CN109211984A - A kind of miniature space hydrogen detection microsensor and preparation method thereof - Google Patents
A kind of miniature space hydrogen detection microsensor and preparation method thereof Download PDFInfo
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- CN109211984A CN109211984A CN201810730089.5A CN201810730089A CN109211984A CN 109211984 A CN109211984 A CN 109211984A CN 201810730089 A CN201810730089 A CN 201810730089A CN 109211984 A CN109211984 A CN 109211984A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
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- 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
- G01K7/183—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 characterised by the use of the resistive element
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Abstract
The invention discloses a kind of miniature space hydrogen to detect microsensor, using palladium-nickel alloy system as hydrogen sensitive material, prepare palladium-nickel alloy resistance hydrogen sensitive device, processing technology is simple and is easily integrated, and efficiently solve pure palladium and adsorbed as crossing for hydrogen sensitive material, the disadvantages of trailing phenomenon and sensitive thin film fall off;Palladium ni-mh sensitive material of the present invention is designed as patterned fold-line-shaped filiform membrane structure, relative to pure palladium material, it can produce more sensitivity sites inside palladium ni-mh sensitive thin film and generate cavity and recess etc. in micro-structure, the specific surface area of palladium ni-mh sensitive thin film is increased to a certain extent, higher signal strength can be obtained, this is that other hydrogen sensors cannot compare under equal conditions;The sensor belongs to space hydrogen atom original position micro detector important component, can be mounted on micro-nano satellite platform, detects the hydrogen atom concentration of extremely low concentration, and low in energy consumption, small in size, light-weight.
Description
Technical field
The invention belongs to gas concentration detection technology fields, and in particular to a kind of miniature space hydrogen detection microsensor and its
Preparation method.
Background technique
The abundance of H element is 95% in space environment, and the detection of H element is for disclosing universe origin, verifying huge explosion reason
Universe Red Shift theory is referred to important learning value and scientific meaning.Atomic hydrogen be in upper space ambient air ingredient most
Main neutral component, composition transfer have aeronomy, solar physics important meaning, for example,
Atmospheric Chemistry, plasma and neutral particle coupling process, the energy dissipation process of magnetosphere and earth magnetism storm are all associated.
In addition, as neutral component most light in atmospheric environment, atomic hydrogen is for being detached from minimum energy required for planetary gravitation, according to estimating
The speed that hydrogen atom escapes into outer space in the meter earth is about 108cm-2s-1, have in the long term for evolution of atmosphere process
There is profound significance.
It different from hydrogen in ground environment is existed in the form of hydrogen, the protium in space environment is deposited due to by plasma
High energy electron in body environment and under the radiation effects of sunlight, is with monatomic H or H2Two states exist, and concentration
It is very low, only 1011A/m3, therefore be difficult to carry out hydrogen detection using conventional method.Therefore hydrogen atom detects especially in-orbit original
Position Detection Techniques belong to more scabrous problem in the world.
Promotion and correlation detection skill of the recent years with countries in the world to space environment and space science cognitive ability
Protium detection demand in earth orbital environment is continuously improved in the continuous development of art, for example, Jianqi Qin in 2016 and
The detection about H atom concentration in earth geocorona that Lara Waldrop et al. is delivered on Nature communications
As a result, the research is for disclosing the detailed research of hydrogen atom distribution progress within the sun different cycles of activity and carrying out
Analysis.It is pointed out in report, the means of protium detection are with sun background the most, by being emitted after absorbing energy to H atom
The spectrum of specific wavelength out is detected.Therefore, the external detection to hydrogen atom is usually hoped using powerful high frequency radio
Remote mirror carries out remote sensing on ground or carries complicated optical imaging system to hydrogen using space shuttle and Large-scale satellite
Element is detected.For example, emitted by the hyperfine structure 21cm forbidden transition that radio telescope is observed in hydrogen atom
Radio radiation detects hydrogen atom.It is this kind of to observe the neutral hydrogen observation for applying in general to low red shift.Another observation of neutral hydrogen
Method be using the celestial body of high red shift as background light source, when these light source celestial bodies in direction of visual lines there are when HI cloud, in
Property hydrogen cloud can generate Absorption Line on the continuous spectrum of light source celestial body, and neutral hydrogen absorber is then inferred according to the feature of Absorption Line
Property.In addition, the geocorona scanning imaging instrument that such as U.S. is carried from rocket nineteen fifty-seven for the first time is to earth atmosphere hydrogen atom
Density is detected, and the research has great importance for disclosing H concentration in geocorona outermost layer environment.The passing of satelline is carried
Geocorona airglow in one solar cycle of GUVI optical spectrum imagers degree carries out imaging analysis, obtains in current geocorona environment
The detailed data that H atom the most accurate is fluctuated with solar cycle.
The features such as distribution of micro-nano satellite constellation type solid and real-time detection, the carrying for being highly suitable as the detection of space hydrogen are flat
Platform.China, which has begun, at present carries out the detection of space hydrogen using micro-nano satellite platform.But due to micro-nano satellite it is light-weight,
The own characteristics such as small in size, the low in energy consumption and service life is short, have stringent limit for the volume, weight and power consumption of load etc.
System.Therefore, the high and low power consumption of detection accuracy is developed, the micro-sensor technologies of small size are to realize micro-nano satellite hydrogen Detection Techniques
It is crucial.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of miniature space hydrogen detection microsensor and preparation method thereof, it can
To obtain higher signal strength, detection accuracy is improved;Preparation method is simply easy to implement.
A kind of miniature space hydrogen detects microsensor, hytrogen sensitive film including substrate and thereon, temperature detecting resistance and
Adding thermal resistance;The hytrogen sensitive film is filiform, and detour is distributed on the substrate;The adding thermal resistance is close to the hydrogen sensitive
Film distribution;The material of the hytrogen sensitive film is palladium-nickel alloy material.
It further, further include pad, for welding drawing for the hytrogen sensitive film, temperature detecting resistance and adding thermal resistance
Line.
Preferably, the temperature detecting resistance and adding thermal resistance use Pt resistance.
Preferably, the temperature detecting resistance and adding thermal resistance are used to the temperature of hydrogen detection microsensor being maintained at 20 DEG C
Within the scope of~50 DEG C.
A kind of preparation method of miniature space hydrogen detection microsensor, includes the following steps:
Step 1 makes substrate using silica, and carries out washing and drying treatment:
Step 2 deposits Si on the substrate3N4Film;
Step 3, in the Si3N4Temperature detecting resistance and temperature resistance are prepared on film;
Step 4, according to the figure of temperature detecting resistance and temperature resistance, respectively the two upper surface deposit Si3N4Film;
Step 5 prepares PdNi hytrogen sensitive film on the substrate;
Step 6 prepares SiO on the PdNi hytrogen sensitive film2Protective layer.
Further, after completing step 6, pad is prepared on the substrate.
Preferably, PdNi hytrogen sensitive film figure is formed on the substrate using photoetching technique first in the step 5;So
Deposit the PdNi film of 80nm on PdNi hytrogen sensitive film figure using magnetically controlled sputter method again afterwards.
Preferably, temperature detecting resistance and temperature resistance figure is formed on the substrate using photoetching technique first in the step 3
Shape;Then the Pt film of 80nm is deposited on figure using magnetically controlled sputter method again.
Preferably, forming SiO on PdNi hytrogen sensitive film using photoetching technique first in the step 62Protective layer figure
Shape;Then the SiO of 50nm is deposited on figure using magnetically controlled sputter method again2Film.
Preferably, ambient anneal heat treatment is carried out after completing step 6, specifically: sample is placed in vacuum annealing furnace
300 DEG C of heat preservation 2h are heated to, wherein heating and temperature-fall period are passed through high pure nitrogen, holding stage is passed through the nitrogen of 2% density of hydrogen
Hydrogen gaseous mixture.
The invention has the following beneficial effects:
The present invention, as hydrogen sensitive material, prepares palladium-nickel alloy resistance hydrogen sensitive device using palladium-nickel alloy system, processes
It is technically simple and be easily integrated, and efficiently solve pure palladium and adsorbed as crossing for hydrogen sensitive material, trailing phenomenon and sensitive thin film
The disadvantages of falling off;Palladium ni-mh sensitive material of the present invention is designed as patterned fold-line-shaped filiform membrane structure, relative to pure palladium material
Expect, can produce more sensitivity sites inside palladium ni-mh sensitive thin film and generates cavity and recess etc. in micro-structure,
The specific surface area of palladium ni-mh sensitive thin film is increased to a certain extent, can obtain higher signal strength, this is equal conditions
Under other hydrogen sensors cannot compare;The sensor belongs to space hydrogen atom original position micro detector important component,
It can be mounted on micro-nano satellite platform, detect the hydrogen atom concentration of extremely low concentration, and low in energy consumption, small in size, light-weight.
In the present invention, hydrogen barrier layer is deposited in the upper and lower surface of temperature detecting resistance and temperature resistance, it can be to avoid hydrogen from base
Bottom side diffuses into Pt temperature detecting resistance and temperature resistance through substrate, so as to cause the variation of Pt resistance, thus improves
Detection accuracy;SiO is deposited in hytrogen sensitive film upper surface2Protective layer can stop other gases and steam to generate sensor
It influences and interferes;Further increase measurement accuracy.
Detailed description of the invention
Fig. 1 is miniature space hydrogen detection microsensor basic block diagram;
Fig. 2 is miniature space hydrogen detection microsensor preparation technology flow chart.
Wherein, 1- substrate, 2- temperature detecting resistance, 3- adding thermal resistance, 4-PdNi hytrogen sensitive film, 5- pad.
Specific embodiment
The present invention will now be described in detail with reference to the accompanying drawings and examples.
A kind of miniature space hydrogen detection microsensor, the sensor include oxidation silicon base 1, PdNi hytrogen sensitive film 4, survey
Warm resistance 2, adding thermal resistance 3, pad 5, the outer dimension of sensor are 3.5mmx3.5mmx0.5mm, as shown in Figure 1.The sensing
Device by measurement absorption hydrogen after sensitive thin film resistance variations can quantitatively acquisition hydrogen concentration, wherein temperature detecting resistance 2 and plus
Thermal resistance 3 guarantees that operating temperature of the sensor in space environment inhales hydrogen within the scope of 20 DEG C~50 DEG C, while for sensor
Quick dehydrogenation afterwards restores.
The substrate 1 uses silica material, the carrying for entire sensor;
Temperature detecting resistance 2 on the sensor uses Pt material, and Pt temperature detecting resistance 2 is detour wire shaped, Pt temperature detecting resistance 2
It is mainly used for the environment temperature and operating temperature of measurement sensor, 2 film of Pt temperature detecting resistance is 100 sides, and resistance value is 100 Ω;
Adding thermal resistance 3 on the sensor uses Pt material, and Pt adding thermal resistance 3 is detour wire shaped, guarantees sensor
Operating temperature in space environment inhales the quick dehydrogenation recovery after hydrogen for sensor within the scope of 20 DEG C~50 DEG C.
3 film of Pt adding thermal resistance is 75 sides, and resistance value is 85 Ω;
The hytrogen sensitive film 4 uses PdNi alloy material, measures for hydrogen.PdNi hydrogen sensitive resistance is that detour is linear
Shape, PdNi hydrogen sensitive resistance film are 95 sides, and resistance value is 750 Ω;To save space, simultaneously in order to enable after sensor suction hydrogen
Quick dehydrogenation restore, adding thermal resistance 3 is distributed close to the hytrogen sensitive film 4, and the two detour shape having the same.
The pad 5 is used for welding lead using golden material, for power supply and data transmission.
Miniature space hydrogen detection microsensor preparation method of the invention comprises the following specific steps that:
Step 1, silica Substrate treatment:
Oxidation silicon chip 1 is cleaned by ultrasonic 15min with acetone, alcohol, deionized water respectively, uses N2Gas dries up silicon wafer table
Face moisture.
Step 2, Si3N4The deposition of film:
Oxidation silicon chip 1 is placed in vacuum chamber, background vacuum is evacuated to by 8x10 by molecular pump-4Pa is hereinafter, first
It is passed through the high-purity argon gas of 30sccm, air pressure is adjusted to open radio frequency source after 1Pa, adjusting RF source power is 200W, pre-sputtering silicon
After target 15min, it is passed through the high pure nitrogen of 5sccm, reaction magnetocontrol sputtering 15min is aoxidizing deposited on silicon substrates a layer thickness about
The Si of 50nm3N4As the barrier layer of hydrogen, hydrogen is avoided to diffuse into Pt temperature detecting resistance and temperature control electricity through substrate from substrate side
Resistance, so as to cause the variation of Pt resistance.
The preparation of step 3, Pt temperature detecting resistance 2 and temperature resistance 3:
Using 4000A positive photoresist, with the uniform whirl coating of 3000r/min on whirl coating platform, photoresist thickness is in 2~3um
Between, 90s post bake is then toasted, with photo-etching machine exposal 4s, is subsequently placed at 45s in developer solution, deionization forms Pt after rinsing and surveys
The figure of warm resistance 2 and temperature resistance 3;On figure simultaneously using the Pt film of Deposited By Dc Magnetron Sputtering a layer thickness about 80nm
Stripping photoresist forms Pt thermometric/temperature resistance.
Step 4, Si3N4The deposition of film:
Using 4000A positive photoresist, with the uniform whirl coating of 3000r/min on whirl coating platform, photoresist thickness is in 2~3um
Between, 90s post bake is then toasted, with photo-etching machine exposal 4s, is subsequently placed at 45s in developer solution, deionization forms Si after rinsing3N4
The figure on barrier layer;Wherein, consistent with the figure of temperature detecting resistance and temperature resistance;Using magnetron sputtering in Si3N4The figure on barrier layer
The Si of a layer thickness about 50nm is deposited in shape3N4As Pt thermometric/temperature resistance hydrogen barrier layer, as a result, in temperature detecting resistance and temperature
The upper and lower surface of control resistance forms complete hydrogen barrier layer, avoids hydrogen and Pt from acting on and Pt thermometric/temperature resistance resistance value is caused to become
Change.
The preparation of step 5, PdNi hytrogen sensitive film 4:
Using 4000A positive photoresist, with the uniform whirl coating of 3000r/min on whirl coating platform, photoresist thickness is in 2~3um
Between, 90s post bake is then toasted, with photo-etching machine exposal 4s, is subsequently placed at 45s in developer solution, deionization forms PdNi after rinsing
The figure of sensitive thin film 4;Deposit a layer thickness about 80nm's on 4 figure of PdNi sensitive thin film using magnetically controlled DC sputtering technology
PdNi film 4 and stripping photoresist formation hydrogen sensitive resistance pattern.
Step 6, SiO2The preparation of protective layer:
Using 4000A positive photoresist, with the uniform whirl coating of 3000r/min on whirl coating platform, photoresist thickness is in 2~3um
Between, 90s post bake is then toasted, with photo-etching machine exposal 4s, is subsequently placed at 45s in developer solution, deionization forms SiO after rinsing2
The figure of protective layer, the SiO of r. f. magnetron sputtering a layer thickness about 50nm2Film and stripping photoresist formation protective layer figure
Shape.Since SiO2 protective layer is porous structure, hydrogen molecule is the smallest gas molecule, so only hydrogen can be protected by SiO2
Layer, other gases and steam can not pass through, therefore can reach and steam and other atmosphere is avoided to have an impact and interfere sensor.
The preparation of step 7, pad 5:
Using 4000A positive photoresist, with the uniform whirl coating of 3000r/min on whirl coating platform, photoresist thickness is at 2~3 μm
Between, subsequent front baking 90s post bake is subsequently placed at 45s in developer solution with photo-etching machine exposal 4s, and deionization forms gold solder after rinsing
The figure of disk, magnetron sputtering deposits the Au film of a layer thickness about 280nm and stripping photoresist forms gold solder disk.Wherein, thermometric
The position at the both ends of resistance and temperature resistance and PdNi sensitive thin film forms pad, for powering and transmitting signal.
Step 8, ambient anneal heat treatment:
Sample is placed in vacuum annealing furnace and is heated to 300 DEG C of heat preservation 2h, wherein heating and temperature-fall period are passed through High Purity Nitrogen
Gas, holding stage are passed through the nitrogen and hydrogen mixture of 2% density of hydrogen.
The isolated sensor chip of step 9, slice.
In conclusion the above is merely preferred embodiments of the present invention, being not intended to limit the scope of the present invention.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of miniature space hydrogen detects microsensor, which is characterized in that hytrogen sensitive film, thermometric including substrate and thereon
Resistance and adding thermal resistance;The hytrogen sensitive film is filiform, and detour is distributed on the substrate;The adding thermal resistance is close to institute
State hytrogen sensitive film distribution;The material of the hytrogen sensitive film is palladium-nickel alloy material.
2. a kind of miniature space hydrogen as described in claim 1 detects microsensor, which is characterized in that further include pad, be used for
Weld the lead of the hytrogen sensitive film, temperature detecting resistance and adding thermal resistance.
3. a kind of miniature space hydrogen as described in claim 1 detects microsensor, which is characterized in that the temperature detecting resistance and
Adding thermal resistance uses Pt resistance.
4. a kind of miniature space hydrogen as described in claim 1 detects microsensor, which is characterized in that the temperature detecting resistance and plus
Thermal resistance is used to for the temperature of hydrogen detection microsensor being maintained within the scope of 20 DEG C~50 DEG C.
5. a kind of a kind of preparation method of miniature space hydrogen detection microsensor as described in claim 1, which is characterized in that packet
Include following steps:
Step 1 makes substrate using silica, and carries out washing and drying treatment:
Step 2 deposits Si on the substrate3N4Film;
Step 3, in the Si3N4Temperature detecting resistance and temperature resistance are prepared on film;
Step 4, according to the figure of temperature detecting resistance and temperature resistance, respectively the two upper surface deposit Si3N4Film;
Step 5 prepares PdNi hytrogen sensitive film on the substrate;
Step 6 prepares SiO on the PdNi hytrogen sensitive film2Protective layer.
6. a kind of preparation method of miniature space hydrogen detection microsensor as claimed in claim 5, which is characterized in that complete step
After rapid 6, the pad is prepared on the substrate.
7. a kind of preparation method of miniature space hydrogen detection microsensor as claimed in claim 5, which is characterized in that the step
In rapid 5, PdNi hytrogen sensitive film figure is formed on the substrate using photoetching technique first;Then existed again using magnetically controlled sputter method
The PdNi film of 80nm is deposited on PdNi hytrogen sensitive film figure.
8. a kind of preparation method of miniature space hydrogen detection microsensor as claimed in claim 5, which is characterized in that the step
In rapid 3, temperature detecting resistance and temperature resistance figure are formed on the substrate using photoetching technique first;Then magnetron sputtering side is used again
Method deposits the Pt film of 80nm on figure.
9. a kind of preparation method of miniature space hydrogen detection microsensor as claimed in claim 5, which is characterized in that the step
In rapid 6, SiO is formed on PdNi hytrogen sensitive film using photoetching technique first2Protect layer pattern;Then magnetron sputtering is used again
Method deposits the SiO of 50nm on figure2Film.
10. a kind of preparation method of miniature space hydrogen detection microsensor as claimed in claim 5, which is characterized in that complete
After step 6, ambient anneal heat treatment is carried out, specifically: sample is placed in vacuum annealing furnace and is heated to 300 DEG C of heat preservation 2h,
Wherein heating and temperature-fall period are passed through high pure nitrogen, and holding stage is passed through the nitrogen and hydrogen mixture of 2% density of hydrogen.
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CN110426422A (en) * | 2019-09-12 | 2019-11-08 | 中国工程物理研究院总体工程研究所 | Membrane bridge pressure type nitrogen atmosphere sensor |
CN111118330A (en) * | 2019-12-16 | 2020-05-08 | 北京凯恩特技术有限公司 | Palladium-based ternary alloy hydrogen-sensitive material, film, element, preparation method and hydrogen sensor |
WO2021036867A1 (en) * | 2019-08-30 | 2021-03-04 | 江苏多维科技有限公司 | Hydrogen gas sensor based on electrically isolated tunnel magnetoresistive sensitive element |
CN112763660A (en) * | 2020-12-28 | 2021-05-07 | 苏州芯镁信电子科技有限公司 | Palladium film hydrogen sensor |
CN116773616A (en) * | 2023-08-25 | 2023-09-19 | 宁德时代新能源科技股份有限公司 | Gas sensor, battery, power consumption device, and gas concentration detection method |
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