CN107677707A - A kind of substrate integration wave-guide formula wireless and passive gas sensor based on LTCC and preparation method thereof - Google Patents
A kind of substrate integration wave-guide formula wireless and passive gas sensor based on LTCC and preparation method thereof Download PDFInfo
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- CN107677707A CN107677707A CN201710735159.1A CN201710735159A CN107677707A CN 107677707 A CN107677707 A CN 107677707A CN 201710735159 A CN201710735159 A CN 201710735159A CN 107677707 A CN107677707 A CN 107677707A
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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
Abstract
The invention belongs to gas sensing techniques field, specifically a kind of substrate integration wave-guide formula wireless and passive gas sensor based on LTCC and preparation method thereof.Solves existing gas sensor wired connection, installation is inconvenient, the problems such as service life is short, including upper surface metal level, lower surface metal layer and the LTCC alumina ceramic plates for being arranged on centre, upper surface metal level, lower surface metal layer and LTCC alumina ceramic plates composition substrate, substrate the week side of boss is provided with the side-wall metallic cylindrical hole of a circle substrate integration wave-guide, structure based on substrate integration wave-guide is formed with this, silver paste is filled with the side-wall metallic cylindrical hole of substrate integration wave-guide, gas sensitive structure is provided with the middle part of substrate, upper surface layer on surface of metal is provided with slot antenna.The present invention, which takes full advantage of substrate integration wave-guide resonator, has the advantages that high quality factor, low-loss, can effectively increase the distance of wireless test.
Description
Technical field
The invention belongs to gas sensing techniques field, specifically a kind of substrate integration wave-guide formula wireless and passive based on LTCC
Gas sensor and preparation method thereof.
Background technology
Under the driving that science and technology and petro chemical industry develop very fast, inflammable, explosive and toxic gas has obtained extensively
General application.These gases will cause personnel to be poisoned among the process transported, store and used, once leakage occurs, and make
Into atmosphere pollution, fire or even blast, life and assets security to people have very big threat.Such as：In some ore deposit holes
In the recovery process of mine, substantial amounts of H can be produced2S, gas inflammable and explosive CO etc., the personal safety to operating personnel are formed
Threaten.When being transported in some chemical plant with storing inflammable volatile poisonous and harmful industrial chemicals, some often occur and lets out
If leakage accident can not timely find that very big danger can be caused, directly influence the health of people or cause the dirt of environment
Dye.In addition, the haze in many cities in China is all very serious at present, causes very big injury to the respiratory tract of human body, such as
Fruit suction for a long time results even in death, thus air pollution problems inherent has become the people and pays high attention to and be badly in need of asking for solution
Topic.Therefore, the detection to these pernicious gases just seems very significant, and studying corresponding air-sensitive detection sensor also becomes
It is more and more significant.
Existing gas sensor, generally by the way of wired connection, these gas sensors have higher detection
Sensitivity, shorter detection response time.But the installation of the mode degree sensor of wired connection causes very big not side
Just, the larger service life for having had a strong impact on sensor of power consumption.And the appearance of wireless and passive gas sensor, it can be very good to solve
Certainly these power consumptions and installation the problem of, so, wireless and passive formula gas sensor design with prepare there is great research
Meaning.In addition, there is high quality factor, low-loss advantage based on substrate integrated morphology, more wireless at a distance survey can be achieved
Examination.
The content of the invention
The present invention is in order to solve existing gas sensor wired connection, the problems such as installation is inconvenient, and service life is short, there is provided
A kind of substrate integration wave-guide formula wireless and passive gas sensor based on LTCC and preparation method thereof.
The present invention takes following technical scheme：A kind of substrate integration wave-guide formula wireless and passive gas sensing based on LTCC
Device, including upper surface metal level, lower surface metal layer and the LTCC alumina ceramic plates for being arranged on centre, upper surface metal
Layer, lower surface metal layer and LTCC alumina ceramic plates composition substrate, substrate the week side of boss are provided with the side wall of a circle substrate integration wave-guide
Metal cylinder through hole, the structure based on substrate integration wave-guide is formed with this, in the side-wall metallic cylindrical hole of substrate integration wave-guide
Filled with silver paste, gas sensitive structure is provided with the middle part of substrate, upper surface layer on surface of metal is provided with slot antenna.
Further, gas sensitive structure is included in the cylindrical hole set on LTCC alumina ceramic plates, table in cylindrical hole
Face scribbles one layer of silver paste, and graphite oxide ene coatings are scribbled on the outside of silver paste.
Further, LTCC alumina ceramic plates are provided with 6 layers.
A kind of preparation method of the substrate integration wave-guide formula wireless and passive gas sensor based on LTCC, specific steps are such as
Under：
1）First, 6 LTCC green bands are got out, the numbering of first layer to layer 6 is 9-14, takes tri- layers of LTCC greens of 9-11
Band carries out the lamination of 20 minutes under 70 DEG C, 21MPa parameter, afterwards by the green band for the 9-11 layers being laminated in medium position
Cut away 25 cylinders.
2）The 9-11 layer green bands for having cut cylinder and 12-14 layer green bands are continued to be laminated, laminating parameters 70
DEG C, the lamination of 20 minutes is carried out under 21MPa parameter.
3）A series of small column through hole is cut away in the position that the week side of boss one for the 9-14 layer green bands being laminated is enclosed, to cutting
The small column removed carries out the filling of silver paste, and the inwall of 25 small columns to being cut off in the first step carries out the brushing of silver paste.
4) the green band that silver paste is printed in the 3rd step is placed in the sintering of 850 DEG C of progress in high temperature furnace, obtains 9-14
The ripe porcelain of layer.
5）Using the technique of silk-screen printing, the printing of silver paste is carried out in the upper surface of the ripe porcelain of 9-14 layers, in high temperature furnace
850 DEG C of sintering is carried out, obtains the upper metal covering and slot antenna configurations of substrate integration wave-guide；In the following table of the ripe porcelain of 9-14 layers
Face carries out the printing of silver paste, and sintering obtains the lower metal covering of substrate integration wave-guide.
6）The preparation of graphene oxide, the 100mL concentrated sulfuric acids and 10mL phosphoric acid is taken to be added sequentially in three-necked bottle；By mixed acid
It is placed in ice-water bath, adds 0.8g crystalline flake graphites and 5g potassium permanganate, stirs 45min；Mixture is placed in 45 ~ 55 DEG C of perseverances
After stirring 35min in reservoir, it is placed in 60 DEG C of constant temperature water tanks and reacts 16h, mixture is in blackish green；50mL5% dioxygen is added dropwise
Water, it is stirred well to mixture and golden yellow is presented；Product is moved in beaker, normal temperature stands cooling, is washed with deionized more
It is secondary until neutral；Product after washing is placed in 60 DEG C of drying in drying box, products therefrom is graphene oxide.
7）The graphene oxide prepared in 6th step is doped with 5% mass ratio with zinc oxide, ground using agate
Alms bowl grinding is uniform, adds deionized water, slurry is modulated into, as gas sensitive.
8）The gas sensitive prepared in the 7th step is taken, is equably spun on the side of 25 cylindrical holes cut off out in the first step
Wall and lower surface, prepare final wireless and passive gas sensor.
In the test process of reality, the side wall of the cylindrical hole of centre 25 of sensor and the gas sensitive of lower surface are to second
Alcohol gas is adsorbed, and changes the effective dielectric constant of cylindrical hole portion, theoretical according to the Medium perturbation of substrate integration wave-guide, is passed
The resonant frequency of sensor is changed, and the resonant frequency for causing sensor is produced in various degree inclined by the gas of various concentrations
Move, the detection to gas concentration is realized with this.
Compared with prior art, the invention has the advantages that：
1）In the present invention, it is proposed that slot antenna is integrated in above substrate integrated wave guide structure, realizes the electromagnetism of wireless and passive
Ripple couples, and under conditions of substrate integration wave-guide magnetic distribution is not changed, is prepared at the center of structure and can be used for carrying
The cylindrical hole of gas sensitive.
2）It is doped the gas sensitive prepared in the present invention with zinc oxide using the graphene oxide prepared, effectively
The adsorption area to gas is increased, compared with the gas sensor that zinc oxide is prepared as sensitive material, there is higher survey
Try sensitivity.
3）The present invention further increases to the spin coating on 25 cylinder side wall metal coverings with the gas sensitive on bottom surface
Gas absorption area, the effective guarantee measurement sensitivity of gas sensor.In addition, it is humorous based on above-mentioned substrate integration wave-guide
Shake the gas sensor of device, in that context it may be convenient to which change is spun on the conductivity type gas sensitive of cylinder side wall metal covering, prepares pair
The sensitive gas sensor of gas with various.
4）The volume size of sensor of the present invention is smaller, base material thickness it is relatively low, more conducively sensor is multiple
Installation under heterocycle border, at the same it is also easily portable.In addition, gas sensor described in patent, takes full advantage of substrate and integrates ripple
Leading resonator has the advantages that high quality factor, low-loss, can effectively increase the distance of wireless test.
Brief description of the drawings
Fig. 1 is the top view of sensor of the invention structure；
Fig. 2 is sensor of the invention structure upward view；
Fig. 3 is the internal anatomy of A-A in Fig. 1；
Fig. 4 is in Fig. 12 top view；
Fig. 5 is the internal anatomy of 2 B-B in Fig. 1；
Fig. 6 is sensor process schematic diagram；
Fig. 7 is the microwave scattering test philosophy figure of the present invention；
In figure：1-slot antenna, 2-gas sensitive structure, the side-wall metallic cylindrical hole of 3-substrate integration wave-guide, 4-on
Surface metal-layer, 5-lower surface metal layer, the metal inner surface for the cylinder that 6-gas sensitive structure is depended on, 7-oxidation stone
Black ene coatings, 9~14-first layers of LTCC ceramics is represented respectively to layer 6,15-wireless and passive gas sensor, 16-
Interrogation antenna, 17-frequency sweep transmission signal, 18-echo reflection signal, 19-gas test platform and wireless and passive gas sensing
Device.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
As shown in Figure 1, 2, 3, a kind of substrate integration wave-guide formula wireless and passive gas sensor based on LTCC, including upper table
Face metal level 4, lower surface metal layer 5 and the LTCC alumina ceramic plates for being arranged on centre, upper surface metal level 4, lower surface
Metal level 5 and LTCC alumina ceramic plates composition substrate, substrate the week side of boss are provided with the side-wall metallic cylinder of a circle substrate integration wave-guide
Through hole 3, the side-wall metallic cylindrical hole 3 of substrate integration wave-guide is interior to be filled with silver paste, and gas sensitive structure is provided with the middle part of substrate
2, the surface of upper surface metal level 4 is provided with slot antenna 1.
As shown in Figure 4,5, described gas sensitive structure 2 is included in the cylindrical hole 6 set on LTCC alumina ceramic plates,
The inner surface of cylindrical hole 6 scribbles one layer of silver paste, and graphite oxide ene coatings 7 are scribbled on the outside of silver paste.
Described LTCC alumina ceramic plates are provided with 6 layers.
As shown in fig. 6, a kind of preparation method of the substrate integration wave-guide formula wireless and passive gas sensor based on LTCC, tool
Body step is as follows：
1）First, 6 LTCC green bands are got out, the numbering of first layer to layer 6 is 9-14, takes tri- layers of LTCC greens of 9-11
Band carries out the lamination of 20 minutes under 70 DEG C, 21MPa parameter, afterwards by the green band for the 9-11 layers being laminated in medium position
Cut away 25 cylinders.
2）The 9-11 layer green bands for having cut cylinder and 12-14 layer green bands are continued to be laminated, laminating parameters 70
DEG C, the lamination of 20 minutes is carried out under 21MPa parameter.
3）A series of small column through hole is cut away in the position that the week side of boss one for the 9-14 layer green bands being laminated is enclosed, to cutting
The small column removed carries out the filling of silver paste, and the inwall of 25 small columns to being cut off in the first step carries out the brushing of silver paste.
4) the green band that silver paste is printed in the 3rd step is placed in the sintering of 850 DEG C of progress in high temperature furnace, obtains 9-14
The ripe porcelain of layer.
5）Using the technique of silk-screen printing, the printing of silver paste is carried out in the upper surface of the ripe porcelain of 9-14 layers, in high temperature furnace
850 DEG C of sintering is carried out, obtains the upper metal covering and slot antenna configurations of substrate integration wave-guide；In the following table of the ripe porcelain of 9-14 layers
Face carries out the printing of silver paste, and sintering obtains the lower metal covering of substrate integration wave-guide.
6）The preparation of graphene oxide, the 100mL concentrated sulfuric acids and 10mL phosphoric acid is taken to be added sequentially in three-necked bottle；By mixed acid
It is placed in ice-water bath, adds 0.8g crystalline flake graphites and 5g potassium permanganate, stirs 45min；Mixture is placed in 45 ~ 55 DEG C of perseverances
After stirring 35min in reservoir, it is placed in 60 DEG C of constant temperature water tanks and reacts 16h, mixture is in blackish green；50mL5% dioxygen is added dropwise
Water, it is stirred well to mixture and golden yellow is presented；Product is moved in beaker, normal temperature stands cooling, is washed with deionized more
It is secondary until neutral；Product after washing is placed in 60 DEG C of drying in drying box, products therefrom is graphene oxide.
7）The graphene oxide prepared in 6th step is doped with 5% mass ratio with zinc oxide, ground using agate
Alms bowl grinding is uniform, adds appropriate deionized water, is modulated into slurry, as gas sensitive.
8）The gas sensitive prepared in the 7th step is taken, is equably spun on the side of 25 cylindrical holes cut off out in the first step
Wall and lower surface, prepare final wireless and passive gas sensor.
As shown in fig. 7, the substrate Integral wireless passive source gas working sensor mode based on microwave scattering, interrogation antenna
16（The ultra-wideband antenna of coplanar wave guide feedback, radiating guide etc. of opening a way）Send comprising the frequency sweep including sensor resonant frequency
Signal 17, received by the slot antenna 1 of substrate integration wave-guide upper surface metal level 4, slot antenna couples a signal to substrate
In integrated waveguide, with wave guide resonance frequency similar in restricting the number substrate integration wave-guide formed standing wave, and the frequency of other parts believe
Numbers 18 are reflected back, be asked antenna reception, and substrate integration wave-guide is arrived by the echo reflection signal for analyzing interrogation antenna
Resonant frequency.In the work process of gas sensor, the gas sensitive structure 2 of spin coating graphene oxide is absorbing gas
Afterwards, the resistivity of inner structural wall changes, according to the perturbation principle of substrate integration wave-guide, the resonance frequency of substrate integration wave-guide
Rate frees change, therefore using analysis of the Network Analyzer to the resonant frequency of the substrate integration wave-guide received of interrogation antenna,
It can be detected the change in concentration situation of gas.
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art,
It can still modify to the technical scheme described in foregoing embodiments, or which part technical characteristic is carried out etc.
With replacing, within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., this should be included in
Within the protection domain of invention.
Claims (4)
- A kind of 1. substrate integration wave-guide formula wireless and passive gas sensor based on LTCC, it is characterised in that：Including upper surface gold Belong to layer（4）, lower surface metal layer（5）And it is arranged on the LTCC alumina ceramic plates of centre, upper surface metal level（4）, following table Face metal level（5）Substrate is formed with LTCC alumina ceramic plates, substrate the week side of boss is provided with the side-wall metallic of a circle substrate integration wave-guide Cylindrical hole（3）, the side-wall metallic cylindrical hole of substrate integration wave-guide（3）It is interior to be filled with silver paste, it is provided with gas in the middle part of substrate Sensitive structure（2）, upper surface metal level（4）Surface is provided with slot antenna（1）.
- 2. the substrate integration wave-guide formula wireless and passive gas sensor according to claim 1 based on LTCC, its feature exist In：Described gas sensitive structure（2）It is included in the cylindrical hole set on LTCC alumina ceramic plates（6）, cylindrical hole（6）Interior table Face scribbles one layer of silver paste, and the gas sensitive coating that graphene oxide mixes with zinc oxide is scribbled on the outside of silver paste（7）.
- 3. the substrate integration wave-guide formula wireless and passive gas sensor according to claim 2 based on LTCC, its feature exist In：Described LTCC alumina ceramic plates are provided with 6 layers.
- A kind of 4. preparation side of the substrate integration wave-guide formula wireless and passive gas sensor based on LTCC as claimed in claim 3 Method, it is characterised in that：Comprise the following steps that：1）First, 6 LTCC green bands are got out, the numbering of first layer to layer 6 is 9-14, takes tri- layers of LTCC greens of 9-11 Band carries out the lamination of 20 minutes under 70 DEG C, 21MPa parameter, afterwards by the green band for the 9-11 layers being laminated in medium position Cut away 25 cylinders；2）The 9-11 layer green bands for having cut cylinder and 12-14 layer green bands are continued to be laminated, laminating parameters be 70 DEG C, The lamination of 20 minutes is carried out under 21MPa parameter；3）A series of small column through hole is cut away in the position that the week side of boss one for the 9-14 layer green bands being laminated is enclosed, to excision Small column carries out the filling of silver paste, and the inwall of 25 small columns to being cut off in the first step carries out the brushing of silver paste；4) the green band that silver paste is printed in the 3rd step is placed in the sintering of 850 DEG C of progress in high temperature furnace, obtains 9-14 layers Ripe porcelain；5）Using the technique of silk-screen printing, the printing of silver paste is carried out in the upper surface of the ripe porcelain of 9-14 layers, is carried out in high temperature furnace 850 DEG C of sintering, obtain the upper metal covering and slot antenna configurations of substrate integration wave-guide；Enter in the lower surface of the ripe porcelain of 9-14 layers The printing of row silver paste, sintering obtain the lower metal covering of substrate integration wave-guide；6）The preparation of graphene oxide, the 100mL concentrated sulfuric acids and 10mL phosphoric acid is taken to be added sequentially in three-necked bottle；Mixed acid is placed in In ice-water bath, 0.8g crystalline flake graphites and 5g potassium permanganate are added, stirs 45min；Mixture is placed in 45 ~ 55 DEG C of thermostatted waters After stirring 35min in case, it is placed in 60 DEG C of constant temperature water tanks and reacts 16h, mixture is in blackish green；50mL5% hydrogen peroxide is added dropwise, It is stirred well to mixture and golden yellow is presented；Product is moved in beaker, normal temperature stands cooling, is washed with deionized repeatedly straight To neutrality；Product after washing is placed in 60 DEG C of drying in drying box, products therefrom is graphene oxide；7）The graphene oxide prepared in 6th step is doped with 5% mass ratio with zinc oxide, ground using agate mortar Mill is uniform, adds deionized water, slurry is modulated into, as gas sensitive；8）Take the gas sensitive prepared in the 7th step, be equably spun on 25 cylindrical holes cut off out in the first step side wall and Lower surface, prepare final wireless and passive gas sensor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387971A (en) * | 2018-03-13 | 2018-08-10 | 清华大学 | Tunable directional couple device based on graphene and nanotube antenna array |
| CN111272831A (en) * | 2020-02-24 | 2020-06-12 | 大连理工大学 | Based on MXene/SnO2Heterojunction passive wireless ammonia gas sensor and preparation method thereof |
| CN113884542A (en) * | 2021-09-06 | 2022-01-04 | 中国科学院上海硅酸盐研究所 | Wireless micro-fluidic sensor based on multilayer ceramic technology |
| RU2770861C1 (en) * | 2021-07-22 | 2022-04-22 | федеральное государственное автономное образовательное учреждение высшего образования «Московский физико-технический институт (национальный исследовательский университет)» | Thermocatalytic sensor based on ceramic mems platform and method for its manufacture |
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| CN103675040A (en) * | 2013-11-20 | 2014-03-26 | 中北大学 | Non-contact passive gas sensor based on low-temperature co-fired ceramic technology |
| CN107085015A (en) * | 2017-04-11 | 2017-08-22 | 中北大学 | Wireless and passive gas, temperature biparameter sensor and preparation method thereof |
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2017
- 2017-08-24 CN CN201710735159.1A patent/CN107677707B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675040A (en) * | 2013-11-20 | 2014-03-26 | 中北大学 | Non-contact passive gas sensor based on low-temperature co-fired ceramic technology |
| CN107085015A (en) * | 2017-04-11 | 2017-08-22 | 中北大学 | Wireless and passive gas, temperature biparameter sensor and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387971A (en) * | 2018-03-13 | 2018-08-10 | 清华大学 | Tunable directional couple device based on graphene and nanotube antenna array |
| CN111272831A (en) * | 2020-02-24 | 2020-06-12 | 大连理工大学 | Based on MXene/SnO2Heterojunction passive wireless ammonia gas sensor and preparation method thereof |
| CN111272831B (en) * | 2020-02-24 | 2021-10-15 | 大连理工大学 | Based on MXene/SnO2Heterojunction passive wireless ammonia gas sensor and preparation method thereof |
| RU2770861C1 (en) * | 2021-07-22 | 2022-04-22 | федеральное государственное автономное образовательное учреждение высшего образования «Московский физико-технический институт (национальный исследовательский университет)» | Thermocatalytic sensor based on ceramic mems platform and method for its manufacture |
| CN113884542A (en) * | 2021-09-06 | 2022-01-04 | 中国科学院上海硅酸盐研究所 | Wireless micro-fluidic sensor based on multilayer ceramic technology |
| CN113884542B (en) * | 2021-09-06 | 2024-02-06 | 中国科学院上海硅酸盐研究所 | Wireless micro-fluidic sensor based on multilayer ceramic technology |
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