CN108975920B - HTCC-based high-temperature heat flow sensor and preparation method thereof - Google Patents

HTCC-based high-temperature heat flow sensor and preparation method thereof Download PDF

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CN108975920B
CN108975920B CN201810526801.XA CN201810526801A CN108975920B CN 108975920 B CN108975920 B CN 108975920B CN 201810526801 A CN201810526801 A CN 201810526801A CN 108975920 B CN108975920 B CN 108975920B
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aluminum nitride
nitride green
tape
filling
heat flow
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CN108975920A (en
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谭秋林
郭彦杰
董和磊
张磊
吕文
熊继军
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North University of China
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B37/00Joining burned ceramic articles with other burned ceramic articles or other articles by heating
    • C04B37/02Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
    • C04B37/021Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01KMEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
    • G01K7/00Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
    • G01K7/02Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6025Tape casting, e.g. with a doctor blade

Abstract

The invention provides a high-temperature heat flow sensor based on HTCC and a preparation method thereof, according to the sensitive mechanism of a thermopile heat flow sensor, a plurality of filling holes are arranged on an aluminum nitride green ceramic tape to integrate a plurality of thermocouples, so that the arrangement density of the thermocouples is increased, the output potential of the thermocouples is increased, and the test sensitivity of the sensor is greatly improved; according to the difference of the heat conduction coefficients of the high-temperature resistant materials, aluminum nitride is selected as a medium material of a substrate and an intermediate layer of the sensor structure, and the response time of the sensor is greatly prolonged by selecting three materials, namely aluminum nitride material, platinum/15% iridium alloy and palladium gold; the sensor has the advantages of simple and convenient manufacturing process, high sensitivity, good response block and stability and more convenient installation, and can realize the detection of the heat flow in high-temperature and large-heat-flow environments such as the interior of aerospace craft and engines.

Description

HTCC-based high-temperature heat flow sensor and preparation method thereof
Technical Field
The invention relates to the field of heat flow sensing, in particular to a high-temperature heat flow sensor based on HTCC and a preparation method thereof.
Background
The modern war has the operational performance requirements on high speed, high precision and high maneuverability of the aircraft, and causes various countries in the world to compete to develop the research and development work of the supersonic aircraft. With the great increase of the flying speed of the supersonic aircraft, the high-temperature heat flow environment generated by pneumatic heating becomes more and more severe.
The parts of the front cone end part, the combustion chamber, the exhaust port and the like of the aerospace craft can generate a local high-temperature area and a high-heat-flow environment which are higher than 1200 ℃. The method is used for monitoring the heat flow on the surface of the aerospace craft and in the engine combustion chamber under the extremely severe environment conditions of ultrahigh temperature and high heat flow, and plays a vital role in the structural design, safety performance and part service life of the aerospace craft. The aerospace craft and the engine thereof are not only in a severe environment with high temperature and large heat flow, but also are accompanied by complex environments such as high spin, vibration, centrifugal force, compound motion and the like, and have strict limitations on the aspects such as weight, volume and the like of the added test equipment in the aspect of aerodynamics, and provide great challenges for realizing real-time and accurate measurement of heat flow characteristic parameters on the surface of the aerospace craft and in the interior of the aerospace craft under the conditions of not influencing the original aerodynamic characteristics and loading.
The existing heat flow sensor applied to the high-temperature and large-heat-flow extreme environment mainly comprises a circular foil type heat flow sensor and a thin film type heat flow sensor. The circular foil type heat flow sensor has the following limitations: the sensitivity coefficient is low, the response time is long, and the method is not suitable for detecting transient heat flow; when the sensor is used in a high-temperature environment, a water cooling mode is needed, and the size is large. The film type heat flow sensor adopts two-dimensional plane layout, only a few thermocouples can be integrated in a certain area relative to a three-dimensional structure, the sensitivity is low, and the requirement of testing in a severe environment with ultra-high temperature (more than 1000 ℃) is difficult to meet.
Disclosure of Invention
The invention aims to avoid the defects of the prior art and provides a high-temperature heat flow sensor based on HTCC and a preparation method thereof.
The object of the invention can be achieved by adopting the following technical measures, and the preparation method of the HTCC-based high-temperature heat flow sensor is designed, and comprises the following steps: providing first to fourth aluminum nitride green porcelain strips, and punching other aluminum nitride green porcelain strips except the first aluminum nitride green porcelain strip to form corresponding filling holes arranged in an array; thermocouple connecting lines are arranged at the hole edges of the two filling holes close to the diagonal positions on the second aluminum nitride green porcelain strip, the first aluminum nitride green porcelain strip is used as a substrate and laminated with the second aluminum nitride green porcelain strip to obtain a first aluminum nitride green porcelain strip lamination, and palladium-gold slurry is filled in the filling holes of the second aluminum nitride green porcelain strip; adhering a third layer of aluminum nitride green porcelain tape to the first aluminum nitride green porcelain tape lamination for lamination to obtain a second aluminum nitride green porcelain tape lamination, and respectively filling palladium-gold and platinum/15% iridium alloy slurry in each filling hole of the third aluminum nitride green porcelain tape in parallel along the hole wall without connection, wherein the palladium-gold and the platinum/15% iridium alloy slurry are in contact with palladium-gold in the second aluminum nitride green porcelain tape filling hole; a fourth layer of aluminum nitride green porcelain tape is stuck to the second aluminum nitride green porcelain tape lamination for lamination, and palladium-gold slurry is filled in each filling hole of the fourth aluminum nitride green porcelain tape; the filling metal in each filling hole of the fourth aluminum nitride green ceramic band is contacted with the two metals in two adjacent filling holes of the third aluminum nitride green ceramic band, so that an aluminum nitride ceramic chip containing an array thermopile structure is obtained; and (3) carrying out laminating, cutting and high-temperature sintering on the aluminum nitride ceramic chip containing the array thermopile structure to obtain the high-temperature heat flow sensor.
And after the step of filling the metal slurry into the filling holes of the second, third and fourth layers of aluminum nitride green porcelain tapes, the steps of drying at high temperature and observing and correcting the structure under a microscope operating platform are also included.
Wherein the high temperature drying temperature is 100 deg.C, and the time is 10 min.
Wherein, after the step of laminating the aluminum nitride green ceramic tape containing the array thermopile structure, the method comprises the following steps: wrapping the laminated aluminum nitride ceramic chip by using a silica gel film, setting the temperature of a laminating machine to be 70 ℃, and setting the static pressure to be 21MPa, and placing the wrapped aluminum nitride ceramic chip containing the array thermopile structure in the laminating machine for isostatic pressing lamination for 20 min.
In the step of high-temperature sintering, each independent array thermopile sensing structure cut from an aluminum nitride ceramic chip is put in a high-temperature furnace with hydrogen protection for high-temperature co-firing.
Wherein, the filling holes on the aluminum nitride green porcelain tape are square holes.
Wherein, in the step of providing four square aluminum nitride green porcelain strips with different thicknesses, the method comprises the following steps: mixing aluminum nitride powder, water and a dispersing agent according to a certain ratio, adjusting the pH value of a system to be 9.0 by using ammonia water, and carrying out first ball milling for 24 hours; adding a binder and a plasticizer for secondary ball milling and mixing, adding a defoaming agent for vacuum defoaming, and preparing a blank sheet; and adjusting the knife edge height and the casting speed of the casting machine, drying and demoulding the blank sheet to obtain four casting sheets with different thicknesses, and slicing the casting sheets.
In the step of setting the thermocouple connecting line, a screen printing technology is utilized, a platinum brush is used for forming the thermocouple connecting line on the edge of the filling hole at the diagonal position of the second aluminum nitride green porcelain strip, and the thermocouple connecting line is connected with metal arranged in the filling hole.
The purpose of the invention can be realized by adopting the following technical measures, and the high-temperature heat flow sensor based on the HTCC is designed and is prepared by the preparation method of the high-temperature heat flow sensor.
Wherein the thicknesses of the first, second, third and fourth aluminum nitride green porcelain tapes are 100 μm, 20 μm, 100 μm and 20 μm, respectively.
Compared with the prior art, the preparation method of the HTCC-based high-temperature heat flow sensor provided by the invention has the advantages that a plurality of filling holes are formed in the aluminum nitride green ceramic tape according to the sensitive mechanism of the thermopile heat flow sensor to integrate a plurality of thermocouples, so that the arrangement density of the thermocouples is increased, the output potential of the thermocouples is increased, and the test sensitivity of the sensor is greatly improved; according to the difference of the heat conduction coefficients of the high-temperature resistant materials, aluminum nitride is selected as a medium material of a substrate and an intermediate layer of the sensor structure, and the response time of the sensor is greatly prolonged by selecting three materials, namely aluminum nitride material, platinum/15% iridium alloy and palladium gold; the sensor has the advantages of simple and convenient manufacturing process, high sensitivity, good response block and stability and more convenient installation, and can realize the detection of the heat flow in high-temperature and large-heat-flow environments such as the interior of aerospace craft and engines.
Drawings
FIG. 1 is a schematic process flow diagram of a method for manufacturing a HTCC-based high-temperature heat flow sensor according to the present invention;
FIG. 2 is a schematic flow chart of a method for manufacturing a HTCC-based high-temperature heat flow sensor according to the present invention;
FIG. 3 is a front plan view of the overall structure of an HTCC-based high temperature heat flux sensor and a fourth aluminum nitride green tape in accordance with the present invention;
FIG. 4 is a schematic structural view of section A-A of FIG. 3 according to the present invention;
FIG. 5 is a side view block diagram of each thermocouple cell structure in an HTCC-based high temperature heat flux sensor according to the present invention;
FIG. 6 is a schematic top view of a third aluminum nitride green tape in an HTCC-based high temperature heat flux sensor according to the present invention;
fig. 7 is a schematic top view of a second alumina porcelain band in an HTCC-based high temperature heat flux sensor according to the present invention.
Detailed Description
The technical solution of the present invention will be further described in more detail with reference to the following embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, fig. 1 is a schematic process flow diagram of a method for manufacturing a HTCC-based high-temperature heat flow sensor according to the present invention; FIG. 2 is a schematic flow chart of a method for manufacturing a HTCC-based high-temperature heat flow sensor according to the present invention. The method comprises the following steps:
s110: providing a first aluminum nitride green porcelain strip, a second aluminum nitride green porcelain strip and a third aluminum nitride green porcelain strip, and punching other aluminum nitride green porcelain strips except the first aluminum nitride green porcelain strip to form corresponding filling holes arranged in an array.
Four square aluminum nitride green porcelain tapes with different thicknesses are provided, and particularly, the finished product can be directly used or the aluminum nitride green porcelain tape can be prepared. The preparation method comprises the following steps: mixing aluminum nitride powder, water and a dispersing agent according to a certain ratio, adjusting the pH value of a system to be 9.0 by using ammonia water, and carrying out first ball milling for 24 hours; adding a binder and a plasticizer for secondary ball milling and mixing, adding a defoaming agent for vacuum defoaming, and preparing a blank sheet; and adjusting the knife edge height and the casting speed of the casting machine, drying and demoulding the blank sheet to obtain four casting sheets with different thicknesses, and slicing the casting sheets.
Four aluminum nitride green ceramic tapes with different thicknesses are obtained by slicing, and in one embodiment of the invention, the thicknesses of the four aluminum nitride green ceramic tapes are respectively 100 micrometers, 20 micrometers, 100 micrometers and 20 micrometers. According to the invention, the filling holes arranged in the aluminum nitride green porcelain strips are all arranged in an array, the cross sections of the filling holes are preferably square, and each aluminum nitride green porcelain strip is arranged in a square with the side length of 9 inches.
S120: and thermocouple connecting lines are arranged at the hole edges of the two filling holes close to the diagonal positions on the second aluminum nitride green porcelain strip, the first aluminum nitride green porcelain strip is used as a substrate and laminated with the second aluminum nitride green porcelain strip to obtain a first aluminum nitride green porcelain strip lamination, and palladium-gold slurry is filled in the filling holes of the second aluminum nitride green porcelain strip.
Setting a first aluminum nitride green porcelain strip with the thickness of 100 mu m as a substrate of a high-temperature heat flow sensor, placing a second aluminum nitride green porcelain strip with the thickness of 20 mu m in a screen printer, brushing a metal lead structure on the edges of two filling holes in the diagonal position of the second aluminum nitride green porcelain strip by using platinum slurry to form a thermocouple connecting line, taking out the second aluminum nitride green porcelain strip from the screen printer, placing the second aluminum nitride green porcelain strip in a 100-DEG C environment for heat preservation for 10min, aligning by using the filling holes on the second aluminum nitride green porcelain strip, laminating the second aluminum nitride green porcelain strip and the first aluminum nitride green porcelain strip serving as the substrate, filling palladium-gold slurry in the filling holes of the second aluminum nitride green porcelain strip to obtain a thermopile bottom layer after filling, placing the thermopile bottom layer in the 100-DEG C environment for heat preservation for 10min, taking out and placing the thermopile bottom layer under a microscope operating table for structure observation and correction. Wherein, the thermocouple connecting wire is connected with the palladium-gold filler arranged in the filling hole close to the thermocouple connecting wire.
S130: and adhering a third layer of aluminum nitride green porcelain strip to the first aluminum nitride green porcelain strip lamination for lamination to obtain a second aluminum nitride green porcelain strip lamination, and respectively filling palladium-gold and platinum/15% iridium alloy slurry in each filling hole of the third aluminum nitride green porcelain strip in parallel along the hole wall without connection, wherein the palladium-gold and the platinum/15% iridium alloy slurry are in contact with the palladium-gold in the second aluminum nitride green porcelain strip filling hole.
And taking a third aluminum nitride green porcelain strip with the single-layer thickness of 100 mu m, and laminating, specifically, laminating with one side of the second aluminum nitride green porcelain strip. And after lamination, taking palladium-gold slurry and platinum/15% iridium alloy slurry, and filling in the filling holes of the third aluminum nitride green ceramic band. Because the filling holes formed in the third aluminum nitride raw porcelain strip are square, in the filling process, the slurry is arranged along the opposite surfaces of the inner walls of the filling holes, so that two different slurries filled in the same filling hole are not contacted with each other, and the filling holes in the third aluminum nitride raw porcelain strip are just opposite to the filling holes in the second aluminum nitride raw porcelain strip, so that the two slurries in the filling holes of the third aluminum nitride raw porcelain strip are respectively contacted with the palladium-gold filled in the corresponding filling holes in the second aluminum nitride raw porcelain strip. After the filling is finished, the glass is placed in an environment with the temperature of 100 ℃ for heat preservation for 10min, and then the glass is taken out and placed under a microscope operating platform for structure observation and correction.
S140: a fourth layer of aluminum nitride green porcelain tape is stuck to the second aluminum nitride green porcelain tape lamination for lamination, and palladium-gold slurry is filled in each filling hole of the fourth aluminum nitride green porcelain tape; and the filling metal in each filling hole of the fourth aluminum nitride green ceramic band is contacted with the two metals in the two adjacent filling holes of the third aluminum nitride green ceramic band, so that the aluminum nitride ceramic chip containing the array thermopile structure is obtained.
Taking a fourth aluminum nitride green porcelain strip with the single-layer thickness of 20 mu m, laminating the fourth aluminum nitride green porcelain strip with the structure prepared in the previous step, and specifically laminating the fourth aluminum nitride green porcelain strip with the surface of the third aluminum nitride green porcelain strip. During lamination, the overlapped position is determined by comparing the relative positions of the filling holes arranged on the third aluminum nitride green porcelain strip and the filling holes arranged on the fourth aluminum nitride green porcelain strip. In the present embodiment, the position of the fourth aluminum nitride green ceramic tape is adjusted so that the metal structure formed by solidifying the palladium-gold slurry and the platinum/15% iridium alloy slurry provided in the filling holes of two adjacent third aluminum nitride green ceramic tapes can be simultaneously seen in the filling holes provided in the fourth aluminum nitride green ceramic tape. In the present embodiment, the filling holes provided in the second, third, and fourth aluminum nitride green ceramic tapes are completely the same. In other embodiments, the shape and area of the filling holes in each aluminum nitride green tape can be set arbitrarily, but it is necessary to ensure that the two metals in the filling holes of the third aluminum nitride green tape are in contact with the metal in the filling holes of the second aluminum nitride green tape, and the metal in the filling holes of the fourth aluminum nitride green tape is in contact with the two metals in the two adjacent filling holes of the third aluminum nitride green tape. After the filling is finished, the glass is placed in an environment with the temperature of 100 ℃ for heat preservation for 10min, and then the glass is taken out and placed under a microscope operating platform for structure observation and correction.
S150: and (3) carrying out laminating, cutting and high-temperature sintering on the aluminum nitride ceramic chip containing the array thermopile structure to obtain the high-temperature heat flow sensor.
And (4) finishing laminating the aluminum nitride green ceramic tapes of each layer to obtain the thermopile. And (3) laminating the thermopile, wrapping the thermopile by using a coating after the lamination is finished, setting the temperature of a laminating machine to be 70 ℃, setting the static pressure to be 21MPa, and placing the ceramic chip wrapped by the coating in the laminating machine for isostatic pressing for 20 min. And after the lamination is finished, taking out the ceramic chip containing the multiple array thermopile structures from the laminator, placing the ceramic chip in a laser drilling machine for cutting, and dividing the high-temperature heat flow sensor unit. During specific cutting, each sensor needs to be ensured to comprise one filling hole of the second aluminum nitride green ceramic tape, the third aluminum nitride green ceramic tape and the fourth aluminum nitride green ceramic tape, so that the high-temperature heat flow sensor is internally provided with a metal structure as shown in fig. 4. And placing the prepared sensor structure in a high-temperature furnace with hydrogen protection for high-temperature co-firing, and finally preparing a plurality of high-temperature heat flow sensor structures.
As shown in fig. 1, the process of manufacturing the HTCC-based high-temperature heat flow sensor according to the present invention includes preparing an aluminum nitride green tape by the aluminum nitride green tape preparing method in step S110, and then slicing the aluminum nitride green tape, for example, preparing 100 μm and 20 μm aluminum nitride green tapes, which are cut to have a side length of 9 inches in slicing. And punching holes on the sliced aluminum nitride green porcelain tape, and arranging a plurality of groups of array holes. As shown in fig. 1, four sets of array holes were provided in the aluminum nitride green tape. And preparing a lead, laminating and filling metal according to the steps, obtaining an aluminum nitride lamination after the lamination is finished, and carrying out laminating, cutting and high-temperature sintering to obtain the high-temperature heat flow sensor.
According to the sensitive mechanism of the thermopile heat flow sensor, a plurality of thermocouples are integrated by utilizing an HTCC (high temperature coefficient carrier) micro-assembly process, so that the arrangement density of the thermocouples is increased, the output potential of the thermocouples is increased, and the test sensitivity of the sensor is greatly improved;
according to the invention, according to the difference of the heat conduction coefficients of high-temperature resistant materials, aluminum nitride is selected as a medium material of a substrate and an intermediate layer of a sensor structure, two metal materials of a thermocouple are palladium-gold and platinum/15% iridium alloy, which are determined by the seebeck coefficients of the two metal materials, and the selection of the aluminum nitride material, the platinum/15% iridium alloy and the palladium-gold greatly improves the response time of the high-temperature heat flow sensor, and finally can reach 500 microseconds or less;
the two metal materials of the thermopile structure selected in the invention are palladium gold and platinum/15% iridium alloy, the intermediate layer medium material of the thermopile is aluminum nitride, the fuse metal material of the high-temperature heat flow sensor is platinum gold, the stable working temperature is above 1500 ℃, and the maximum working temperature of the prepared high-temperature heat flow sensor is ensured to be more than 1200 ℃;
the sensor has the advantages of reasonable structural design, simple and convenient manufacturing process, high sensitivity, good stability and convenient installation, and can realize the detection of the heat flow in high-temperature and high-heat-flow environments such as the interior of aerospace craft and engines.
Referring to fig. 4, fig. 4 is a schematic structural diagram of a cross section of a high-temperature heat flow sensor based on HTCC according to the present invention. The high-temperature heat flow sensor is prepared by the preparation method of the high-temperature heat flow sensor in the technical scheme. Specifically, the ceramic tape comprises a first aluminum nitride green ceramic tape 1 as a substrate; a second aluminum nitride green porcelain strip 2 serving as a thermopile bottom layer, thermocouple wires 9 and 10 arranged on the second aluminum nitride green porcelain strip, and a thermopile bottom layer metal material 8 arranged in the second aluminum nitride green porcelain strip filling hole, as shown in fig. 6, which is a schematic plan view of the second aluminum nitride green porcelain strip 2; a third aluminum nitride green ceramic tape 3 serving as a thermopile middle layer, and a thermopile middle layer metal a material 6 and a metal B material 7 disposed in the filling hole, as shown in fig. 7, are schematic top views of the third aluminum nitride green ceramic tape 3; as shown in fig. 1, a schematic plan view of the fourth aluminum nitride green ceramic tape 4 is shown as a fourth aluminum nitride green ceramic tape as the thermopile top layer and the thermopile top layer metal material 5 provided in the filling hole.
The thermopile top layer metal material 5 and the thermopile bottom layer metal material 8 are both obtained by solidifying palladium-gold slurry, the thermopile middle layer metal A material 6 and the metal B material 7 are obtained by solidifying palladium-gold and platinum/15% iridium alloy slurry, and the thermocouple connecting wires 9 and 10 are formed by utilizing a screen printing technology and using a platinum brush. By adjusting the structure of the filling holes and the relative positions of the filling holes in different layers, two metals in the filling holes of the third aluminum nitride green porcelain strip 3 are in contact with the metals in the filling holes of the second aluminum nitride green porcelain strip 2, and the metals in the filling holes of the fourth aluminum nitride green porcelain strip 4 are in contact with the two metals in two adjacent filling holes on the third aluminum nitride green porcelain strip 3, so that the thermopile with the unit structure section as shown in FIG. 5 is formed.
Compared with the prior art, the preparation method of the HTCC-based high-temperature heat flow sensor provided by the invention has the advantages that a plurality of filling holes are formed in the aluminum nitride green ceramic tape according to the sensitive mechanism of the thermopile heat flow sensor to integrate a plurality of thermocouples, so that the arrangement density of the thermocouples is increased, the output potential of the thermocouples is increased, and the test sensitivity of the sensor is greatly improved; according to the difference of the heat conduction coefficients of the high-temperature resistant materials, aluminum nitride is selected as a medium material of a substrate and an intermediate layer of the sensor structure, and the response time of the sensor is greatly prolonged by selecting three materials, namely aluminum nitride material, platinum/15% iridium alloy and palladium gold; the sensor has the advantages of simple and convenient manufacturing process, high sensitivity, good response block and stability and more convenient installation, and can realize the detection of the heat flow in high-temperature and large-heat-flow environments such as the interior of aerospace craft and engines.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by using the contents of the present specification and the accompanying drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. A preparation method of a high-temperature heat flow sensor based on HTCC is characterized by comprising the following steps:
providing first to fourth aluminum nitride green porcelain strips, and punching other aluminum nitride green porcelain strips except the first aluminum nitride green porcelain strip to form corresponding filling holes arranged in an array;
thermocouple connecting lines are arranged at the hole edges of the two filling holes close to the diagonal positions on the second aluminum nitride green porcelain strip, the first aluminum nitride green porcelain strip is used as a substrate and laminated with the second aluminum nitride green porcelain strip to obtain a first aluminum nitride green porcelain strip lamination, and palladium-gold slurry is filled in the filling holes of the second aluminum nitride green porcelain strip;
adhering a third layer of aluminum nitride green porcelain tape to the first aluminum nitride green porcelain tape lamination for lamination to obtain a second aluminum nitride green porcelain tape lamination, and respectively filling palladium-gold and platinum/15% iridium alloy slurry in each filling hole of the third aluminum nitride green porcelain tape in parallel along the hole wall without connection, wherein the palladium-gold and the platinum/15% iridium alloy slurry are in contact with palladium-gold in the second aluminum nitride green porcelain tape filling hole;
a fourth layer of aluminum nitride green porcelain tape is stuck to the second aluminum nitride green porcelain tape lamination for lamination, and palladium-gold slurry is filled in each filling hole of the fourth aluminum nitride green porcelain tape; the filling metal in each filling hole of the fourth aluminum nitride green ceramic band is contacted with the two metals in two adjacent filling holes of the third aluminum nitride green ceramic band, so that an aluminum nitride ceramic chip containing an array thermopile structure is obtained;
and (3) carrying out laminating, cutting and high-temperature sintering on the aluminum nitride ceramic chip containing the array thermopile structure to obtain the high-temperature heat flow sensor.
2. The method of claim 1, further comprising the steps of baking at high temperature, and observing and correcting the structure under a microscope stage after the step of filling the metal slurry into the filling holes of the second, third and fourth aluminum nitride green tape layers.
3. The method of claim 2, wherein the high temperature oven drying is performed at 100 ℃ for 10 min.
4. The method of claim 1, wherein the step of laminating the aluminum nitride green ceramic tape containing the arrayed thermopile structure is followed by the steps of: wrapping the laminated aluminum nitride ceramic chip by using a silica gel film, setting the temperature of a laminating machine to be 70 ℃, and setting the static pressure to be 21MPa, and placing the wrapped aluminum nitride ceramic chip containing the array thermopile structure in the laminating machine for isostatic pressing lamination for 20 min.
5. The method of claim 1, wherein the step of sintering at high temperature is carried out by co-firing each individual array thermopile sensing structure cut from an aluminum nitride wafer in a hydrogen-protected high temperature furnace.
6. The method of claim 1, wherein the aluminum nitride green tape has square holes for the filling holes.
7. The method of claim 1, wherein the step of providing square aluminum nitride green ceramic strips of four different thicknesses comprises the steps of:
mixing aluminum nitride powder, water and a dispersing agent according to a certain ratio, adjusting the pH value of a system to be 9.0 by using ammonia water, and carrying out first ball milling for 24 hours; adding a binder and a plasticizer for secondary ball milling and mixing, adding a defoaming agent for vacuum defoaming, and preparing a blank sheet; and adjusting the knife edge height and the casting speed of the casting machine, drying and demoulding the blank sheet to obtain four casting sheets with different thicknesses, and slicing the casting sheets.
8. The method of claim 1, wherein the step of providing the thermocouple wires comprises forming the thermocouple wires by a screen printing process using a platinum brush on the edges of the filling holes diagonally opposite to the second alumina green ceramic tape, and connecting the thermocouple wires to the metal provided in the filling holes.
9. An HTCC-based high-temperature heat flow sensor, which is prepared by the preparation method of the high-temperature heat flow sensor according to any one of claims 1 to 8.
10. The HTCC-based high temperature heat flow sensor according to claim 9, wherein the first, second, third and fourth aluminum nitride green ceramic strips have a thickness of 100 μ ι η, 20 μ ι η, 100 μ ι η and 20 μ ι η, respectively.
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