CN105294074A - Method for preparing oxide film type thermocouple by using screen printing technology - Google Patents
Method for preparing oxide film type thermocouple by using screen printing technology Download PDFInfo
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- CN105294074A CN105294074A CN201510772034.7A CN201510772034A CN105294074A CN 105294074 A CN105294074 A CN 105294074A CN 201510772034 A CN201510772034 A CN 201510772034A CN 105294074 A CN105294074 A CN 105294074A
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Abstract
The invention relates to a method for preparing an oxide film type thermocouple by using screen printing technology. The screen printing technology is employed for deposition of the oxide thick-film thermocouple used for high temperature measurement on a high temperature ceramic substrate. The thick-film thermocouple can be directly pasted on the surface of the ceramic substrate, is applicable to an oxidation atmosphere and can stably work at a high temperature of 1000 to 1250 DEG C for a long time.
Description
[technical field]
The present invention relates to sensor technology of preparing and high-temperature temperature field of measuring technique, be specially a kind of method adopting silk-screen printing technique to prepare sull type thermopair.
[background technology]
In Aeroengine Design and confirmatory experiment, in order to the design of the efficiency of combustion and cooling system of verifying engine, need the temperature at the positions such as accurate test engine turbine blade surface, Inner Wall of Combustion Chamber.Linearly to compare with block shape thermopair with traditional, pyroceramic type thick film thermocouple has the features such as thermal capacity is little, volume is little, fast response time, transient temperature change can be caught, thick film thermocouple can be directly deposited on the surface of measurand simultaneously, do not destroy unit under test structure, and little on the impact of unit under test Working environment.Therefore be more suitable for for surface transient temperature measuring.Hot-end component surface temperature distribution situation accurately can be understood by thick film thermocouple, heat transfer, cooling scheme design can be optimized, and then ensure that engine operation is in optimum working order, raising motor efficiency, for the design of new-generation fighter and airline carriers of passengers provides reliable basis.
Research at present to NiCr/NiSi film thermocouple, relative maturity, but its Range of measuring temp is low, only adapts to test occasion with medium and low temperature.In high temperature test field, usually adopt the precious metal such as platinum, rhodium to be thin-film material, but there is the problems such as cost is high, error is large, severe environment are oxidizable due to it.Therefore, in the urgent need to developing a kind of new ceramics film thermocouple of high temperature resistant, stable performance.In existing research, ITO and In of film-type
2o
3material is expected to become pyrometric core preferred material.Be expected to the important breakthrough point becoming development of new ceramic base film thermocouple.
[summary of the invention]
The present invention be directed to the defect of current material system and higher application demand, provide a kind of method adopting silk-screen printing technique to prepare sull type thermopair, be applicable to thick film thermocouple of pyroceramic substrate and preparation method thereof.
To achieve these goals, technical scheme of the present invention:
Adopt silk-screen printing technique to prepare a method for sull type thermopair, comprise the following steps:
1) respectively to adding organic solvent in tin-doped indium oxide ceramic powder and Indium sesquioxide ceramic powder and additive makes two groups of ceramic sizes, as two thermode materials of oxide thickness membranous type thermopair;
2) in conjunction with graphical mould plate technique, design respectively and there is thermode one and supporting a pair screen printing screens of thermode two figure, choose one of them screen printing screens to place on a ceramic substrate, getting one group of ceramic size is again placed in above screen printing screens, adopt printing scraper to apply pressure at ceramic size position to make it to move from one end of screen printing screens to the other end, under the effect of printing scraper, ceramic size is through the mesh on screen printing screens, print out a thermode, and 80 ~ 100 DEG C of dryings 2 ~ 5 hours, obtain a dried printing heat electrode,
3) another screen printing screens supporting with thermode in step 2 is chosen, according to step 2) identical technique prepares another printing heat electrode on a ceramic substrate, namely obtains thermode one that silk-screen printing technique makes and thermode two;
4) shaping oxide thickness membranous type thermopair is obtained through high-temperature heat treatment again; High-temperature heat treatment condition is: in air or oxygen atmosphere, and 1000-1200 DEG C of process 3-5 hour, heat-up rate is 3-5 DEG C/min.
As a further improvement on the present invention, in tin-doped indium oxide ceramic powder, Theil indices is 5-10%.
As a further improvement on the present invention, ceramic powder granularity is 50-500 nanometer, and purity is more than 99%.
As a further improvement on the present invention, organic solvent is Terpineol 350, and additive is ethyl cellulose or 2-Butoxyethyl acetate.
As a further improvement on the present invention, often organize in ceramic size, the weight of ceramic powder accounts for the 40%-60% of ceramic powder and organic solvent gross weight, additive add the 9%-11% that weight is ceramic powder weight.
As a further improvement on the present invention, the screen mesh printing plate specification that silk-screen printing technique is used is 200-300 order.
As a further improvement on the present invention, thermode one and thermode two are that specular is arranged along ceramic substrate medullary ray, and two groups of thermode overlap joints form U-shaped structure or V-structure, and thermode one and thermode two one end portion overlap overlap joint form hot junction.
As a further improvement on the present invention, the length of two groups of thermodes is 8-40cm, and width is 3mm-12mm, and thickness is 1-50 μm.
As a further improvement on the present invention, the length in two thermode overlap joint coincidence districts is 0.5-3cm.
As a further improvement on the present invention, ceramic substrate is the structural ceramics of aluminum oxide, mullite or SiC.
Relative to prior art, the present invention has the following advantages:
Adopt silk-screen printing technique to prepare a method for sull type thermopair, adopt silk-screen printing technique, preparation technology is simple, can be used for the oxide compound thick film thermocouple of high-temperature temperature measurement in the preparation of pyroceramic deposition on substrate.Adopt ceramic to prepare thick film, the sticking power between thermode rete and substrate can be improved well.Due to the existence of powder granule, between thick film thermode and ceramic substrate, the anchor at interface increases, under the effect of additive, contact area between them increases, easier in mechanical interlocked or other physicochemical change of interface generation, finally make the physical strength of thick film improve, sticking power significantly improves.High-temperature service performance for thick film has good improvement result.The acting in conjunction of these two aspects, for the long-time use at high temperature of thick-film type thermopair, all has obvious advantage.This thick film thermocouple adopt directly mount or be deposited on ceramic substrate surface, can be used in oxidizing atmosphere, can under 1000 DEG C of-1250 DEG C of high temperature long-term stable operation.The present invention adopts new ceramics thermocouple material, compares common K type thermopair, has temperature-measuring range wider, and can adapt to the advantage of oxidation and acid or alkali environment; Compare the resistance to thermocouple material of other types as platinum rhodium etc., within the scope of identical temperature test, its thermopair cost is low, and is applicable to the extreme ambient temperature test in fields such as space flight and aviation.
Further, adopt the good ceramic of grain development to prepare thick film in this technique, the size of powder is in 50-500nm scope.Owing to adopting, grain development is good, the ceramic of compact structure, its heat shock resistance and adaptability to changes significantly strengthen, macrobead decomposes and the possibility of directly volatilization reduces, the thermal evaporation effect affecting film heat stability weakens, thus effectively keeps the high temperature resistant and military service performance of thick film thermode.
[accompanying drawing explanation]
The ITO-In that Fig. 1 adopts silk-screen printing technique to prepare
2o
3thick film thermocouple structure iron;
The ITO-In that Fig. 2 adopts silk-screen printing technique to prepare
2o
3thick film thermocouple cross-section structure;
The ITO-In that Fig. 3 silk-screen printing technique prepares
2o
3the XRD result of thick film;
The section SEM result of 10% content ITO thick film thermode of preparation in Fig. 4 specific embodiment 1;
The ITO-In that Fig. 5 silk-screen printing technique prepares
2o
3the temperature-voltage curve of thick film thermocouple;
In figure, 1-ceramic substrate, 2-hot junction, 3-thermode one, 4-thermode two, (wherein thermode one and thermode two are respectively ITO and In
2o
3one), 5-lead end.
[embodiment]
Below in conjunction with the drawings and specific embodiments, the present invention will be further described, the invention is not restricted to following examples.
A kind of oxide thickness membranous type thermopair comprises ceramic substrate 1 and ceramic thermoelectric pole layer, and described ceramic thermoelectric pole layer is by be that the thermode 1 of specular setting and thermode 24 form along ceramic substrate 1 medullary ray; Thermode 1 and thermode 24 form the hot junction 2 of this thermopair by overlap.
The base substrate layer that described ceramic thick film thermopair is arranged from bottom to top and function thermode layer.Hot thermocouple electrode all adopts silk-screen printing technique to realize.Wherein thermode 1 is tin-doped indium oxide (ITO) ceramic thick film, and the content of its stannic oxide is within the scope of 5-10%, and described thermode 24 is pure Indium sesquioxide (In
2o
3) ceramic thick film.The raw material adopted respectively during concrete enforcement is ITO and In
2o
3ceramic powder, the size range of powder is in 20-200 nanometer, and purity is more than 99%; The content of powder and organic ink is than being 30-60%, and operational organic ink has the mixing solutions of the superpolymer such as ethyl cellulose, Terpineol 350,2-Butoxyethyl acetate.
The thickness of thick film thermode prepared in the present invention is in 1.0-50 micrometer range, and the length of thick film thermode is between 8-40cm.The thickness of thick film is larger, can time of hot operation longer.The thick film of deposition preparation needs through (1000-1200 DEG C) high-temperature heat treatment 3-5 hour to improve the density of thick film.
In the present invention, the ceramic substrate selected by thick film thermocouple of required preparation can be the high-temperature structural ceramics such as aluminum oxide, mullite, SiC.
Embodiment 1
The ITO oxide thermoelectricity pole component selected to be Theil indices be 10% indium tin oxide material, Indium sesquioxide thermode component is the single oxide of purity 99%, adopt silk-screen printing technique at thickness be 3mm aluminium oxide ceramic substrate on deposit thick film thermode, the ceramic size for silk screen printing is made up of the powder of ITO and the powder of Indium sesquioxide respectively.The granularity of powder is 100nm, adopt terpineol solution as organic solvent, by ceramic powder and Terpineol 350 according to the quality of 1:1 than Homogeneous phase mixing, and add the ethyl cellulose of ceramic powder quality 10%, and carry out strong stirring mixing, as the ceramic size for silk screen printing.Good graphical in order to obtain, choosing thermode length is 12cm, and width is the silk screen printing preparation that the U-shaped structure mask plate of 4mm carries out thick film thermode, and half tone used is 200 orders.First on substrate, print ITO thick film, and then print Indium sesquioxide thick film, after two kinds of thick-film materials all deposit and terminate, by the 1200 DEG C of thermal treatment 4 hours in retort furnace of thick film sample, heat-up rate remains on 3 DEG C/min, finally prepares the ITO-In with U-shaped structure that film thickness is 50 microns
2o
3thick-film type thermopair.The ITO-In that Fig. 3 silk-screen printing technique prepares
2o
3the XRD result of thick film, Fig. 4 is the section SEM photo of the ITO thick film adopting this technique to prepare.The ITO-In that Fig. 5 silk-screen printing technique prepares
2o
3the temperature-voltage curve of thick film thermocouple.Show that this oxide compound thick film thermocouple can 1250 DEG C of steady operations more than 10 hours.
Embodiment 2
The ITO oxide thermoelectricity pole component selected to be Theil indices be 5% indium tin oxide material, Indium sesquioxide thermode component is the single oxide of purity 99%, adopt silk-screen printing technique at thickness be 5mm aluminium oxide ceramic substrate on deposit thick film thermode, the ceramic size for silk screen printing is made up of the powder of ITO and the powder of Indium sesquioxide respectively.The granularity of powder is 200nm, adopt terpineol solution as organic solvent, by ceramic powder and Terpineol 350 according to the quality of 2:3 than Homogeneous phase mixing, and add the ethyl cellulose of ceramic powder quality 9%, and carry out strong stirring mixing, as the ceramic size for silk screen printing.As the ceramic size for silk screen printing.Good graphical in order to obtain, choosing thermode length is 25cm, and width is the silk screen printing preparation that the U-shaped structure mask plate of 5mm carries out thick film thermode.First on substrate, print In
2o
3thick film, and then print ITO thick film, after two kinds of thick-film materials all deposit and terminate, by the 1200 DEG C of thermal treatment 5 hours in retort furnace of thick film sample, heat-up rate remains on 3 DEG C/min, finally prepares the ITO-In with U-shaped structure that film thickness is 40 microns
2o
3thick-film type thermopair.
Embodiment 3
The ITO oxide thermoelectricity pole component selected to be Theil indices be 10% indium tin oxide material, Indium sesquioxide thermode component is the single oxide of purity 99%, adopt silk-screen printing technique at thickness be 10mm aluminium oxide ceramic substrate on deposit thick film thermode, the ceramic size for silk screen printing is made up of the powder of ITO and the powder of Indium sesquioxide respectively.The granularity of powder is 200nm, adopt terpineol solution as organic solvent, by ceramic powder and Terpineol 350 according to the quality of 3:2 than Homogeneous phase mixing, and add the ethyl cellulose of ceramic powder quality 11%, and carry out strong stirring mixing, as the ceramic size for silk screen printing.As the ceramic size for silk screen printing.Good graphical in order to obtain, choosing thermode length is 20cm, and width is the silk screen printing preparation that the U-shaped structure mask plate of 1.0cm carries out thick film thermode.First on substrate, print ITO thick film, and then print Indium sesquioxide thick film, after two kinds of thick-film materials all deposit and terminate, by the 1100 DEG C of thermal treatment 4 hours in retort furnace of thick film sample, heat-up rate remains on 3 DEG C/min, finally prepares the ITO-In with U-shaped structure that film thickness is 50 microns
2o
3thick-film type thermopair.
Embodiment 4
The ITO oxide thermoelectricity pole component selected to be Theil indices be 5% indium tin oxide material, Indium sesquioxide thermode component is the single oxide of purity 99%, adopt silk-screen printing technique at thickness be 10mm aluminium oxide ceramic substrate on deposit thick film thermode, the ceramic size for silk screen printing is made up of the powder of ITO and the powder of Indium sesquioxide respectively.The granularity of powder is 50nm, adopt terpineol solution as organic solvent, by ceramic powder and Terpineol 350 according to the quality of 1:1 than Homogeneous phase mixing, and add the ethyl cellulose of ceramic powder quality 10%, and carry out strong stirring mixing, as the ceramic size for silk screen printing.As the ceramic size for silk screen printing.Good graphical in order to obtain, choosing thermode length is 20cm, and width is the silk screen printing preparation that the V-structure mask plate of 5mm carries out thick film thermode.First on substrate, print In
2o
3thick film, and then print ITO thick film, after two kinds of thick-film materials all deposit and terminate, by the 1000 DEG C of thermal treatment 5 hours in retort furnace of thick film sample, heat-up rate remains on 5 DEG C/min, finally prepares the ITO-In with V-structure that film thickness is 30 microns
2o
3thick-film type thermopair.
Claims (10)
1. adopt silk-screen printing technique to prepare a method for sull type thermopair, it is characterized in that, comprise the following steps:
1) respectively to adding organic solvent in tin-doped indium oxide ceramic powder and Indium sesquioxide ceramic powder and additive makes two groups of ceramic sizes, as two thermode materials of oxide thickness membranous type thermopair;
2) in conjunction with graphical mould plate technique, design respectively and there is thermode one (3) and supporting a pair screen printing screens of thermode two (4) figure, choosing one of them screen printing screens is placed on ceramic substrate (1), getting one group of ceramic size is again placed on screen printing screens, adopt printing scraper to apply pressure at ceramic size position to make it to move from one end of screen printing screens to the other end, under the effect of printing scraper, ceramic size is through the mesh on screen printing screens, print out a thermode, and 80 ~ 100 DEG C of dryings 2 ~ 5 hours, obtain a dried printing heat electrode,
3) another screen printing screens supporting with thermode in step 2 is chosen, according to step 2) identical technique prepares another printing heat electrode on ceramic substrate (1), namely obtains thermode one (3) that silk-screen printing technique makes and thermode two (4);
4) shaping oxide thickness membranous type thermopair is obtained through high-temperature heat treatment again; High-temperature heat treatment condition is: in air or oxygen atmosphere, and 1000-1200 DEG C of process 3-5 hour, heat-up rate is 3-5 DEG C/min.
2. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, is characterized in that: in tin-doped indium oxide ceramic powder, Theil indices is 5-10%.
3. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, it is characterized in that: ceramic powder granularity is 50-500 nanometer, purity is more than 99%.
4. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, it is characterized in that: organic solvent is Terpineol 350, additive is ethyl cellulose or 2-Butoxyethyl acetate.
5. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, it is characterized in that: often organize in ceramic size, the weight of ceramic powder accounts for the 40%-60% of ceramic powder and organic solvent gross weight, additive add the 9%-11% that weight is ceramic powder weight.
6. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, is characterized in that: silk-screen printing technique screen mesh printing plate specification used is 200-300 order.
7. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, it is characterized in that: thermode one (3) and thermode two (4) are that specular is arranged along ceramic substrate (1) medullary ray, two groups of thermode overlap joints form U-shaped structure or V-structure, and thermode one (3) and thermode two (4) one end portion overlap overlap joint form hot junction (2).
8. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 7, it is characterized in that: the length of two groups of thermodes is 8-40cm, and width is 3mm-12mm, thickness is 1-50 μm.
9. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 7, is characterized in that: the length in two thermode overlap joint coincidence districts is 0.5-3cm.
10. a kind of method adopting silk-screen printing technique to prepare sull type thermopair according to claim 1, is characterized in that: ceramic substrate is the structural ceramics of aluminum oxide, mullite or SiC.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107063492A (en) * | 2017-04-20 | 2017-08-18 | 武汉大学 | A kind of sign for safe evacuation of printed form temperature sensor and the application temperature sensor |
| CN112174678A (en) * | 2020-09-23 | 2021-01-05 | 中国科学院金属研究所 | High-strength two-dimensional ceramic silk screen material and preparation method thereof |
| CN112729580A (en) * | 2020-12-23 | 2021-04-30 | 西安交通大学 | Flexible temperature sensor and preparation method thereof |
| CN113959574A (en) * | 2021-09-26 | 2022-01-21 | 西安交通大学 | Thin-film thermocouple based on indium oxide composite material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007057260A (en) * | 2005-08-22 | 2007-03-08 | Osaka City | Temperature sensor element and method of manufacturing same |
| CN103900728A (en) * | 2014-04-23 | 2014-07-02 | 大连交通大学 | Ceramic thin film thermocouple and manufacture method thereof |
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- 2015-11-12 CN CN201510772034.7A patent/CN105294074B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007057260A (en) * | 2005-08-22 | 2007-03-08 | Osaka City | Temperature sensor element and method of manufacturing same |
| CN103900728A (en) * | 2014-04-23 | 2014-07-02 | 大连交通大学 | Ceramic thin film thermocouple and manufacture method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107063492A (en) * | 2017-04-20 | 2017-08-18 | 武汉大学 | A kind of sign for safe evacuation of printed form temperature sensor and the application temperature sensor |
| CN112174678A (en) * | 2020-09-23 | 2021-01-05 | 中国科学院金属研究所 | High-strength two-dimensional ceramic silk screen material and preparation method thereof |
| CN112729580A (en) * | 2020-12-23 | 2021-04-30 | 西安交通大学 | Flexible temperature sensor and preparation method thereof |
| CN113959574A (en) * | 2021-09-26 | 2022-01-21 | 西安交通大学 | Thin-film thermocouple based on indium oxide composite material and preparation method thereof |
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