CN107162441B - A kind of glass and preparation method thereof of doped ITO nanoparticle - Google Patents
A kind of glass and preparation method thereof of doped ITO nanoparticle Download PDFInfo
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- CN107162441B CN107162441B CN201710295438.0A CN201710295438A CN107162441B CN 107162441 B CN107162441 B CN 107162441B CN 201710295438 A CN201710295438 A CN 201710295438A CN 107162441 B CN107162441 B CN 107162441B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
Abstract
The invention discloses a kind of glass and preparation method thereof of doped ITO nanoparticle, using being evenly distributed with nanometer level microporous cellular glass, prepare ITO nanoparticle in situ in micropore, the size of particle can effectively be limited, and makes ITO nanoparticle in glass there is preferable dispersibility, its simple process, preparation are convenient, after high temperature sintering, cellular glass duct closure, the intensity of glass greatly improves, it is evenly dispersed in glass to have ITO nanoparticle, the shortwave luminescent properties of glass can be made to significantly improve.ITO nanoparticle is uniformly distributed in glass matrix by the present invention, in conjunction with the high chemical stability of silica glass, it can preferably play the characteristics such as the distinctive non-linear, plasma characteristics of ITO itself and defect luminescence and be applied to the fields such as nonlinear optics, fluorescence enhancement, surface plasma sensing, photocatalysis, fiber optic communication.
Description
Technical field
The invention belongs to the preparation fields of glass, more specifically to a kind of doped ITO (tin indium oxide) nanoparticle
Glass and preparation method thereof.
Background technique
The composite material that doped semiconductor oxide nano-particles obtain can realize exciton emission at room temperature, generate close purple
Outer shortwave shines, and has the effects such as piezoelectricity, photoelectricity, can be used for the development of the devices such as light source, detector, optical waveguide.In addition, half
The composite material that conducting oxide and rare earth ion are co-doped with can realize energy transmission etc., promote shining for rare earth ion, this is in light
The communications field has great significance.The composite material that certain doped semiconductor oxide nano-particles obtain also has catalytic
Can, it means a great in photocatalysis field.The compound of certain doped semiconductor oxide nano-particles is in terms of gas sensing
There is important application.
Currently, preparing the equally distributed main preparation method of conductor oxidate nanoparticle in glass matrix has:
Fusion method, sol-gal process etc., these techniques are relatively mature.But but there is shortcomings for these methods, such as:
Melting method needs to melt at high temperature after mixing conductor oxidate and frit, since glass system viscosity is big,
Realize that conductor oxidate nanoparticle is evenly dispersed relatively difficult in glass matrix；And sol-gal process is preparing glass
The salting liquid containing semiconductor is mixed with glass melten gel simultaneously, doped semiconductor oxidate nano can be obtained by post-processing
Particle glass, the dispersed phase of conductor oxidate nanoparticle is to more uniform, but this preparation method, complex process, production
Period is compared with long, pollution is big, and the intensity of glass is relatively low, and the requirement of practical application is not achieved.
ITO (tin indium oxide) is a kind of N-type semiconductor of height degeneracy, its two-dimensional film material is saturating with high visible light
It crosses rate and infrared reflection rate, excellent electric conductivity and preferable etching performance and is widely used in liquid crystal display, solar energy
The fields such as battery, transparent electrode, anti-reflective film, the preparation method of the ITO (tin indium oxide) of film-form be mainly magnetron sputtering and
Spin-coating method, but the ITO of film-form (tin indium oxide) can not play its research and application value completely.
In recent years, the non-linear of ITO (tin indium oxide), plasma characteristics and its defect luminescence, many researchers are based on
Research emphasis is transferred to ITO (tin indium oxide) nanoparticle.And the preparation of ITO (tin indium oxide) nanoparticle of the prior art
Method includes mechanical mixing, sol-gal process, spray heating decomposition, coprecipitation, hydrothermal synthesis method etc..Wherein mechanical mixture
It is easily mixed into more impurity during method preparation, and the production cycle is longer；The sol-gal process period is long, the agglutinating property of particle is poor, holds
It is easy to reunite；Spray heating decomposition condition is difficult to control, reaction process is complicated, the high requirements on the equipment；Precipitating reagent in coprecipitation
Addition may generate local concentration it is excessively high and cause reunite and not enough uniformly；Hydrothermal synthesis method is needed in the anti-of good seal
It answers in kettle and carries out, non-visuality.In addition, using these methods by ITO nanoparticle evenly spread in glass matrix can be real
Existing property is poor.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of doped ITOs (tin indium oxide) to receive
Glass of rice corpuscles and preparation method thereof, the ITO nanoparticle prepared are evenly distributed, and simple process, preparation are conveniently,
Thus solve prior art doped semiconductor oxide nano-particles method for glass preparation realizability it is poor, cannot really by
Conductor oxidate nanoparticle doped enters in glass matrix；Conductor oxidate nanoparticle disperses unevenly in glass,
Or pollution is big, complex process, the technical problem that the production cycle is longer, strength of glass is more low.
To achieve the above object, according to one aspect of the present invention, a kind of glass of doped ITO nanoparticle is provided
Preparation method includes the following steps:
(1) indium salts and pink salt are soluble in water, prepare the mixed solution containing indium ion and tin ion；
(2) cellular glass is placed in the mixed solution containing indium ion and tin ion and is at least impregnated 24 hours, obtained
Cellular glass after to immersion；
(3) cellular glass after the immersion is placed in air atmosphere and is sintered, doped ITO nanoparticle is prepared
Glass.
Preferably, indium ion concentration range is 0.1mol/L~2.5mol/L, tin ion in step (1) described mixed solution
Concentration range is 0.01~0.25mol/L, and the indium ion concentration is 9~10 times of the tin ion concentration.
Preferably, step (1) indium salts are four water indium trichlorides, and the pink salt is stannic chloride pentahydrate.
Preferably, the cellular glass is silica glass, and the inside glass is evenly distributed with nanometer micropore, individually
The pore size of the micropore is 5~50 nanometers, in the cellular glass volume of micropore account for cellular glass total volume 30~
35%.
Preferably, step (2) soaking process carries out ultrasonic vibration simultaneously.
Preferably, step (3) sintering uses following sintering procedure:
(1) 550~650 DEG C are warming up to the heating rate of 0.5~1.5 DEG C/min, then keep the temperature 2~4h；
(2) 700~800 DEG C are warming up to the heating rate of 0.5~1.5 DEG C/min again, then keep the temperature 1~3h；
(3) 900~1000 DEG C are warming up to the heating rate of 0.5~1.0 DEG C/min again, then keep the temperature 0.5~1h；
(4) 1150~1200 DEG C are warming up to the heating rate of 1.5~2.5 DEG C/min again, then keep the temperature 1~3h；
(5) last furnace cooling is to room temperature.
Preferably, step (3) the sintering specific steps are as follows:
(1) 600 DEG C are warming up to the heating rate of 1 DEG C/min, then keep the temperature 3h；
(2) 700 DEG C are warming up to the heating rate of 1 DEG C/min again, then keep the temperature 1h；
(3) 950 DEG C are warming up to the heating rate of 0.8 DEG C/min again, then keep the temperature 0.5h；
(4) 1150 DEG C are warming up to the heating rate of 2.2 DEG C/min again, then keep the temperature 1h；
(5) last furnace cooling is to room temperature.
Other side according to the invention provides a kind of glass of doped ITO nanoparticle, according to the system
Preparation Method is prepared.
Preferably, doped with ITO nanoparticle in the glass, the size of the ITO nanoparticle is 5~30nm.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect.
The preparation method of the glass of doped ITO (tin indium oxide) nanoparticle of the invention, using being evenly distributed with nanometer
The cellular glass of grade micropore, it is in situ in micropore by the ultrasonic vibration and soaking time and high temperature sintering program especially groped
ITO (tin indium oxide) nanoparticle is prepared, can effectively limit the size of particle, and makes ITO (tin indium oxide) nanoparticle
Son has preferable dispersibility in glass, and simple process, preparation are convenient, after 1150 DEG C of high temperature sinterings, cellular glass duct
Closure, the intensity of glass greatly improves, evenly dispersed in glass to have ITO nanoparticle, can make the shortwave luminescent properties of glass
It significantly improves.
ITO nanoparticle is uniformly distributed in glass matrix by the present invention for the first time, in conjunction with the height chemistry of silica glass
Stability can preferably play the characteristics such as the distinctive non-linear, plasma characteristics of ITO itself and defect luminescence and be applied to
The fields such as nonlinear optics, fluorescence enhancement, surface plasma sensing, photocatalysis, fiber optic communication are also other semiconductor dopings
Provide a kind of new thinking.
Detailed description of the invention
Fig. 1 is the SEM picture of cellular glass of the present invention；
Fig. 2 is the XRD test map of sample prepared by the embodiment of the present invention 1；
Fig. 3 is the TEM (Transmission Electron Microscope) for the sample that the embodiment of the present invention 1 obtains
Picture；
Fig. 4 is fluorescence spectra of the sample prepared by the embodiment of the present invention 1 under the excitation of 325nm laser.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
A kind of preparation method of the glass of doped ITO (tin indium oxide) nanoparticle provided by the invention, including following steps
It is rapid:
(1) indium salts and pink salt are soluble in water, prepare the mixed solution containing indium ion and tin ion；
(2) cellular glass is placed in the mixed solution containing indium ion and tin ion and is at least impregnated 24 hours, and
Carry out ultrasonic vibration simultaneously, it is prolonged impregnate and ultrasonic vibration so that ion in solution well into cellular glass hole
Cellular glass in road, after being impregnated；
(3) cellular glass after the immersion is placed in air atmosphere and is sintered, prepare the glass of the nanoparticle containing ITO
Glass.
The step of step (1) preparation is containing a certain proportion of mixed solution containing indium ion and tin ion are as follows: weigh one
Determine the compound containing indium ion of quality and the compound containing tin ion of corrresponding quality, making indium ion concentration is tin ion concentration
9~10 times, above two compound is dissolved in solvent, is configured to indium ion concentration range in 0.1mol/L~2.5mol/
L, for tin ion concentration range in the solution containing indium ion, tin ion of 0.01~0.25mol/L, the indium ion compound is four
Water indium trichloride, the tin ion compound are stannic chloride pentahydrate, and the solvent is water.
In the preparation method of the glass of doped ITO of the present invention (tin indium oxide) nanoparticle, the immersion step
Suddenly are as follows: cellular glass is placed in the mixed solution containing a certain proportion of indium ion and tin ion and is impregnated, and simultaneously into
Row ultrasonic vibration is impregnated and sonic oscillation 1~3 day with promoting infiltration and diffusion of the mixed solution in glass microporous, containing indium from
Then the mixed solution of son and tin ion dries in the air cellular glass taking-up naturally vertically well into the micropore to cellular glass
It is dry.
Here ultrasonic vibration, which refers to, to be placed in appearance immersed with the mixed solution containing indium ion and tin ion of cellular glass
In device, and the container is placed in the ultrasonic device of such as ultrasonic cleaner and carries out ultrasonic vibration, mixed solution is promoted to enter
In glass microporous.Cellular glass is soaked in the time in mixed solution not shorter than 24 hours by the present invention, just can guarantee that mixing is molten
Liquid is by gradually penetrating into the micropore of cellular glass.
The high temperature sintering described in the preparation method of the glass of doped ITO of the present invention (tin indium oxide) nanoparticle
Program is (sintering atmosphere is air):
(1) 550~650 DEG C are warming up to the heating rate of 0.5~1.5 DEG C/min, then keep the temperature 2~4h；
(2) 700~800 DEG C are warming up to the heating rate of 0.5~1.5 DEG C/min again, then keep the temperature 1~3h；
(3) 900~1000 DEG C are warming up to the heating rate of 0.5~1.0 DEG C/min again, then keep the temperature 0.5~1h；
(4) 1150~1200 DEG C are warming up to the heating rate of 1.5~2.5 DEG C/min again, then keep the temperature 1~3h；
(5) last furnace cooling is to room temperature.
By this high-temperature sintering process, the duct in cellular glass is closed, and nanoparticle is wrapped in the duct of closure.
Sintering procedure is preferably (sintering atmosphere is air):
(1) 600 DEG C are warming up to the heating rate of 1 DEG C/min, then keep the temperature 3h；
(2) 700 DEG C are warming up to the heating rate of 1 DEG C/min again, then keep the temperature 1h；
(3) 950 DEG C are warming up to the heating rate of 0.8 DEG C/min again, then keep the temperature 0.5h；
(4) 1150 DEG C are warming up to the heating rate of 2.2 DEG C/min again, then keep the temperature 1h；
(5) last furnace cooling is to room temperature.
In the preparation method of the glass of doped ITO of the present invention (tin indium oxide) nanoparticle, the porous
Micropore is evenly distributed in glass, the pore size of single micropore is 5~50 nanometers, and the volume of micropore accounts for porous in cellular glass
The 30~35% of glass total volume.
The cellular glass is that the raw material by receiving containing silica, boron oxide, oxidation is shaped by high-temperature fusion, chilling, cut
Piece polishing, split-phase, acid processing are made, and wherein the quality of silica accounts for 70% or so of glass gross weight, after peracid treatment,
Sodium boron mutually disappears in glass, leaves behind silica, and the sodium boron phase to disappear then forms in glass 30~35% nano pore.
Pass through high temperature sintering in the preparation method of the glass of doped ITO of the present invention (tin indium oxide) nanoparticle
Later, indium ion and tin ion fabricated in situ ITO (tin indium oxide) are present in the microchannel of cellular glass closure, so that porous
The duct of glass is closed.
High temperature sintering program of the invention is to find out to come on the basis of many experiments, and sintering heating should not be too fast,
Otherwise the crystal characteristic peak of ITO cannot be detected.The four water indium trichloride meeting between 30-200 DEG C of indium salts used due to the present invention
Slow dehydration becomes the indium trichloride containing only a crystallization water, and the removing of the last one crystallization water then needs 300 DEG C or more
Temperature, indium oxide can be generated by continuing heating in air.And stannic chloride pentahydrate is dissolved in water and generates stannic acid, stannic acid passes through in air
Tin oxide can be generated by crossing 400~600 DEG C of high-temperature calcination.The process that oxide is hydrolyzed and generated in conjunction with the two, has selected this hair
Bright above-mentioned sintering procedure, only can be final especially under preferred sintering procedure by above-mentioned sintering procedure
The crystal peak of tin indium oxide nanoparticle is detected in cellular glass matrix.Here the slow heating-up time of cold stage be for
Guarantee that four water indium trichlorides and stannic chloride pentahydrate sufficiently generate its corresponding oxide, and tin ion is allowed to be dissolved into oxidation
Form oxide ITO in the lattice of indium, the temperature-rise period and soak process of hot stage are to allow the hole of cellular glass
Road is slowly closed, to form the high-intensitive silica glass containing ITO nanoparticle.
The following are embodiments:
Embodiment 1
Under room temperature environment, four water indium trichlorides and stannic chloride pentahydrate are dissolved in deionized water, compound concentration is
The indium trichloride of 0.48mol/L and the tin tetrachloride solution 10ml of 0.05mol/L, solution are placed in sample bottle, by porous
Glass, which is put into, impregnates and is placed in ultrasonic cleaner progress ultrasonic vibration for 24 hours in indium tin mixed solution, wherein distribution in cellular glass
Have micropore, the thickness of the cellular glass is about 1mm so that the mixed solution containing indium ion and tin ion well into arrive porous
In the micropore of glass, cellular glass is then taken out into vertical naturally dry.Then high temperature burning is carried out to the cellular glass after immersion
Knot, specific sintering procedure are (sintering atmosphere is air):
(1) 600 DEG C are warming up to the heating rate of 1 DEG C/min, then keep the temperature 3h；
(2) 700 DEG C are warming up to the heating rate of 1 DEG C/min again, then keep the temperature 1h；
(3) 950 DEG C are warming up to the heating rate of 0.8 DEG C/min again, then keep the temperature 0.5h；
(4) 1150 DEG C are warming up to the heating rate of 2.2 DEG C/min again, then keep the temperature 1h；
(5) last furnace cooling is to room temperature.
Take out the glass of as doped ITO (tin indium oxide) nanoparticle.
SEM (scanning electron microscope) picture of cellular glass used is given as shown in Figure 1.From
Fig. 1 can be seen that the aperture of cellular glass used in 5~50nm, and be uniformly distributed, which ensure that subsequent
Doped ITO nanoparticle is uniformly distributed in glass, in cellular glass the volume of micropore account for cellular glass total volume 30~
35%.
It is given as shown in Figure 2 according to the obtained sample of the present embodiment (solid line in figure) and blank undoped with glass (figure
Middle dotted line) XRD (X-ray Diffraction, X-ray diffraction, the mainly composition of reference standard spectrum analysis nanoparticle)
Test result, for the spectrum shape of made sample, several characteristic peaks (222) of ITO in X-ray diffraction peak and document report
(400) (440) (622) meet, and characteristic peak is obvious, illustrate containing ITO nanoparticle in the glass prepared, and scheme
Dot-dashed line is the XRD spectrum of undoped glass as blank reference.
TEM (the Transmission Electron according to the obtained sample of the present embodiment is given as shown in Figure 3
Microscope) picture, it can be seen that ITO nanoparticle is uniformly distributed in glass matrix, and 5~30nm of particle size is differed,
This is consistent with the pore size of script in glass.
It gives as shown in Figure 4 according to the obtained sample of the present embodiment (solid line) and blank undoped with glass (pecked line)
Fluorescence spectra under the excitation of 325nm laser, figure 4, it is seen that the shortwave of the glass doped with ITO nanoparticle
Luminescent properties are significantly improved relative to undoped glass.
Embodiment 2
Under room temperature environment, four water indium trichlorides and stannic chloride pentahydrate are dissolved in deionized water, configuration concentration is
The indium trichloride of 0.96mol/L and the tin tetrachloride solution 10ml of 0.1mol/L, solution are placed in sample bottle, by cellular glass
It is put into immersion and ultrasonic vibration 36h in indium tin mixed solution, so that the mixed solution containing indium salts and pink salt is porous well into arriving
In the micropore of glass, cellular glass is then taken out into vertical naturally dry.Then high temperature is carried out to the cellular glass after immersion
Sintering, specific sintering procedure are (sintering atmosphere is air):
(1) 600 DEG C are warming up to the heating rate of 1 DEG C/min, then keep the temperature 3h；
(2) 700 DEG C are warming up to the heating rate of 1 DEG C/min again, then keep the temperature 1h；
(3) 950 DEG C are warming up to the heating rate of 0.8 DEG C/min again, then keep the temperature 0.5h；
(4) 1150 DEG C are warming up to the heating rate of 2.2 DEG C/min again, then keep the temperature 1h；
(5) last furnace cooling is to room temperature.
Take out the glass of as doped ITO (tin indium oxide) nanoparticle, the doped ITO prepared (tin indium oxide) nanometer
The glass of particle is evenly distributed with ITO nanoparticle, X-ray diffraction peak and document report in the micropore that cellular glass is closed
Several characteristic peaks (222) (400) (440) (622) of middle ITO meet.
Embodiment 3
Under room temperature environment, four water indium trichlorides and stannic chloride pentahydrate are dissolved in deionized water, configuration concentration is
The indium trichloride of 1.44mol/L and the tin tetrachloride solution 10ml of 0.14mol/L, solution are placed in sample bottle, by porous
Glass is put into immersion and ultrasonic vibration 48h in indium tin mixed solution, so that the mixed solution containing indium salts and pink salt is more well into arriving
In the micropore of hole glass, cellular glass is then taken out into vertical naturally dry.Then to the cellular glass after immersion in air
Middle carry out high temperature sintering, specific sintering procedure are (sintering atmosphere is air):
(1) 600 DEG C are warming up to the heating rate of 1 DEG C/min, then keep the temperature 3h；
(2) 700 DEG C are warming up to the heating rate of 1 DEG C/min again, then keep the temperature 1h；
(3) 950 DEG C are warming up to the heating rate of 0.8 DEG C/min again, then keep the temperature 0.5h；
(4) 1150 DEG C are warming up to the heating rate of 2.2 DEG C/min again, then keep the temperature 1h；
(5) last furnace cooling is to room temperature.
Take out the glass of as doped ITO (tin indium oxide) nanoparticle, the doped ITO prepared (tin indium oxide) nanometer
The glass of particle is evenly distributed with ITO nanoparticle, X-ray diffraction peak and document report in the micropore that cellular glass is closed
Several characteristic peaks (222) (400) (440) (622) of middle ITO meet
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of the glass of doped ITO nanoparticle, which comprises the steps of:
(1) indium salts and pink salt are soluble in water, prepare the mixed solution containing indium ion and tin ion；
(2) cellular glass is placed in the mixed solution containing indium ion and tin ion and is at least impregnated 24 hours, soaked
Cellular glass after bubble；
(3) cellular glass after the immersion is placed in air atmosphere and is sintered, the glass of doped ITO nanoparticle is prepared
Glass；
Step (3) sintering uses following sintering procedure:
(1) 550~650 DEG C are warming up to the heating rate of 0.5~1.5 DEG C/min, then keep the temperature 2~4h；
(2) 700~800 DEG C are warming up to the heating rate of 0.5~1.5 DEG C/min again, then keep the temperature 1~3h；
(3) 900~1000 DEG C are warming up to the heating rate of 0.5~1.0 DEG C/min again, then keep the temperature 0.5~1h；
(4) 1150~1200 DEG C are warming up to the heating rate of 1.5~2.5 DEG C/min again, then keep the temperature 1~3h；
(5) last furnace cooling is to room temperature.
2. preparation method as described in claim 1, which is characterized in that indium ion concentration model in step (1) described mixed solution
It encloses for 0.1mol/L~2.5mol/L, tin ion concentration range is 0.01~0.25mol/L, and the indium ion concentration is described
9~10 times of tin ion concentration.
3. preparation method as described in claim 1, which is characterized in that step (1) indium salts are four water indium trichlorides, described
Pink salt is stannic chloride pentahydrate.
4. preparation method as described in claim 1, which is characterized in that the cellular glass is silica glass, the glass
Nanometer micropore is evenly distributed with inside glass, the pore size of the single micropore is 5~50 nanometers, micropore in the cellular glass
Volume account for the 30~35% of cellular glass total volume.
5. preparation method as described in claim 1, which is characterized in that step (2) soaking process carries out ultrasonic shake simultaneously
It swings.
6. preparation method as described in claim 1, which is characterized in that step (3) the sintering specific steps are as follows:
(1) 600 DEG C are warming up to the heating rate of 1 DEG C/min, then keep the temperature 3h；
(2) 700 DEG C are warming up to the heating rate of 1 DEG C/min again, then keep the temperature 1h；
(3) 950 DEG C are warming up to the heating rate of 0.8 DEG C/min again, then keep the temperature 0.5h；
(4) 1150 DEG C are warming up to the heating rate of 2.2 DEG C/min again, then keep the temperature 1h；
(5) last furnace cooling is to room temperature.
7. a kind of glass of doped ITO nanoparticle, which is characterized in that it is according to as described in claim 1~6 any one
Preparation method is prepared.
8. glass as claimed in claim 7, which is characterized in that doped with ITO nanoparticle in the glass, the ITO is received
The size of rice corpuscles is 5~30nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1717374A (en) * | 2002-11-29 | 2006-01-04 | 独立行政法人科学技术振兴机构 | Luminescent glass |
| CN1785873A (en) * | 2005-10-21 | 2006-06-14 | 中国科学院上海光学精密机械研究所 | Manufacturing method of erbium doped high silicon oxygen infrared luminous glass |
| CN101993199A (en) * | 2009-08-10 | 2011-03-30 | 海洋王照明科技股份有限公司 | Cellular glass containing palladium nanoparticles and preparation method thereof |
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2017
- 2017-04-28 CN CN201710295438.0A patent/CN107162441B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1717374A (en) * | 2002-11-29 | 2006-01-04 | 独立行政法人科学技术振兴机构 | Luminescent glass |
| CN1785873A (en) * | 2005-10-21 | 2006-06-14 | 中国科学院上海光学精密机械研究所 | Manufacturing method of erbium doped high silicon oxygen infrared luminous glass |
| CN101993199A (en) * | 2009-08-10 | 2011-03-30 | 海洋王照明科技股份有限公司 | Cellular glass containing palladium nanoparticles and preparation method thereof |
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