CN112268632B - 1000 ℃ high-temperature-resistant metal film thermal resistor with adjustable temperature coefficient and preparation method thereof - Google Patents

1000 ℃ high-temperature-resistant metal film thermal resistor with adjustable temperature coefficient and preparation method thereof Download PDF

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CN112268632B
CN112268632B CN202011121722.4A CN202011121722A CN112268632B CN 112268632 B CN112268632 B CN 112268632B CN 202011121722 A CN202011121722 A CN 202011121722A CN 112268632 B CN112268632 B CN 112268632B
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temperature
layer
lead
resistor
bonding pad
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CN112268632A (en
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杨永超
王大兴
皮倩倩
刘玺
刘志远
于海超
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Beijing Mechanical And Electrical Engineering General Design Department
CETC 49 Research Institute
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
    • G01K7/16—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements
    • G01K7/18—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using resistive elements the element being a linear resistance, e.g. platinum resistance thermometer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment

Abstract

The invention discloses a 1000 ℃ high-temperature resistant metal film thermal resistor with an adjustable temperature coefficient and a preparation method thereof, belongs to the technical field of temperature sensors, and particularly relates to a high-temperature metal film thermal resistor and a preparation method thereof. The invention aims to solve the problems that the existing Pt film has poor structural stability under the high-temperature environment of 1000 ℃, the surface protection of the Pt film is weak in the high-temperature environment, the temperature coefficient is difficult to regulate and control, and the connection reliability of a high-temperature lead is low. The 1000 ℃ high-temperature resistant metal film thermal resistor with the adjustable temperature coefficient comprises a high-temperature resistant substrate layer, a high-stability temperature sensing layer, a high-temperature resistant protective layer and a high-reliability lead protective layer, and is integrated into a whole. The method comprises the following steps: cleaning the ceramic wafer; 2. preparing a high-stability temperature sensing layer; 3. preparing a high-temperature-resistant protective layer; 4. welding a lead; 5. and preparing a high-reliability lead protection layer. The invention realizes stable measurement in high temperature environment by three-layer temperature sensing film protection technology.

Description

1000 ℃ high-temperature-resistant metal film thermal resistor with adjustable temperature coefficient and preparation method thereof
Technical Field
The invention belongs to the technical field of temperature sensors, and particularly relates to a high-temperature metal film thermal resistor and a preparation method thereof.
Background
The temperature change of the environment and the object is detected by a temperature sensing device, and the main temperature measuring methods in the current market comprise a thermistor, a thermocouple, a metal film thermal resistor and the like. The metal film thermal resistor has the advantages of simple structure, good stability, high precision, good linearity, simple use, low price and the like, and can be widely applied to various high-precision temperature measurement and control devices, including the fields of environment, satellite, meteorology, medical treatment, military, automobile electronics and the like. In the metal film thermal resistor, platinum metal has the advantages of corrosion resistance, stable structure, high temperature coefficient and the like, and is a rational material for manufacturing the metal film thermal resistor. At present, the germany, switzerland, japan and other companies propose platinum film thermal resistance technical products for measuring and controlling the temperature of the environment and the object, but due to the limitation of the manufacturing method, the platinum film thermal resistance only realizes the stable temperature measurement of only 600 ℃, and the temperature measurement of the environment of 1000 ℃ is difficult to realize, such as an engine control system, an industrial temperature control system and the like. The standard platinum thermal resistance temperature coefficient is 3851ppm/k, and the temperature coefficient is difficult to meet the high-temperature measurement and control field aiming at the special requirement of the temperature coefficient.
Disclosure of Invention
The invention aims to solve the problems that the existing Pt film thermal resistor has poor structural stability of the Pt film under the high-temperature environment of 1000 ℃, the surface protection of the Pt film under the high-temperature environment is weak, the temperature coefficient is difficult to regulate and control, and the high-temperature lead connection reliability is low, and provides a 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient and a preparation method thereof.
A1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient comprises a high-temperature resistant substrate layer, a high-stability temperature sensing layer, a high-temperature resistant protective layer and a high-reliability lead protective layer, which are integrated into a whole;
the high-temperature resistant substrate layer is a high-temperature resistant ceramic wafer with a polished surface;
the high-stability temperature sensing layer comprises a temperature sensing resistor strip, a resistor fine adjustment area, a first lead bonding pad, a second lead bonding pad, a first lead and a second lead; one end of the temperature sensing resistor strip is communicated with one end of the first lead bonding pad; the other end of the temperature sensing resistor strip is communicated with one end of the second lead bonding pad; the resistor fine adjustment area is communicated with the temperature sensing resistor strip; the first lead is communicated with the other end of the first lead bonding pad; the second lead is communicated with the other end of the second lead bonding pad;
the high-temperature-resistant protective layer comprises an aluminum oxide layer, a high-temperature glass sealing layer and a ceramic sealing layer; the high-temperature glass sealing layer covers the alumina layer; the ceramic sealing layer covers the high-temperature glass sealing layer;
the high-reliability lead protection layer is made of high-temperature-resistant glass; the main components of the high-temperature resistant glass consist of O, al and Si, and the resistant temperature reaches 1100 ℃;
the high-stability temperature sensing layer is arranged on the upper surface of the high-temperature resistant substrate layer, the aluminum oxide layer covers the upper surfaces of the temperature sensing resistor strip and the resistor fine adjustment area, and the high-reliability lead protection layer covers the resistor fine adjustment area, the first lead pad and the second lead pad.
A preparation method of a 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient is completed according to the following steps:
1. cleaning:
firstly, adopting a mixed solution of concentrated sulfuric acid and potassium dichromate to cook the ceramic wafer, wherein the cooking temperature is 60-100 ℃, the cooking time is 30-60 min, then using deionized water to wash the ceramic wafer to be neutral, and finally drying at 80 ℃ to obtain a high-temperature resistant ceramic wafer with a polished surface, namely a high-temperature resistant substrate layer;
the mass fraction of the concentrated sulfuric acid in the step one is 98%; the potassium dichromate mixed solution is formed by mixing concentrated sulfuric acid, potassium dichromate and water, wherein the volume ratio of the mass of the potassium dichromate to the concentrated sulfuric acid is (0.8-1.2 g) - (15 mL-25 mL), the volume ratio of the mass of the potassium dichromate to the water is (0.8-1.2 g) - (15 mL-25 mL), and the mass fraction of the concentrated sulfuric acid is 98%;
2. preparing a high-stability temperature sensing layer:
(1) preparing a high-stability temperature-sensing metal film layer on the surface of the high-temperature-resistant substrate layer by adopting a physical vapor deposition technology, and carrying out heat treatment at the temperature of 1000-1300 ℃ for 2-3 h to obtain a heat-treated high-stability temperature-sensing metal film layer;
the high-stability temperature-sensing metal film layer in the step two (1) is a Pt film or an Rh-doped Pt film, and the thickness of the high-stability temperature-sensing metal film layer is 0.5-2.0 mu m;
(2) forming a temperature sensing resistor strip, a resistor fine adjustment area, a first lead bonding pad and a second lead bonding pad by the high-stability temperature sensing metal film layer through photoetching and etching processes; introducing a layer of high-temperature metal slurry on the first lead bonding pad and the second lead bonding pad by adopting a screen printing process, and sintering at the high temperature of 1100-1300 ℃ to realize the solidification of the high-temperature metal slurry;
the high-temperature metal slurry in the step two (2) is Pt slurry;
3. preparing a high-temperature-resistant protective layer:
firstly, forming an alumina film layer on the upper surfaces of the temperature sensing resistor strips and the resistor fine adjustment area by adopting a physical vapor deposition technology; then coating high-temperature glass slurry on the surface of an alumina film layer by adopting a silk screen technology, sticking a ceramic sheet to the high-temperature glass slurry by using an automatic chip mounter, completely covering a resistor strip and a resistor fine adjustment area, and finally sintering at the high temperature of 1100-1200 ℃ for 10-30 min, wherein the sintered alumina film layer is an alumina layer, the sintered high-temperature glass slurry is a high-temperature glass sealing layer, the sintered ceramic sheet is a ceramic sealing layer, and the alumina layer, the high-temperature glass sealing layer and the ceramic sealing layer realize high-temperature protection on the temperature sensing resistor strip and the resistor fine adjustment area;
the main components of the high-temperature glass slurry in the third step are composed of O, al and Si, and the tolerance temperature reaches 1100 ℃;
the ceramic wafer in the third step is an aluminum nitride ceramic wafer or an aluminum oxide ceramic wafer;
4. and (3) lead welding:
welding the first lead and a first lead bonding pad by adopting a precision welding technology, and welding the second lead and a second lead bonding pad;
the first lead wire in the fourth step is a Pt wire or a Pt-Rh wire;
the second lead wire in the fourth step is a Pt wire or a Pt-Rh wire;
5. preparing a high-reliability lead protection layer:
coating high-temperature glass slurry to cover the ceramic sealing layer, the first lead bonding pad and the second lead bonding pad above the resistor fine adjustment area, sintering at 1100-1300 ℃, and forming a high-reliability lead protection layer after vitrification of the high-temperature glass slurry to finish reinforcement and sealing of a lead so as to form a complete 1000 ℃ high-temperature resistant metal thin film thermal resistor with an adjustable temperature coefficient;
the main components of the high-temperature glass slurry in the step five are composed of O, al and Si, and the tolerance temperature reaches 1100 ℃.
The principle and the advantages of the invention are as follows:
1. aiming at the technical difficulties, the invention adopts a doping process to improve the stability of the high-temperature structure of the metal platinum film, and simultaneously realizes the regulation and control of the temperature coefficient of the platinum thermal resistance through the doping process, thereby meeting the technical requirements in different temperature measurement and control fields; the high temperature resistance of the temperature sensing doped platinum film is ensured by adopting a high temperature resistant surface protection technology, the stability of the temperature sensing film is kept when the temperature sensing doped platinum film works in a high temperature environment for a long time, the high temperature reliability of a product is obviously enhanced, and the use requirement under the high temperature environment of 1000 ℃ can be met. In addition, the product manufacturing process is mature and controllable, and batch production can be realized;
2. the high-stability temperature sensing layer is a Pt film or an Rh-doped Pt film, and a thermal resistor prepared from the Rh-doped Pt film has high-temperature resistance, so that the stability measurement of the environment temperature of 1000 ℃ can be realized, and the temperature measurement range is greatly widened; by changing the doping concentration of Rh, the temperature coefficient 3700-3851ppm/k of the thermal resistance can be effectively regulated and controlled, and the high-temperature measurement and control requirements in different technical fields are met;
3. the invention realizes stable measurement in high temperature environment by three-layer temperature sensing film protection technology; the thermal resistor has the advantages of high temperature measurement temperature and controllable temperature coefficient, and can be widely applied to the field of industrial high-temperature environment measurement and control and the field of high-temperature measurement and control with special temperature coefficient requirements; the 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient is designed and manufactured based on MEMS technology, and the manufacturing process is mature and easy for batch production.
The invention can obtain the 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient.
Drawings
FIG. 1 is a schematic diagram illustrating a layered structure of a 1000 ℃ high-temperature-resistant metal thin-film thermal resistor with adjustable temperature coefficient according to a first embodiment;
fig. 2 is a schematic structural diagram of the second embodiment after the fine resistance tuning area in the middle and high stable temperature sensing layer is modified.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, steps or conditions of the present invention may be made without departing from the spirit of the invention.
The first embodiment is as follows: the embodiment is that a 1000 ℃ high-temperature resistant metal thin film thermal resistor with adjustable temperature coefficient comprises a high-temperature resistant substrate layer 1, a high-stability temperature sensing layer 2, a high-temperature resistant protective layer 3 and a high-reliability lead protective layer 4, which are integrated into a whole;
the high-temperature resistant substrate layer 1 is a high-temperature resistant ceramic wafer with a polished surface;
the high-stability temperature sensing layer 2 comprises a temperature sensing resistor strip 2-1, a resistor fine adjustment area 2-2, a first lead bonding pad 2-3, a second lead bonding pad 2-4, a first lead 2-5 and a second lead 2-6; one end of the temperature sensing resistor strip 2-1 is communicated with one end of the first lead bonding pad 2-3; the other end of the temperature sensing resistor strip 2-1 is communicated with one end of a second lead bonding pad 2-4; the resistor fine adjustment area 2-2 is communicated with the temperature sensing resistor strip 2-1; the first lead 2-5 is communicated with the other end of the first lead bonding pad 2-3; the second lead 2-6 is communicated with the other end of the second lead bonding pad 2-4;
the high-temperature-resistant protective layer 3 comprises an aluminum oxide layer 3-1, a high-temperature glass sealing layer 3-2 and a ceramic sealing layer 3-3; the high-temperature glass sealing layer 3-2 covers the alumina layer 3-1; the ceramic sealing layer 3-3 covers the high-temperature glass sealing layer 3-2;
the high-reliability lead protection layer 4 is made of high-temperature-resistant glass; the main components of the high-temperature resistant glass consist of O, al and Si, and the resistant temperature reaches 1100 ℃;
the high-stability temperature sensing layer 2 is arranged on the upper surface of the high-temperature resistant substrate layer 1, the aluminum oxide layer 3-1 covers the upper surfaces of the temperature sensing resistor strips 2-1 and the resistor fine adjustment area 2-2, and the high-reliability lead protection layer 4 covers the resistor fine adjustment area 2-2, the first lead bonding pad 2-3 and the second lead bonding pad 2-4.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the thickness of the high-temperature resistant substrate layer 1 is 0.1 mm-1 mm; the ceramic wafer is an aluminum nitride ceramic wafer or an aluminum oxide ceramic wafer. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the high-stability temperature sensing layer (2) is a Pt film or an Rh-doped Pt film, and the thickness is 0.5-2.0 μm; the mass fraction of Rh doping in the Rh-doped Pt film is 0.0001-0.1%, and the temperature coefficient is adjusted within the range of 3700 ppm/k-3851 ppm/k through the difference of the mass fraction of Rh doping in the Rh-doped Pt film. The other steps are the same as those in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the first lead bonding pad 2-3 is communicated with the first lead 2-5 through high-temperature metal paste, and the second lead bonding pad 2-4 is communicated with the second lead 2-6 through high-temperature metal paste; the high-temperature metal slurry is Pt slurry. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and the first to the fourth embodiments is: the resistor fine adjustment area 2-2 can adjust the resistance value of the 1000 ℃ resistant metal film thermal resistor through precise adjustment. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the thickness of the aluminum oxide layer 3-1 is 5-20 μm; the thickness of the high-temperature glass sealing layer 3-2 is 10-40 μm; the thickness of the ceramic sealing layer 3-3 is 100-500 μm. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the embodiment provides a preparation method of a 1000 ℃ high-temperature resistant metal film thermal resistor with an adjustable temperature coefficient, which is completed according to the following steps:
1. cleaning:
firstly, adopting a mixed solution of concentrated sulfuric acid and potassium dichromate to cook the ceramic wafer, wherein the cooking temperature is 60-100 ℃, the cooking time is 30-60 min, then using deionized water to wash the ceramic wafer to be neutral, and finally drying the ceramic wafer at 80 ℃ to obtain a high-temperature resistant ceramic wafer with a polished surface, namely a high-temperature resistant substrate layer 1;
the mass fraction of the concentrated sulfuric acid in the step one is 98%; the potassium dichromate mixed solution is formed by mixing concentrated sulfuric acid, potassium dichromate and water, wherein the volume ratio of the mass of potassium dichromate to the concentrated sulfuric acid is (0.8-1.2 g) - (15 mL-25 mL), the volume ratio of the mass of potassium dichromate to the volume of water is (0.8-1.2 g) - (15 mL-25 mL), and the mass fraction of the concentrated sulfuric acid is 98%;
2. preparing a high-stability temperature sensing layer:
(1) preparing a high-stability temperature-sensing metal film layer on the surface of the high-temperature-resistant substrate layer 1 by adopting a physical vapor deposition technology, and carrying out heat treatment at the temperature of 1000-1300 ℃ for 2-3 h to obtain a heat-treated high-stability temperature-sensing metal film layer;
the high-stability temperature-sensing metal film layer in the step two (1) is a Pt film or an Rh-doped Pt film, and the thickness of the high-stability temperature-sensing metal film layer is 0.5-2.0 mu m;
(2) forming a temperature sensing resistor strip 2-1, a resistor fine adjustment area 2-2, a first lead bonding pad 2-3 and a second lead bonding pad 2-4 by the high-stability temperature sensing metal film layer through photoetching and etching processes; introducing a layer of high-temperature metal slurry on the first lead bonding pad 2-3 and the second lead bonding pad 2-4 by adopting a screen printing process, and sintering at the high temperature of 1100-1300 ℃ to realize the solidification of the high-temperature metal slurry;
the high-temperature metal slurry in the second step (2) is Pt slurry;
3. preparing a high-temperature-resistant protective layer:
firstly, forming an alumina film layer on the upper surfaces of a temperature sensing resistor strip 2-1 and a resistor fine adjustment area 2-2 by adopting a physical vapor deposition technology; then, coating high-temperature glass slurry on the surface of an alumina film layer by adopting a silk screen technology, pasting an alumina or aluminum nitride ceramic sheet on the high-temperature glass slurry by using an automatic chip mounter, completely covering a resistor strip 2-1 and a resistor fine adjustment area 2-2, and finally sintering at the high temperature of 1100-1200 ℃ for 10-30 min, wherein the sintered alumina film layer is an alumina layer 3-1, the sintered high-temperature glass slurry is a high-temperature glass sealing layer 3-2, the sintered ceramic sheet is a ceramic sealing layer 3-3, the alumina layer 3-1, the high-temperature glass sealing layer 3-2 and the ceramic sealing layer 3-3 realize high-temperature protection on the temperature sensing resistor strip 2-1 and the resistor fine adjustment area 2-2;
the main components of the high-temperature glass slurry in the third step are composed of O, al and Si, and the tolerance temperature reaches 1100 ℃;
the ceramic wafer in the third step is an aluminum nitride ceramic wafer or an aluminum oxide ceramic wafer;
4. and (3) lead welding:
welding a first lead 2-5 with a first lead bonding pad 2-3 and welding a second lead 2-6 with a second lead bonding pad 2-4 by adopting a precision welding technology;
the first lead 2-5 in the fourth step is a Pt wire or a Pt-Rh wire;
the second lead 2-6 in the fourth step is Pt wire or Pt-Rh wire;
5. preparing a high-reliability lead protection layer:
coating high-temperature glass slurry to cover the ceramic sealing layer 3-3, the first lead bonding pad 2-3 and the second lead bonding pad 2-4 above the resistor fine adjustment area 2-2, sintering at 1100-1300 ℃, forming a high-reliability lead protection layer 4 after the high-temperature glass slurry is vitrified, completing the reinforcement and sealing of the lead, and forming a complete 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient;
the main components of the high-temperature glass slurry in the step five are composed of O, al and Si, and the tolerance temperature reaches 1100 ℃.
The principle and advantages of the embodiment are as follows:
1. aiming at the technical difficulties, the embodiment adopts a doping process to improve the stability of the high-temperature structure of the metal platinum film, and simultaneously realizes the regulation and control of the temperature coefficient of the platinum thermal resistance through the doping process, thereby meeting the technical requirements in different temperature measurement and control fields; the high temperature resistance of the temperature sensing doped platinum film is ensured by adopting a high temperature resistant surface protection technology, the stability of the temperature sensing film is kept when the temperature sensing doped platinum film works in a high temperature environment for a long time, the high temperature reliability of a product is obviously enhanced, and the use requirement under the high temperature environment of 1000 ℃ can be met. In addition, the product manufacturing process is mature and controllable, and batch production can be realized;
2. in the embodiment, the high-stability temperature sensing layer 2 is a Pt film or an Rh-doped Pt film, and a thermal resistor prepared by the Rh-doped Pt film has high temperature resistance, so that the stability measurement of the environment temperature of 1000 ℃ can be realized, and the temperature measurement range is greatly widened; by changing the doping concentration of Rh, the temperature coefficient 3700-3851ppm/k of the thermal resistance can be effectively regulated and controlled, and the high-temperature measurement and control requirements in different technical fields are met;
3. the embodiment realizes stable measurement in a high-temperature environment by a three-layer temperature sensing film protection technology; the thermal resistor has the advantages of high temperature measurement temperature and controllable temperature coefficient, and can be widely applied to the field of industrial high-temperature environment measurement and control and the field of high-temperature measurement and control with special temperature coefficient requirements; the 1000 ℃ high-temperature resistant metal film thermal resistor with the adjustable temperature coefficient, which is prepared by the embodiment, is designed and manufactured based on the MEMS technology, and the manufacturing process is mature and is easy for batch production.
The embodiment can obtain the 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient.
The specific implementation mode eight: the seventh embodiment is different from the first embodiment in that: preparing the Pt film in the step two (1) by adopting a magnetron sputtering deposition system, wherein a target material is a platinum target, the sputtering power is 200-1000W, the sputtering time is 30-70 min, the sputtering gas is Ar, and the sputtering pressure is 0.1-5.0 Pa; the Rh-doped Pt film is prepared by a single-target magnetron sputtering technology or a double-target magnetron co-sputtering technology, wherein the Rh-doped mass fraction in the Rh-doped Pt film is 0.0001-0.1%; the single-target magnetron sputtering technology is prepared by adopting a magnetron sputtering deposition system, the target material is a platinum target with Rh doping mass fraction of 0.0001-0.1%, the sputtering power is 200-1000W, the sputtering time is 30-70 min, the sputtering gas is Ar, and the sputtering pressure is 0.1-5.0 Pa; the double-target magnetron co-sputtering technology adopts a platinum target and an Rh target to co-sputter, wherein the sputtering power of the Pt target is 200W-1000W, the sputtering power of the Rh target is 5W-50W, the sputtering time is 30 min-70 min, the sputtering gas is Ar, and the sputtering pressure is 0.1 Pa-5.0 Pa. The other steps are the same as those in the seventh embodiment.
The specific implementation method nine: the seventh to eighth embodiments are different from the first to eighth embodiments in that: and in the step two (2), the resistor fine adjustment area 2-2 is accurately adjusted through photoetching, etching process and laser adjustment, so that the resistance value and the resistance value accuracy of the 1000 ℃ resistant metal thin film thermal resistor are adjusted. The other steps are the same as those of the seventh to eighth embodiments.
The detailed implementation mode is ten: the seventh to ninth differences from the present embodiment are as follows: in the third step, a magnetron sputtering deposition technology is adopted to form an alumina film layer with a thickness on the upper surfaces of the temperature sensing resistor strips 2-1 and the resistor fine adjustment area 2-2, and the specific preparation method comprises the following steps: the preparation method adopts a magnetron sputtering deposition system, the target material is an alumina target, and the technological parameters are as follows: the sputtering power is 200W-1000W; the sputtering time is 10 min-30 min, the sputtering gas is Ar, and the sputtering pressure is 0.1 Pa-5.0 Pa. The other steps are the same as those in the seventh to ninth embodiments.
The present invention will be described in detail with reference to the accompanying drawings 1 to 2 and examples.
The first embodiment is as follows: a1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient comprises a high-temperature resistant substrate layer 1, a high-stability temperature sensing layer 2, a high-temperature resistant protective layer 3 and a high-reliability lead protective layer 4, which are integrated into a whole;
the high-temperature resistant substrate layer 1 is a high-temperature resistant ceramic wafer with a polished surface;
the high-stability temperature sensing layer 2 comprises temperature sensing resistor strips 2-1, a resistor fine adjustment area 2-2, a first lead bonding pad 2-3, a second lead bonding pad 2-4, a first lead 2-5 and a second lead 2-6; one end of the temperature sensing resistor strip 2-1 is communicated with one end of the first lead bonding pad 2-3; the other end of the temperature sensing resistor strip 2-1 is communicated with one end of a second lead bonding pad 2-4; the resistor fine adjustment area 2-2 is communicated with the temperature sensing resistor strip 2-1; the first lead 2-5 is communicated with the other end of the first lead bonding pad 2-3; the second lead 2-6 is communicated with the other end of the second lead bonding pad 2-4;
the high-temperature-resistant protective layer 3 comprises an aluminum oxide layer 3-1, a high-temperature glass sealing layer 3-2 and a ceramic sealing layer 3-3; the high-temperature glass sealing layer 3-2 covers the alumina layer 3-1; the ceramic sealing layer 3-3 covers the high-temperature glass sealing layer 3-2;
the high-reliability lead protection layer 4 is made of high-temperature-resistant glass; the main components of the high-temperature resistant glass consist of O, al and Si, and the resistant temperature reaches 1100 ℃;
the high-stability temperature sensing layer 2 is arranged on the upper surface of the high-temperature resistant substrate layer 1, the aluminum oxide layer 3-1 covers the temperature sensing resistor strips 2-1 and covers the upper surface of the resistor fine adjustment area 2-2, and the high-reliability lead protection layer 4 covers the resistor fine adjustment area 2-2, the first lead bonding pad 2-3 and the second lead bonding pad 2-4;
the thickness of the high-temperature resistant substrate layer 1 is 0.5mm; the ceramic plate is an aluminum nitride ceramic plate;
the high-stability temperature sensing layer 2 is an Rh-doped Pt film with the thickness of 1.5 mu m; the mass fraction of Rh doping in the Rh-doped Pt film is 0.001%;
the first lead bonding pad 2-3 is communicated with the first lead 2-5 through high-temperature metal paste, and the second lead bonding pad 2-4 is communicated with the second lead 2-6 through high-temperature metal paste; the high-temperature metal slurry is platinum slurry;
a preparation method of a 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient is completed according to the following steps:
1. cleaning:
firstly, adopting a mixed solution of concentrated sulfuric acid and potassium dichromate to cook the ceramic wafer, wherein the cooking temperature is 80 ℃, the cooking time is 40min, then using deionized water to wash the ceramic wafer to be neutral, and finally drying at the temperature of 80 ℃ to obtain a high-temperature-resistant ceramic wafer with a polished surface, namely a high-temperature-resistant substrate layer 1;
the mass fraction of the concentrated sulfuric acid in the step one is 98%;
2. preparing a high-stability temperature sensing layer:
(1) preparing a high-stability temperature-sensing metal film layer on the surface of the high-temperature-resistant substrate layer 1 by adopting a physical vapor deposition technology, and performing heat treatment at the temperature of 1200 ℃ for 3 hours to obtain a heat-treated high-stability temperature-sensing metal film layer;
the high-stability temperature-sensing metal film layer in the step two (1) is an Rh-doped Pt film;
(2) forming a temperature sensing resistor strip 2-1, a resistor fine adjustment area 2-2, a first lead bonding pad 2-3 and a second lead bonding pad 2-4 by the high-stability temperature sensing metal film layer through photoetching and etching processes; introducing a layer of high-temperature metal slurry on the first lead bonding pad 2-3 and the second lead bonding pad 2-4 by adopting a screen printing process, and sintering at high temperature of 1200 ℃ to realize the solidification of the high-temperature metal slurry;
the high-temperature metal slurry in the second step (2) is platinum slurry;
3. preparing a high-temperature-resistant protective layer:
firstly, forming an alumina film layer on the upper surfaces of a temperature sensing resistor strip 2-1 and a resistor fine adjustment area 2-2 by adopting a physical vapor deposition technology; then, coating high-temperature glass slurry on the surface of an alumina film layer by adopting a silk screen technology, pasting an alumina ceramic sheet on the high-temperature glass slurry by using an automatic chip mounter, completely covering the resistor strip 2-1 and the resistor fine adjustment area 2-2, and finally sintering at 1150 ℃ for 20min at high temperature, wherein the sintered alumina film layer is an alumina layer 3-1, the sintered high-temperature glass slurry is a high-temperature glass sealing layer 3-2, the sintered ceramic sheet is a ceramic sealing layer 3-3, and the alumina layer 3-1, the high-temperature glass sealing layer 3-2 and the ceramic sealing layer 3-3 realize high-temperature protection on the temperature sensing resistor strip 2-1 and the resistor fine adjustment area 2-2;
the main components of the high-temperature glass slurry in the third step are composed of O, al and Si, and the tolerance temperature reaches 1100 ℃;
4. and (3) lead welding:
welding a first lead 2-5 and a first lead bonding pad 2-3 by adopting a precision welding technology, and welding a second lead 2-6 and a second lead bonding pad 2-4 by adopting a precision welding technology;
the first lead 2-5 in the fourth step is Pt wire;
the second lead 2-6 in the fourth step is Pt wire;
5. preparing a high-reliability lead protection layer:
coating high-temperature glass slurry to cover the ceramic sealing layer 3-3, the first lead bonding pad 2-3 and the second lead bonding pad 2-4 above the resistor fine adjustment area 2-2, sintering at 1200 ℃, and vitrifying the high-temperature glass slurry to form a high-reliability lead protection layer 4 to finish reinforcing and sealing a lead so as to form a complete 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient;
the main components of the high-temperature glass slurry in the step five are composed of O, al and Si, and the tolerance temperature reaches 1100 ℃;
the Rh doping mass fraction of the Rh doping Pt film in the step two (1) is 0.001%, and the Rh doping Pt film is prepared by a single-target magnetron sputtering technology or a double-target magnetron co-sputtering technology; the single-target magnetron sputtering technology is prepared by adopting a magnetron sputtering deposition system, the target material is a platinum target with Rh doping mass fraction of 0.001%, the sputtering power is 500W, the sputtering time is 50min, the sputtering gas is Ar, and the sputtering pressure is 2.0Pa;
in the third step, a magnetron sputtering deposition technology is adopted to form an alumina film layer with a thickness on the upper surfaces of the temperature sensing resistor strips 2-1 and the resistor fine adjustment area 2-2, and the specific preparation method comprises the following steps: the preparation method adopts a magnetron sputtering deposition system, the target material is an alumina target, and the technological parameters are as follows: the sputtering power is 500W; the sputtering time is 20min, the sputtering gas is Ar, and the sputtering pressure is 2.0Pa.
FIG. 1 is a schematic diagram illustrating a layered structure of a 1000 ℃ high-temperature-resistant metal thin-film thermal resistor with adjustable temperature coefficient according to a first embodiment;
the temperature coefficient of the 1000 ℃ high-temperature resistant metal film thermal resistor with the adjustable temperature coefficient obtained in the first embodiment is 3770 +/-12 ppm/k, and the temperature measurement of a 1000 ℃ environment can be realized.
Example two: the present embodiment is different from the first embodiment in that: and in the step two (2), the resistor fine adjustment area 2-2 is accurately adjusted through photoetching, etching process and laser adjustment, so that the resistance value and the resistance value accuracy of the 1000 ℃ resistant metal thin film thermal resistor are adjusted. Other steps and parameters are the same as those in the first embodiment, as shown in FIG. 2;
fig. 2 is a schematic structural diagram of the second embodiment of the invention after the fine resistance adjustment area in the middle and high stable temperature sensing layer 2 is modified.
The temperature coefficient of the 1000 ℃ high-temperature resistant metal film thermal resistor with the adjustable temperature coefficient obtained in the second embodiment is 3770 +/-12 ppm/k, and the temperature measurement of a 1000 ℃ environment can be realized.

Claims (6)

1. A preparation method of a 1000 ℃ high-temperature resistant metal film thermal resistor with an adjustable temperature coefficient is characterized in that the 1000 ℃ high-temperature resistant metal film thermal resistor with the adjustable temperature coefficient comprises a high-temperature resistant substrate layer (1), a high-stability temperature sensing layer (2), a high-temperature resistant protective layer (3) and a high-reliability lead protective layer (4), and is integrated into a whole;
the high-temperature resistant substrate layer (1) is a high-temperature resistant ceramic wafer with a polished surface;
the high-stability temperature sensing layer (2) comprises a temperature sensing resistor strip (2-1), a resistor fine adjustment area (2-2), a first lead bonding pad (2-3), a second lead bonding pad (2-4), a first lead (2-5) and a second lead (2-6); one end of the temperature sensing resistor strip (2-1) is communicated with one end of the first lead bonding pad (2-3); the other end of the temperature sensing resistor strip (2-1) is communicated with one end of the second lead bonding pad (2-4); the resistor fine adjustment area (2-2) is communicated with the temperature sensing resistor strip (2-1); the first lead (2-5) is communicated with the other end of the first lead bonding pad (2-3); the second lead (2-6) is communicated with the other end of the second lead bonding pad (2-4);
the high-temperature-resistant protective layer (3) comprises an aluminum oxide layer (3-1), a high-temperature glass sealing layer (3-2) and a ceramic sealing layer (3-3); the high-temperature glass sealing layer (3-2) covers the aluminum oxide layer (3-1); the ceramic sealing layer (3-3) covers the high-temperature glass sealing layer (3-2);
the high-reliability lead protection layer (4) is made of high-temperature-resistant glass;
the high-stability temperature sensing layer (2) is arranged on the upper surface of the high-temperature resistant substrate layer (1), the aluminum oxide layer (3-1) covers the upper surfaces of the temperature sensing resistor strips (2-1) and the resistor fine adjustment area (2-2), and the high-reliability lead protection layer (4) covers the resistor fine adjustment area (2-2), the first lead bonding pad (2-3) and the second lead bonding pad (2-4);
a preparation method of a 1000 ℃ high-temperature resistant metal film thermal resistor with an adjustable temperature coefficient is completed according to the following steps:
1. cleaning:
firstly, adopting a mixed solution of concentrated sulfuric acid and potassium dichromate to cook the ceramic wafer, wherein the cooking temperature is 60-100 ℃, the cooking time is 30-60 min, then using deionized water to wash the ceramic wafer to be neutral, and finally drying the ceramic wafer at 80 ℃ to obtain a high-temperature resistant ceramic wafer with a polished surface, namely a high-temperature resistant substrate layer (1);
the mass fraction of the concentrated sulfuric acid in the step one is 98%; the potassium dichromate mixed solution is formed by mixing concentrated sulfuric acid, potassium dichromate and water, wherein the volume ratio of the mass of the potassium dichromate to the concentrated sulfuric acid is (0.8-1.2 g) - (15 mL-25 mL), the volume ratio of the mass of the potassium dichromate to the water is (0.8-1.2 g) - (15 mL-25 mL), and the mass fraction of the concentrated sulfuric acid is 98%;
2. preparing a high-stability temperature sensing layer:
(1) preparing a high-stability temperature sensing layer (2) on the surface of a high-temperature resistant substrate layer (1) by adopting a physical vapor deposition technology, and performing heat treatment at the temperature of 1000-1300 ℃ for 2-3 h to obtain the heat-treated high-stability temperature sensing layer (2);
the high-stability temperature sensing layer (2) in the step two (1) is a Pt film or an Rh-doped Pt film, and the thickness of the high-stability temperature sensing layer is 0.5-2.0 mu m;
(2) the high-stability temperature sensing layer (2) forms a temperature sensing resistor strip (2-1), a resistor fine adjustment area (2-2), a first lead bonding pad (2-3) and a second lead bonding pad (2-4) through photoetching and etching processes; introducing a layer of high-temperature metal slurry on the first lead bonding pad (2-3) and the second lead bonding pad (2-4) by adopting a screen printing process, and sintering at the high temperature of 1100-1300 ℃ to realize the solidification of the high-temperature metal slurry;
the high-temperature metal slurry in the step two (2) is Pt slurry;
3. preparing a high-temperature-resistant protective layer:
firstly, forming an alumina film layer on the upper surfaces of a temperature sensing resistor strip (2-1) and a resistor fine adjustment area (2-2) by adopting a physical vapor deposition technology; then, coating high-temperature glass slurry on the surface of an alumina film layer by adopting a silk screen technology, pasting a ceramic sheet on the high-temperature glass slurry by using an automatic chip mounter, completely covering a resistor strip (2-1) and a resistor fine adjustment area (2-2), and finally sintering at the high temperature of 1100-1200 ℃ for 10-30 min, wherein the sintered alumina film layer is an alumina layer (3-1), the sintered high-temperature glass slurry is a high-temperature glass sealing layer (3-2), the sintered ceramic sheet is a ceramic sealing layer (3-3), the alumina layer (3-1), the high-temperature glass sealing layer (3-2) and the ceramic sealing layer (3-3) realize high-temperature protection on the temperature sensing resistor strip (2-1) and the resistor fine adjustment area (2-2);
the ceramic wafer in the third step is an aluminum nitride ceramic wafer or an aluminum oxide ceramic wafer;
4. welding a lead:
welding a first lead (2-5) and a first lead bonding pad (2-3) by adopting a precision welding technology, and welding a second lead (2-6) and a second lead bonding pad (2-4);
the first lead (2-5) in the fourth step is a Pt wire or a Pt-Rh wire;
the second lead (2-6) in the fourth step is a Pt wire or a Pt-Rh wire;
5. preparing a high-reliability lead protection layer:
coating high-temperature glass slurry to cover the ceramic sealing layer (3-3), the first lead bonding pad (2-3) and the second lead bonding pad (2-4) above the resistor fine adjustment area (2-2), sintering at 1100-1300 ℃, forming a high-reliability lead protection layer (4) after the high-temperature glass slurry is vitrified, completing the reinforcement and sealing of the lead, and forming a complete 1000 ℃ high-temperature resistant metal film thermal resistor with adjustable temperature coefficient.
2. The method for preparing the 1000 ℃ high-temperature resistant metal thin film thermal resistor with the adjustable temperature coefficient according to claim 1, wherein the thickness of the high-temperature resistant substrate layer (1) is 0.1 mm-1 mm.
3. The method for preparing the metal thin film thermal resistor with adjustable temperature coefficient and high temperature resistance of 1000 ℃ according to claim 1, wherein the thickness of the aluminum oxide layer (3-1) is 5-20 μm; the thickness of the high-temperature glass sealing layer (3-2) is 10-40 μm; the thickness of the ceramic sealing layer (3-3) is 100-500 μm.
4. The method for preparing the 1000 ℃ high-temperature-resistant metal thin film thermal resistor with the adjustable temperature coefficient according to claim 1, wherein the Pt film in the step two (1) is prepared by a magnetron sputtering deposition system, a target material is a platinum target, sputtering power is 200W-1000W, sputtering time is 30 min-70 min, sputtering gas is Ar, and sputtering pressure is 0.1 Pa-5.0 Pa; the Rh-doped Pt film has the mass fraction of Rh doping of 0.0001-0.1%, and is prepared by a single-target magnetron sputtering technology or a double-target magnetron co-sputtering technology; the single-target magnetron sputtering technology is prepared by adopting a magnetron sputtering deposition system, the target material is a platinum target with Rh doping mass fraction of 0.0001-0.1%, the sputtering power is 200-1000W, the sputtering time is 30-70 min, the sputtering gas is Ar, and the sputtering pressure is 0.1-5.0 Pa; the double-target magnetron co-sputtering technology adopts a platinum target and an Rh target to co-sputter, wherein the sputtering power of the Pt target is 200W-1000W, the sputtering power of the Rh target is 5W-50W, the sputtering time is 30 min-70 min, the sputtering gas is Ar, and the sputtering pressure is 0.1 Pa-5.0 Pa.
5. The method for preparing the metal film thermal resistor with the adjustable temperature coefficient and the resistance temperature of 1000 ℃ according to claim 1, wherein in the second step (2), the resistor fine tuning area (2-2) is precisely tuned through photoetching, etching process and laser tuning, so that the resistance value and the resistance value precision of the metal film thermal resistor with the adjustable temperature coefficient and the resistance temperature of 1000 ℃ can be adjusted.
6. The preparation method of the metal thin film thermal resistor with the adjustable temperature coefficient and the high temperature resistance of 1000 ℃ according to claim 1, wherein in the third step, a magnetron sputtering deposition technology is adopted to form an alumina film layer with a thickness on the upper surfaces of the temperature sensing resistor strips (2-1) and the resistor fine tuning area (2-2), and the preparation method specifically comprises the following steps: the preparation method adopts a magnetron sputtering deposition system, the target material is an alumina target, and the technological parameters are as follows: the sputtering power is 200W-1000W; the sputtering time is 10min to 30min, the sputtering gas is Ar, and the sputtering pressure is 0.1Pa to 5.0Pa.
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