CN103487155B - A kind of SiCN pottery wireless and passive temperature sensor and preparation method thereof - Google Patents
A kind of SiCN pottery wireless and passive temperature sensor and preparation method thereof Download PDFInfo
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Abstract
A kind of SiCN pottery wireless and passive temperature sensor and preparation method thereof, relates to temperature sensor.Described temperature sensor is provided with cylindrical SiCN amorphous ceramic temperature sensing element, is provided with refractory metal layer on the surface of cylindrical SiCN amorphous ceramic temperature sensing element and forms resonator cavity, being provided with slot antenna on resonator cavity surface.1) the cylindrical SiCN amorphous ceramic temperature sensing element of preparation；(1) SiCN pottery element embryo is first prepared；(2) under inert gas shielding, SiCN pottery element embryo is pyrolyzed, after re-annealing processes, obtains temperature sensing element SiCN amorphous ceramic body；2) the slot antenna region Kapton Tape at temperature sensing element SiCN amorphous ceramic body upper surface is protected; at temperature sensing element SiCN amorphous ceramic surface metal cladding; after again Kapton Tape being removed; stayed region is the slot antenna of transceiving electromagnetic ripple signal, obtains cylindrical SiCN pottery wireless and passive temperature sensor.
Description
Technical field
The present invention relates to temperature sensor, especially relate to a kind of SiCN pottery wireless and passive temperature sensor and preparation method thereof.
Background technology
Internal work environment very severe during turbine engine combustion, extreme temperatures (> 1000 DEG C), existing temperature sensor system many employings optical fiber (J.H.Wo, Q.Z.Sun, H.Liu, et.al, OpticalFiberTechnology19 (2013) 289-292) or the working method (M.A.Fonseca of low-frequency active, J.M.English, andM.G.Allen, J.Microelectromech.Syst.11 (2002) 337-343), cannot normally work under such rugged environment at all, thus turbogenerator internal temperature field data famine, seriously limit the development of aero-engine equipment technology.Meanwhile, wired active system of existing temperature sensor, it is impossible to be arranged on movable member (such as engine blade) and be operated.Therefore, be badly in need of to develop the superhigh temperature resistant (> 800 DEG C that can be applicable to harsh environments) radio temperature sensor, this sensor especially can be operated on engine blade.The predicament of hyperthermic temperature sensor research and development is preparation and the exploitation of corresponding wireless signal collection mode of high temperature resistant sensing element.
Polymer precursor pyrolysismethod preparation pottery is to utilize the features such as mobility, mouldability, machinability and structure designability that polymer precursor is good, polymer precursor carries out high temperature pyrolysis and prepares a kind of novel forming method of advanced ceramics material.Ceramic material prepared by polymer precursor pyrolysismethod is high temperature resistant, antioxidation, corrosion-resistant, manufacturing process is easy, with low cost simultaneously, and sintering temperature can be reduced to 1000 DEG C, is the focus material studied in the world.SiCN ceramic high-temperature resistant prepared by polymer precursor polysilazane, anticorrosive, radiation hardness, it it is a kind of novel semi-conducting material, the more important thing is that this SiCN pottery Jie's temperature characteristics under microwave frequency band presents good linear relationship, therefore this material can be used for developing novel super-high temperature wireless and passive temperature sensor.
Summary of the invention
Present invention aims to the temperature sensing element operating temperature existing for existing temperature sensor relatively low, wired measuring is difficult to bear the technical problems such as high-temperature corrosion environment, it is provided that a kind of SiCN pottery wireless and passive temperature sensor that can use under the adverse circumstances such as hot and humid soda acid and preparation method thereof.
SiCN pottery wireless and passive temperature sensor of the present invention is provided with cylindrical SiCN amorphous ceramic temperature sensing element, is provided with refractory metal layer on the surface of cylindrical SiCN amorphous ceramic temperature sensing element and forms resonator cavity, being provided with slot antenna on resonator cavity surface.
The diameter of described cylindrical SiCN amorphous ceramic temperature sensing element can be 9～15mm, and thickness can be 1～5mm.Cylindrical SiCN amorphous ceramic temperature sensing element can be prepared by polymer precursor conversion method, and described cylindrical SiCN amorphous ceramic is resistant to 1400 DEG C of temperature the most higher.
Described refractory metal layer refers to the fusing point metal level more than 1000 DEG C；The thickness of described refractory metal layer can be 8～25 μm.
When launch signal end give a frequency 5～15GHz wideband microwave signal, this signal is received by slot antenna, and in resonator cavity internal resonance frequency-selecting, after frequency-selecting, the signal of (resonant frequency 10.6GHz) sends receiver module circuit to further through slot antenna, complete radio temperature sensor information gathering, this sensor carries out the transmission of signal by microwave electromagnetic field, overcome wiring problem, having the little light weight of volume need not the feature of any electric power system, high-temp in-situ can be realized measure, the measurement on movable member can be realized again, significantly widen the range of temperature sensor.
The preparation method of described SiCN pottery wireless and passive temperature sensor, comprises the following steps:
1) the cylindrical SiCN amorphous ceramic temperature sensing element of preparation；
(1) first preparing SiCN pottery element embryo, concrete grammar is as follows:
Method 1: after being mixed with thermal initiator cumyl peroxide (DCP) by precursor polysilazane, carry out heat cross-linking so that it is become the polysilazane of solid-state from the polysilazane of liquid, pulverize last, is pressed into SiCN pottery element embryo；
Method 2: after being mixed with light trigger by polysilazane, puts into and carries out UV-crosslinked in mould, obtain faint yellow SiCN pottery element embryo；
Method 3: after polysilazane is mixed with light trigger, carry out UV-crosslinked after, pulverize last, be pressed into SiCN pottery element embryo；
(2) under inert gas shielding, SiCN pottery element embryo is pyrolyzed, after re-annealing processes, obtains temperature sensing element SiCN amorphous ceramic body；
2) the slot antenna region Kapton Tape at temperature sensing element SiCN amorphous ceramic body upper surface is protected; at temperature sensing element SiCN amorphous ceramic surface metal cladding; after again Kapton Tape being removed; stayed region is the slot antenna of transceiving electromagnetic ripple signal, so far prepares cylindrical SiCN pottery wireless and passive temperature sensor.
In the method 1 of step 1) (1st) part, described polysilazane can be 1 with the mass ratio of thermal initiator: (0～0.1)；The temperature of described heat cross-linking can be 120～400 DEG C, and the time of heat cross-linking can be 1～4h；The particle diameter of described powder can be 0.5～2 μm.
In the method 2 of step 1) (1st) part, described light trigger can use I819 light trigger etc.；Described polysilazane can be 1 with the mass ratio of light trigger: (0.005～0.05)；Described mould can use PDMS mould, and the diameter of mould can be 4～25mm, and the height of mould can be 1～5mm；Described UV-crosslinked condition can be: under uviol lamp, irradiation carries out UV-crosslinked, and the power of described uviol lamp can be 250W, and centre wavelength can be 326nm, and the UV-crosslinked time can be 0.25～2h.
In the method 3 of step 1) (1st) part: described light trigger can use I819 light trigger etc.；Described polysilazane can be 1 with the mass ratio of light trigger: (0.005～0.05)；Described UV-crosslinked condition can be: under uviol lamp, irradiation carries out UV-crosslinked, and the power of described uviol lamp can be 250W, and centre wavelength can be 326nm, and the UV-crosslinked time can be 0.25～2h；The particle diameter of described powder can be 0.5～2 μm.
In step 1) (2nd) part, described noble gas can use nitrogen or argon etc.；The temperature of described pyrolysis can be 800～1000 DEG C, and the time of pyrolysis can be 1～4h, and the temperature of described annealing can be 1000～1400 DEG C, and the time of annealing can be 1～4h；Obtained temperature sensing element SiCN amorphous ceramic body is the temperature sensing element SiCN amorphous ceramic body of a kind of densification, and its density is 2.6～3.0g/cm3。
In step 2) in, described at temperature sensing element SiCN amorphous ceramic surface metal cladding, can be by the method for plating or evaporation at SiCN ceramic surface metal cladding；Described metal can use platinum or titanium etc.；The thickness of described metal level can be 8～25 μm.The size and location of described slot antenna determines according to operating frequency, the size of SiCN pottery and selected surface metal, but finally requires that the load impedance that slot antenna causes reaches to mate with the intrinsic impedance of the resonator cavity of cylindrical SiCN pottery formation.
SiCN pottery, refractory metal material and slot antenna that the SiCN pottery wireless and passive temperature sensor of the present invention is prepared by polymer precursor conversion method are constituted, using amorphous Si CN pottery as temperature sensing material, material surface parcel refractory metal also forms resonator cavity with temperature sensing material, opening suitable slot antenna on this resonator cavity surface, the resonator cavity of band slot antenna defines the wireless sourceless sensor being resistant to 800 DEG C to 1400 DEG C.SiCN pottery prepared by polymer precursor conversion method linearly changes in microwave frequency band dielectric constant with temperature, and in the case of resonant cavity size is fixing, resonant frequency is determined by SiCN ceramic dielectric constant, and then realizes the corresponding relation of resonant frequency and temperature.When transmitting signal end gives a wideband microwave signal, and this signal is received by slot antenna, and in resonator cavity internal resonance frequency-selecting, the signal after frequency-selecting sends receiver module circuit to further through slot antenna, and this Antenna Design can effectively reduce the volume of sensor.The SiCN pottery wireless and passive temperature sensor of the present invention, the method using microwave receiving on the basis of using high temperature resistant temperature sensing material, having the little light weight of volume need not the feature of any electric power system, high-temp in-situ can be realized measure, the measurement on movable member can be realized again, significantly widened the range of temperature sensor.
Accompanying drawing explanation
Fig. 1 is the structure composition schematic diagram of SiCN pottery wireless and passive temperature sensor embodiment of the present invention.
Fig. 2 is the top view of Fig. 1.
Fig. 3 is the A-A profile of Fig. 2.
In the drawings, respectively it is labeled as: 1, cylindrical SiCN amorphous ceramic temperature sensing element；2, metal level；3, slot antenna.
Detailed description of the invention
Following example will the present invention is further illustrated in conjunction with accompanying drawing.
Embodiment 1
The preparation method seeing Fig. 1～3, SiCN pottery wireless and passive temperature sensor is as follows:
1,5g polysilazane and 0.3g thermal initiator cumyl peroxide mixed liquor mix 2h, the thick white shape liquid being uniformly mixed on 60 DEG C of magnetic stirrers.
2, the thick white shape liquid of mix homogeneously is poured in tinfoil paper carton, put into 70 DEG C of baking oven inside holding 2h, then temperature is risen to 140 DEG C of insulation 4h mixed liquor is carried out heat cross-linking, obtain solid-state polysilazane.
3, the solid-state polysilazane ball mill grinding obtained is become powder, particle diameter 1 μm.Ball mill uses QP-3SP2 vibrator, and frequency is 300Hz, and Ball-milling Time is 1h.
4, powder good for ball milling and stock solution being mixed with 6: 1 ratios, mixed particle requirement is less than 5 μm.Fine powder is poured in Φ 13 disk mould, be slowly forced into 18MPa, pressurize 3min, obtain pottery element embryo sheet.
5, the pottery element embryo sheet pressed is put in aluminium oxide porcelain boat; it is sintered under high temperature process furnances high pure nitrogen is protected; being incubated 4h after being warming up to 1000 DEG C with 0.5 DEG C/min of heating rate, prepared flawless densification thickness is 5mm, the SiCN ceramic disks of a diameter of 11.32mm.
6, the surface Kapton Tape in cylindrical SiCN ceramic disks blocks to stay a slot antenna, the position of slot antenna is to be at 2.66mm at the upper surface of resonator cavity away from axial location, the cuboid of a width of 1mm of the longest 8.5mm, thickness is identical with metal layer thickness.
7, make ceramic surface metallization by plating or evaporation, at the metal platinum layer of SiCN one layer of 15 μ m-thick of ceramic disks plated surface, form resonator cavity.
8, remove Kapton Tape, form SiCN pottery wireless and passive temperature sensor.
The structure of gained SiCN pottery wireless and passive temperature sensor sees Fig. 1, described SiCN pottery wireless and passive temperature sensor is provided with cylindrical SiCN amorphous ceramic temperature sensing element 1, it is provided with refractory metal layer 2 on the surface of cylindrical SiCN amorphous ceramic temperature sensing element 1 and forms resonator cavity, being provided with slot antenna 3 on resonator cavity surface.
In figs 2 and 3, the diameter 2r=11.66mm of SiCN ceramic disks, highly h=1.1mm, the operating frequency of SiCN pottery wireless and passive temperature sensor is 10.6GHz, and metal is platinum, the thickness t=15 μm of metal platinum layer, therefore the position of slot antenna is x=3mm, l=8.5mm, w=1mm.
Embodiment 2
1, taking the polysilazane precursor of 5g and light trigger (I819) mixing of 0.3g, mixed liquor is placed on magnetic stirrer and carries out heating magnetic agitation, and heating-up temperature is 60 DEG C, and mixing time is 1～2h, obtains faint yellow mixed liquor after mix homogeneously.
2,5g polydimethylsiloxane (PDMS) is taken, 0.5g cross-linking agent, magnetic agitation makes its mix homogeneously, evacuation or supersound process 10～30min remove bubble removing, a diameter of Φ 13 disk is put in PDMS solution, it is heating and curing, takes out master mold afterwards, obtain the PDMS mould of die cavity with master mold shape.
3, mixed liquor is poured in PDMS mould, and be placed under 250W uviol lamp and carry out UV-crosslinked 1h, polysilazane element embryo wafer thickness 2～5mm.
4, the polysilazane element embryo disk being cured is separated with PDMS mould, it is placed in aluminium oxide porcelain boat, put in tube-type atmosphere furnace and be sintered, being incubated 4h after making temperature be to slowly warm up to 1000 DEG C, polysilazane element embryo disk to reduce sintering heating rate to ensure gas release completely during sintering.Choose at this is the heating rate of 0.5 DEG C/min.Sintering process is passed through high pure nitrogen as protective gas.Finally prepare the fine and close thickness of free from flaw in 3mm, the SiCN ceramic disks of a diameter of 10mm.
5, the surface Kapton Tape in cylindrical SiCN ceramic disks blocks to stay a slot antenna, and the position of slot antenna is to be at 2.66mm at the upper surface of resonator cavity away from axial location, the cuboid of a width of 1mm of the longest 8.5mm, thickness 20 μm.
6, by electroplating or evaporating the titanium layer in SiCN ceramic disks plated surface last layer 20 μm, complete surface metalation, form resonator cavity.
7, remove Kapton Tape, obtain SiCN pottery wireless and passive temperature sensor.
Embodiment 3
1, taking the polysilazane precursor of 5g and the light trigger mixing of 0.3g, mixed liquor is placed on magnetic stirrer and carries out heating magnetic agitation, and heating-up temperature is 60 DEG C, and mixing time is 2h, obtains faint yellow mixed liquor after mix homogeneously.
2, mixed liquor is poured in tinfoil paper carton, put into 70 DEG C of baking oven inside holding 1～2h, to remove the bubble in mixed liquor and little molecule, or supersound process 30min removes bubble removing, being placed on and carry out UV-crosslinked under 250W uviol lamp, crosslinking time is 1.5h, obtains solid-state polysilazane element embryo.
3, the solid-state polysilazane element embryo obtained is smashed to pieces in glass grinds alms bowl, it is desirable to grain diameter is less than 4mm.With ball mill, particulate abrasive is powdered, particle diameter 0.5 μm.Ball mill uses QP-3SP2 vibrator, and frequency is 300Hz, and Ball-milling Time is 1h.
4, powder good for ball milling and stock solution being mixed with the ratio of 3: 1, mixed particle requirement is less than 5 μm.Fine powder is poured in Φ 13 disk mould, slowly it is forced into 18MPa, difference depending on sheeting thickness, give the different dwell times, particularly polysilazane element flake thickness sheet (thickness is 3～6mm), in order to obtain without being layered crackless polysilazane element flake thickness sheet, the dwell time is the shortest, and the dwell time can be 5s.
5, the polysilazane element embryo sheet pressed is put in aluminium oxide porcelain boat, high-temperature tubular atmosphere furnace stove is sintered, being incubated 1h after making temperature be to slowly warm up to 1000 DEG C, polysilazane element flake thickness sheet to reduce sintering heating rate to ensure gas release completely during sintering.Choose at this is the heating rate of 0.5 DEG C/min.Sintering process is passed through high pure nitrogen as protective gas.Finally prepare the fine and close thickness of free from flaw in 3mm, the SiCN ceramic disks of a diameter of 11mm.
6, the surface Kapton Tape at cylindrical SiCN pottery blocks to stay a slot antenna, and the position of slot antenna is to be at 2.66mm at the upper surface of resonator cavity away from axial location, and the cuboid of a width of 1mm of the longest 8.5mm, thickness is 10 μm.
7, plate layer of metal by plating or evaporation at SiCN ceramic surface, complete surface metalation, form resonator cavity.Metal uses titanium material, and thickness is 10 μm.
8, remove Kapton Tape, obtain SiCN pottery wireless and passive temperature sensor.
The final hyperthermic temperature sensor (operating temperature 800～1400 DEG C) prepared, the demarcation of temperature to be carried out, determine the corresponding relation between its resonant frequency and temperature.
Claims (10)
1. a SiCN pottery wireless and passive temperature sensor, it is characterized in that being provided with cylindrical SiCN amorphous ceramic temperature sensing element, it is provided with refractory metal layer on the surface of cylindrical SiCN amorphous ceramic temperature sensing element and forms resonator cavity, being provided with slot antenna on resonator cavity surface.
2. a kind of SiCN pottery wireless and passive temperature sensor, it is characterised in that a diameter of the 9～15mm of described cylindrical SiCN amorphous ceramic temperature sensing element, thickness is 1～5mm.
3. a kind of SiCN pottery wireless and passive temperature sensor, it is characterised in that described refractory metal layer refers to the fusing point metal level more than 1000 DEG C；The thickness of described refractory metal layer is 8～25 μm.
4. the preparation method of SiCN pottery wireless and passive temperature sensor as claimed in claim 1, it is characterised in that comprise the following steps:
1) the cylindrical SiCN amorphous ceramic temperature sensing element of preparation；
(1) first preparing SiCN pottery element embryo, concrete grammar is as follows:
Method 1: after being mixed with thermal initiator cumyl peroxide (DCP) by precursor polysilazane, carry out heat cross-linking so that it is become the polysilazane of solid-state from the polysilazane of liquid, pulverize last, is pressed into SiCN pottery element embryo；Or
Method 2: after being mixed with light trigger by polysilazane, puts into and carries out UV-crosslinked in mould, obtain faint yellow SiCN pottery element embryo；Or
Method 3: after polysilazane is mixed with light trigger, carry out UV-crosslinked after, pulverize last, be pressed into SiCN pottery element embryo；
(2) under inert gas shielding, SiCN pottery element embryo is pyrolyzed, after re-annealing processes, obtains temperature sensing element SiCN amorphous ceramic body；
2) the slot antenna region Kapton Tape at temperature sensing element SiCN amorphous ceramic body upper surface is protected; at temperature sensing element SiCN amorphous ceramic surface metal cladding; after again Kapton Tape being removed; stayed region is the slot antenna of transceiving electromagnetic ripple signal, so far prepares cylindrical SiCN pottery wireless and passive temperature sensor.
5. the preparation method of as claimed in claim 4 SiCN pottery wireless and passive temperature sensor, it is characterised in that in step 1) (1st) part method 1 in, described polysilazane is 1 with the mass ratio of thermal initiator: (0～0.1)；The temperature of described heat cross-linking is 120～400 DEG C, and the time of heat cross-linking is 1～4h；The particle diameter of described powder is 0.5～2 μm.
6. the preparation method of as claimed in claim 4 SiCN pottery wireless and passive temperature sensor, it is characterised in that in step 1) (1st) part method 2 in, described light trigger uses I819 light trigger；Described polysilazane is 1 with the mass ratio of light trigger: (0.005～0.05)；Described mould uses PDMS mould, and a diameter of the 4 of mould～25mm, the height of mould is 1～5mm；Described UV-crosslinked condition is: under uviol lamp, irradiation carries out UV-crosslinked, and the power of described uviol lamp is 250W, and centre wavelength is 326nm, and the UV-crosslinked time is 0.25～2h.
7. the preparation method of as claimed in claim 4 SiCN pottery wireless and passive temperature sensor, it is characterised in that in step 1) (1st) part method 3 in: described light trigger uses I819 light trigger；Described polysilazane is 1 with the mass ratio of light trigger: (0.005～0.05)；Described UV-crosslinked condition is: under uviol lamp, irradiation carries out UV-crosslinked, and the power of described uviol lamp is 250W, and centre wavelength is 326nm, and the UV-crosslinked time is 0.25～2h；The particle diameter of described powder is 0.5～2 μm.
8. the preparation method of as claimed in claim 4 SiCN pottery wireless and passive temperature sensor, it is characterised in that in step 1) in (2nd) part, described noble gas uses nitrogen or argon；The temperature of described pyrolysis is 800～1000 DEG C, and the time of pyrolysis is 1～4h.
9. the preparation method of as claimed in claim 4 SiCN pottery wireless and passive temperature sensor, it is characterised in that in step 1) in (2nd) part, the temperature of described annealing is 1000～1400 DEG C, and the time of annealing is 1～4h；Obtained temperature sensing element SiCN amorphous ceramic body is the temperature sensing element SiCN amorphous ceramic body of a kind of densification, and its density is 2.6～3.0g/cm3。
10. the preparation method of SiCN pottery wireless and passive temperature sensor as claimed in claim 4, it is characterized in that in step 2) in, described at temperature sensing element SiCN amorphous ceramic surface metal cladding, it is that the method by plating or evaporation is at SiCN ceramic surface metal cladding；Described metal uses platinum or titanium；The thickness of described metal level is 8～25 μm.
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| CN109678519B (en) * | 2018-12-13 | 2021-09-07 | 西南交通大学 | High-temperature pressure sensor based on polymer precursor ceramic |
| CN110672222A (en) * | 2019-10-09 | 2020-01-10 | 天津大学 | Dielectric resonator type temperature sensor for high-temperature measurement |
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