CN107085015B - Wireless and passive gas, temperature biparameter sensor and preparation method thereof - Google Patents
Wireless and passive gas, temperature biparameter sensor and preparation method thereof Download PDFInfo
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- CN107085015B CN107085015B CN201710232914.4A CN201710232914A CN107085015B CN 107085015 B CN107085015 B CN 107085015B CN 201710232914 A CN201710232914 A CN 201710232914A CN 107085015 B CN107085015 B CN 107085015B
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/227—Sensors changing capacitance upon adsorption or absorption of fluid components, e.g. electrolyte-insulator-semiconductor sensors, MOS capacitors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/34—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using capacitative elements
- G01K7/343—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using capacitative elements the dielectric constant of which is temperature dependant
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/221—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance by investigating the dielectric properties
- G01N2027/222—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance by investigating the dielectric properties for analysing gases
Abstract
The invention belongs to sensor technical fields, for solve that existing gas sensor stability is poor, reuse rate is low and need power supply power supply cause the sensor life-time time limit it is short, cannot be the hot operation the technical issues of, provide a kind of wireless and passive gas, temperature biparameter sensor and preparation method thereof, sensor includes medium substrate, the side setting gas test inductance coil and interdigital capacitor of medium substrate, the inside of gas test inductance coil is arranged in interdigital capacitor, and interdigital capacitor is connected with the inner ring of gas test inductance coil, GO/In is adhered on interdigital capacitor surface2O3Temperature test coil is arranged in air-sensitive film, the other side of medium substrate, and temperature test coil and its own existing parasitic capacitance form a LC resonance circuit.The configuration of the present invention is simple is reasonable, is measured using the method for wireless and passive, improves the stability of measurement, reduces power consumption, easy to process conducive to integration, the micromation for realizing gas, temperature biparameter sensor, low in cost.
Description
Technical field
The invention belongs to sensor technical fields, and in particular to a kind of wireless and passive gas, temperature biparameter sensor and
Preparation method.
Background technique
With the development of the social economy, industrialized progress, more and more toxic gases are continuously emerged, and threaten to people
The existence and health of class.Most of gas sensor is all metal-oxide gas transducer at present, with higher sensitive
Degree, response is rapid and uses the features such as simple, but its stability is poor, lower reusable rate etc., and traditional gas
Body sensor be all it is active, need power supply power supply, this results in the sensor life-time time limit is short, cannot work at high temperature,
Its application field is limited by very large.In recent years, with the development of wireless and passive technology and the promotion of environmental protection life, nothing
Line passive source gas sensor has become the new direction of future studies.
Summary of the invention
The present invention is that the existing gas sensor stability of solution is poor, reuse rate is low and power supply power supply is needed to cause to sense
The device service life time limit is short, cannot provide a kind of wireless and passive gas, temperature biparameter sensor the hot operation the technical issues of
And preparation method thereof.
The technical solution adopted by the invention is as follows:
A kind of wireless and passive gas, temperature biparameter sensor, are prepared using magnetron sputtering technique, including are used
Medium substrate made of ltcc substrate, the side setting gas test inductance coil and interdigital capacitor of medium substrate are described interdigital
The inside of gas test inductance coil is arranged in capacitor, and interdigital capacitor is connected with the inner ring of gas test inductance coil, interdigital
Capacitive surface adheres to GO/In2O3Temperature test coil, the temperature test is arranged in the other side of air-sensitive film, the medium substrate
Coil and its own existing parasitic capacitance form a LC resonance circuit.
The preparation method of a kind of wireless and passive gas, temperature biparameter sensor, comprising the following steps: first in LTCC base
Metallic vias is processed on plate, the interconnection for gas test inductance coil and interdigital capacitor；It will be golden using the technology of magnetron sputtering
Gold atom on target is splashed to the front and back of ltcc substrate, sputters gas test inductor wire in the front of ltcc substrate
Circle and interdigital capacitor, go out temperature test coil in the back spatter of ltcc substrate；Graphene oxide is prepared using Hummers method
GO；Pale yellow powder In is prepared using the method for collosol and gel2O3, obtained pale yellow powder is ground in agate mortar
The nanometer In refined2O3Particle；By the GO prepared and the nanometer In prepared2O3Particle is doped, and is coated to interdigital
On capacitor, interdigital capacitor is completely covered.
The specific preparation step of wireless and passive gas, temperature biparameter sensor are as follows:
(1) metallic vias is processed on ltcc substrate first, for the interconnection of gas test inductance coil and interdigital capacitor,
The technology of lamination is recycled to be integrally formed two layers of ltcc substrate lamination；
(2) first with sol evenning machine in the even layer photoresist in front for preparing integral ltcc substrate, by gas test
Inductance coil removes the photoresist on ltcc substrate using litho machine with interdigital capacitor mask plate, then uses magnetic control sputtering device handle
Gold atom is splashed on substrate, and finally extra photoresist is washed with acetone, leaves gas test inductance coil and fork
Refer to capacitor；The sputtering of temperature test coil is got at the ltcc substrate back side using technique same as ltcc substrate front, is formed
The wireless sourceless sensor of gas, temperature biparameter；
(3) preparation of graphene oxide takes the 100mL concentrated sulfuric acid and 10mL phosphoric acid to be added sequentially in three-necked bottle；It will mixing
Acid is placed in ice-water bath, is slow added into 0.8g crystalline flake graphite and 5g potassium permanganate, stirs 45min；Mixture is placed in 45 ~
It after stirring 35min in 55 DEG C of constant temperature water tanks, is placed in 60 DEG C of constant temperature water tanks and reacts 16h, mixture is in blackish green；It is slowly added dropwise
The hydrogen peroxide of 50mL5% is stirred well to mixture and golden yellow is presented；Product is moved in beaker, room temperature stands cooling, spends
Ion water washing is repeatedly until neutral；Product after washing is placed in 60 DEG C of drying in drying box, products therefrom is oxidation stone
Black alkene；
(4) InCl of 1.5g is weighed3•4H2O is dissolved in the distilled water of 20ml, and 2% polyethylene glycol is added, and mixing is stirred
Mix a period of time；The NH of 1mol/L is slowly added dropwise into solution at room temperature3•H2O is simultaneously slowly stirred until during the pH value of solution is
Property, jelly is obtained, sol solution placement is become into gel in static 2 hours at room temperature；It is repeatedly washed after filtering with deionized water
Wash, by washed gel be placed in drying box 100 DEG C at a temperature of dry 3 hours, then with 300 in high temperature furnace
DEG C temperature calcination 1 hour, obtained pale yellow powder, obtained pale yellow powder is ground to obtain diameter in agate mortar be
The nano indium oxide particle of 15-45nm；
(5) by the GO prepared and the nanometer In prepared2O3Particle is doped in 1.5% ratio, is ground using agate
Alms bowl grinding uniformly, is added suitable deionized water and is tuned into slurry；The slurry mixed up is coated to interdigital electricity by the way of being coated with
Interdigital capacitor is completely covered Rong Shang, it is ensured that thickness is uniform, places dry in the cool at room temperature；It, will after being completely dried
Sensor, which is placed in 260 DEG C of high temperature furnaces, is sintered 2 h；Finally by the sensor prepared 24 h of aging in air.
Beneficial effects of the present invention: compared with prior art, gas of the present invention, temperature biparameter sensor use
LC resonance principle (such as Fig. 1) utilizes gas sensitization layer GO/ In2O3Physical absorption object gas, so that the electricity between interdigital capacitor
Appearance, resistance change with the difference of adsorbed gas concentration, measure to realize the wireless and passive of gas, sensor base
The dielectric constant at bottom is temperature sensitive, and when extraneous temperature changes, the parasitic capacitance size of sensor also changes,
It eventually leads to sensor resonant frequency to change with temperature, realizes the wireless and passive measurement to temperature.The present invention is by gas
Measurement and temperature measurement combine, and two measurement methods are measured using the method for wireless and passive, are improved
The stability of measurement, reduces power consumption, realizes the measurement to gas, temperature biparameter, and dimensionally has very
Big flexibility.
The configuration of the present invention is simple is reasonable, conducive to integration, the micromation for realizing gas, temperature biparameter sensor, is convenient for
Processing, it is low in cost.
Detailed description of the invention
Fig. 1 is test schematic of the invention；
Fig. 2 is that LTCC material is laminated process flow diagram；
Fig. 3 is magnetron sputtering front flow diagram；
Fig. 4 is magnetron sputtering back side flow diagram；
Fig. 5 is concrete structure schematic diagram of the invention；
In figure: 1- sensor；2- Network Analyzer；3- interrogation antenna；4- gas test inductance coil；5- interdigital capacitor；
6- temperature test coil；7- medium substrate；8- punching；The filling of 9- metal；10- lamination；11- cofiring；12- spin coating；13- photoetching；
14- sputtering；15- removes photoresist；16-GO/ In2O3Air-sensitive film.
Specific embodiment
As shown in figure 5, a kind of wireless and passive gas, temperature biparameter sensor, are prepared using magnetron sputtering technique,
Including medium substrate 7, the medium substrate 7 is made of ltcc substrate, and gas test inductor wire is arranged in the side of medium substrate 7
Circle 4 and interdigital capacitor 5, the inside of gas test inductance coil 4 is arranged in the interdigital capacitor 5, and interdigital capacitor 5 and gas are surveyed
The inner ring for trying inductance coil 4 is connected, and GO/In is adhered on 5 surface of interdigital capacitor2O3Air-sensitive film 16, the medium substrate 7 it is another
Temperature test coil 6 is arranged in side, and the temperature test coil 6 forms a LC resonance with its own existing parasitic capacitance and returns
Road.
The preparation method of wireless and passive gas, temperature biparameter sensor of the invention, specifically includes the following steps:
(1) metallic vias is processed on ltcc substrate first, for the interconnection of gas test inductance coil and interdigital capacitor,
The technology of lamination is recycled to be integrally formed two layers of ltcc substrate lamination, as shown in Figure 2.
It (2), will be designed first with sol evenning machine in the even layer photoresist in front for preparing integral ltcc substrate
Gas test inductance coil and interdigital capacitor mask plate remove the photoresist on ltcc substrate to obtain desired using litho machine
Gold atom, is then splashed to substrate with magnetic control sputtering device by structure (i.e. the structure of gas test inductance coil and interdigital capacitor)
On, extra photoresist is washed with acetone finally, leaves gas test inductance coil and interdigital capacitor, as shown in Figure 3；
The sputtering of temperature test coil is got at the ltcc substrate back side using technique same as ltcc substrate front, as shown in figure 4, shape
At gas, the wireless sourceless sensor of temperature biparameter.
(3) preparation of graphene oxide takes the 100mL concentrated sulfuric acid and 10mL phosphoric acid to be added sequentially in three-necked bottle；It will mixing
Acid is placed in ice-water bath, is slow added into 0.8g crystalline flake graphite and 5g potassium permanganate, stirs 45min；Mixture is placed in 45 ~
It after stirring 35min in 55 DEG C of constant temperature water tanks, is placed in 60 DEG C of constant temperature water tanks and reacts 16h, mixture is in blackish green；It is slowly added dropwise
The hydrogen peroxide of 50mL5% is stirred well to mixture and golden yellow is presented；Product is moved in beaker, room temperature stands cooling, spends
Ion water washing is repeatedly until neutral；Product after washing is placed in 60 DEG C of drying in drying box, products therefrom is oxidation stone
Black alkene.
(4) InCl of 1.5g is weighed3•4H2O is dissolved in the distilled water of 20ml, and 2% polyethylene glycol is added, and mixing is stirred
Mix a period of time；The NH of 1mol/L is slowly added dropwise into solution at room temperature3•H2O is simultaneously slowly stirred until during the pH value of solution is
Property, jelly is obtained, sol solution placement is become into gel in static 2 hours at room temperature；It is repeatedly washed after filtering with deionized water
Wash, by washed gel be placed in drying box 100 DEG C at a temperature of dry 3 hours, then with 300 in high temperature furnace
DEG C temperature calcination 1 hour, obtained pale yellow powder, obtained pale yellow powder is ground to obtain diameter in agate mortar be
The nano indium oxide particle of 15-45nm.
(5) by the GO prepared and the nanometer In prepared2O3Particle is doped in 1.5% ratio, is ground using agate
Alms bowl grinding uniformly, is added suitable deionized water and is tuned into slurry；The slurry mixed up is coated to interdigital electricity by the way of being coated with
As shown in figure 5, interdigital capacitor is completely covered in appearance, it is ensured that thickness is uniform, places dry in the cool at room temperature, avoids sunlight
Direct projection prevents air-sensitive film cracking from falling off；After being completely dried, places a sensor at and is sintered 2 h in 260 DEG C of high temperature furnaces,
With the stability of reinforcement material and it is completely dried air-sensitive film；Finally by the sensor prepared 24 h of aging in air,
To improve its performance.
Compared with prior art, gas of the present invention, temperature biparameter sensor are using LC resonance principle (as schemed
1) gas sensitization layer GO/ In, is utilized2O3Physical absorption object gas, so that the capacitor, resistance between interdigital capacitor are with adsorbed gas
The difference of bulk concentration and change, the wireless and passive of gas is measured to realize, the dielectric constant of sensor base is to temperature
Degree is sensitive, and when extraneous temperature changes, the parasitic capacitance size of sensor also changes, and it is humorous to eventually lead to sensor
Vibration frequency changes with temperature, realizes the wireless and passive measurement to temperature.The present invention ties gasmetry and temperature measurement
Altogether, and two measurement methods are measured using the method for wireless and passive, improve the stability of measurement, are reduced
Power consumption, realizes the measurement to gas, temperature biparameter, and dimensionally have very big flexibility.
The configuration of the present invention is simple is reasonable, conducive to integration, the micromation for realizing gas, temperature biparameter sensor, is convenient for
Processing, it is low in cost.
Claims (1)
1. the preparation method of a kind of wireless and passive gas, temperature biparameter sensor, it is characterised in that specific step are as follows:
(1) metallic vias is processed on ltcc substrate first, for the interconnection of gas test inductance coil and interdigital capacitor, then benefit
Two layers of ltcc substrate lamination is integrally formed with the technology of lamination；
(2) gold atom on gold target material is splashed to the front and back of ltcc substrate using the technology of magnetron sputtering, in LTCC
The front of substrate sputters gas test inductance coil and interdigital capacitor, goes out temperature test line in the back spatter of ltcc substrate
Circle；Specially first with sol evenning machine in the even layer photoresist in front for preparing integral ltcc substrate, by gas test electricity
Sense coil removes the photoresist on ltcc substrate using litho machine with interdigital capacitor mask plate, then with magnetic control sputtering device gold
On atom sputtering to substrate, finally extra photoresist is washed with acetone, leave gas test inductance coil with it is interdigital
Capacitor；The sputtering of temperature test coil is got at the ltcc substrate back side using technique same as ltcc substrate front, is formd
The wireless sourceless sensor of gas, temperature biparameter；
(3) graphene oxide GO is prepared using Hummers method, the 100mL concentrated sulfuric acid and 10mL phosphoric acid is specially taken to sequentially add
Into three-necked bottle；Mixed acid is placed in ice-water bath, 0.8g crystalline flake graphite and 5g potassium permanganate are slow added into, is stirred
45min；Mixture is placed in 45 ~ 55 DEG C of constant temperature water tanks after stirring 35min, is placed in 60 DEG C of constant temperature water tanks and reacts 16h, mixed
Object is in blackish green；The hydrogen peroxide of 50mL5% is slowly added dropwise, is stirred well to mixture and golden yellow is presented；Product is moved into beaker
In, room temperature stands cooling, is washed with deionized repeatedly until neutral；Product after washing is placed in 60 DEG C of bakings in drying box
Dry, products therefrom is graphene oxide；
(4) pale yellow powder In is prepared using the method for collosol and gel2O3, by obtained pale yellow powder in agate mortar
Grind the nanometer In refined2O3Particle；Specially weigh the InCl of 1.5g3•4H2O is dissolved in the distilled water of 20ml,
2% polyethylene glycol is added, a period of time is mixed；The NH of 1mol/L is slowly added dropwise into solution at room temperature3•H2O simultaneously delays
Slow stirring is neutrality until the pH value of solution, obtains jelly, and sol solution placement is become solidifying in static 2 hours at room temperature
Glue；It is repeatedly washed after filtering with deionized water, washed gel is placed in drying box in 100 DEG C of at a temperature of drying 3
A hour, then with temperature calcination 1 hour of 300 DEG C in high temperature furnace, obtained pale yellow powder, the yellowish toner that will be obtained
It grinds to obtain the nano indium oxide particle that diameter is 15-45nm in agate mortar in end；
(5) by the GO prepared and the nanometer In prepared2O3Particle is doped, and is coated on interdigital capacitor, by interdigital capacitor
It is completely covered；Specially by the GO prepared and the nanometer In prepared2O3Particle is doped in 1.5% ratio, utilizes Ma
Nao mortar grinder is uniform, and suitable deionized water is added and is tuned into slurry；The slurry mixed up is coated to fork by the way of being coated with
Refer on capacitor, interdigital capacitor is completely covered, it is ensured that thickness is uniform, places dry in the cool at room temperature；Wait be completely dried with
Afterwards, it places a sensor at and is sintered 2 h in 260 DEG C of high temperature furnaces；Finally by the sensor prepared 24 h of aging in air.
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| CN107677707B (en) * | 2017-08-24 | 2020-02-18 | 中北大学 | LTCC-based substrate integrated waveguide type wireless passive gas sensor and preparation method thereof |
| CN108387610A (en) * | 2018-01-19 | 2018-08-10 | 上海交通大学 | marker detection device and detection method |
| CN108975920B (en) * | 2018-03-12 | 2021-05-18 | 中北大学 | HTCC-based high-temperature heat flow sensor and preparation method thereof |
| CN109238313B (en) * | 2018-09-18 | 2020-12-01 | 东南大学 | Multi-parameter LC sensor for monitoring state of rotating structure |
| CN110174181B (en) * | 2019-06-05 | 2020-09-18 | 中北大学 | Temperature/thermal flow state testing method for rotating part |
| CN110426064B (en) * | 2019-07-18 | 2021-07-20 | 东南大学 | Wireless passive sensor and wireless passive sensing method |
| CN110542455B (en) * | 2019-09-16 | 2021-11-05 | 中北大学 | HTCC composite microsensor for pressure/vibration synchronous measurement and preparation method thereof |
| CN111238544B (en) * | 2020-03-12 | 2022-10-21 | 江苏林洋能源股份有限公司 | Microwave sensor based on LC type resonator and applied to temperature/humidity environment detection |
| CN112378424B (en) * | 2020-11-13 | 2022-06-14 | 中北大学 | Wireless passive strain and temperature dual-parameter sensor and preparation method thereof |
| CN113092545B (en) * | 2021-04-13 | 2022-12-09 | 哈尔滨理工大学 | Based on CuO/In 2 O 3 Preparation method of modified graphene MEMS gas sensor |
| CN113418969B (en) * | 2021-06-07 | 2023-04-25 | 武汉大学 | High-sensitivity millimeter wave dielectric resonance sensor for biomedical detection |
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