles and amorphous Ta2O5Form crystal/amorphous contact.
The amorphous Ta2O5Shell thickness is usually 5~20 nanometers.
The crystal Cu2The size of O nano particles is usually 2~20 nanometers.
Prepare above-mentioned crystal Cu2O/ amorphous Ta2O5The method of nano-heterogeneous structure hollow ball, includes the following steps：
1）Ta adsorbent solutions are configured：By TaCl5It is dissolved in anhydrous ethanol solvent, being configured to Ta ion molar concentrations is
The adsorbent solution A of 0.001~10M；
2）Absorption：There is the carbon ball template of carboxyl and hydroxyl to immerse in adsorbent solution A surface, carbon ball template consumption is
1g/L ~ 100g/L, ultrasound is fully dispersed to carbon ball template, and the carbon after isolating absorption is centrifuged or filtered after 2 ~ 48h of stirring and adsorbing
Ball template, in 40~100 DEG C of dry 2~48h；
3）Cu adsorbent solutions are configured：By CuCl2It is dissolved in anhydrous ethanol solvent, being configured to Cu ion molar concentrations is
The adsorbent solution B of 0.001~10M；
4）Second adsorption:By step 2）Carbon ball that treated is immersed in adsorbent solution B, and it is 1g/L ~ 100g/ to make its content
L, ultrasound is fully dispersed to carbon ball, centrifuges or filters after 2 ~ 48h of stirring and adsorbing and isolates the carbon ball after second adsorption, 40~
100 DEG C of dry 2~48h；
5）Removing template：By step 4）Carbon ball that treated handles 3~60h removal carbon ball templates at 300~450 DEG C, obtains
Obtain crystal CuO/ amorphous Ta2O5Nano-heterogeneous structure hollow ball；
6）Reduction：By step 5）Hollow ball obtained hydrogen annealing 2~20 hours, hydrogen flowing quantity at 100~200 DEG C are
100-200sccm, then 2~20h of laughing gas annealing at 100~200 DEG C, laughing gas flow are 5-55sccm, obtain crystal Cu2O/
Amorphous Ta2O5Nano-heterogeneous structure hollow ball.
In the present invention, the preparation method that the surface has the carbon ball template of carboxyl and hydroxyl can refer to Sun, X.;
Li, Y., Angewandte Chemie International Edition 2004,43 (29), 3827-3831。
The beneficial effects of the present invention are：The crystal Cu of the present invention2O/ amorphous Ta2O5Nano-heterogeneous structure hollow ball, due to
Its unique crystal/amorphous contact, eliminates in crystal/crystal hetero-junctions intrinsic crystal lattice mismatch and electronic mismatch, makes
Nano heterojunction photo-generate electron-hole separative efficiency close to 100%.The hollow ball large specific surface area of the present invention, hetero-junctions are thick
Spend small, preparation method is simple, cost is relatively low, is conducive to the application of industrialization.
Description of the drawings
Fig. 1 is crystal Cu2O/ amorphous Ta2O5The XRD diffraction pictures of nano-heterogeneous structure hollow ball.
Fig. 2 is crystal Cu2O/ amorphous Ta2O5The transmission picture of nano-heterogeneous structure hollow ball.
Fig. 3 is crystal Cu2O/ amorphous Ta2O5The high-resolution transmission picture of nano-heterogeneous structure hollow ball.
Fig. 4 is crystal Cu2O/ amorphous Ta2O5The visible ray of nano-heterogeneous structure hollow ball half an hour decomposes water performance map entirely.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples.
Embodiment 1
1）Ta adsorbent solutions are configured：By TaCl5It is dissolved in anhydrous ethanol solvent, being configured to Ta ion molar concentrations is
The adsorbent solution A of 0.01M；
2）Absorption：There is the carbon ball template of carboxyl and hydroxyl to immerse in adsorbent solution A surface, carbon ball template consumption is
10g/L, ultrasound is fully dispersed to carbon ball template, and stirring and adsorbing centrifuges or filter afterwards for 24 hours the carbon ball template after isolating absorption,
80 DEG C of dryings are for 24 hours；
3）Cu adsorbent solutions are configured：By CuCl2It is dissolved in anhydrous ethanol solvent, being configured to Cu ion molar concentrations is
The adsorbent solution B of 0.01M；
4）Second adsorption:By step 2）Carbon ball that treated is immersed in adsorbent solution B, makes its content for 10g/L, ultrasound
Fully dispersed to carbon ball, stirring and adsorbing, which is centrifuged or filtered afterwards for 24 hours, isolates the carbon ball after second adsorption, in 80 DEG C of dryings for 24 hours；
5）Removing template：By step 4）Carbon ball that treated handles 30h removal carbon ball templates at 400 DEG C, obtains crystal
CuO/ amorphous Ta2O5Nano-heterogeneous structure hollow ball；
6）Reduction：By step 5）Hollow ball obtained hydrogen annealing 10 hours at 150 DEG C, hydrogen flowing quantity 150sccm,
Then the laughing gas annealing 10h at 150 DEG C, laughing gas flow are 30sccm, obtain crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure is empty
Bulbus cordis.
Crystal Cu made from this example2O/ amorphous Ta2O5The XRD diffraction picture of nano-heterogeneous structure hollow ball as shown in Figure 1,
Transmission picture and high-resolution transmission the picture difference of its spherical shell are as shown in Figures 2 and 3, it can be seen that amorphous Ta in the hollow ball2O5
The thickness of spherical shell is dispersed with crystal Cu in 5-20nm thereon2O nano particles, size 2-20nm；It is empty made from this example
The visible ray of bulbus cordis decomposes the performance map of water entirely as shown in figure 4, it has very high photo-generate electron-hole separative efficiency.
Embodiment 2
1）Ta adsorbent solutions are configured：By TaCl5It is dissolved in anhydrous ethanol solvent, being configured to Ta ion molar concentrations is
The adsorbent solution A of 0.001M；
2）Absorption：There is the carbon ball template of carboxyl and hydroxyl to immerse in adsorbent solution A surface, carbon ball template consumption is
1g/L, ultrasound is fully dispersed to carbon ball template, is centrifuged after stirring and adsorbing 2h or filters the carbon ball template after isolating absorption, 40
DEG C dry 48h；
3）Cu adsorbent solutions are configured：By CuCl2It is dissolved in anhydrous ethanol solvent, being configured to Cu ion molar concentrations is
The adsorbent solution B of 0.001M；
4）Second adsorption:By step 2）Carbon ball that treated is immersed in adsorbent solution B, makes its content for 100g/L, ultrasound
It is fully dispersed to carbon ball, it centrifuges or filters after stirring and adsorbing 48h and isolate the carbon ball after second adsorption, in 40 DEG C of dry 48h；
5）Removing template：By step 4）Carbon ball that treated handles 3h removal carbon ball templates at 450 DEG C, obtains crystal CuO/
Amorphous Ta2O5Nano-heterogeneous structure hollow ball；
6）Reduction：By step 5）Hollow ball obtained hydrogen annealing 2 hours at 200 DEG C, hydrogen flowing quantity 200sccm,
Then the laughing gas annealing 20h at 100 DEG C, laughing gas flow are 5sccm, obtain crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure is empty
Bulbus cordis.
Embodiment 3
1）Ta adsorbent solutions are configured：By TaCl5It is dissolved in anhydrous ethanol solvent, is configured to Ta ions molar concentration as 10M
Adsorbent solution A；
2）Absorption：There is the carbon ball template of carboxyl and hydroxyl to immerse in adsorbent solution A surface, carbon ball template consumption is
100g/L, ultrasound is fully dispersed to carbon ball template, and the carbon ball template after isolating absorption is centrifuged or filtered after stirring and adsorbing 48h,
In 100 DEG C of dry 2h；
3）Cu adsorbent solutions are configured：By CuCl2It is dissolved in anhydrous ethanol solvent, is configured to Cu ions molar concentration as 10M
Adsorbent solution B；
4）Second adsorption:By step 2）Carbon ball that treated is immersed in adsorbent solution B, and making its content, ultrasound is extremely for 1g/L
Carbon ball is fully dispersed, centrifuges or filters after stirring and adsorbing 2h and isolate the carbon ball after second adsorption, in 100 DEG C of dry 2h；
5）Removing template：By step 4）Carbon ball that treated handles 60h removal carbon ball templates at 300 DEG C, obtains crystal
CuO/ amorphous Ta2O5Nano-heterogeneous structure hollow ball；
6）Reduction：By step 5）Hollow ball obtained hydrogen annealing 20 hours at 100 DEG C, hydrogen flowing quantity 100sccm,
Then the laughing gas annealing 2h at 200 DEG C, laughing gas flow are 55sccm, obtain crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure is empty
Bulbus cordis.
Claims (2)
1. a kind of crystal Cu2O/ amorphous Ta2O5Nano-heterogeneous structure hollow ball, it is characterised in that the spherical shell of the hollow ball is non-
Brilliant Ta2O5, crystal Cu is distributed in spherical shell surface2O nano particles, crystal Cu2O nano particles and amorphous Ta2O5Form crystal/amorphous
Contact；The amorphous Ta2O5Shell thickness is 5~20 nanometers, crystal Cu2The size of O nano particles is 2~20 nanometers.
2. prepare crystal Cu as described in claim 12O/ amorphous Ta2O5The method of nano-heterogeneous structure hollow ball, feature exist
In including the following steps：
1）Ta adsorbent solutions are configured：By TaCl5Be dissolved in anhydrous ethanol solvent, be configured to Ta ions molar concentration for 0.001~
The adsorbent solution A of 10M；
2）Absorption：The carbon ball template that surface has carboxyl and hydroxyl is immersed in adsorbent solution A, carbon ball template consumption for 1g/L ~
100g/L, ultrasound is fully dispersed to carbon ball template, and the carbon ball mould after isolating absorption is centrifuged or filtered after 2 ~ 48h of stirring and adsorbing
Plate, in 40~100 DEG C of dry 2~48h；
3）Cu adsorbent solutions are configured：By CuCl2Be dissolved in anhydrous ethanol solvent, be configured to Cu ions molar concentration for 0.001~
The adsorbent solution B of 10M；
4）Second adsorption:By step 2）Carbon ball that treated is immersed in adsorbent solution B, its content is made to surpass for 1g/L ~ 100g/L
Sound is fully dispersed to carbon ball, centrifuges or filters after 2 ~ 48h of stirring and adsorbing and isolate the carbon ball after second adsorption, at 40~100 DEG C
Dry 2~48h；
5）Removing template：By step 4）Carbon ball that treated handles 3~60h removal carbon ball templates at 300~450 DEG C, obtains brilliant
Body CuO/ amorphous Ta2O5Nano-heterogeneous structure hollow ball；
6）Reduction：By step 5）Hollow ball obtained hydrogen annealing 2~20 hours at 100~200 DEG C, hydrogen flowing quantity 100-
200sccm, then 2~20h of laughing gas annealing at 100~200 DEG C, laughing gas flow are 5-55sccm, obtain crystal Cu2O/ amorphous
Ta2O5Nano-heterogeneous structure hollow ball.
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