CN1225898A - Nanometer indium oxide medium porosity assembling system and manufacturing method thereof - Google Patents
Nanometer indium oxide medium porosity assembling system and manufacturing method thereof Download PDFInfo
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- CN1225898A CN1225898A CN 99114003 CN99114003A CN1225898A CN 1225898 A CN1225898 A CN 1225898A CN 99114003 CN99114003 CN 99114003 CN 99114003 A CN99114003 A CN 99114003A CN 1225898 A CN1225898 A CN 1225898A
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- mesoporous
- medium porosity
- assembling system
- nanometer
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Abstract
The preparation method of nanometre indium oxide (In2O3) mesoporous assembly system uses the processes of soaking and thermal decomposition of indium sulfate to obtain the nanometre indium oxide (In2O3) mesoporous assembly system in which the particles of indium oxide (In2O3) are fine and small, uniform in particle size (diameter is about 2-8 nm), and highly-dispersed and distributed in the mesopores of the mesoporous solid and its composite content can be controlled. Said invention develops the new property of the In2O3 material, and said assembly system is different from In2O3 thin film in fluorescence which can be randomly regulated and controlled in a wide band from near ultraviolet to whole visible region, and possesses extensive application in the fields of microelectronic, photoelectric and sensing devices, etc..
Description
The present invention relates to nano indium oxide (In
2O
3) medium porosity assembling system and preparation method thereof.
Electrically conducting transparent broad stopband oxide semiconductor In
2O
3A kind of very important microelectronic material and gas sensitive.Because of its unique excellent photoelectric properties (on the one hand, because its forbidden band is wide transparent in whole visible region; On the other hand, have high conductivity mixing or exist in the situation of oxygen defect), recent two decades has obtained big quantity research, and is widely used in solar cell, liquid crystal display and alarm etc.But these application only limit to In
2O
3Thin-film material, and research mainly lays particular emphasis on method for manufacturing thin film and electric property.Under the room temperature, In pure, that satisfy stoichiometric proportion
2O
3Not luminous, although In in recent years
2O
3The accidental report of the fluorescence phenomenon of film, but In
2O
3The research of the characteristics of luminescence and use less.Be pointed out that In in the film
2O
3Particle size is bigger, and mutually reunites between particle.
Under study for action, we utilize the confinement effect in the hole of mesoporous solid, design and obtained In
2O
3Nanometer In in the hole that particle is tiny, size uniform, highly dispersed are distributed in mesoporous solid
2O
3Medium porosity assembling system, and observe this system and In occurred
2O
3The unexistent strong fluorescence phenomenon of film, namely along with the variation of heat-treat condition, fluorescence can be near ultraviolet to whole visible region broad frequency range in arbitrarily regulation and control.The discovery of this phenomenon will promote In greatly
2O
3The application of (particularly luminous) aspect optics.
The object of the invention provides nanometer In
2O
3Medium porosity assembling system and preparation method thereof.
The foregoing invention purpose is achieved in that mesoporous solid is soaked in indium sulfate solution, after treating fully to soak thoroughly, takes out mesoporous solid, carries out drying and annealing heat treatment, namely obtains In
2O
3The nanometer In that particle is tiny, size uniform, highly dispersed distribute
2O
3Medium porosity assembling system.
The present invention is described in detail in detail below: adopt sol-gel technology make mesoporous solid (also can be without sol-gel process, as long as the aperture of the mesoporous solid that makes 2～50nm can); It is soaked in the indium sulfate [In of 0.25mol/L
2(SO
4)
3] in the solution, soak a week (or longer time) under the room temperature after, take out mesoporous solid, 100-120 ℃ carry out drying after, through 450-1000 ℃ of different temperatures annealing, namely obtain In
2O
3The nanometer In that particle is tiny, size uniform, highly dispersed distribute
2O
3Medium porosity assembling system.
The used mesoporous solid of the present invention can be mesoporous SiO
2, TiO
2And the aperture is in the orderly template of 2～50nm.
The inventive method also can utilize other to contain oxygen indium salt [such as In (NO
3)
3] or alkali [In (OH)
3] replacement In
2(SO
4)
3Carry out thermal decomposition.
The inventive method, also available change In
2(SO
4)
3The method of the concentration of solution obtains the nanometer In of different composite amount
2O
3Medium porosity assembling system.Solution concentration is more high, and compound quantity is more big, otherwise compound quantity reduces.
Characteristics of the present invention are nanometer In
2O
3The preparation technology of medium porosity assembling system is simple, only needs the method with simple thermal decomposition, just can carry out under air atmosphere, normal pressure; Low to the experimental facilities requirement, only need common electric furnace, be convenient to generation in enormous quantities; The assembly system uniform particles of preparing, highly dispersed distribute.The present invention has developed In
2O
3The new capability of material, this system has broad application prospects in fields such as microelectronics, photoelectricity, Sensitive Apparatuses, for the preparation of other oxide semiconductor provide a kind of economical convenient, be worth the method used for reference, and lay a good foundation for the development of semiconductor Quantum Device, quantum dot light emitting device.
Embodiment 1. (1) silicon-dioxide (SiO
2) preparation of colloidal sol
In 1000 ml beakers, add 200 milliliters of ethyl orthosilicates and 214 milliliters of absolute ethyl alcohols, obtain the water white transparency supernatant liquid.Magnetic stirring apparatus stirs, and slowly add 380 ml deionized water (being tetraethoxy, dehydrated alcohol, deionized water three mol ratio about 1: 4: 15～24), solution begins to be shallow oyster white muddiness, continue to stir, and add a small amount of rare nitric acid and make catalyzer, regulating the pH value is 1.0, and solution is clear gradually.Amount of heat is emitted in this reaction, makes the walls of beaker heating.Continue to stir under the room temperature 2 hours, treat the solution cooling after, pack into small beaker or surface plate (the high about 7-8 millimeter of liquid level) seal for subsequent use with transparent adhesive tape.This clear solution is SiO
2Colloidal sol.(2) block mesoporous SiO
2The preparation of solid
The SiO of small beaker will pack into
2Colloidal sol is put into baking oven, and after 72 hours, colloidal sol solidifies through 60 ℃ of dryings, is the translucent wet gel of oyster white.Temperature is risen to 90 ℃, make gel aging, after 24 hours, the gel cracking.The transparent adhesive tape of sealing is opened an aperture, moisture is slowly emitted.Continue to keep 90 ℃ and wore out 72 hours, gel shrinks, and volume reduces.Be warming up to 100 ℃ of dryings after 24 hours, SiO in the beaker
2The a large amount of contraction.Through 120 ℃ of dryings several hours, promptly obtain the mesoporous SiO of water white transparency afterwards
2Block.Isothermal nitrogen absorption BET equation shows that its specific surface area is up to 780m
2/ g, porosity is about 50%, and bore dia mainly is distributed between the 2-8nm.(3) nanometer In
2O
3With the mesoporous SiO of block
2The preparation of assembly system: get In
2(SO
4)
312.94 gram dissolves in 100 ml deionized water, is made into the In that concentration is 0.25mol/L
2(SO
4)
3Solution.With the mesoporous SiO of block
2Be soaked in this In
2(SO
4)
3Solution, SiO
2Acutely emit a large amount of bubbles, and be cleaved into fritter.Take out SiO after the about week
2, (quick-drying purpose was to avoid In in the hole as far as possible through rapid draing in 100-120 ℃, 2～3 hours then
2(SO
4)
3The escape of particle and evaporation).With the mesoporous SiO of above-mentioned immersion by drying
2Carry out 450-1000 ℃ of annealing heat treatment, namely obtain In
2O
3Particle is tiny, and diameter is 2-8nm, size uniform, and highly dispersed is distributed in the mesoporous SiO of block
2Nanometer In among the solid pores
2O
3Medium porosity assembling system.
Description of drawings:
Fig. 1 be assembly system Electronic Speculum pattern with diffraction mutually.
Embodiment 2. (1) silica (SiO2) preparation of colloidal sol: with embodiment 1. (2) the mesoporous SiO of sheet2The preparation of solid:
The SiO of surface plate will pack into2Colloidal sol is put in people's baking oven, through 60 ℃ of dryings after 72 hours, Colloidal sol solidifies, and is the translucent wet gel of milky. Prick an aperture at transparent adhesive tape, use syringe Slowly add suitable deionized water to cover SiO to surface plate2Gel surface. Seal up aperture, baking The case temperature keeps 60 ℃. After one week, baking oven is slowly risen to 90 ℃, make gel aging, 48 After hour, the gel cracking. With the transparent adhesive tape thorn several apertures of pin in sealing, make wherein moisture Slowly emit. Continue to keep 90 ℃ and wore out 72 hours, it is little to be warming up to afterwards 100 ℃ of dryings 24 The time, finally by 120 ℃ of dryings several hours, namely obtain even thickness (about 2-3 millimeter), colourless The mesoporous SiO of bright sheet2Solid. The mesoporous SiO of this sheet2Solid is through 700 ℃ of annealing 1 hour, no Cracking. The mesoporous SiO of this sheet2Solid specific surface, porosity and pore-size distribution and massive phase are worked as. (3) nanometer In2O
3With the mesoporous SiO of sheet2The preparation of assembly system:
With embodiment 1, get In2(SO
4)
312.94 gram dissolves in 100 ml deionized water, is made into the In that concentration is 0.25mol/L2(SO
4)
3Solution. With the mesoporous SiO of sheet2Be soaked in this In2(SO
4)
3Solution, SiO2Sharply emit a large amount of bubbles, but do not ftracture. Take out SiO after the about week2, (quick-drying purpose was to avoid In in the hole as far as possible through rapid draing in 100-120 ℃, 2～3 hours then2(SO
4)
3The escape of particle and evaporation). With the mesoporous SiO of above-mentioned immersion by drying2Carry out 450-1000 ℃ of annealing heat treatment, namely obtain In2O
3Particle is tiny, and diameter is 2-8nm, size uniform, and highly dispersed is distributed in the mesoporous SiO of sheet2Nanometer In among the solid pores2O
3Mesoporous group The dress system.
Claims (6)
1. nano indium oxide (In
2O
3) preparation method of medium porosity assembling system, comprise the preparation of mesoporous solid, it is characterized in that, with soak, thermal decomposition indium sulfate [In
2(SO
4)
3] method, namely obtain nanometer In
2O
3Medium porosity assembling system.
2. the method for claim 1 is characterized in that, the preparation of mesoporous solid can be used sol-gel process, also can, but the aperture of the mesoporous solid that makes should at 2-50nm, be soaked in In with it again
2(SO
4)
3In the solution, soak under the room temperature more than the week, take out mesoporous solid, 100-120 ℃ carry out drying after, through 450-1000 ℃ of different temperatures annealing, obtain at last nanometer In again
2O
3Medium porosity assembling system.
3. method as claimed in claim 2 is characterized in that, as long as change In
2(SO
4)
3The concentration of solution just can obtain the assembly system of different composite amount, and solution concentration is more high, and compound quantity is more big, otherwise compound quantity is more little.
4. the method for claim 1 is characterized in that, also can utilize other to contain oxygen indium salt or alkali replacement In
2(SO
4)
3Carry out thermal decomposition.
5. the method for claim 1 is characterized in that, used mesoporous solid can be mesoporous SiO
2, TiO
2And the aperture is in the orderly template of 2～50nm.
6. the nanometer In of method as claimed in claim 1 preparation
2O
3Medium porosity assembling system is characterized in that, nanometer In
2O
3In in the medium porosity assembling system
2O
3Particle is tiny, size uniform diameter 2-8nm, highly dispersed are distributed in the hole of mesoporous solid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114003 CN1225898A (en) | 1999-01-04 | 1999-01-04 | Nanometer indium oxide medium porosity assembling system and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99114003 CN1225898A (en) | 1999-01-04 | 1999-01-04 | Nanometer indium oxide medium porosity assembling system and manufacturing method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1225898A true CN1225898A (en) | 1999-08-18 |
Family
ID=5277135
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 99114003 Pending CN1225898A (en) | 1999-01-04 | 1999-01-04 | Nanometer indium oxide medium porosity assembling system and manufacturing method thereof |
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| Country | Link |
|---|---|
| CN (1) | CN1225898A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2800300A1 (en) * | 1999-11-02 | 2001-05-04 | Rhodia Chimie Sa | MESOSTRUCTURE MATERIAL INCORPORATING NANOMETRIC PARTICLES |
| CN100422730C (en) * | 2005-11-14 | 2008-10-01 | 中国科学院合肥物质科学研究院 | Nano-structural ordered porous thin-film type gas sensor and method for preparing same |
-
1999
- 1999-01-04 CN CN 99114003 patent/CN1225898A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2800300A1 (en) * | 1999-11-02 | 2001-05-04 | Rhodia Chimie Sa | MESOSTRUCTURE MATERIAL INCORPORATING NANOMETRIC PARTICLES |
| WO2001032558A1 (en) * | 1999-11-02 | 2001-05-10 | Rhodia Chimie | Mesostructured material incorporating particles of nanometric dimensions |
| US6866925B1 (en) | 1999-11-02 | 2005-03-15 | Rhodia Chimie | Mesostructured material incorporating particles of nanometric dimensions |
| CN100422730C (en) * | 2005-11-14 | 2008-10-01 | 中国科学院合肥物质科学研究院 | Nano-structural ordered porous thin-film type gas sensor and method for preparing same |
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