CN104651805B - Ultrasonic atomizing microwave tube furnace and application thereof - Google Patents
Ultrasonic atomizing microwave tube furnace and application thereof Download PDFInfo
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- CN104651805B CN104651805B CN201510057826.6A CN201510057826A CN104651805B CN 104651805 B CN104651805 B CN 104651805B CN 201510057826 A CN201510057826 A CN 201510057826A CN 104651805 B CN104651805 B CN 104651805B
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Abstract
The invention discloses an ultrasonic atomizing microwave tube furnace and the application thereof and belongs to the fields of oxide film preparation by use of spray pyrolysis and powder metallurgy. The invention also provides a method for preparing an ITO film and a powder simultaneously by heating by use of the ultrasonic atomizing microwave tube furnace. The method is characterized in that an indium-tin precursor saline solution is atomized by use of the ultrasonic wave, next, the atomized liquid drops are fed into a horizontal microwave heating tube furnace by use of a carrier gas for a flash pyrolytic reaction, and forming a layer of ITO film when the atomized drops come into contact with a high-temperature quartz glass sheet. Meanwhile, other atomized drops are formed into superfine ITO powder which is large in surface area, good in dispersity and good in appearance. The method is simple in process operation and low in cost; the materials are utilized reasonable; compared with the traditional method of spraying on a high-temperature glass sheet substrate, the waste of the materials is reduced. As a result, simultaneous preparation of the ITO film and the ITO powder by combining the ultrasonic atomizing pyrolysis method and the microwave heating tube furnace is possible.
Description
Technical field
The present invention relates to a kind of ultrasonic atomization microwave tube type oven and utilization, belong to powder metallurgy with thin-film material green system
Standby Technical Development Area.
Background technology
Ultra-fine ITO powders and film, are widely used in solid state flat panel display（Such as liquid crystal display, plasma
Display screen, EL panel etc.）, solar cell, electromagnetic wave shielding and transparent conductive material, inorganic functional material, coating, rubber
The fields such as glue, glass, ceramics, plastics, military affairs, photochemical catalyst, cell tracker agent, gas sensitive device, short wavelength's device, capacitor.
And the target in these fields is mainly by ITO powders and thin film fabrication, so ITO powders also just become pendulum wide with the preparation of film
Important topic in face of big scientific worker.
As ITO powders and thin-film material are widely applied, ITO powders increasingly cause people with the technology of preparing of film
Attention, the technology of preparing of current powder mainly has hydrothermal synthesis method, sol-gel method, chemical coprecipitation], spraying-combustion
Burning method, spray pyrolysis etc., wherein spray pyrolysis law technology are a kind of aerosol technologies of synthesizing superfine powder.But former
Spray pyrolysis prepare in ITO powders and film.All it is separate preparation, the present invention makes mist by ultrasonic wave, by carrier gas
Drop is directly entered under predetermined high temperature and directly carry out rapid evaporation dry thermal cracking reaction, so that in the target temperature of quartz glass plate
The lower direct reaction of degree forms film.Due in droplet mass transport process, it is impossible to which all drops are all completely in high quartz glass
React on piece, be solves the problems, such as tail gas and remaining drop how handling problems, the present invention is made using heating using microwave diamond heating
Whole drops in high quartz pipe with react and collected in pipe tail receiving flask under microwave field.Wherein heating using microwave
Technology have selective heating, firing rate it is fast, it is pollution-free the features such as, greatly increased the efficiency of experiment, shorten experiment
In the reaction time of middle drop internal solvent evaporation drying pyrolysis, to significantly reduce and quickly form solid powder under energy consumption and low temperature
Body.
The present invention mainly uses two salts substances of ultrasonic atomization and descends Jing solvents according to a certain ratio（Water dissolves）It is mixed
Precursor solution is closed, using air droplet is sent into as carrier gas and meet high quartz sheet glass in heating microwave tube type oven burner hearth and send out
Heat solution simultaneously aoxidizes acquisition ito thin film and is molded on quartz glass plate, and pipe tail receiving flask obtains spherical ITO powders, whole reaction
All it is carry out in closed quartz ampoule, it is to avoid other wastes of spray droplet, has accomplished to be sprayed used in microwave tube type oven
Pyrolysismethod disposably obtains the breakthrough of ito thin film and ITO powders on 600 DEG C of high-temperatures, for spray pyrolysis are in high-temperature
Lower preparation prepares sull with powder there is provided feasibility Experiment method simultaneously, adopts this experimental technique, significantly reduces
Energy resource consumption in heating process, simplifies operating process, has greatly saved production cost, decreases environmental pollution,
Generate significant economy and ecological benefits.The category that film and powder are prepared under spray pyrolysis high temperature is expanded.
The content of the invention
The present invention relates to a kind of ultrasonic atomization microwave tube type oven, realizes under spray pyrolysis high temperature while preparing
ITO powders and ito thin film, specifically include：Air pressure pump 1, spinner device 2, ultrasonic sprayer 3, ultrasonic wave are made mist and are shaken
Moving plate 4, droplet 5, quartz glass conduit 6, quartz glass tube 7, microwave heating equipment 8, microwave generator 9, quartz glass plate 10,
Auxiliary heating material 11, insulation material 12, powder buffering sedimentation bottle 13, powder 14, powder receiving flask 15, first order alkali liquor absorption
Tail gas unit 16, second level alkali liquor absorption tail gas unit 17, air pressure pump 1 is by spinner device 2 and ultrasonic sprayer 3
It is connected, the bottom of ultrasonic sprayer 3 is provided with ultrasonic wave and makes mist vibrating disk 4, and ultrasonic sprayer 3 is led by quartz glass
Pipe 6 is connected with quartz glass tube 7；Quartz glass tube 7 be internally provided with quartz glass plate 10 and auxiliary heating material 11, stone
The outside of English glass tube 7 is provided with microwave heating equipment 8, and between microwave heating equipment 8 and quartz glass tube 7 insulation material is provided with
12, microwave generator 9 is provided with microwave heating equipment 8；The other end powder buffering sedimentation bottle 13 of quartz glass tube 7, powder
Buffering sedimentation bottle 13 is connected with powder receiving flask 15；Powder receiving flask 15, first order alkali liquor absorption tail gas unit 16 and second
Level alkali liquor absorption tail gas unit 17 is sequentially connected logical.
Another object of the present invention is to provide the ultrasonic atomization microwave tube type oven for while preparing ITO powder
Body and ito thin film method, specifically include following steps：
（1）To be dissolved in absolute ethyl alcohol with inidum chloride and stannous chloride and prepare precursor solution, chlorine in precursor solution
The concentration for changing indium is 0.1-1mol/L, the concentration of stannous chloride is 0.1-1mol/L；
（2）Precursor solution is added to into ultrasonic sprayer（3）In carry out making mist, wherein, ultrasonic frequency 1.3-
1.7MHz, atomization quantity is 0.3-0.7L/h；
（3）Using air as carrier gas, flow rate of carrier gas 0.2-0.8l/min, droplet is sent into by heating using microwave reaction by carrier gas
Area（500~750℃）Carry out the evaporation drying pyrolysis of droplet and form ito thin film on high quartz sheet glass, continuing by carrying
The powder for being formed is sent into and formed in afterbody receiving flask ITO powders by gas.
Beneficial effects of the present invention：
（1）Ultrasonic atomization microwave tube type oven of the present invention, realizes under spray pyrolysis high temperature while preparing
ITO powders and ito thin film, simplify practical operation step, it is to avoid former spray pyrolysis prepare droplet during ito thin film
The situation with environmental pollution is wasted, the even particle size distribution of Scientific Outlook on Development ITO powder, favorable dispersibility has effectively been put into practice；
（2）This method simple production process, it is with low cost, by bringing-up section heating using microwave select the solvent inside droplet
Property is preferentially inhaled ripple and integrally heats and become vapor and decompose rapidly, and droplet quickly finishes evaporation drying under microwave reinforced heating
And film forming is assembled with afterbody receiving flask powder on quartz glass plate, the method makes mist, microwave tube type oven using ultrasonic wave
Plus heat integration prepares ITO powders and ito thin film.
（2）This methods described reduces traditional spray pyrolysismethod and prepares in film directly beats the mistake on the very little bottom of high temperature by drop
Drop in journey is wasted and environmental pollution, and the present invention can allow the drop that film is not formed on high quartz sheet glass direct
By under the mass transfer of carrier gas under high temperature oxidative atmosphere fast pyrogenation and formed ITO powders and in afterbody receiving flask collect；Simultaneously
The tail gas produced in pyrolytic process has also obtained safety dumping；Belong to powder metallurgy with thin-film material green technology of preparing exploitation
Field.
Description of the drawings
Fig. 1 is the structural representation of lateral ultrasonic wave spraying microwave tube type oven of the present invention；
Fig. 2 is the structural representation of longitudinal ultrasonic ripple spraying microwave tube type oven of the present invention；
Fig. 3 is the XRD of the ITO powders that embodiment 1 ~ 4 is prepared；
Fig. 4 is the XRD of the ito thin film that embodiment 1 ~ 4 is prepared；
Fig. 5 is the scanning electron microscope (SEM) photograph of the ITO powders that embodiment 1 ~ 4 is prepared；
Fig. 6 is the scanning electron microscope (SEM) photograph of the ito thin film that embodiment 1 ~ 4 is prepared.
Fig. 1, in 2：1- air pressure pumps；2- spinner devices；3- ultrasonic sprayers；4- ultrasonic waves make mist vibrating disk；
5- droplets；6- quartz glass conduits；7- quartz glass tubes；8- microwave heating equipments；9- microwave generators；10- quartz glass plates；
11-SiC aids in heating material 12- insulation materials；13- powders buffering sedimentation bottle；14- powders；15- powder receiving flasks；16- first
Level alkali liquor absorption tail gas unit；17- second level alkali liquor absorption tail gas unit.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is described in further detail with specific embodiment, but protection scope of the present invention is simultaneously
It is not limited to the content.
In embodiment XRD be Rigaku D/Max2200 types, Cu target Ka lines, tube voltage 40kV, tube current 80mA, test
Angular range（2θ）For 10 ° ~ 90 °；SEM Electronic Speculum is Philips, model XL-30E, and transmission electron microscope is JEOL, model JEM-
2100。
Embodiment 1
Ultrasonic atomization microwave tube type oven described in the present embodiment is horizontal（As shown in Figure 1）, specifically include：Air compresses
Pump 1, spinner device 2, ultrasonic sprayer 3, ultrasonic wave make mist vibrating disk 4, droplet 5, quartz glass conduit 6, quartz glass
Pipe 7, microwave heating equipment 8, microwave generator 9, quartz glass plate 10, auxiliary heating material 11, insulation material 12, powder buffering
Sedimentation bottle 13, powder 14, powder receiving flask 15, first order alkali liquor absorption tail gas unit 16, second level alkali liquor absorption tail gas unit
17, air pressure pump 1 is connected by spinner device 2 with ultrasonic sprayer 3, and the bottom of ultrasonic sprayer 3 is provided with
Ultrasonic wave makes mist vibrating disk 4, and ultrasonic sprayer 3 is connected by quartz glass conduit 6 with quartz glass tube 7；Quartz glass
Pipe 7 is internally provided with quartz glass plate 10 and auxiliary heating material 11, and the outside of quartz glass tube 7 is provided with heating using microwave dress
8 are put, insulation material 12 is provided between microwave heating equipment 8 and quartz glass tube 7, microwave is provided with microwave heating equipment 8 and is sent out
Raw device 9；The other end powder buffering sedimentation bottle 13 of quartz glass tube 7, powder buffering sedimentation bottle 13 is connected with powder receiving flask 15
It is logical；Powder receiving flask 15, first order alkali liquor absorption tail gas unit 16 are sequentially connected logical with second level alkali liquor absorption tail gas unit 17.
Ultrasonic atomization microwave tube type oven described in the present embodiment is used to prepare ITO powders and ito thin film side simultaneously
Method, specifically includes following steps：
（1）To be dissolved in absolute ethyl alcohol with inidum chloride and stannous chloride and prepare precursor solution, chlorine in precursor solution
The concentration for changing indium is 0.1mol/L, the concentration of stannous chloride is 0.1mol/L；
（2）Precursor solution is added to into ultrasonic sprayer（3）In carry out making mist, wherein, ultrasonic frequency 1.3MHz,
Atomization quantity is 0.3L/h）；
（3）Using air as carrier gas, flow rate of carrier gas 0.2L/min, droplet is sent into by heating using microwave reaction zone by carrier gas
500 DEG C carry out the evaporation drying pyrolysis of droplet and form ito thin film on high quartz sheet glass, by carrier gas will formed
Powder send into afterbody receiving flask in formed ITO powders.
The XRD of the ITO powders that the present embodiment is prepared as shown in figure 3, the XRD of the ito thin film for preparing such as
Shown in Fig. 4, as seen from the figure：The scanning electron microscope (SEM) photograph such as Fig. 5 for the ITO powders that the present embodiment is prepared（a）It is shown, it is prepared into
The scanning electron microscope (SEM) photograph of the ito thin film for arriving such as Fig. 6（a）It is shown, as seen from the figure：The present embodiment has obtained the particle diameter of good dispersion
Uniform powder also has the film of certain good compactness.
Embodiment 2
Ultrasonic atomization microwave tube type oven described in the present embodiment is longitudinal direction（As shown in Figure 2）, specifically include：Air compresses
Pump 1, spinner device 2, ultrasonic sprayer 3, ultrasonic wave make mist vibrating disk 4, droplet 5, quartz glass conduit 6, quartz glass
Pipe 7, microwave heating equipment 8, microwave generator 9, quartz glass plate 10, auxiliary heating material 11, insulation material 12, powder buffering
Sedimentation bottle 13, powder 14, powder receiving flask 15, first order alkali liquor absorption tail gas unit 16, second level alkali liquor absorption tail gas unit
17, air pressure pump 1 is connected by spinner device 2 with ultrasonic sprayer 3, and the bottom of ultrasonic sprayer 3 is provided with
Ultrasonic wave makes mist vibrating disk 4, and ultrasonic sprayer 3 is connected by quartz glass conduit 6 with quartz glass tube 7；Quartz glass
Pipe 7 is internally provided with quartz glass plate 10 and auxiliary heating material 11, and the outside of quartz glass tube 7 is provided with heating using microwave dress
8 are put, insulation material 12 is provided between microwave heating equipment 8 and quartz glass tube 7, microwave is provided with microwave heating equipment 8 and is sent out
Raw device 9；The other end powder buffering sedimentation bottle 13 of quartz glass tube 7, powder buffering sedimentation bottle 13 is connected with powder receiving flask 15
It is logical；Powder receiving flask 15, first order alkali liquor absorption tail gas unit 16 are sequentially connected logical with second level alkali liquor absorption tail gas unit 17.
Ultrasonic atomization microwave tube type oven described in the present embodiment is used to prepare ITO powders and ito thin film side simultaneously
Method, specifically includes following steps：
（1）To be dissolved in absolute ethyl alcohol with inidum chloride and stannous chloride and prepare precursor solution, chlorine in precursor solution
The concentration for changing indium is 1mol/L, the concentration of stannous chloride is 0.4mol/L；
（2）Precursor solution is added to into ultrasonic sprayer（3）In carry out making mist, wherein, ultrasonic frequency 1.7MHz,
Atomization quantity is 0.7L/h；
（3）Using air as carrier gas, flow rate of carrier gas 0.8/min, droplet is sent into by heating using microwave reaction zone 600 by carrier gas
DEG C carry out the evaporation drying pyrolysis of droplet and form ito thin film on high quartz sheet glass, continuing to be formed by carrier gas
Powder is sent into and formed in afterbody receiving flask ITO powders.
The XRD of the ITO powders that the present embodiment is prepared as shown in figure 3, the XRD of the ito thin film for preparing such as
Shown in Fig. 4, as seen from the figure：Powder and appearance peak corresponding with ITO standard cards in film XRD spectral lines, it is miscellaneous without other
Mass peak；The scanning electron microscope (SEM) photograph such as Fig. 5 for the ITO powders that the present embodiment is prepared（b）Shown, the ito thin film for preparing is swept
Retouch electron microscope such as Fig. 6（b）It is shown, as seen from the figure：The ITO morphology microstructures that the present embodiment is prepared all compare with dispersiveness
It is good；Ito thin film crystallization very completely, defines the film of high-compactness.
Embodiment 3
Ultrasonic atomization microwave tube type oven described in the present embodiment is horizontal（As shown in Figure 1）, specifically include：Air compresses
Pump 1, spinner device 2, ultrasonic sprayer 3, ultrasonic wave make mist vibrating disk 4, droplet 5, quartz glass conduit 6, quartz glass
Pipe 7, microwave heating equipment 8, microwave generator 9, quartz glass plate 10, auxiliary heating material 11, insulation material 12, powder buffering
Sedimentation bottle 13, powder 14, powder receiving flask 15, first order alkali liquor absorption tail gas unit 16, second level alkali liquor absorption tail gas unit
17, air pressure pump 1 is connected by spinner device 2 with ultrasonic sprayer 3, and the bottom of ultrasonic sprayer 3 is provided with
Ultrasonic wave makes mist vibrating disk 4, and ultrasonic sprayer 3 is connected by quartz glass conduit 6 with quartz glass tube 7；Quartz glass
Pipe 7 is internally provided with quartz glass plate 10 and auxiliary heating material 11, and the outside of quartz glass tube 7 is provided with heating using microwave dress
8 are put, insulation material 12 is provided between microwave heating equipment 8 and quartz glass tube 7, microwave is provided with microwave heating equipment 8 and is sent out
Raw device 9；The other end powder buffering sedimentation bottle 13 of quartz glass tube 7, powder buffering sedimentation bottle 13 is connected with powder receiving flask 15
It is logical；Powder receiving flask 15, first order alkali liquor absorption tail gas unit 16 are sequentially connected logical with second level alkali liquor absorption tail gas unit 17.
Ultrasonic atomization microwave tube type oven described in the present embodiment is used to prepare ITO powders and ito thin film side simultaneously
Method, specifically includes following steps：
（1）To be dissolved in absolute ethyl alcohol with inidum chloride and stannous chloride and prepare precursor solution, chlorine in precursor solution
The concentration for changing indium is 0.4mol/L, the concentration of stannous chloride is 0.6mol/L；
（2）Precursor solution is added to into ultrasonic sprayer（3）In carry out making mist, wherein, ultrasonic frequency 1.4
MHz, atomization quantity is 0.5L/h；
（3）Using air as carrier gas, flow rate of carrier gas 0.4l/min, droplet is sent into by heating using microwave reaction zone by carrier gas
700 DEG C carry out the evaporation drying pyrolysis of droplet and form ito thin film on high quartz sheet glass, by carrier gas will formed
Powder send into afterbody receiving flask in formed ITO powders.
The XRD of the ITO powders that the present embodiment is prepared as shown in figure 3, the XRD of the ito thin film for preparing such as
Shown in Fig. 4, as seen from the figure：Powder and appearance peak corresponding with ITO standard cards in film XRD spectral lines, it is miscellaneous without other
Mass peak；The scanning electron microscope (SEM) photograph such as Fig. 5 for the ITO powders that the present embodiment is prepared（c）Shown, the ito thin film for preparing is swept
Retouch electron microscope such as Fig. 6（c）It is shown, as seen from the figure：The ITO morphology microstructures that the present embodiment is prepared all compare with dispersiveness
It is good；Ito thin film crystallization very completely, defines the film of high-compactness.
Embodiment 4
Ultrasonic atomization microwave tube type oven described in the present embodiment is longitudinal direction（As shown in Figure 2）, specifically include：Air compresses
Pump 1, spinner device 2, ultrasonic sprayer 3, ultrasonic wave make mist vibrating disk 4, droplet 5, quartz glass conduit 6, quartz glass
Pipe 7, microwave heating equipment 8, microwave generator 9, quartz glass plate 10, auxiliary heating material 11, insulation material 12, powder buffering
Sedimentation bottle 13, powder 14, powder receiving flask 15, first order alkali liquor absorption tail gas unit 16, second level alkali liquor absorption tail gas unit
17, air pressure pump 1 is connected by spinner device 2 with ultrasonic sprayer 3, and the bottom of ultrasonic sprayer 3 is provided with
Ultrasonic wave makes mist vibrating disk 4, and ultrasonic sprayer 3 is connected by quartz glass conduit 6 with quartz glass tube 7；Quartz glass
Pipe 7 is internally provided with quartz glass plate 10 and auxiliary heating material 11, and the outside of quartz glass tube 7 is provided with heating using microwave dress
8 are put, insulation material 12 is provided between microwave heating equipment 8 and quartz glass tube 7, microwave is provided with microwave heating equipment 8 and is sent out
Raw device 9；The other end powder buffering sedimentation bottle 13 of quartz glass tube 7, powder buffering sedimentation bottle 13 is connected with powder receiving flask 15
It is logical；Powder receiving flask 15, first order alkali liquor absorption tail gas unit 16 are sequentially connected logical with second level alkali liquor absorption tail gas unit 17.
Ultrasonic atomization microwave tube type oven described in the present embodiment is used to prepare ITO powders and ito thin film side simultaneously
Method, specifically includes following steps：
（1）To be dissolved in absolute ethyl alcohol with inidum chloride and stannous chloride and prepare precursor solution, chlorine in precursor solution
The concentration for changing indium is 0.6mol/L, the concentration of stannous chloride is 1mol/L；
（2）Precursor solution is added to into ultrasonic sprayer（3）In carry out making mist, wherein, ultrasonic frequency 1.5MHz,
Atomization quantity is 0.6L/h；
（3）Using air as carrier gas, flow rate of carrier gas 0.6/min, droplet is sent into by heating using microwave reaction zone 750 by carrier gas
DEG C carry out the evaporation drying pyrolysis of droplet and form ito thin film on high quartz sheet glass, continuing to be formed by carrier gas
Powder is sent into and formed in afterbody receiving flask ITO powders.
The XRD of the ITO powders that the present embodiment is prepared as shown in figure 3, the XRD of the ito thin film for preparing such as
Shown in Fig. 4, as seen from the figure：Powder and appearance peak corresponding with ITO standard cards in film XRD spectral lines, it is miscellaneous without other
Mass peak；The scanning electron microscope (SEM) photograph such as Fig. 5 for the ITO powders that the present embodiment is prepared（d）Shown, the ito thin film for preparing is swept
Retouch electron microscope such as Fig. 6（d）It is shown, as seen from the figure：The ITO morphology microstructures that the present embodiment is prepared all compare with dispersiveness
It is good；Ito thin film crystallization very completely, defines the film of high-compactness.
Claims (4)
1. a kind of ultrasonic atomization microwave tube type oven, it is characterised in that include：Air pressure pump（1）, spinner device（2）, it is super
Sonic nebulizer（3）, ultrasonic wave make mist vibrating disk（4）, droplet（5）, quartz glass conduit（6）, quartz glass tube（7）, microwave
Heater（8）, microwave generator（9）, quartz glass plate（10）, auxiliary heating material（11）, insulation material（12）, powder delay
Punching sedimentation bottle（13）, powder（14）, powder receiving flask（15）, first order alkali liquor absorption tail gas unit（16）, second level alkali lye inhale
Ending device of air（17）, air pressure pump（1）By spinner device（2）And ultrasonic sprayer（3）It is connected, ultrasonic wave spray
Day with fog（3）Bottom be provided with ultrasonic wave and make mist vibrating disk（4）, ultrasonic sprayer（3）By quartz glass conduit（6）With stone
English glass tube（7）It is connected；Quartz glass tube（7）Be internally provided with quartz glass plate（10）, quartz glass plate（10）After
Face is provided with auxiliary heating material（11）, quartz glass tube（7）Outside be provided with microwave heating equipment（8）, heating using microwave dress
Put（8）With quartz glass tube（7）Between be provided with insulation material（12）, microwave heating equipment（8）On be provided with microwave generator
（9）；Quartz glass tube（7）The other end powder buffering sedimentation bottle（13）, powder buffering sedimentation bottle（13）With powder receiving flask
（15）It is connected；Powder receiving flask（15）, first order alkali liquor absorption tail gas unit（16）With second level alkali liquor absorption tail gas unit
（17）It is sequentially connected logical.
2. ultrasonic atomization microwave tube type oven according to claim 1, it is characterised in that：Ultrasonic atomization microwave tube type oven
For transversely or longitudinally.
3. ultrasonic atomization microwave tube type oven described in claim 1 is used to prepare the side of ITO powders and ito thin film simultaneously
Method, it is characterised in that specifically include following steps：
（1）To be dissolved in absolute ethyl alcohol with inidum chloride and stannous chloride and prepare precursor solution, inidum chloride in precursor solution
Concentration be 0.1-1mol/L, stannous chloride concentration be 0.1-1mol/L；
（2）Precursor solution is added to into ultrasonic sprayer（3）In carry out making mist, wherein, ultrasonic frequency 1.3-1.7MHz,
Atomization quantity is 0.3-0.7L/h；
（3）Using air as carrier gas, flow rate of carrier gas 0.2-0.8L/min, droplet feeding heating using microwave reaction zone is entered by carrier gas
The evaporation drying pyrolysis of row droplet simultaneously forms ito thin film on high quartz sheet glass, is continuing the powder for being formed by carrier gas
Send into and formed in afterbody receiving flask ITO powders.
4. the method for preparing ITO powders and ito thin film simultaneously according to claim 3, it is characterised in that：The microwave
The temperature in heating response area is 500 ~ 750 DEG C.
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| CN106984256B (en) * | 2017-03-30 | 2019-12-17 | 重庆文理学院 | Spray cracking system and application method thereof |
| CN107285383B (en) * | 2017-06-29 | 2018-10-23 | 宁波吉电鑫新材料科技有限公司 | A kind of one-step synthesis double-perovskite kalium ion battery negative material and preparation method thereof |
| CN109168212B (en) * | 2018-07-11 | 2020-08-04 | 南京三乐微波技术发展有限公司 | Solid waste microwave treatment equipment |
| CN112107873B (en) * | 2020-08-31 | 2023-03-17 | 武汉市格勒特新材料有限公司 | Vertical device and method for preparing superfine powder through spray pyrolysis |
| CN114949890A (en) * | 2022-05-27 | 2022-08-30 | 杭州东日节能技术有限公司 | Microwave-heated filler type evaporator and method for concentrating fluorine-containing dilute sulfuric acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Ultrasonic atomizing preparation of superfine powder |
| CN103590022A (en) * | 2013-11-27 | 2014-02-19 | 昆明理工大学 | Method for making film through ultrasonic atomization-microwave pyrolysis |
| CN203678371U (en) * | 2013-11-27 | 2014-07-02 | 昆明理工大学 | Device for preparing nano powder by using ultrasonic atomization-microwave pyrolysis combined method |
| CN204849025U (en) * | 2015-02-04 | 2015-12-09 | 昆明理工大学 | Ultrasonic wave spraying microwave tube -like stove |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57158369A (en) * | 1981-03-26 | 1982-09-30 | Semiconductor Energy Lab Co Ltd | Formation of dielectric film by plasma vapor phase method |
| JPH01265414A (en) * | 1988-04-15 | 1989-10-23 | Furukawa Electric Co Ltd:The | Manufacture of oxide superconductive wire rod |
-
2015
- 2015-02-04 CN CN201510057826.6A patent/CN104651805B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1040932A (en) * | 1988-09-08 | 1990-04-04 | 清华大学 | Ultrasonic atomizing preparation of superfine powder |
| CN103590022A (en) * | 2013-11-27 | 2014-02-19 | 昆明理工大学 | Method for making film through ultrasonic atomization-microwave pyrolysis |
| CN203678371U (en) * | 2013-11-27 | 2014-07-02 | 昆明理工大学 | Device for preparing nano powder by using ultrasonic atomization-microwave pyrolysis combined method |
| CN204849025U (en) * | 2015-02-04 | 2015-12-09 | 昆明理工大学 | Ultrasonic wave spraying microwave tube -like stove |
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