CN102944321A - Preparation method of high-precision thick-film type thermocouple group for measuring micro-distance temperature difference - Google Patents
Preparation method of high-precision thick-film type thermocouple group for measuring micro-distance temperature difference Download PDFInfo
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- CN102944321A CN102944321A CN2012105221355A CN201210522135A CN102944321A CN 102944321 A CN102944321 A CN 102944321A CN 2012105221355 A CN2012105221355 A CN 2012105221355A CN 201210522135 A CN201210522135 A CN 201210522135A CN 102944321 A CN102944321 A CN 102944321A
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- negative pole
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Abstract
The invention relates to a preparation method of a high-precision thick-film type thermocouple group for measuring micro-distance temperature difference. Positive and negative pole slurry is sintered on a ceramic substrate, the negative poles are of vertical lines which are vertically parallel to the horizontal plane, the figures of the positive poles are a plurality of oblique lines which are parallel mutually, each oblique line is at a 45-degree angle with a horizontal plane, and the negative poles and the positive poles are arranged in a staggered way; and the negative poles and the positive poles which are adjacent to each other are connected end to end, the negative pole at a terminal is connected with a platinum thermocouple wire, and the positive pole at the terminal is connected with a platinum-rhodium thermocouple wire. The high-precision thick-film type thermocouple group prepared by the method is used for measuring the temperature difference between two points with a millimetre-sized distance in the aerospace field and has the advantage of high measurement precision.
Description
Technical field
The present invention relates to a kind of thermocouple assembly of the measuring distance temperature for aerospace field, particularly a kind of preparation method of the high-precision thick membranous type thermopair group for measuring the distance element temperature difference.
Background technology
Along with the development of science and technology and the needs of modern industrial technology, thermometry also constantly improves and improves, temperature-measuring range is more and more wider, and the kind of temperature element is also more and more more, and temperature measurer commonly used in the commercial production has resistance thermometer, temperature difference heat galvanic couple etc.Wherein the thick-film type thermopair is the brand-new temperature element of a kind of structure that utilizes the preparation of thick film screen printing technique.This process has that material consumption is low, the parameter adjustment cycle is short, can realize the characteristics such as large batch of mechanization production.
Needing with measuring distance in the aerospace field is the millimetre-sized point-to-point transmission temperature difference.Yet because heat radiation is very fast, the point-to-point transmission temperature difference of this slight distance is less, and considerably beyond the minimum resolution of traditional temperature measurer, the differential temperature survey error is larger.
Summary of the invention
Purpose of the present invention is exactly for the deficiencies in the prior art, provide a kind of high-precision thick membranous type thermopair group for measuring the distance element temperature difference the preparation method, it is the millimetre-sized point-to-point transmission temperature difference that the thermopair group of this method preparation is used for the aerospace field measuring distance, and the high advantage of measuring accuracy is arranged.
For achieving the above object, technical solution of the present invention is as follows:
Be used for to measure the distance element temperature difference high-precision thick membranous type thermopair group the preparation method, following steps are arranged:
1) preparation of slip:
Cathode size comprises pure platinum powder, glass dust and organic solvent, behind three's mixing, makes cathode size, and wherein, the weight ratio of pure platinum powder, glass dust and organic solvent is 12:3:10; Anodal slip comprises pure platinum powder, pure rhodium powder, glass dust and organic solvent, after evenly mixing four, makes anode sizing agent, and wherein the weight ratio of pure platinum powder and pure rhodium powder is 9:1, and the weight ratio of platinum rhodium metal powder, glass dust and organic solvent is 12:3:10;
In its positive and negative electrode in the glass dust percentage by weight of each component be: 8%～11%Al
2O
3, 3%～6%MgO, 19%～22%BaO, 43%～46%H
3BO
3, 20%～23%SiO
2The percentage by weight of each component is in the organic solvent: ethyl cellulose 12 ~ 14%, butyl acetate 7 ~ 9 %, terpinol 72 ~ 75%, normal butyl alcohol 4 ~ 6 %.
2) making of negative pole:
Cathode size is printed on the ceramic substrate, sintering, forming thickness is the platinum layer negative pole of 30-40 μ m, and sintering temperature is: 1100 ℃, sintering time is 25min, and negative pole is many vertical lines with the surface level vertical parallel;
3) anodal making:
The positive electrode slurry is printed on the ceramic substrate that is printed on negative pole, sintering, forming thickness is the platinum rhodium layer positive pole of 30-40 μ m, the anodal junction temperature that burns is 1300 ℃, sintering time is 35min, many oblique lines that are parallel to each other just very, every oblique line is horizontal by 45° angle, and the quantity of anodal oblique line is identical with the quantity of negative pole vertical line;
Negative pole and positive pole are staggered, and adjacent negative pole and positive pole are end-to-end, and the negative pole of termination is connected with the platinum thermocouple silk, and positive pole is connected with the platinum rhodium thermocouple silk, make for the high-precision thick membranous type thermopair group of measuring the distance element temperature difference.
Pure platinum powder resistance ratio is 1.3851 described in the step 1), and particle diameter is 20～80 μ m.
The particle diameter of pure platinum powder and pure rhodium powder described in the step 1) is 20～80 μ m.
Step 2) length of every negative pole vertical line is for intending measuring the length of distance element in, and the spacing between adjacent cathode two vertical lines is 100～1000um.
The length of every positive pole is 1.41 times of length that intend to measure distance element in the step 3), and the spacing between adjacent two oblique lines is 100～1000um.
Described ceramic substrate contains 95% Al
2O
3
The making of thick film thermocouple group is printed first the platinum negative pole through twice printing and twice sintering for preventing that high temperature from polluting to adopt, 1100 ℃ of sintering, and the rear printing platinum rhodium utmost point, 1300 ℃ of sintering platinum rhodiums are anodal.
Behind the sintering, organic solvent volatilizees fully, only remains glass dust and metal powder (platinum powder or platinum rhodium powder), and wherein glass dust sticks in Al as connecting material with metal powder
2O
3On the ceramic substrate.
The present invention adopts the printing slurry technology that 100～1000 pairs of S type thermopairs are formed series circuit, therefore the thermoelectric force signal that will intend the point-to-point transmission of measurement has amplified 100～1000 times, the potential value that gathers is the mean value of point-to-point transmission thermoelectric force divided by the logarithm of thermopair group, has so greatly improved the precision of thermometric.Wherein the point-to-point transmission temperature difference spacing of the printing length of every pair of thermopair for intending measuring can be regulated printing length according to technical need, as: need to measure the temperature difference at 2 mm spacing places, then the printing length of thermopair group is 2mm; Measure the temperature difference at 5mm spacing place, then the printing length of thermopair group is 5mm.
It is 99.99% commercially available prod that platinum powder of the present invention, rhodium powder all adopt content; Al
2O
3, MgO, BaO, H
3BO
3, SiO
2And organic solvent all adopts analytically pure commercially available prod.
The present invention is further illustrated below in conjunction with accompanying drawing, but therefore do not limit the present invention among the described scope of embodiments.
Description of drawings
Fig. 1 is that N is to the structural representation for the high-precision thick membranous type thermopair group of measuring the distance element temperature difference.
Embodiment
Referring to Fig. 1.
It is the point-to-point transmission temperature difference of 2mm that embodiment 1 intends measuring distance:
Be 1.3851 with resistance ratio, particle diameter is 30 μ m, 12g platinum powder, 3g glass dust (9%Al
2O
3, 5%MgO, 20%BaO, 45%H
3BO
3, 21%SiO
2) and evenly mixing of 10g organic solvent (ethyl cellulose 13 %, butyl acetate 9 %, terpinol 73%, normal butyl alcohol 5 %), make the negative material slurry.With 10.8 g platinum powders, 1.2g rhodium powder, 3g glass dust (9%Al
2O
3, 5%MgO, 20%BaO, 45%H
3BO
3, 21%SiO
2) and evenly mixing of 10g organic solvent (ethyl cellulose 13 %, butyl acetate 9 %, terpinol 73%, normal butyl alcohol 5 %), evenly be mixed and made into the positive electrode slurry.Adopt the traditional silk-screened technology, the printed pattern exposure scribbling on the silk screen of photoresist, is made image substrate, then utilize this figure that cathode size is printed on and contain 95% Al
2O
3Ceramic substrate on.The printed pattern of cathode size is, 100 with the mutual parallel vertical lines of the vertical cut of surface level, every vertical line length H is 2mm, the space D of adjacent two vertical lines is 200um.Then carry out the cathode size sintering, sintering temperature is: 1000 ℃, sintering time is 25min, and forming thickness is the platinum layer negative pole 1 of 30～40 μ m.Screen printing technique is adopted in the printing of anode sizing agent equally, and the printed pattern exposure scribbling on the silk screen of photoresist, is made image substrate, then utilizes this figure that anode sizing agent is printed on the ceramic substrate that is printed on negative pole thermopair slurry.The printed pattern of anode sizing agent is 100 parallel oblique lines, every oblique line is horizontal by 45° angle, length is 2.82 mm, the spacing of adjacent two oblique lines is 200 um, the sintering temperature of anodal platinum powder slurry is: 1300 ℃, sintering time is 35min, and forming thickness is the platinum rhodium layer positive pole 2 of 30～40 μ m.Negative pole and positive pole are staggered, and adjacent negative pole and positive pole are end-to-end, and the negative pole of termination is connected with platinum thermocouple silk S, and positive pole is connected with platinum rhodium thermocouple silk S '.Be the impact of the spuious electromotive force that prevents the compensation lead of thermocouple exit, adopt diameter be the S type thermocouple wire of 0.4mm as extended line, directly freeze at the thermopair end and to draw the measurement extended line.
Be 1.3851 with resistance ratio, particle diameter is 30 μ m, 12g platinum powder, 3g glass dust (9%Al
2O
3, 5%MgO, 20%BaO, 45%H
3BO
3, 21%SiO
2) and evenly mixing of 10g organic solvent (ethyl cellulose 13 %, butyl acetate 9 %, terpinol 73%, normal butyl alcohol 5 %), make the negative material slurry.With 10.8 g platinum powders, 1.2g rhodium powder, 3g glass dust (9%Al
2O
3, 5%MgO, 20%BaO, 45%H
3BO
3, 21%SiO
2) and evenly mixing of 10g organic solvent (ethyl cellulose 13 %, butyl acetate 9 %, terpinol 73%, normal butyl alcohol 5 %), evenly be mixed and made into the positive electrode slurry.Adopt the traditional silk-screened technology, the printed pattern exposure scribbling on the silk screen of photoresist, is made image substrate, then utilize this figure that cathode size is printed on and contain 95% Al
2O
3Ceramic substrate on.The printed pattern of cathode size is, 500 with the mutual parallel vertical lines of the vertical cut of surface level, every vertical line length is 4mm, the spacing of adjacent two vertical lines is 400um.Then carry out the cathode size sintering, sintering temperature is: 1000 ℃, sintering time is 25min, and forming thickness is the platinum layer negative pole of 30～40 μ m.Screen printing technique is adopted in the printing of anode sizing agent equally, and the printed pattern exposure scribbling on the silk screen of photoresist, is made image substrate, then utilizes this figure that anode sizing agent is printed on the ceramic substrate that is printed on negative pole thermopair slurry.The printed pattern of anode sizing agent is 500 parallel oblique lines, every oblique line is horizontal by 45° angle, length is 5.68 mm, the spacing of adjacent two oblique lines is 400um, the sintering temperature of anodal platinum powder slurry is: 1300 ℃, sintering time is 35min, and forming thickness is the platinum rhodium layer positive pole of 30～40 μ m.Negative pole and positive pole are staggered, and adjacent negative pole and positive pole are end-to-end, and the negative pole of termination is connected with platinum thermocouple silk S, and positive pole is connected with platinum rhodium thermocouple silk S ˊ.Be the impact of the spuious electromotive force that prevents the compensation lead of thermocouple exit, adopt diameter be the type thermocouple wire of 0.4mm as extended line, directly freeze at thermocouple cold junction and to draw the measurement extended line.
Embodiment 3
Intending measuring distance is the point-to-point transmission temperature difference of 10 mm:
Be 1.3851 with resistance ratio, particle diameter is 30 μ m, 12g platinum powder, 3g glass dust (9%Al
2O
3, 5%MgO, 20%BaO, 45%H
3BO
3, 21%SiO
2) and evenly mixing of 10g organic solvent (ethyl cellulose 13 %, butyl acetate 9 %, terpinol 73%, normal butyl alcohol 5 %), make the negative material slurry.With 10.8 g platinum powders, 1.2g rhodium powder, 3g glass dust (9%Al
2O
3, 5%MgO, 20%BaO, 45%H
3BO
3, 21%SiO
2) and evenly mixing of 10g organic solvent (ethyl cellulose 13 %, butyl acetate 9 %, terpinol 73%, normal butyl alcohol 5 %), evenly be mixed and made into the positive electrode slurry.Adopt the traditional silk-screened technology, the printed pattern exposure scribbling on the silk screen of photoresist, is made image substrate, then utilize this figure that cathode size is printed on and contain 95% Al
2O
3Ceramic substrate on.The printed pattern of cathode size is, 1000 with the mutual parallel vertical lines of the vertical cut of surface level, every vertical line length is 10 mm, the spacing of adjacent two vertical lines is 800um.Then carry out the cathode size sintering, sintering temperature is: 1000 ℃, sintering time is 25min, and forming thickness is the platinum layer negative pole of 30～40 μ m.Screen printing technique is adopted in the printing of anode sizing agent equally, and the printed pattern exposure scribbling on the silk screen of photoresist, is made image substrate, then utilizes this figure that anode sizing agent is printed on the ceramic substrate that is printed on negative pole thermopair slurry.The printed pattern of anode sizing agent is 1000 parallel oblique lines, every oblique line is horizontal by 45° angle, length is 14.14 mm, the spacing of adjacent two oblique lines is 800 um, the sintering temperature of anodal platinum powder slurry is: 1300 ℃, sintering time is 35min, and forming thickness is the platinum rhodium layer positive pole of 30～40 μ m.Be the impact of the spuious electromotive force that prevents the compensation lead of thermocouple exit, adopt diameter be the S type thermocouple wire of 0.4mm as extended line, directly freeze at thermocouple cold junction and to draw the measurement extended line.
The thermopair group that adopts embodiment 1-3 to make, after testing test all can be satisfied the technical requirement to the distance element temperature measurement accuracy.
Claims (5)
1. preparation method who be used for to measure the high-precision thick membranous type thermopair group of the distance element temperature difference is characterized in that following steps are arranged:
1) preparation of slip:
Cathode size by pure platinum powder, glass dust and organic solvent mixing after, make cathode size, wherein, the weight ratio of pure platinum powder, glass dust and organic solvent is 12:3:10; Anodal slip is made anode sizing agent after evenly being mixed by pure platinum powder, pure rhodium powder, glass dust and organic solvent, and wherein the weight ratio of pure platinum powder and pure rhodium powder is 9:1, and the weight ratio of platinum rhodium metal powder, glass dust and organic solvent is 12:3:10;
Wherein,
In the positive and negative electrode in the glass dust percentage by weight of each component be: 8%～11%Al
2O
3, 3%～6%MgO, 19%～22%BaO, 43%～46%H
3BO
3, 20%～23%SiO
2
The percentage by weight of each component is in the organic solvent: ethyl cellulose 12 ~ 14%, butyl acetate 7 ~ 9 %, terpinol 72 ~ 75%, normal butyl alcohol 4 ~ 6 %;
2) making of negative pole:
Cathode size is printed on the ceramic substrate, sintering, forming thickness is the platinum layer negative pole of 30-40 μ m, and sintering temperature is: 1100 ℃, sintering time is 25min, and negative pole is some the vertical lines with the surface level vertical parallel;
3) anodal making:
The positive electrode slurry is printed on the ceramic substrate that is printed on negative pole, sintering, forming thickness is the platinum rhodium layer positive pole of 30-40 μ m, the anodal junction temperature that burns is 1300 ℃, sintering time is 35min, many oblique lines that are parallel to each other just very, every oblique line is horizontal by 45° angle, and the quantity of anodal oblique line is identical with the quantity of negative pole vertical line;
Negative pole and positive pole are staggered, and adjacent negative pole and positive pole are end-to-end, and the negative pole of termination is connected with the platinum thermocouple silk, and positive pole is connected with the platinum rhodium thermocouple silk, make for the high-precision thick membranous type thermopair group of measuring the distance element temperature difference.
2. method according to claim 1, it is characterized in that: the particle diameter of pure platinum powder and pure rhodium powder described in the step 1) is 20～80 μ m.
3. thick film thermocouple group according to claim 1 is characterized in that: step 2) in the length of every negative pole vertical line for intend measuring the length of distance element, the spacing between adjacent cathode two vertical lines is 100～1000um.
4. thick film thermocouple group according to claim 1 is characterized in that: the length of every anodal oblique line is 1.41 times of distance between 2 temperature difference intending measuring in the step 3), and the spacing of adjacent two oblique lines is 100～1000um.
5. thick film thermocouple group according to claim 1, it is characterized in that: described ceramic substrate contains 95% Al
2O
3
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2012
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