CN1402594A - Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray - Google Patents
Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray Download PDFInfo
- Publication number
- CN1402594A CN1402594A CN 02139432 CN02139432A CN1402594A CN 1402594 A CN1402594 A CN 1402594A CN 02139432 CN02139432 CN 02139432 CN 02139432 A CN02139432 A CN 02139432A CN 1402594 A CN1402594 A CN 1402594A
- Authority
- CN
- China
- Prior art keywords
- film
- heating
- sno
- substrate
- ultrasonic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
SnO2:F transparent conducting film is evenly prepared on the inner wall of fire resistant borosilicate glass tube so as to form the heating tube of the electric heat film used to heat liquid. Comparing with other filming technique, the technique provides the advantages of simple device, low material cost, good evenness and repeatability. The film is acid and alkali resistant, providing the performances: resistivity lower as 4X10 to the power -4 ohm.cm, degree of transparency of the visible light 91%, power density as high 35W/cm2. With heated in air for 7200 hours, the film still keeps the high hardness. The film can be coated on the surface of the substrate so as to produce the product of the ceramic plate of the electric heating film.
Description
One, affiliated technical field
The invention belongs to the new process of film preparation, relate to a kind of preparation of electrothermal film heating pipe, particularly a kind of with supersonic spraying with SnO
2: the F Electric radiant Heating Film prepares the technology of high temperature resistant Pyrex inside pipe wall.
Two, background technology
To SnO
2The research of film, preparation and application are in recent years in continuous development.Common SnO
2Film is a polycrystalline material, diamond lattic structure, and conductivity can reach 10
3Ω
-1Cm
-1Existing multiple preparation SnO
2The method of film is broadly divided into physical vaporous deposition (PVD), chemical vapour deposition technique (CVD), sol-gel process (Sol-Gel) and spray pyrolysis method etc.PVD method and CVD method are divided into many kinds of methods such as radio frequency sputtering, direct magnetic control cathodic sputtering method, MOPECVD method etc. again.The Sol-Gel thin films does not need PVD method and the such complex and expensive equipment of CVD method, it is easy that it has technology, equipment requirements is low and be suitable for large tracts of land system film, and the film chemical ratio of components is easier to control, can be well suited for the polynary composition sull of preparation from characteristics such as molecular level design preparation materials.It is simple that spray pyrolysis method has equipment, and process cycle is short, and the characteristics that the production prices of raw and semifnished materials are cheap can be prepared and the suitable high-quality thin film of physical deposition method performance.Traditional spray pyrolysis method is by spray gun source solution atomization and the substrate that is carried into heating to be carried out pyrolytic reaction by means of high pressure carrier gas.
When at common SnO
2The people can make its conductivity improve an order of magnitude for mixing elements such as Sb, F, P in the film, prepares SnO and mix F
2: the conductivity of F film is than mixing the taller of Sb film.Yet, adopt various PVD methods, CVD method, not only apparatus expensive, technology are loaded down with trivial details, and film can not be plated on the inwall of glass tube; Though the heating tube uniformity of Sol-Gel method preparation is better, internal and external walls all has conducting film, uses dangerous, and the film of Sol-Gel method preparation is relatively poor to the adhesive force of substrate, have crack performance in the film, film is a cellular, and the resulting thickness that at every turn circulates is thin etc.; Traditional spray pyrolysis method is by spray gun source solution atomization and the substrate that is carried into heating to be carried out pyrolytic reaction by means of high pressure carrier gas, the performance of prepared film be subjected to such as spray gun atomizing uniformity, high-pressure atomization droplet flow to the shape of the rapid influence of underlayer temperature, spray tip and nozzle governing screw under high pressure draught easily loosening and change spray influence of various factors such as the flow of liquid and jet length, randomness is bigger.Therefore, the technology controlling and process of spray gun spray pyrolysis method is difficulty, the uniformity of prepared film performance and poor repeatability.
Three, summary of the invention
According to defective or deficiency that above-mentioned prior art exists, the present invention aims to provide a kind of with SnO
2: the F transparent electric heating film is plated in resistant to elevated temperatures Pyrex inside pipe wall equably, the process of preparation high power heating tube.
To achieve these goals, the technical scheme that the present invention takes is that supersonic spraying prepares SnO
2: the technology of F electrothermal film heating pipe, carry out according to the following steps: the 1) cleaning of backing material
With clear water substrate surface is cleaned up earlier, again substrate is put into potassium bichromate (K
2CrO
7) the concentrated sulfuric acid (H
2SO
4) in the saturated solution behind the dipping 2h-4h, put into ultrasonic cleaning machine and clean 30min with distilled water, take out and place clean baking oven dry for standby; 2) preparation of source solution
Take by weighing 22g～30g SnCl
45H
2O. in beaker, the adding volume ratio is 8: 1～12: 1 H
2O and CH
3Mixed liquid to the solid of OH just dissolves, and adds 1g～6g NH again
4The F aqueous solution stirs, and pours in the ultrasonic atomizatio generator; 3) preparation of film
Design temperature control make between 380 ℃～450 ℃ of underlayer temperatures, nozzle and substrate apart from 6mm～12mm, stepping motor gait of march 0.5m/s～2.5m/s, atomization quantity 1800dm
3h
-1～2500dm
3h
-1And carrier gas air pressure 1.2 * 10
5Pa～2.0 * 10
5Behind the Pa, open stepping motor and ultrasonic atomizer, the ultrasonic vibration of piezoelectric ceramic transducer is with the solution atomization that is prepared, be carried into the nozzle of ultrasonic atomizer by carrier gas, under Stepping Motor Control, the soup droplet is delivered to the Pyrex inside pipe wall substrate of heating equably, and chemical reaction takes place on substrate source solution under the high temperature, can deposit go out uniform SnO on substrate
2: the F film; 4) annealing in process
Close fire door, the 30min that anneals under 400 ℃～480 ℃ temperature slowly cools to room temperature and gets final product; 5) encapsulation
Coat skim annular silver slurry equably at the two ends of heating tube inwall.Behind the airing, starch the heating curve of 20 ℃～600 ℃ of variations of requirement, sintering 1h～3h under the room temperature by used silver; Welding lead on two electrodes is used the insulative water-proof material package again.
Supersonic spraying involved in the present invention prepares SnO
2: the process of F electrothermal film heating pipe, adopt the ultrasonic atomizatio technology, can remedy the deficiency of spray gun spraying effectively, can be effectively at the zone of required film forming (as the Pyrex inside pipe wall substrate) film that processability is good.Compare with other coating process, this technology has that equipment is simple, technology is simple, the advantage of uniformity and good reproducibility.Institute's made membrane acid-alkali-corrosive-resisting, resistivity is low to moderate 4 * 10
-4Ω cm, visible light transmissivity are up to 91%, and power density is up to 35W/cm
2, heating is 7200 hours in air, the performance no change, the hardness height, with quartzy, topaz is suitable, strong adhesion, graduating with cutter are not down.This coating process also can reach the identical effect of other coating method, as is plated on substrate surface, thereby makes products such as electro-thermal film ceramic sheet, Electric radiant Heating Film coffee pot.
Four, description of drawings
Fig. 1 is ullrasonic spraying deposit SnO
2: the device schematic diagram of F film; Each symbol is expressed as respectively among the figure: 1 carrier gas (air), 2 flowmeters, the control of 3 times, 4 solution, 5 ultrasonic transducers, 6 stepping motors, 7 quartz ampoule nozzles, 8 gas vents, 9 borosilicate glass tubes, 10 thermal reaction chambers, 11 thermocouples, 12 supports, 13 Muffle furnaces, 14 temperature controllers and display.
Fig. 2 (a) is stereoscan photograph (SEM); (b), (c) is scanning tunnel microscope photo (STM);
Fig. 3 is made up of a heating tube for adopting single electrothermal film heating pipe of the present invention's preparation, and electrothermal tube is immersed in the heated liquid, and energized can heat, and power of alterating and direct current all can use.
Fig. 4 is formed in parallel by some single tubes for adopting the combination electrothermal film heating pipe of the present invention's preparation.Can be according to the single tube of corresponding radical in the power demand parallel connection.Also each single tube can be connected on the different switches, by the power of switch control combination pipe.
Fig. 5 is for adopting the transparent electric heating film heating ceramic sheet of the present invention's preparation, is to be substrate with the highly heat-conductive carbon/ceramic ceramics, plates one deck SnO thereon
2: F makes.It is big that this sheet has power, the advantage that volume is little, and it is narrow and small and need area heated carry out the power heating to can be used for the space.
Five, embodiment
Comply with the embodiment that technical scheme of the present invention is finished below in conjunction with accompanying drawing and inventor, the present invention is described in further detail.5.1 instrument and equipment
As Fig. 1 is ullrasonic spraying deposit SnO
2: the experimental provision of F film.Each symbol is expressed as respectively among the figure: 1 carrier gas (air), 2 flowmeters, 3 time controllers, 4 solution, 5 ultrasonic transducers, 6 stepping motors, 7 quartz ampoule nozzles, 8 gas vents, 9 borosilicate glass tubes, 10 thermal reaction chambers, 11 thermocouples, 12 supports, 13 Muffle furnaces, 14 temperature controllers and display.
Thermal reactor is new RJM resistance furnace, the wide 17cm of fire door, and high 10cm, the dark 30cm of stove, its temperature is adjustable in ℃ scope of room temperature～1200.Tubular nozzle in borosilicate glass tube operating rate and the cycle by step motor control.Underlayer temperature is detected by thermocouple.Carrier gas (air) is produced by air compressor, and throughput is controlled by Pressure gauge.The ultrasonic vibration frequency 1.7MHz of emission type piezoelectric ceramic transducer wafer, diameter 25mm, atomization quantity 400～500dm
3h
-1This experimental provision has 6 Φ 25 piezoelectric ceramic transducers, by the starting of oscillation number size of regulating atomization quantity of control transducer.The spraying deposition time is controlled by the time relay.5.2 the cleaning of technical process 5.2.1 backing material
With clear water substrate surface is cleaned up earlier, again substrate is put into potassium bichromate (K
2CrO
7) the concentrated sulfuric acid (H
2SO
4) in the saturated solution behind the dipping 2h-4h, the ultrasonic cleaning machine of putting into supersonic frequency and be 20kHz-40kHz cleans 30min with distilled water.Taking-up places clean baking oven dry for standby.5.2.2 the preparation of source solution
Take by weighing the SnCl of 25g～30g
45H
2O was with 10: 1 H
2O and CH
3OH is mixed with solution, adds the NH of 3g～5g again
4The F aqueous solution stirs, and pours in the ultrasonic atomizatio generator.
SnCl
45H
2O can be between 22g～30g, H
2O and CH
3OH can be between 8: 1～12: 1, NH
4The F aqueous solution can be between 1g～6g; 5.2.3 the preparation of film
Set experiment parameters such as the size of distance, nozzle operating rate and cycle between underlayer temperature, nozzle and substrate, atomization quantity and carrier gas air pressure, as between 380 ℃～450 ℃ of underlayer temperatures, nozzle and substrate apart from 6mm～12mm, stepping motor gait of march 0.5m/s～2.5m/s, atomization quantity 1800dm
3h
-1～2500dm
3h
-1And carrier gas air pressure 1.2 * 10
5Pa～2.0 * 10
5Pa; Open stepping motor and ultrasonic atomizer, the ultrasonic vibration of piezoelectric ceramic transducer is with the solution atomization that is prepared, be carried into the Pyrex substrate of heating by carrier gas, complicated chemical reaction takes place in source solution under the high temperature on substrate, can deposit go out uniform SnO on substrate
2: the F film.Under the constant situation of atomization quantity, to SnO
2: the experiment parameter that the deposition rate of F film and light, electrical characteristics have the greatest impact is the F/Sn ratio of underlayer temperature and solution.5.2.4 annealing in process
Close fire door, the 30min that anneals under 400 ℃～480 ℃ temperature slowly cools to room temperature.5.2.5 encapsulation
The electrode of conductive film not only plays the effect that is connected with power supply, and different design (as size and position), can change the power of heating tube.Coat skim annular silver slurry equably at the two ends of heating tube inwall.Behind the airing, press the heating curve sintering regular hour of setting under the room temperature.Welding lead on two electrodes is used the insulative water-proof material package again.5.3 atomization process
When piezoelectric ceramic transducer wafer during, above near the solution the center wafer, evoke the water column that is similar to fountain with certain frequency vibration.Meanwhile, because the vibration of supersonic frequency produces cavitation on the water column surface, make solution be atomized into a large amount of suspended particulates.The diameter of this atomized particles is relevant with the frequency of ultrasonic vibration with the kind of solution (surface tension and density).For the solution that oneself prepares, the diameter of atomized particles depends on the frequency of ultrasonic vibration.For example, when the frequency of ultrasonic vibration was 800kHz, the atomized particles diameter of the aqueous solution was 4.5 μ m, and the atomized particles diameter of butanol solution then is 3.6 μ m.Therefore, the size of source solution ultrasonic atomization particulate can be regulated by the frequency of ultrasonic vibration, and the uniformity of atomized particles is much better than the effect of any spray gun spraying.Clearly, the diameter of the flow rate of carrier gas of ullrasonic spraying and solution atomization particulate is irrelevant, only works to carry atomized particles.Spray gun then is to rely on the air blast sprayed solution to produce atomizing, and the diameter of atomized particles reduces with the increase of air-flow.So the ullrasonic spraying carrier gas flux can be much smaller than the required carrier gas of gun spraying; Like this, in preparation during film, the ullrasonic spraying air-flow is to the influence of the underlayer temperature situation much smaller than the spray gun spraying, makes the control of ultrasonic atomizatio depositing technics with relatively easy to the control that becomes diaphragm area.5.4 the effect 5.4.1 XRD analysis of invention
With RAX-12 type X-ray diffractometer to SnO
2: the F film carries out material phase analysis, the X-ray target CuK α of experiment usefulness, tube voltage 40kV, tube current 100mA, counter tube voltage 800V.The result shows, SnO
2: the F film is mainly polycrystalline structure and a small amount of amorphous state is formed, and its (200) and (110) crystal face diffracted intensity are bigger.Can try to achieve SnO according to the diffraction index and the angle of diffraction that XRD analysis provides
2: the lattice parameter of F film is a=4.7183, and c=3.1736 is with SnO
2The lattice parameter a=4.7355 of standard card, the c=3.1846 basically identical.SnO
2: the interplanar distance d of F film and the interplanar distance of standard crystal be basically identical also, sees Table 1 (SnO
2: the F film interplanar distance and the standard interplanar distance table of comparisons).The SnO that under various substrate, prepares
2: the XRD analysis of F film shows, all samples is maximum and along with the relative diffracted intensity of rising (200) crystal face of underlayer temperature increases at the diffracted intensity of (200) crystal face, sees Table 2 (SnO
2: F film crystal face diffracted intensity is with the variation of underlayer temperature).
Table 1 SnO
2: the F film interplanar distance and the standard interplanar distance table of comparisons
5.4.2 SEM and STM analyze
| Interplanar distance d | Sample | Standard |
| ??(110) | ????3.2875 | ????3.350 |
| ??(101) | ????2.6121 | ????2.644 |
| ??(200) | ????2.3362 | ????2.369 |
| ??(211) | ????1.7508 | ????1.765 |
Usually, because SnO
2The conductivity of film is not high enough, so before carrying out the SEM morphology observation, also will be to SnO
2Film vapor deposition conductive layer (as golden film), the conductivity that increases sample is with the tolerance electron bombard.For prepared SnO
2: F film, resistivity only are 4 * 10
-4Ω cm, conductivity is quite high.Therefore, under the situation of not doing any increase conductivity processing, carry out the SEM morphology observation, obtained relatively clear photograph, see Fig. 2 (a).Stereoscan photograph the analysis showed that, with the SnO of ullrasonic spraying method deposit
2: though F film compactness is good, but still has hole, and average grain diameter is about 50nm, is in the good uniformity of discrete island and film basically.With STM to SnO
2: the F film has carried out morphology analysis, sees Fig. 2 (b), (c).Table 2 SnO
2: F film crystal face diffracted intensity is with the variation of underlayer temperature
5.4.3 heat efficiency comparative analysis
| Crystal face (hkl) | Underlayer temperature (℃) | |||
| ????400 | ????430 | ????460 | ????490 | |
| ????(110) ????(101) ????(200) ????(211) ????(310) ????(301) | ????61 ????58 ????100 ????64 ????0 ????18 | ????34 ????80 ????100 ????79 ????6 ????43 | ????9 ????10 ????100 ????19 ????10 ????12 | ????8 ????6 ????100 ????17 ????16 ????14 |
SnO with 300W
2: F transparent electric heating film heating pipe and heating wire heating tube (immersion heater) are the contrast experiment that heats up water, water 300ml, 16 ℃ of initial temperatures, 100 ℃ of final temperatures.Calculate institute's calorific requirement by formula:
Q＝CV(T
2-T
1)＝105.3?kJ?????????①
Test result sees Table 3 (SnO
2: F electrothermal film heating pipe and the heating wire immersion heater heat efficiency contrast experiment that heats up water).
Table 3 SnO
2: F electrothermal film heating pipe and the heating wire immersion heater heat efficiency contrast experiment that heats up water
| Power (W) | Initial temperature (℃) | The heater element final temperature (℃) | Voltage (V) | Resistance (Ω) | Time Δ t heats up water | Produce heat Q '=U 2At/R ????(kJ) | Heat efficiency Q/Q ' % | |
| SnO 2: the F Electric radiant Heating Film | ??300 | ??16 | ????121 | ?220 | ?161 | ?6’30” | ????117.1 | ??89.92％ |
| The heating wire immersion heater | ??300 | ??16 | ????330 | ?220 | ?165 | ?11’1” | ????193.8 | ??54.33％ |
Experiment shows, SnO
2: the thermal efficiency ratio heating wire heating tube of F transparent electric heating film heating pipe is high by 35.6%.5.4.4 resistivity is referring to table 4 table 4 SnO
2: the resistivity of F transparent conductive film
5.4.5 visible light transmissive counting rate meter 5 SnO
2: the visible light transmissivity of F transparent conductive film
5.4.6 power density
| Sample 1 (Ω cm) | Sample 2 (Ω cm) | Sample 3 (Ω cm) | Sample 4 (Ω cm) |
| ????6.7×10 -4 | ????4.3×10 -4 | ????4.0×10 -4 | ????5.2×10 -4 |
| Sample 1 (%) | Sample 2 (%) | Sample 3 (%) | Sample 4 (%) |
| ????92.1 | ????88.6 | ????89.7 | ????91.5 |
Table 6 SnO
2: F electrothermal film heating pipe power density
5.5 comparison 5.5.1 electric conversion efficiency height, energy saving with other heating elements
| Sample 1 (W/cm 2) | Sample 1 (W/cm 2) | Sample 1 (W/cm 2) | Sample 1 (W/cm 2) |
| ????34.6 | ????36.2 | ????35.5 | ????34.9 |
Electric radiant Heating Film is planar exothermic material, forms thermal conductive surface to greatest extent with heated object, and heat transfer resistance is little, during the energising heating, heat energy can be passed to heated object very soon, and Electric radiant Heating Film does not have, and rubescent, scorching hot phenomenon produces, the radiation heat loss is very little, and the heat efficiency is quite high, generally about 90%.And traditional heating wire, because radiating surface is little, in the electric heating transfer process, the heat energy that electric energy produced can not be passed to heated object very soon, cause on the heating wire heat too concentrated, become scorching hot, rubescent very soon, the considerable part of electric energy becomes the luminous energy of various wavelength and scatters and disappears, and causes electric conversion efficiency low.In the contrast experiment, boil the synthermal water of equivalent with same power, same container, Electric radiant Heating Film is than heating wire (immersion heater) 35.6% (the seeing Table 3) of will economizing on electricity.5.5.2 the life-span is long, not fragile
General heating wire always uses under scorching hot, rubescent state, so be easy to produce oxidation, cause and opens circuit.And Electric radiant Heating Film in when work because area of dissipation is big, heat conduction is fast, so self temperature is lower, this has just solved the autoxidation problem of electrothermal film material under "on" position, has prolonged useful life.On the other hand, the physics of transparent electric heating film, chemical property are very stable, and himself fusing point is more than 1000 ℃, and heat resisting temperature is very high, Heat stability is good.The Electric radiant Heating Film corrosion resistance is extremely strong, soaks 72 hours the performance no change in concentrated hydrochloric acid, red fuming nitric acid (RFNA), the concentrated sulfuric acid or strong base solution.Continuously non-oxidation phenomenon, performance no change are used in 7200 hours processes in energising.In addition, the anti-wear performance of transparent electric heating film is fabulous, and is suitable with hardness quartzy, topaz, and the friction in general the use is had no effect to transparent electric heating film.5.5.3 the outward appearance selectivity is strong, applied widely
Transparent electric heating film directly on the insulating bodies such as coated glass, pottery, mica, is not subjected to the restriction of matrix surface shape, but the equal coated of various complicated vessel or working surface, and this specific character of Electric radiant Heating Film makes its scope of application more widely than the traditional electrical thermal element.5.5.4 thermal inertia is little
The transparent electric heating film thickness accumulates heat hardly less than 1 micron during use, thermal inertia is little.For example boil water with strip heater or boil milk, when reaching the boiling point outage, water can continue boiling because of thermal inertia, milk then overflow.And with the transparent electric heating film heater when water or milk reach the boiling point outage owing to seethe with excitement and promptly end in the little outage of thermal inertia back, milk can not overflow.5.5.5 the flames of anger, safe and reliable
Often have naked light to produce during heating wire energising heating, the chance combustibles are promptly on fire.The transparent electric heating film heating pipe can not produce naked light when heating liquid, when heater was in 100 ℃ of boiling water states, Electric radiant Heating Film can burnt paper, cotton, and timber contacts with it also and can not ignite.Therefore, Electric radiant Heating Film is well suited for some needs heat tracing, does not allow the special occasions of naked light again.5.5.6 product Miniaturizable, slimming
The thickness of Electric radiant Heating Film is less than 1 micron, and coated can make product miniaturization, slimming on electric heating appliance.Convenient transportation is lightly attractive in appearance.5.5.7 processing technology is simple, simple in structure, cost is low
Replace traditional electrical thermal elements such as heating wire, electric hot tray, electrothermal tube with Electric radiant Heating Film, can save many auxiliary material, thereby the electric heating element structure is greatly simplified.The Electric radiant Heating Film manufacturing process is simple, and weight and cost can reduce significantly, and the Electric radiant Heating Film raw material are the general industry raw material, and are with low cost.5.6 use embodiment
Embodiment 1: industrial acid-washed need are heated to about 80 ℃, and heat with the titanium heating tube of acid corrosion-resistant in this field at present.Titanium costs an arm and a leg, 500～600 yuan of titanium heating tubes.And adopt the single tube shown in the accompanying drawing 3,4 can reach the effect identical fully with the titanium heating tube with compound tube, and its cost dozens of yuan only reduces industrial cost greatly.
Embodiment 2: for solving oil dripping phenomenon in certain product, obtain area 1cm with heating wire on mica sheet
2Thickness is used for the atomizing of carburetor to oil droplet less than the high temperature that the heating plate of 1mm is kept more than 300 ℃ local space, but there is the shortcoming of easy oxidation fracture of wire in heating wire.Adopt the electro-thermal film ceramic sheet in the accompanying drawing 5, can keep high temperature for a long time, address the above problem.
Claims (4)
1. supersonic spraying prepares SnO
2: the technology of F electrothermal film heating pipe, it is characterized in that, use the ullrasonic spraying method with SnO
2: the F Electric radiant Heating Film prepares equably at resistant to elevated temperatures Pyrex inside pipe wall, makes to be used for the particularly heating tube of corrosive liquids heating of liquid; Carry out according to the following steps: the 1) cleaning of backing material
With clear water substrate surface is cleaned up earlier, again substrate is put into potassium bichromate (K
2CrO
7) the concentrated sulfuric acid (H
2SO
4) in the saturated solution behind the dipping 2h-4h, put into ultrasonic cleaning machine and clean 30min with distilled water, take out and place clean baking oven dry for standby; 2) preparation of source solution
Take by weighing the SnCl of 22g～30g
45H
2O places beaker, and the adding volume ratio is 8: 1～12: 1 H
2O and CH
3OH mixes liquid, adds 1g～6g NH again
4The F aqueous solution stirs, and pours in the ultrasonic atomizatio generator; The surperficial coated layer protecting film of ultrasonic atomizatio piezoelectric ceramic wafer is to prevent the corrosion of soup to piezoelectric ceramic wafer; 3) preparation of film
Design temperature control makes 380 ℃～450 ℃ of underlayer temperatures; Between nozzle and substrate apart from 6mm～12mm, stepping motor gait of march 0.5m/s～2.5m/s, atomization quantity 1800dm
3h
-1～2500dm
3h
-1And carrier gas air pressure 1.2 * 10
5Pa～2.0 * 10
5Behind the Pa, open stepping motor and ultrasonic atomizer, the ultrasonic vibration of piezoelectric ceramic transducer is with the solution atomization that is prepared, be carried into the nozzle of ultrasonic atomizer by carrier gas, under Stepping Motor Control, the soup droplet is delivered to the Pyrex substrate of heating equably, and chemical reaction takes place on substrate source solution under the high temperature, can deposit go out uniform SnO on substrate
2: the F film; 4) annealing in process
Close fire door, the 30min that anneals under 400 ℃～480 ℃ temperature slowly cools to room temperature and gets final product; 5) encapsulation
Coat skim annular silver slurry equably at the two ends of heating tube inwall.Behind the airing, starch the heating curve of 20 ℃～600 ℃ of variations of requirement, sintering 1h～3h under the room temperature by used silver; Welding lead on two end electrodes is used the insulative water-proof material package again.
2. supersonic spraying according to claim 1 prepares SnO
2: the technology of F electrothermal film heating pipe is characterized in that described piezoelectric ceramic transducer has 6, by the starting of oscillation number size of regulating atomization quantity of control transducer.
3. supersonic spraying according to claim 1 prepares SnO
2: the technology of F electrothermal film heating pipe is characterized in that the supersonic frequency of described ultrasonic cleaning machine is 20kHz-40kHz.
4. supersonic spraying according to claim 2 prepares SnO
2: the technology of F electrothermal film heating pipe, it is characterized in that described piezoelectric ceramic transducer wafer is an emission type, its ultrasonic vibration frequency is 1.7MHz.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021394326A CN1153506C (en) | 2002-09-20 | 2002-09-20 | Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021394326A CN1153506C (en) | 2002-09-20 | 2002-09-20 | Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1402594A true CN1402594A (en) | 2003-03-12 |
| CN1153506C CN1153506C (en) | 2004-06-09 |
Family
ID=4750079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021394326A Expired - Fee Related CN1153506C (en) | 2002-09-20 | 2002-09-20 | Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1153506C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441055C (en) * | 2005-03-23 | 2008-12-03 | 冷同桂 | Composite metal electrothermal film sol and method for producing electroheating tube with the same |
| CN102235945A (en) * | 2010-04-23 | 2011-11-09 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| CN102735522A (en) * | 2011-04-12 | 2012-10-17 | 金华职业技术学院 | Apparatus for preparing single-molecule sample by supersonic wave |
| CN107698171A (en) * | 2017-08-31 | 2018-02-16 | 浙江大学 | A kind of preparation method of TiN coated glasses |
| CN109768118A (en) * | 2018-12-27 | 2019-05-17 | 浙江师范大学 | The preparation method of arsenic and fluorin-doped tin oxide Position-Sensitive Detector |
| CN109862631A (en) * | 2019-04-04 | 2019-06-07 | 浙江大学 | A kind of preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film |
| CN111646708A (en) * | 2020-07-07 | 2020-09-11 | 浙江山蒲照明电器有限公司 | Spraying mechanism for inner wall of glass tube |
| CN114272936A (en) * | 2021-12-28 | 2022-04-05 | 中国科学院宁波材料技术与工程研究所 | Multi-element metal oxide film and preparation method and application thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1784087B (en) * | 2004-11-30 | 2010-05-05 | 林正平 | Tubular internal electric heating film heater and its electrode structure |
-
2002
- 2002-09-20 CN CNB021394326A patent/CN1153506C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100441055C (en) * | 2005-03-23 | 2008-12-03 | 冷同桂 | Composite metal electrothermal film sol and method for producing electroheating tube with the same |
| CN102235945A (en) * | 2010-04-23 | 2011-11-09 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| CN102235945B (en) * | 2010-04-23 | 2013-02-20 | 昆明物理研究所 | Method for preparing amorphous film sample for transmission electron microscope research |
| CN102735522A (en) * | 2011-04-12 | 2012-10-17 | 金华职业技术学院 | Apparatus for preparing single-molecule sample by supersonic wave |
| CN107698171A (en) * | 2017-08-31 | 2018-02-16 | 浙江大学 | A kind of preparation method of TiN coated glasses |
| CN109768118A (en) * | 2018-12-27 | 2019-05-17 | 浙江师范大学 | The preparation method of arsenic and fluorin-doped tin oxide Position-Sensitive Detector |
| CN109768118B (en) * | 2018-12-27 | 2020-06-23 | 浙江师范大学 | Preparation method of arsenic and fluorine co-doped tin oxide position sensitive detector |
| CN109862631A (en) * | 2019-04-04 | 2019-06-07 | 浙江大学 | A kind of preparation method of NEW TYPE OF COMPOSITE plate Electric radiant Heating Film |
| CN111646708A (en) * | 2020-07-07 | 2020-09-11 | 浙江山蒲照明电器有限公司 | Spraying mechanism for inner wall of glass tube |
| CN114272936A (en) * | 2021-12-28 | 2022-04-05 | 中国科学院宁波材料技术与工程研究所 | Multi-element metal oxide film and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1153506C (en) | 2004-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4727355B2 (en) | Deposition method | |
| Yadav et al. | Electrical, structural and optical properties of SnO2: F thin films: Effect of the substrate temperature | |
| CN201751427U (en) | Linear evaporation source | |
| CN1153506C (en) | Process of mfg. electrothermal SnO2:F film heating pipe by ultrasonic spray | |
| CN101164689A (en) | Nanocrystalline porous TiO2 film and preparation method thereof | |
| CN101003420B (en) | Technique for preparing Nano Sn02/Ti02 composite film in use for photovoltaic conversion | |
| JP6529615B2 (en) | Planar heating element and electrically conductive thin film | |
| CN102761995B (en) | Semiconductor electrothermal membrane preparation method | |
| CN1032673C (en) | Semiconductor electric-heating thin film and manufacture thereof | |
| JP6614764B2 (en) | Piezoelectric thin film and manufacturing method thereof, piezoelectric thin film manufacturing apparatus, and liquid discharge head | |
| TW201034991A (en) | Conductive film formation on glass | |
| US5009928A (en) | Method for forming a transparent conductive metal oxide film | |
| CN1670252A (en) | Device and method for preparing nanometer oxide nesa by ultrasound rapid deposition method | |
| CN103332870B (en) | A kind of preparation method of nano-titanium dioxide film | |
| CN105142250A (en) | Preparation method for semiconductor thermoelectric film | |
| CN103781209A (en) | Nano electric heating plate using chemical vapor deposition technology and manufacturing method thereof | |
| CN107963805B (en) | Method for preparing self-cleaning and anti-fog glass by using annealing process | |
| JP2005116391A (en) | Apparatus of manufacturing substrate for transparent electrode | |
| JPS62213281A (en) | Transparent conductive film | |
| Gunasekaran et al. | Modulation of ZnO film thickness and formation of water-hyacinth nanostructure | |
| JP2006016273A (en) | Film deposition system based on spray pyrolysis method | |
| CN101724815B (en) | Method for preparing energy-saving heating films | |
| KR101694751B1 (en) | Apparatus for supplying precursors for forming thin film and film forming apparatus having the same | |
| JPH0645888B2 (en) | Deposited film formation method | |
| CN102842636A (en) | Substrate heating base used for chemical vapor deposition system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |