CN117665061A - Carbon thick film atomic oxygen sensor and preparation method thereof - Google Patents
Carbon thick film atomic oxygen sensor and preparation method thereof Download PDFInfo
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 127
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 29
- 230000008569 process Effects 0.000 claims abstract description 17
- 238000007650 screen-printing Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 18
- 238000007639 printing Methods 0.000 claims description 16
- 230000009471 action Effects 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 9
- -1 dicarboxylic acid ester Chemical class 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052737 gold Inorganic materials 0.000 claims description 9
- 239000010931 gold Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000004513 sizing Methods 0.000 claims description 7
- 229920002433 Vinyl chloride-vinyl acetate copolymer Polymers 0.000 claims description 6
- 238000005520 cutting process Methods 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 claims description 3
- 229920001225 polyester resin Polymers 0.000 claims description 3
- 239000004645 polyester resin Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000003999 initiator Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 11
- 238000005259 measurement Methods 0.000 abstract description 5
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
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- 239000000126 substance Substances 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- 229910052762 osmium Inorganic materials 0.000 description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
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- 229910000489 osmium tetroxide Inorganic materials 0.000 description 1
- 239000012285 osmium tetroxide Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a carbon thick film atomic oxygen sensor and a preparation method thereof. An atomic oxygen sensor with carbon film thickness in the range of 3-200 mu m is prepared by adopting a screen printing process, so that the detection accuracy and the service life of the atomic oxygen sensor are improved. The invention solves the problems of the process and flow of preparing the carbon thick film atomic oxygen sensor, improves the uniformity, stability and printability of the carbon film, has the characteristics of simple process, less types of required raw materials, less environmental pollution, good stability and the like, can realize mass production, and ensures smaller difference between different batches. The carbon thick film atomic oxygen sensor prepared by the invention has the advantages of long service life, good performance and the like, and is more suitable for on-orbit long-time atomic oxygen detection and measurement.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a carbon thick film atomic oxygen sensor and a preparation method thereof.
Background
Atomic oxygen is an important component of the low earth orbit space atmospheric environment, and has high energy (about 5 eV) and high number density, so that under the long-term action, the atomic oxygen can generate serious chemical degradation effect on the surface material of the low earth orbit spacecraft, so that the performance of the material is degraded or invalid, and the performance of the spacecraft is influenced. Therefore, the research and detection of the space atomic oxygen environment are very necessary.
In mass spectrometry, mass loss test, chemical heat detection, film thickness measurement, semiconductor detection, resistance analysis and other atomic oxygen detection methods, the resistance analysis method has the characteristics of low cost, light detector mass, low power consumption, capability of measuring atomic oxygen fluence (flux density), simple circuit and the like, and is widely applied to space atomic oxygen detection.
The working principle of the resistance analysis method is as follows: the conductive film sensitive to the atomic oxygen is used as a sensor, the thickness of the conductive film is thinned under the action of the atomic oxygen, the resistance is increased, the resistance variation of the sensor is linearly related to the accumulated atomic oxygen flux received by the conductive film, and after calibration, the accumulated atomic oxygen flux can be obtained by measuring the real-time resistance of the sensor under the action of the atomic oxygen. Common conductive film materials include silver films, osmium films, and carbon films. The silver film reacts with atomic oxygen to generate solid oxide, so that the atomic oxygen is prevented from continuously reacting with the inner silver film, and the service life is short; osmium membrane and the osmium tetroxide generated by the reaction of atomic oxygen are toxic and are not popularized and utilized; carbon films react with atomic oxygen to produce gaseous substances and are widely used as atomic oxygen conductive films.
The current carbon film atomic oxygen sensor can be classified into a thick film atomic oxygen sensor and a thin film atomic oxygen sensor based on the thickness of the carbon film, which are different in that: firstly, the thickness is different, thick film generally means that the thickness of the carbon film ranges from 1 μm to 200 μm, and thin film is generally hundreds of nm; secondly, the processing technology is different, the thin film atomic oxygen sensor can be prepared by magnetron sputtering or plasma sputtering deposition and other technologies, and the thick film atomic oxygen sensor can only be prepared by screen printing technology; thirdly, the service life is different, the service life of the thin film atomic oxygen sensor is shorter under the same atomic oxygen environment, and the thin film atomic oxygen sensor can be generally used for only a few months, and the thick film atomic oxygen sensor can be used for a few years. Compared with a thin film atomic oxygen sensor, the thick film atomic oxygen sensor has longer service life, is more suitable for on-orbit long-time atomic oxygen environment monitoring, and can be manufactured in large batches.
At present, although a carbon film atomic oxygen sensor with a carbon film thickness of 28 mu m is developed abroad, the performance of the carbon film atomic oxygen sensor under the action of atomic oxygen is not ideal (see figure 5), namely the relative change of resistance R under the action of atomic oxygen 0 The dependence of R on the atomic oxygen flux F does not exhibit a good linear relationship. Compared with foreign countries, the carbon thick film atomic oxygen sensor with ideal performance has not been developed in China, and the research and application in the aspect in China have a larger gap.
Disclosure of Invention
Therefore, the invention aims to solve the technical problems that the atomic oxygen sensor with a thick carbon film and good performance is difficult to obtain in the prior art, and meets the requirements of the atomic oxygen sensor with long service life and long in-orbit atomic oxygen detection operation, thereby providing the carbon thick film atomic oxygen sensor and the preparation method thereof.
In order to achieve the above purpose, the present invention provides the following technical solutions:
in a first aspect, the invention provides a method for preparing a carbon thick film atomic oxygen sensor, comprising the following steps:
step 1, providing a substrate, ultrasonically cleaning with alcohol for 5-10 min, taking out, and drying with an infrared mesh belt drying furnace for later use;
step 2, printing an organic gold electrode on the dried substrate through a screen printing process, transferring to an infrared mesh belt drying furnace after finishing, drying for 8-10 min at 150 ℃, transferring to a high-temperature infrared mesh belt sintering furnace, cutting off a power supply of the high-temperature infrared mesh belt sintering furnace, naturally cooling to room temperature, and taking out for later use, wherein the sintering peak temperature is 850 ℃;
step 3, printing silver-palladium slurry bonding pads on the gold electrode through a screen printing process, transferring to an infrared mesh belt drying furnace after printing, drying for 8-10 min at 150 ℃, transferring to a high-temperature infrared mesh belt sintering furnace, sintering for 8-10 min at 850 ℃, cutting off a power supply of the high-temperature infrared mesh belt sintering furnace, naturally cooling to room temperature, and taking out for later use;
step 4, preparing a prefabricated slurry;
step 5, printing a carbon film by adopting the pre-sizing agent through a screen printing process, transferring to a hot air circulation oven after printing, and curing for 60-90 min at 140 ℃;
and 6, detecting, screening, welding leads, inspecting finished products, packaging and warehousing to obtain the carbon thick film atomic oxygen sensor.
Further, in step 4, the preparing the pre-slurry includes:
step 401, preparation of intermediate a: mixing the vinyl chloride-vinyl acetate copolymer and the dicarboxylic acid ester according to the weight ratio of 1:1, heating and stirring at 50-80 ℃, stopping heating and stirring after complete dissolution, and standing for standby;
step 402, preparation of intermediate B: mixing polyester resin and dicarboxylic acid ester according to the weight ratio of 1:1, heating and stirring at 50-80 ℃, stopping heating and stirring after complete dissolution, and standing for standby;
step 403, preparing the following components in percentage by weight: 30-50% of intermediate A, 5-15% of intermediate B, 0-6% of conductive carbon powder A, 0-6% of conductive carbon powder B, 0.1-0.5% of silane coupling agent and 10-40% of dicarboxylic acid ester;
step 404, fully mixing the prepared components by adopting a double-planetary power mixer, wherein the rotation speed is 800-1500 r/min, the revolution speed is 10-20 r/min, the cooling target temperature is 20-25 ℃, and the mixing time is 30-60 min;
step 405, grinding 15-30 times at 50-60 Hz frequency by adopting a three-roller grinder;
and 406, filtering and vacuum defoaming by using a screen with 150-400 meshes to obtain the prefabricated slurry.
Further, in the step (1), the substrate is a 96% alumina ceramic sheet, and the dimensions of the substrate are 60mm×45mm×3mm (length×width×thickness).
Further, in the step (2), the dimensions of the gold electrode were 5mm×5mm×0.5 μm (length×width×thickness).
Further, in the step (3), the size of the pad is 3mm×3mm×0.5 μm (length×width×thickness).
Further, in the step (5), the size of the carbon film is 40mm×5mm×3 to 200 μm (length×width×thickness).
Further, step (5) is performed 1 time, the thickness of the carbon film is 3 to 20 μm; executing the step (5) 2 times, wherein the thickness of the carbon film is 6-40 mu m; and similarly, 10 times of the step (5) are performed, wherein the thickness of the carbon film can reach 200 mu m at maximum.
Further, in the step (401), the vinyl chloride-vinyl acetate copolymer is prepared by copolymerizing vinyl chloride and vinyl acetate under the action of an initiator.
Further, the intermediate a prepared in the step (401) belongs to an ester polymer compound, and the intermediate B prepared in the step (402) belongs to an ester polymer compound.
In a second aspect, the present invention provides a carbon thick film atomic oxygen sensor prepared by the method of preparation.
Further, the carbon film thickness of the carbon thick film atomic oxygen sensor is 3-200 μm.
The technical scheme of the invention has the following advantages:
the invention adopts screen printing technology to prepare the carbon thick film atomic oxygen sensor with the carbon film thickness in the range of 3-200 mu m. According to the ground atomic oxygen simulation test result, the carbon thick film atomic oxygen sensor prepared by the process has good linear relation between the relative variable quantity of resistance and the accumulated atomic oxygen flux received by the sensor, namely, the response characteristic to the atomic oxygen effect is good, so that the test accuracy of the atomic oxygen flux is high, and the detection and measurement requirements of the atomic oxygen flux can be met.
In the invention, the intermediate A has the characteristics of low viscosity and good solubility in the prefabricated sizing agent, is favorable for uniform distribution of conductive carbon powder in the prefabricated sizing agent, and increases the adhesive force of the carbon powder to a base material, thereby improving the consistency of the conductive performance of the carbon film. In addition, intermediate a also has good flowability and is easy to screen print. The intermediate B enables the prepared carbon film to have better flexibility and processability, improves the chemical stability of the carbon film, and has stable and consistent reaction rate when reacting with atomic oxygen.
The invention solves the problems of the process and flow of preparing the carbon thick film atomic oxygen sensor, improves the uniformity, stability and printability of the carbon film, has the characteristics of simple process, less types of required raw materials, less environmental pollution, good stability and the like, can realize mass production, and ensures smaller difference between different batches. The carbon thick film atomic oxygen sensor prepared by the invention has good performance, high accuracy of atomic oxygen flux test results and long service life, and is more suitable for on-orbit long-time atomic oxygen detection and measurement application.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings used in the embodiments of the present application or the description of the prior art will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of a carbon thick film atomic oxygen sensor according to an embodiment of the present application.
Reference numerals: 1-1, an alumina substrate; 1-2, carbon film; 1-3, silver/palladium pads; 1-4, a gold electrode.
FIG. 2 is a graph showing the relative change R in resistance of a carbon thick film atomic oxygen sensor with a carbon film thickness of 25 μm according to an embodiment of the present application 0 Graph of R versus atomic oxygen cumulative flux F.
Reference numerals: A. a carbon film A having a thickness of 25 μm; B. a carbon film B having a thickness of 25 μm; C. a carbon film C having a thickness of 25 μm.
FIG. 3 is a graph showing the relative change R in resistance of a carbon thick film atomic oxygen sensor with a carbon film thickness of 50 μm according to an embodiment of the present application 0 Graph of R versus atomic oxygen cumulative flux F.
Reference numerals: a. a carbon film a having a thickness of 50 μm; b. a carbon film b having a thickness of 50 μm; c. a carbon film c having a thickness of 50 μm.
FIG. 4 is a graph showing the relative change R in resistance of a carbon thick film atomic oxygen sensor with a carbon film thickness of 200 μm according to an embodiment of the present application 0 Graph of R versus atomic oxygen cumulative flux F.
FIG. 5 shows the relative change R in resistance of a 28 μm atomic oxygen sensor atom developed by the university of south Ancompton under the action of atomic oxygen 0 Graph of R versus atomic oxygen cumulative flux F.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth such as the particular system architecture, techniques, etc., in order to provide a thorough understanding of the embodiments of the present invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present invention with unnecessary detail.
In the description of the present invention, "/" means "or" unless otherwise indicated, for example, A/B may mean A or B. "and/or" herein is merely an association relationship describing an association object, and means that three relationships may exist, for example, a and/or B may mean: a exists alone, A and B exist together, and B exists alone. Further, "at least one", "a plurality" means two or more. The terms "first," "second," and the like do not limit the number and order of execution, and the terms "first," "second," and the like do not necessarily differ.
In the embodiments of the present application, words such as "exemplary" or "such as" are used to mean serving as examples, illustrations, or descriptions. Any embodiment or design described herein as "exemplary" or "for example" should not be construed as preferred or advantageous over other embodiments or designs. Rather, the use of words such as "exemplary" or "such as" is intended to present related concepts in a concrete fashion that may be readily understood.
Furthermore, references to the terms "comprising" and "having" and any variations thereof in the description of the present application are intended to cover a non-exclusive inclusion. For example, a process, method, system, article, or apparatus that comprises a list of steps or modules is not limited to only those steps or modules but may, alternatively, include other steps or modules not listed or inherent to such process, method, article, or apparatus.
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the following description will be made with reference to the accompanying drawings of the present invention by way of specific embodiments.
Example 1
Referring to fig. 1, an embodiment of the present application provides a carbon thick film atomic oxygen sensor, the structure of which is shown in fig. 1, and the preparation method thereof includes:
(1) Taking 96% alumina ceramic chip as a substrate 1-1, wherein the size of the substrate 1-1 is 60mm multiplied by 45mm multiplied by 3mm (length multiplied by width multiplied by thickness), taking out after ultrasonic cleaning with alcohol for 5min, and drying with an infrared mesh belt drying furnace for standby;
(2) Printing an organic gold electrode 1-4 on the dried substrate through a screen printing process, wherein the size of the electrode 1-4 is 5mm multiplied by 0.5 mu m (length multiplied by width multiplied by thickness), transferring the substrate to an infrared mesh belt drying furnace after printing is finished, drying the substrate for 10min at 150 ℃, transferring the substrate to a high-temperature infrared mesh belt sintering furnace, sintering the substrate for 10min at the peak temperature of 850 ℃, cutting off the power supply of the high-temperature infrared mesh belt sintering furnace, naturally cooling the substrate to room temperature, and taking the substrate out for later use;
(3) Printing silver-palladium slurry bonding pads 1-3 on the gold electrodes 1-4 through a screen printing process, wherein the dimensions of the bonding pads 1-3 are 3mm multiplied by 0.5 mu m (length multiplied by width multiplied by thickness), transferring to an infrared mesh belt drying furnace after printing is finished, drying for 10min at 150 ℃, transferring to a high-temperature infrared mesh belt sintering furnace, sintering for 10min at the peak temperature of 850 ℃, cutting off the power supply of the high-temperature infrared mesh belt sintering furnace, naturally cooling to room temperature, and taking out for later use;
(4) Preparing a prefabricated slurry;
(5) Printing a carbon film 1-2 by using the prefabricated sizing agent prepared in the step (4) through a screen printing process, wherein the size of the carbon film 1-2 is 40mm multiplied by 5mm multiplied by 15 mu m (length multiplied by width multiplied by thickness), transferring the prefabricated sizing agent to a hot air circulation oven after printing is finished, and curing the prefabricated sizing agent at 140 ℃ for 60 minutes;
(6) And detecting, screening, welding leads, inspecting finished products, packaging and warehousing to obtain the carbon thick film atomic oxygen sensor.
Specifically, in the step (4), the preparation of the pre-slurry includes:
(401) Preparation of intermediate a: mixing the vinyl chloride-vinyl acetate copolymer and the dicarboxylic acid ester according to the weight ratio of 1:1, heating and stirring at 50-80 ℃, stopping heating and stirring after complete dissolution, and standing for standby;
(402) Preparation of intermediate B: mixing polyester resin and dicarboxylic acid ester according to the weight ratio of 1:1, heating and stirring at 50-80 ℃, stopping heating and stirring after complete dissolution, and standing for standby;
(403) The preparation method comprises the following steps of: 50% of the intermediate A, 15% of the intermediate B, 3% of conductive carbon black ECP-600JD, 3% of conductive carbon black EC-300J, 5600.3% of a coupling agent KH and 33.7% of dicarboxylic acid ester;
(404) Fully mixing the prepared components by adopting a double-planetary power mixer, wherein the rotation speed is 800r/min, the revolution speed is 10r/min, the cooling target temperature is 25 ℃, and the mixing time is 30min;
(405) Grinding 15 times at 50Hz by adopting a three-roller grinder;
(406) Filtering and vacuum defoaming by using a 300-mesh screen to obtain the prefabricated slurry.
Example 2
Referring to fig. 1, an embodiment of the present application provides a carbon thick film atomic oxygen sensor, whose structure is shown in fig. 1, and a preparation method thereof may refer to embodiment 1, except that: (5) In this step, screen printing was repeated twice, and the dimensions of the carbon film 1-2 were 40 mm. Times.5 mm. Times.25. Mu.m (length. Times.width. Times.thickness).
Example 3
Referring to fig. 1, an embodiment of the present application provides a carbon thick film atomic oxygen sensor, whose structure is shown in fig. 1, and a preparation method thereof may refer to embodiment 1, except that: (5) In this step, screen printing was repeated three times, and the dimensions of the carbon film 1-2 were 40 mm. Times.5 mm. Times.50. Mu.m (length. Times.width. Times.thickness).
Example 4
Referring to fig. 1, an embodiment of the present application provides a carbon thick film atomic oxygen sensor, whose structure is shown in fig. 1, and a preparation method thereof may refer to embodiment 1, except that: (5) In this step, screen printing was repeated ten times, and the dimensions of the carbon film 1-2 were 40 mm. Times.5 mm. Times.200. Mu.m (length. Times.width. Times.thickness).
Comparative example
An atomic oxygen sensor developed by the university of south Anton with a carbon film thickness of 28 μm was used for comparison. Comparative example relative change in resistance of atomic oxygen sensor under the action of atomic oxygen R 0 The relationship of R to the atomic oxygen cumulative flux F is shown in FIG. 5.
Test case
The atomic oxygen sensors of examples 2 to 4, in which the carbon films were 25 μm, 50 μm and 200 μm thick, were respectively subjected to performance tests in an atomic oxygen environment using a ground atomic oxygen test apparatus, and the test results are shown in fig. 2 to 4, respectively.
Principle of measuring atomic oxygen flux by resistance analysis: atomic oxygen flux is measured using the reactivity of the carbon film with atomic oxygen. The carbon film gradually thins and increases in resistance under the atomic oxygen environment. By measuring the change in resistance of the carbon film, the flux density of atomic oxygen was calculated. The formula is as follows:
wherein F is atomic oxygen cumulative flux (atom/cm) 2 ) K is a constant (atom/cm) related to the atomic oxygen sensor 2 )，R 0 The initial resistance (Ω) of the carbon film, and R is the resistance (Ω) of the carbon film after the atomic oxygen action.
Referring to FIGS. 2, 3 and 4, response curves of atomic oxygen sensors with carbon film thicknesses of 25 μm, 50 μm and 200 μm, respectively, under the action of atomic oxygen, R except for a part of data 0 A good linear relationship is shown between R and the atomic oxygen cumulative flux F, which is consistent with the principle of measuring the atomic oxygen flux by a resistance analysis method. It can be seen that the carbon thick film atomic oxygen sensor prepared according to the embodiment of the application can be used for measuring atomic oxygen flux after being calibrated.
Referring to FIG. 5, R of atomic oxygen sensor (carbon film thickness of 28 μm) developed by university of south Amton abroad 0 The curve of R as a function of atomic oxygen action time t is shown by a black thick solid line in the figure, and a black dotted line in the figure is a result of linear fitting according to the curve. As shown in FIG. 5, R of the thick film atomic oxygen sensor 0 The curve of R as a function of t shows more burrs and the curve differs greatly from the result of the linear fitting, so that the accuracy of the test result of atomic oxygen flux F is not very high. As shown in FIGS. 2 to 4, R of the atomic oxygen sensor prepared according to the method of the present invention 0 The change curve of R with the action time t of atomic oxygen is smooth and has little difference from the result of linear fitting. As can be seen by comparing fig. 2-4 with fig. 5: the carbon thick film atomic oxygen sensor prepared by the method has good response performance to atomic oxygen action and is suitable forThe test result of atomic oxygen flux is more accurate. Therefore, the carbon thick film atomic oxygen sensor prepared by the method has better performance and long service life, and is more suitable for on-orbit long-time detection and measurement of atomic oxygen flux.
In fig. 2 and 3, the curves of the atomic oxygen sensors having the same carbon film thickness cannot be completely overlapped, because: during the test, each carbon film atomic oxygen sensor was at a different distance from the center of the sample stage. The flux density of the atomic oxygen beam generated by the atomic oxygen simulation test equipment is maximum at the center position, and the flux density of the atomic oxygen beam is reduced along with the increase of the distance from the center of the sample table, so that the response curves of the carbon film atomic oxygen sensors with the same carbon film thickness cannot be completely overlapped.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (9)
1. The preparation method of the carbon thick film atomic oxygen sensor is characterized by comprising the following steps of:
step 1, providing a substrate, ultrasonically cleaning with alcohol for 5-10 min, taking out, and drying with an infrared mesh belt drying furnace for later use;
step 2, printing an organic gold electrode on the dried substrate through a screen printing process, transferring to an infrared mesh belt drying furnace after finishing, drying for 8-10 min at 150 ℃, transferring to a high-temperature infrared mesh belt sintering furnace, cutting off a power supply of the high-temperature infrared mesh belt sintering furnace, naturally cooling to room temperature, and taking out for later use, wherein the sintering peak temperature is 850 ℃;
step 3, printing silver-palladium slurry bonding pads on the gold electrode through a screen printing process, transferring to an infrared mesh belt drying furnace after printing, drying for 8-10 min at 150 ℃, transferring to a high-temperature infrared mesh belt sintering furnace, sintering for 8-10 min at 850 ℃, cutting off a power supply of the high-temperature infrared mesh belt sintering furnace, naturally cooling to room temperature, and taking out for later use;
step 4, preparing a prefabricated slurry;
step 5, printing a carbon film by adopting the pre-sizing agent through a screen printing process, transferring to a hot air circulation oven after printing, and curing for 60-90 min at 140 ℃;
and 6, detecting, screening, welding leads, inspecting finished products, packaging and warehousing to obtain the carbon thick film atomic oxygen sensor. Wherein,
in step 4, the preparing the pre-slurry includes:
step 401, preparation of intermediate a: mixing the vinyl chloride-vinyl acetate copolymer and the dicarboxylic acid ester according to the weight ratio of 1:1, heating and stirring at 50-80 ℃, stopping heating and stirring after complete dissolution, and standing for standby;
step 402, preparation of intermediate B: mixing polyester resin and dicarboxylic acid ester according to the weight ratio of 1:1, heating and stirring at 50-80 ℃, stopping heating and stirring after complete dissolution, and standing for standby;
step 403, preparing the following components in percentage by weight: 30-50% of intermediate A, 5-15% of intermediate B, 0-6% of conductive carbon powder A, 0-6% of conductive carbon powder B, 0.1-0.5% of silane coupling agent and 10-40% of dicarboxylic acid ester;
step 404, fully mixing the prepared components by adopting a double-planetary power mixer, wherein the rotation speed is 800-1500 r/min, the revolution speed is 10-20 r/min, the cooling target temperature is 20-25 ℃, and the mixing time is 30-60 min;
step 405, grinding 15-30 times at 50-60 Hz frequency by adopting a three-roller grinder;
and 406, filtering and vacuum defoaming by using a screen with 150-400 meshes to obtain the prefabricated slurry.
2. The method of manufacturing a carbon thick film atomic oxygen sensor according to claim 1, wherein in step (1), the substrate is preferably 96% alumina ceramic sheet, and the dimensions of the substrate are preferably 60mm x 45mm x 3mm (length x width x thickness).
3. The method for producing a carbon thick film atomic oxygen sensor according to claim 1, wherein in the step (2), the dimensions of the gold electrode are 5mm x 0.5 μm (length x width x thickness).
4. The method of manufacturing a carbon thick film atomic oxygen sensor according to claim 1, wherein in step (3), the dimensions of the pads are 3mm x 0.5 μm (length x width x thickness).
5. The method for producing a carbon thick film atomic oxygen sensor according to claim 1, wherein in the step (5), the carbon film has dimensions of 40mm×5mm×3 to 200 μm (length×width×thickness).
6. The method for manufacturing a carbon thick film atomic oxygen sensor according to claim 1, wherein step (5) is performed 1 time, the thickness of the carbon film being 3 to 20 μm; executing the step (5) 2 times, wherein the thickness of the carbon film is 6-40 mu m; and similarly, 10 times of the step (5) are performed, wherein the thickness of the carbon film can reach 200 mu m at maximum.
7. The method for manufacturing a carbon thick film atomic oxygen sensor according to claim 1, wherein in the step (401), the vinyl chloride-vinyl acetate copolymer is adopted to prepare the vinyl chloride-vinyl acetate copolymer under the action of an initiator, the intermediate a prepared in the step (401) belongs to an ester polymer compound, and the intermediate B prepared in the step (402) belongs to an ester polymer compound.
8. A carbon thick film atomic oxygen sensor, characterized in that it is produced by the method according to any one of claims 1 to 8.
9. The carbon thick film atomic oxygen sensor of claim 8, wherein a carbon film thickness of the carbon thick film atomic oxygen sensor is 3 to 200 μm.
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