CN113981396A - Method for preparing film heat flow meter by reactive magnetron sputtering - Google Patents

Method for preparing film heat flow meter by reactive magnetron sputtering Download PDF

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Publication number
CN113981396A
CN113981396A CN202111247766.6A CN202111247766A CN113981396A CN 113981396 A CN113981396 A CN 113981396A CN 202111247766 A CN202111247766 A CN 202111247766A CN 113981396 A CN113981396 A CN 113981396A
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sputtering
sensitive layer
substrate
layer
preparing
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邓元
王林斌
姜一
张玉蕾
赵未昀
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Hangzhou Innovation Research Institute of Beihang University
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Hangzhou Innovation Research Institute of Beihang University
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    • 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
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive 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
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • 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
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • 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
    • G01K7/02—Measuring 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
    • 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

Abstract

The invention discloses a method for preparing a film heat flow meter by reactive magnetron sputtering and the film heat flow meter. The film heat flow meter prepared by the invention can effectively reduce the size of the heat flow meter; the multi-heat-insulating layer with different materials can meet the requirement of heat flow direction detection.

Description

Method for preparing film heat flow meter by reactive magnetron sputtering
Technical Field
The invention relates to the technical field of high-temperature films, in particular to a method for preparing a film heat flow meter by reactive magnetron sputtering and the film heat flow meter.
Background
At present, the density of heat flow passing through a material locally in a unit time and an area caused by thermal radiation, thermal convection, thermal conduction and the like is generally analyzed and detected by a heat flow meter. Due to the reasons of large size of devices, thermal resistance of bodies and the like, the traditional heat flow meter generally has the problems of low measurement precision, slow response, poor sensitivity, limited application scene and the like when measuring the heat flow density. Particularly, the development of domestic heat flow meter devices is late, the size of the whole device is in a larger volume stage, the performance is poor when the device faces the environment with high temperature and high heat flow density, and the problems of response signal lag, low sensitivity and the like also exist.
In addition, the general heat flow meter only adopts the same material as a heat insulation layer at the outer side of the measuring end, so that signals output in different heat flow directions have no difference, and the heat flow conduction direction cannot be detected.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention aims to provide a method for preparing a thin film heat flow meter by reactive magnetron sputtering and the thin film heat flow meter prepared by the method, wherein the thin film heat flow meter prepared by the method can effectively improve the size of the heat flow meter, improve the measurement precision and sensitivity and reduce the response time.
The invention discloses a method for preparing a film heat flow meter by reactive magnetron sputtering, which adopts the technical scheme that the method comprises the following steps:
processing the substrate: processing grooves with uniform depth on a substrate according to a pre-designed pattern;
preparing a lower heat insulation layer: filling a groove filling material into the groove of the substrate with the groove processed through reactive magnetron sputtering, wherein the heat conductivity coefficient of the groove filling material is different from that of the substrate material, and the filled groove and the substrate form a lower heat insulation layer;
preparing a sensitive layer: sputtering on the lower heat insulation layer by adopting a two-step patterning mask to obtain a sensitive layer, wherein the sensitive layer comprises a first sensitive layer part and a second sensitive layer part which are connected together and symmetrical, the graphs of the first sensitive layer part and the second sensitive layer part are partially positioned on the surface of the groove and partially positioned on the surface of the substrate outside the groove, the material for preparing the first sensitive layer part is different from the material for preparing the second sensitive layer part, the groove filling material and the substrate material, and the material for preparing the second sensitive layer part is different from the material for preparing the first sensitive layer part, the groove filling material and the substrate material;
preparing an upper heat insulation layer: and performing reactive magnetron sputtering on the sensitive layer by adopting a two-step patterned mask to obtain an upper thermal insulation layer, wherein the upper thermal insulation layer comprises a first thermal resistance layer and a second thermal resistance layer, the pattern and the position of the first thermal resistance layer are the same as those of the filled groove, the second thermal resistance layer surrounds the first thermal resistance layer, covers the part of the first sensitive layer and the part of the second sensitive layer, which is positioned outside the groove, except for the pattern of an external connecting line, the material for preparing the first thermal resistance layer is the same as that of the substrate, and the material for preparing the second thermal resistance layer is the same as that of the groove filling material.
Further, in the step of processing the substrate, grooves with uniform depth are processed on the substrate according to a pre-designed pattern by using a laser etching method.
Further, the substrate is an alumina material substrate.
Furthermore, the parameters of the laser etching method are that the single pulse energy is 5-80 muJ, and the repetition frequency is 50-150 kHz.
Further, the groove filling material is silicon dioxide.
Further, in the step of preparing the lower thermal insulation layer, the parameter of the reactive magnetron sputtering is the purity of the silicon target material>4N, degree of vacuum of back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 50: 1-1: 1, the total air pressure is 1.0-4.0Pa, the sputtering power is 20-300W, the sputtering temperature is less than 400 ℃, the sputtering time is 2-24h, and annealing is carried out for 5-300min under the air or nitrogen atmosphere at 1500 ℃ and 550 ℃ after the sputtering is finished.
Further, the material of the first sensitive layer part and the material of the second sensitive layer part adopt platinum and platinum rhodium (10).
Further, the following are mentionedIn the step of preparing the sensitive layer, the sputtering parameter is the purity of the target material of platinum/platinum rhodium (10)>4N, degree of vacuum of back bottom<8*10-4Pa, argon pressure of 1.0-3.0Pa, sputtering power of 20-80W, sputtering temperature of less than 300 ℃ and sputtering time of 3-20 h.
Further, in the step of preparing the upper thermal insulation layer, the parameter of the first upper thermal insulation layer part of the reactive magnetron sputtering is the purity of the aluminum target material>4N, degree of vacuum of back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 9: 1-2: 1, the total air pressure is 1.5-3.0Pa, the sputtering power is 20-300W, the sputtering temperature is less than 400 ℃, the sputtering time is 2-24h, annealing is carried out for 5-300min in the atmosphere of air or nitrogen at 1500 ℃ after the sputtering is finished, and the parameter of the second upper thermal interlayer part of the reactive magnetron sputtering is the purity of the silicon target material>4N, degree of vacuum of back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 50: 1-1: 1, the total air pressure is 1.0-4.0Pa, the sputtering power is 20-300W, the sputtering temperature is less than 400 ℃, the sputtering time is 2-24h, and annealing is carried out for 5-300min under the air or nitrogen atmosphere at 1500 ℃ and 550 ℃ after the sputtering is finished.
The invention discloses a film heat flow meter, which comprises a lower heat interlayer, an upper heat interlayer and a sensitive layer positioned between the lower heat interlayer and the upper heat interlayer, and is prepared by adopting the method.
The invention has the following beneficial effects: the film heat flow meter prepared by the invention can effectively reduce the size of the heat flow meter, and the heat flow meter has lower response time due to the good combination between the covered heat interlayer and the sensitive layer, no gap and the thickness of only several micrometers without energy accumulation; the multi-logarithm sensitive layer is integrated in a small size range, and compared with a single pair of thermocouple signals, the multi-logarithm sensitive layer can be output in multiples, so that the measurement precision is improved; the sensitive layer adopts high-temperature-resistant platinum and platinum-rhodium (10) (namely Pt-PtRh (10)) series, and the material enables the heat flow meter to have excellent high-temperature-resistant and high-heat-flow-density-resistant performance, can work for a long time at high temperature and meets the measurement requirements on high precision and instantaneous heat flow density; the two ends of the sensitive layer are composed of different thermal impedance layers, the two thermal impedance layers are used for forming temperature difference output electric signals on the two ends of the thermocouple, the signal output is positive and negative, the heat flow direction is indicated, the measurement of the multidimensional heat flow density is possible, and the requirement for detecting the heat flow direction can be met.
Drawings
FIG. 1 is a schematic diagram of a preparation process of the preparation method of the present invention;
fig. 2 is a schematic view of a heat flow meter according to the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings and examples.
As shown in fig. 2, the thin film heat flow meter of the present embodiment includes a lower heat insulation layer, a sensitive layer, and an upper heat insulation layer sequentially stacked from bottom to top, where the lower heat insulation layer includes a substrate and a portion filled in a groove of the substrate, the substrate is an alumina substrate in the present embodiment, the groove is filled with silica to form a base silica layer, and the two form the lower heat insulation layer. The sensitive layer comprises a first sensitive layer part and a second sensitive layer part which are connected together symmetrically, the patterns of the first sensitive layer part and the second sensitive layer part are partially positioned on the surface of the groove and partially positioned on the surface of the substrate outside the groove, and an external connection wire is reserved, and in the embodiment, the material of the first sensitive layer part and the material of the second sensitive layer part adopt platinum and platinum rhodium (10). The upper thermal insulation layer is prepared on the sensitive layer and comprises a first thermal resistance layer and a second thermal resistance layer, the pattern and the position of the first thermal resistance layer are the same as those of the filled groove, the material is aluminum oxide and is the same as that of the substrate, the second thermal resistance layer surrounds the first thermal resistance layer, covers the pattern of the first sensitive layer part and the second sensitive layer part which are positioned in the groove except for the pattern of the external connecting line, the material is silicon dioxide, and the pattern of the second thermal resistance layer is the same as that of the groove filling material.
The thin film heat flow meter has the advantages that the heat interlayer and the sensitive layer which are covered with the thin film heat flow meter are well combined, no gap exists, the thickness is only several micrometers, energy is not accumulated, and the heat flow meter has low response time. The multi-logarithm sensitive layer is integrated in a small size range, and compared with a single pair of thermocouple signals, the multi-logarithm sensitive layer can be output in a multiple mode, and the measurement accuracy is improved. The sensitive layer adopts a high-temperature resistant Pt-PtRh (10) series, and the material enables the heat flow meter to have excellent high-temperature resistance and high-heat-flow-density resistance, so that the heat flow meter can work for a long time at high temperature, and the measurement requirements on high precision and instantaneous heat flow density are met; the two ends of the sensitive layer are composed of different thermal impedance layers, the two thermal impedance layers are different in heat conduction rate, so that temperature difference output electric signals are formed at the two ends of the thermocouple, when the thermocouple radiates from the front, the outer end of the thermocouple passes through silicon dioxide, the inner end of the thermocouple passes through aluminum oxide, the temperature of the inner end of the thermocouple is high, and at the moment, the output is a positive signal; when radiation is carried out on the reverse side, the outer end passes through alumina, the inner end passes through silica, the temperature of the inner end is low, the temperature difference is opposite to that of the inner end, and the output is a negative signal. Therefore, the heat flow direction can be indicated by outputting positive and negative signals through the signal, so that the measurement of the multi-dimensional heat flow density becomes possible, and the requirement of heat flow direction detection can be met
As shown in fig. 1, the preparation method of the thin film heat flow meter mainly includes four steps, specifically as follows:
step 1: processing of alumina substrates
The aluminum oxide substrate with the grooves with a certain depth is prepared by a laser etching method, the laser processing technological parameters are that the single pulse energy is 5-80 muJ, the repetition frequency is 50-150kHz, the processing speed is 20-200mm/s, the processing times are 1-10, the processing patterns are linearly filled, and the filling interval is 2-20μm, so that the substrate with the grooves with uniform depth is obtained, and the groove depth is 1-50μm. It will be appreciated that the grooves can also be made by methods known in the art such as machining, but that precision control is less desirable than laser etching.
In this embodiment, the pattern of the grooves is rectangular. It is understood that the pattern can be designed in advance according to actual situations, such as a circle, a triangle, etc.
Step 2: preparation of lower thermal barrier layer
After the processing is finished, silicon dioxide is filled in the groove through reactive magnetron sputtering to obtain a substrate silicon dioxide layer, and the specific sputtering technological parameter is a silicon target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 50: 1-1: 1, the total air pressure is 1.0-4.0Pa, the direct current power sputtering power is 20-300W, the sputtering temperature is between normal temperature and 400 ℃, the sputtering time is 2-24h, and annealing is carried out for 5-300min under the air or nitrogen atmosphere at the temperature of 1500 ℃ after the sputtering is finished. The substrate dioxygenThe silicon layer and the substrate form a lower thermal isolation layer.
In this embodiment, the substrate material is an aluminum oxide substrate, and the groove filling material is silicon dioxide. In practice, the groove filling material and the substrate material may be other high temperature resistant non-conductive materials, but the thermal conductivity of the groove filling material and the substrate material cannot be the same, and preferably the difference is larger than 20W/(m · K).
And step 3: preparation of the sensitive layer
The sensitive layer comprises a first sensitive layer part and a second sensitive layer part which are connected together symmetrically, and is prepared by sputtering through a two-step patterned mask, wherein the first sensitive layer part is prepared firstly, and the second sensitive layer part is prepared secondly. The first sensitive layer part and the second sensitive layer part are respectively made of different materials, and platinum/platinum rhodium (10) is adopted in the embodiment. The specific sputtering technological parameter is Pt/PtRh (10) target material (purity)>4N，>4N for purity higher than 99.99%), vacuum degree on back<8*10- 4Pa, argon pressure of 1.0-3.0Pa, direct current power supply sputtering power of 20-80W, sputtering temperature of normal temperature-300 ℃ and sputtering time of 3-20 h. The patterns of the first sensitive layer part and the second sensitive layer part are partially positioned on the surface of the groove and partially positioned on the surface of the substrate outside the groove, and an external connecting wire is reserved.
The material of the sensitive layer in this embodiment is Pt-PtRh (10) series. In practice, other materials, such as Pt-PtRh (13), Pt Rh (6) -PtRh (30), NiCr-NiSi, pure Cu-CuNi, Fe-CuNi, NiCr-Si-NiSi, NiCr-CuNi, etc. may be used. The materials have good high-temperature stability and signal output stability.
And 4, step 4: preparation of the Upper thermal Barrier
The upper thermal insulation layer comprises two layers of pattern structures, comprises a first thermal resistance layer and a second thermal resistance layer, and is prepared by sputtering through a two-step patterning mask, wherein the first thermal resistance layer is prepared in the first step, and the second thermal resistance layer is prepared in the second step. The materials of the first thermal resistance layer and the second thermal resistance layer correspond to the materials of the substrate and the groove, that is, the material of the first thermal resistance layer is alumina in the embodiment, an upper alumina layer is formed, and the second thermal resistance layerThe material of (2) is silicon dioxide, forming an upper silicon dioxide layer. The pattern and position of the first thermal resistance layer are the same as those of the filled groove, and the second thermal resistance layer surrounds the first thermal resistance layer, covers the first sensitive layer part and the second sensitive layer part, is positioned in the groove and is not opposite to the pattern of the external connecting line. Wherein the sputtering technological parameters of the upper silicon dioxide layer are the same as those in the step 1, and the reaction magnetron sputtering preparation technological parameters of the upper aluminum oxide layer are aluminum target materials (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 9: 1-2: 1, the total air pressure is 1.5-3.0Pa, the sputtering power of a direct current power supply is 20-300W, the sputtering temperature is between normal temperature and 400 ℃, and the sputtering time is 2-24 h. Annealing for 5-300min at 550-1500 ℃ in air or nitrogen atmosphere after the sputtering is finished.
The above is the thin film heat flowmeter of the present embodiment and the related manufacturing method, and the following gives specific examples of the manufacturing process.
Example 1
And (3) carrying out laser etching to obtain the aluminum oxide substrate with the pattern grooves, and cleaning. The laser processing technological parameters are as follows: the single pulse energy is 5 muJ, the repetition frequency is 150kHz, the processing speed is 20mm/s, the processing times are 5, the processing pattern is filled in a straight line, and the filling interval is 10 mu m. A substrate having grooves of uniform depth, the grooves having a depth of 1 μm, was obtained. Filling reactive magnetron sputtering silicon dioxide to obtain a substrate silicon dioxide layer, wherein the specific sputtering technological parameters are as follows: silicon target (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 50: 1, the total air pressure is 4.0Pa, the direct-current power supply sputtering power is 20W, the sputtering temperature is 400 ℃, and the sputtering time is 24 h. And annealing for 300min at 550 ℃ in an air atmosphere after the sputtering is finished. The sensitive layer is prepared by sputtering through a two-step patterning mask. Platinum/platinum rhodium (10) sputtering process parameters: Pt/PtRh (10) target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the argon pressure is 3.0Pa, the direct-current power supply sputtering power is 60W, the sputtering temperature is 200 ℃, and the sputtering time is 10 h. And preparing an upper heat insulation layer of a two-layer pattern structure by adopting two-step patterning mask sputtering. The reaction magnetron sputtering preparation process parameters of the upper alumina layer are as follows: aluminum target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 2: 1, total pressure 1.5Pa, direct currentThe source sputtering power is 20W, the sputtering temperature is 400 ℃, and the sputtering time is 24 h. And annealing for 300min at 550 ℃ in an air atmosphere after the sputtering is finished.
Example 2
And (3) carrying out laser etching to obtain the aluminum oxide substrate with the pattern grooves, and cleaning. The laser processing technological parameters are as follows: the single pulse energy is 40 muJ, the repetition frequency is 50kHz, the processing speed is 200mm/s, the processing times are 10, the processing pattern is filled in a straight line, and the filling interval is 20μm. A substrate having grooves of a uniform depth, the grooves having a depth of 50 μm, was obtained. Filling reactive magnetron sputtering silicon dioxide to obtain a substrate silicon dioxide layer, wherein the specific sputtering technological parameters are as follows: silicon target (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 1: 1, the total air pressure is 1.0Pa, the direct-current power supply sputtering power is 300W, the sputtering temperature is 100 ℃, and the sputtering time is 2 h. And annealing for 150min at 850 ℃ in a nitrogen atmosphere after the sputtering is finished. The sensitive layer is prepared by sputtering through a two-step patterning mask. Platinum/platinum rhodium (10) sputtering process parameters: Pt/PtRh (10) target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the argon pressure is 2.0Pa, the direct-current power supply sputtering power is 20W, the sputtering temperature is 300 ℃, and the sputtering time is 20 h. And preparing an upper heat insulation layer of a two-layer pattern structure by adopting two-step patterning mask sputtering. The reaction magnetron sputtering preparation process parameters of the upper alumina layer are as follows: aluminum target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 9: 1, the total air pressure is 2.0Pa, the direct-current power supply sputtering power is 300W, the sputtering temperature is 100 ℃, and the sputtering time is 2 h. And annealing for 150min at 850 ℃ in a nitrogen atmosphere after the sputtering is finished.
Example 3
And (3) carrying out laser etching to obtain the aluminum oxide substrate with the pattern grooves, and cleaning. The laser processing technological parameters are as follows: the single pulse energy is 80 muJ, the repetition frequency is 120kHz, the processing speed is 70mm/s, the processing times are 1, the processing pattern is linearly filled, and the filling interval is 2μm. A substrate having grooves of uniform depth, 25 μm deep, was obtained. Filling reactive magnetron sputtering silicon dioxide to obtain a substrate silicon dioxide layer, wherein the specific sputtering technological parameters are as follows: silicon target (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 17: 5, total air pressure is 2.2Pa, direct current power sputteringThe power is 150W, the sputtering temperature is normal temperature, and the sputtering time is 4 h. And annealing at 1500 ℃ for 5min in an air atmosphere after the sputtering is finished. The sensitive layer is prepared by sputtering through a two-step patterning mask. Platinum/platinum rhodium (10) sputtering process parameters: Pt/PtRh (10) target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, argon pressure of 1.0Pa, direct-current power supply sputtering power of 80W, sputtering temperature of normal temperature and sputtering time of 3 h. And preparing an upper heat insulation layer of a two-layer pattern structure by adopting two-step patterning mask sputtering. The reaction magnetron sputtering preparation process parameters of the upper alumina layer are as follows: aluminum target material (purity)>4N), degree of vacuum of the back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 4: 1, the total air pressure is 3.0Pa, the sputtering power of a direct-current power supply is 150W, the sputtering temperature is normal temperature, and the sputtering time is 4 h. And annealing at 1500 ℃ for 5min in an air atmosphere after the sputtering is finished.
The above description is only a preferred embodiment of the present invention, and should not be construed as limiting the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.

Claims (10)

1. A method for preparing a film heat flow meter by reactive magnetron sputtering is characterized by comprising the following steps:
processing the substrate: processing grooves with uniform depth on a substrate according to a pre-designed pattern;
preparing a lower heat insulation layer: filling a groove filling material into the groove of the substrate with the groove processed through reactive magnetron sputtering, wherein the heat conductivity coefficient of the groove filling material is different from that of the substrate material, and the filled groove and the substrate form a lower heat insulation layer;
preparing a sensitive layer: sputtering on the lower heat insulation layer by adopting a two-step patterning mask to obtain a sensitive layer, wherein the sensitive layer comprises a first sensitive layer part and a second sensitive layer part which are connected together and symmetrical, the graphs of the first sensitive layer part and the second sensitive layer part are partially positioned on the surface of the groove and partially positioned on the surface of the substrate outside the groove, and an external connecting line is reserved, wherein the material for preparing the first sensitive layer part is different from the material for preparing the second sensitive layer part, the groove filling material and the substrate material, and the material for preparing the second sensitive layer part is different from the material for preparing the first sensitive layer part, the groove filling material and the substrate material;
preparing an upper heat insulation layer: and performing reactive magnetron sputtering on the sensitive layer by adopting a two-step patterned mask to obtain an upper thermal insulation layer, wherein the upper thermal insulation layer comprises a first thermal resistance layer and a second thermal resistance layer, the pattern and the position of the first thermal resistance layer are the same as those of the filled groove, the second thermal resistance layer surrounds the first thermal resistance layer, covers the part of the first sensitive layer and the part of the second sensitive layer, which is positioned outside the groove, except for the pattern of an external connecting line, the material for preparing the first thermal resistance layer is the same as that of the substrate, and the material for preparing the second thermal resistance layer is the same as that of the groove filling material.
2. The method of claim 1, wherein the step of processing the substrate includes processing the substrate with a groove having a uniform depth in a pre-designed pattern by laser etching.
3. The method of claim 2, wherein the substrate is an alumina material substrate.
4. The method of claim 1 in which the laser etching process has parameters of a single pulse energy of 5-80 μ J and a repetition frequency of 50-150 kHz.
5. The method of claim 3, wherein the recess filling material is silicon dioxide.
6. The method of claim 5, wherein the preparing is performed with a thermal current meterIn the step of interlayer, the parameter of the reactive magnetron sputtering is the purity of the silicon target material>4N, degree of vacuum of back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 50: 1-1: 1, the total air pressure is 1.0-4.0Pa, the sputtering power is 20-300W, the sputtering temperature is less than 400 ℃, the sputtering time is 2-24h, and annealing is carried out for 5-300min under the air or nitrogen atmosphere at 1500 ℃ and 550 ℃ after the sputtering is finished.
7. The method of claim 5, wherein the materials of the first sensitive layer and the second sensitive layer are platinum and platinum-rhodium (10).
8. The method of claim 7, wherein in the step of forming the sensitive layer, the sputtering parameter is the purity of the target material of Pt/Rh (10)>4N, degree of vacuum of back bottom<8*10-4Pa, argon pressure of 1.0-3.0Pa, sputtering power of 20-80W, sputtering temperature of less than 300 ℃ and sputtering time of 3-20 h.
9. The method of claim 7, wherein the step of forming the upper thermal barrier layer comprises the step of reactive magnetron sputtering the first upper thermal barrier layer portion with a parameter of aluminum target purity>4N, degree of vacuum of back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 9: 1-2: 1, the total air pressure is 1.5-3.0Pa, the sputtering power is 20-300W, the sputtering temperature is less than 400 ℃, the sputtering time is 2-24h, annealing is carried out for 5-300min in the atmosphere of air or nitrogen at 1500 ℃ after the sputtering is finished, and the parameter of the second upper thermal interlayer part of the reactive magnetron sputtering is the purity of the silicon target material>4N, degree of vacuum of back bottom<8*10-4Pa, the gas flow ratio of argon to oxygen is 50: 1-1: 1, the total air pressure is 1.0-4.0Pa, the sputtering power is 20-300W, the sputtering temperature is less than 400 ℃, the sputtering time is 2-24h, and annealing is carried out for 5-300min under the air or nitrogen atmosphere at 1500 ℃ and 550 ℃ after the sputtering is finished.
10. A thin film heat flow meter comprising a lower heat barrier layer, an upper heat barrier layer and a sensitive layer between the lower heat barrier layer and the upper heat barrier layer, wherein the thin film heat flow meter is prepared by the method of any one of claims 1 to 9.
CN202111247766.6A 2021-10-26 2021-10-26 Method for preparing film heat flow meter by reactive magnetron sputtering Pending CN113981396A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060228897A1 (en) * 2005-04-08 2006-10-12 Timans Paul J Rapid thermal processing using energy transfer layers
CN106017696A (en) * 2016-07-13 2016-10-12 上海交通大学 Thermal resistance-type thin film thermopile-type transient heat flow meter and manufacturing method
CN111609951A (en) * 2020-06-09 2020-09-01 华中科技大学 Conformal preparation method of thick film heat flow meter and product
CN113091956A (en) * 2021-03-12 2021-07-09 上海交通大学 Double-layer thermal resistance type thin film thermopile type heat flowmeter and preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060228897A1 (en) * 2005-04-08 2006-10-12 Timans Paul J Rapid thermal processing using energy transfer layers
CN106017696A (en) * 2016-07-13 2016-10-12 上海交通大学 Thermal resistance-type thin film thermopile-type transient heat flow meter and manufacturing method
CN111609951A (en) * 2020-06-09 2020-09-01 华中科技大学 Conformal preparation method of thick film heat flow meter and product
CN113091956A (en) * 2021-03-12 2021-07-09 上海交通大学 Double-layer thermal resistance type thin film thermopile type heat flowmeter and preparation method

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