CN1721571A - Method for preparing sensitive membrane on acoustic surface wave liquid phase array sensor - Google Patents
Method for preparing sensitive membrane on acoustic surface wave liquid phase array sensor Download PDFInfo
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- CN1721571A CN1721571A CN 200510085895 CN200510085895A CN1721571A CN 1721571 A CN1721571 A CN 1721571A CN 200510085895 CN200510085895 CN 200510085895 CN 200510085895 A CN200510085895 A CN 200510085895A CN 1721571 A CN1721571 A CN 1721571A
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- liquid
- surface wave
- acoustic surface
- liquid phase
- sensor
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- 239000007791 liquid phase Substances 0.000 title claims abstract description 9
- 239000012528 membrane Substances 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 238000004549 pulsed laser deposition Methods 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 11
- 238000010897 surface acoustic wave method Methods 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 abstract description 30
- 238000001514 detection method Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 9
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 230000000979 retarding effect Effects 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 230000000644 propagated effect Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000005387 chalcogenide glass Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910012463 LiTaO3 Inorganic materials 0.000 description 1
- 230000005515 acousto electric effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000003321 atomic absorption spectrophotometry Methods 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
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Abstract
The present invention is the preparation process of sensitive film for acoustic surface wave liquid phase array sensor. The sensor consists of several acoustic surface wave delay line sensors. By means of opening and shorting the delay line, the overall electric characteristic parameters of liquid may be detected; and by means of pulse laser deposition (PLD) technology, sensitive film may be prepared on the delay line for analyzing metal components in liquid. The present invention may be used in the quantitative and qualitative detection of liquid electric parameters and metal ions in food, industry, biomedicine and other fields.
Description
Technical field
The present invention relates to preparation method with the sensitive membrane on acoustic surface wave liquid phase array sensor of acoustic measurement while tracer liquid electrical characteristic and metal ion composition.
Background technology
Heavy metal ion can produce harmful even fatal influence to human body, so the detection by quantitative of heavy metal has very important meaning at aspects such as medicine, food, clinical and environmental monitorings; The electrical characteristic (specific conductivity etc.) of liquid also are to describe an important parameter of liquid background value simultaneously.Present detection method (as atomic absorption spectrophotometry, mass spectroscopy) can only perform an analysis to heavy metal ion, and the detection means complexity is definite, although salometer, conductivitimeter can be measured the electrical characteristic of liquid simultaneously, but also exist repeatability bad, the shortcoming of electrodes maintenance complexity.And do not have at present to be applied to the instrument that industry spot detects in real time.
Summary of the invention
In order to do check and analysis to electrical characteristic and each metal ion species of liquid simultaneously, the purpose of this invention is to provide a kind of preparation method of sensitive membrane on acoustic surface wave liquid phase array sensor.
The technical solution used in the present invention is:
1. acoustic surface wave liquid phase array sensor: comprise copper coin, piezoelectric substrate, insert and refer to electrode pair, retarding line passage, wear ring and test chamber lid.Described slotting finger electrode pair has n right, the retarding line passage has n, comprise that 1 open channel that forms by the piezoelectric substrate that exposes on the retarding line, 1 short-channel that passes through to form with the metallic substance short-circuited delay line and the film for preparing on the piezoelectric on n-2 the retarding line the different metal sensitivity by pulsed laser deposition (PLD) technology form the individual responsive passage of n-2, each passage composes in parallel on same piezoelectric substrate by Y direction order successively; Protection is housed around on the retarding line inserts the wear ring that refers to electrode, the test chamber lid is housed on the wear ring, the intake-outlet of test chamber lid connects plastic catheter.
The surperficial sensor array of said sound comprises 4 sound surface delay line sensors, i.e. n=4.
2. the preparation method of sensitive membrane on acoustic surface wave liquid phase array sensor:
Adopt pulsed laser deposition (PLD) technology on the SAW (Surface Acoustic Wave) delay line sensor array, to prepare sensing unit, that is: pulsed laser deposition equipment mainly is made up of laser generator, lens and vacuum chamber, by vacuum pump vacuum chamber is being evacuated, is charging into N by inflation inlet then
2Gas, piezoelectric substrate is warmed up to 100 ℃, preheating 20 minutes, produce laser by laser apparatus, scioptics, utilization is radiated at the plasma atmosphere that back on the target material of different metal ion-sensitive is formed and target material is deposited on the piezoelectric substrate of sensing unit, and deposition finishes the back and kept 10 minutes, cooling naturally in vacuum chamber then.Processing parameter is:
| Energy density | Wavelength | Pulse width | Repetition rate | Depositing time | Pressure (N 2) | Base reservoir temperature |
| 0.2J/cm 2 | 248nm | ?30ns | ?1.4Hz | ?30min | ?0.2mbar | ?423K |
The present invention compares with background technology, and the useful effect that has is: it adopts surface acoustic wave sensor can make detection means little, and signal disturbs little; Multichannel structure can be done to measure simultaneously to liquid electric performance and metal ion.This transmitter can carry out the qualitative and quantitative analysis of dynamic real-time to liquid electric performance and metal ion in the fields such as (as blood, body fluid) in food, industry, biomedicine.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples;
Fig. 1 is a structure vertical view of the present invention;
Fig. 2 is the structure vertical view that adds the test chamber lid of the present invention;
Fig. 3 is an assembling synoptic diagram of the present invention;
Fig. 4 is the I-I ' sectional view of Fig. 2;
Fig. 5 is a detection system synoptic diagram of the present invention;
Fig. 6 prepares the schematic diagram of sensor sensing passage for PLD;
Fig. 7 typical sensor dynamic response curve;
Fig. 8 is Fe
3+Responsive passage is to Fe
3+The response curve of ionic concn;
Fig. 9 is contrast experiment's curve of responsive passage and open channel;
Figure 10 is the response curve of open channel to the total salinity of liquid;
Figure 11 is the response curve of open channel to the liquor alcoholic strength;
Figure 12 is the response curve of open channel to gasoline water mixing rate.
Among the figure: 1 is copper coin, and 2 is piezoelectric substrate, and 3 is wear ring, and 4 is the sensitive membrane material, 5 is metal level, and 6 is responsive passage, and 7 is short-channel, 8 is open channel, and 9 are the test chamber lid, and 10 is water-in, 11 is water outlet, and 12 is lens, and 13 is vacuum pump, 14 is vacuum chamber, and 15 is target material, and 16 is the plasma atmosphere, 17 is inflation inlet, and 18 is sensor base, and 19 is laser generator.A is a computer, and B is a high-frequency oscillating circuits, and C is the mixing low pass circuit, and D is a sweeter, and E is a transmitter, and F is a waste liquid tank, and G is a sampling device, and H is a peristaltic pump.
Embodiment
1, the structure of transmitter:
As Fig. 1, Fig. 2, Fig. 3, Fig. 4, shown in Figure 5: acoustic surface wave liquid phase array sensor, comprise copper coin 1, piezoelectric substrate 2, insert and refer to electrode pair, the retarding line passage, it is characterized in that: described slotting finger electrode pair has n right, the retarding line passage has n, comprise 1 open channel 8 that forms by the piezoelectric substrate that exposes on the retarding line, form n-2 responsive passage 6 by 1 short-channel 7 that forms with the metallic substance short-circuited delay line and the sensitive membrane 4 for preparing on the piezoelectric on n-2 the retarding line the different metal sensitivity by pulsed laser deposition (PLD) technology, each passage composes in parallel on same piezoelectric substrate by Y direction order successively; Protection is housed around the retarding line inserts the wear ring 3 that refers to electrode, test chamber lid 9 is housed on the wear ring 3, the intake-outlet 10,11 of test chamber lid 9 connects plastic catheter.
2, transmitter preparation:
Sensor parameters: select 36 ° of Y cuttings for use, the LiTaO that directions X is propagated
3Piezoquartz is as base material, size 16.5 * 9.5 * 1mm of piezoelectric substrate
3Test chamber is of a size of 3 * 20 * 1mm
3Each channel parameters is: input and output IDT be singly refer to, the isometric slotting finger transducer of 100 couple; IDT cycle 60um, mid-frequency 50MHz; IDT aperture 2.43mm, between centers 12mm; The short circuit metal level is the Al film, and thickness is 3000 .
The sensitive membrane preparation:
This programme is with Fe
3+Ion-sensitive material filming technology is that example specifies.Select Fe
1.2(Ge
28Sb
12Se
60)
98.8Chalcogenide glass is Fe
3+The ionic sensitive material.Adopt pulsed laser deposition (PLD) technology on the SAW (Surface Acoustic Wave) delay line sensor array, to prepare sensing unit, pulsed laser deposition equipment mainly is made up of laser generator 11, lens 12 and vacuum chamber 14, vacuum chamber being evacuated, charge into N by inflation inlet 17 then by vacuum pump 13
2Gas, transmitter 18 is warmed up to 100 ℃, preheating 20 minutes, produce laser by laser apparatus, scioptics 12, utilization is radiated at the plasma atmosphere 16 that back on the target material 15 of different metal ion-sensitive is formed and target material 15 is deposited on the piezoelectric 18 of sensing unit, and deposition finishes the back and kept 10 minutes, cooling naturally in vacuum chamber then.Processing parameter is:
| Energy density | Wavelength | Pulse width | Repetition rate | Depositing time | Pressure (N 2) | Base reservoir temperature |
| 0.2J/cm 2 | ?248nm | ?30ns | ?1.4Hz | ?30min | ?0.2mbar | ?423K |
Transmitter is connected with detection system:
As shown in Figure 5, each passage passes through separately, and the slotting finger of the input and output electrode at two ends links to each other with the input and output of high-frequency oscillating circuits B respectively, the signal of the signal of open channel and n-2 responsive passage links to each other with the input port of separately mixing low pass circuit C respectively, another input port of all mixing low pass circuits and the signal of short-channel link to each other, and the n-1 of an acquisition difference frequency signal sends computer A to after being detected by sweeter D.
Fundamentals of Sensors:
36 ° of Y cuttings, the LiTaO3 piezoquartz that directions X is propagated can effectively excite horizontal shear wave, and this wave mode is propagated and little energy decrement in liquid.Under the certain prerequisite of surface liquid physical property, the phase velocity of sound wave depends on the electrical characteristic of liquid in the piezoelectric.Because the electrical short sound channel is zero to the response of electrical characteristic, so can reflect the specific conductivity and the specific inductivity of liquid by the frequency of sound wave difference that detects two sound channels.The principle formula of acoustoelectric effect is:
K
s, ε
p T, δ ', ε
r', ε
0Be respectively the electromechanical coupling factor of piezoelectric and specific inductivity, the specific conductivity of liquid, the specific inductivity of liquid, the specific inductivity of air, the change of oscillation frequency has embodied the electrical characteristic of liquid.
The principle formula of electromechanical effect is
H, p be the thickness of adsorbent and density on responsive passage respectively.
The working process of system:
Start high-frequency oscillating circuits B, mixing low pass circuit C and sweeter work; Computer A is opened the deionization water valve, closes sample liquid valve, opens peristaltic pump H simultaneously, to the transmitter E ionized water of entering; Treat that liquid enters fully that computer A behind the transmitter E is opened and the communication of sweeter D; Wait for that transmitter is to stable (the deviation of reading scope in the 10s＜20Hz), perhaps control certain sample injection time (as 20s) of the response of deionized water; Open sample liquid valve then and close the deionization water valve,, wait for that transmitter E is to stable (the deviation of reading scope in the 10s＜20Hz), perhaps control certain sample injection time (as 20s) of the response of sample liquid to transmitter E sample introduction liquid.So just finished the one-time detection process.The liquid of outflow transmitter E after tested flows to waste liquid tank F.Get transmitter E the difference of both stable state frequency responses is the response value to sample liquid, i.e. y=f (sample liquid)-f (water), as shown in Figure 7.
Sensor characteristic is described:
By 10
-2～10
-6The concentration of mol/l is 10 times of proportioning Fe (NO at interval
3)
3Solution is selected Fe
1.2(Ge
28Sb
12Se
60)
98.8Chalcogenide glass prepares the sensitive membrane material with pulsed laser deposition (PLD) technology on responsive passage.Fig. 8 is that the sensor sensing passage is to above-mentioned concentration Fe (NO
3)
3The response curve of solution, Fig. 9 are that sensor sensing passage and open sensor passage are to 10
-3Fe (the NO of mol/l
3)
3Solution contrast response curve.Responsive passage is to Fe (NO
3)
3Solution detects lower limit can reach 10
-5Mol/l.
Demarcate the KCl solution of 0.024S/m, 0.039S/m, 0.1S/m, 0.18S/m, 0.32S/m, 0.58S/m with conductivitimeter, they are measured, can obtain curve as shown in figure 10, be limited to 1.2 * 10 under the detection of transmitter with open channel
-4S/m.
35 degree, 36 degree, 37 degree, 38 degree and 39 liquor of spending as sample liquid, are detected with open channel, can obtain curve as shown in figure 11.The detection sensitivity of transmitter is the 1.5KHz/ degree, and accuracy of detection is 0.2 degree.
For edible oil, mix the back as sample liquid in water mixing ratio 2%, 5%, 10%, 15% and 20%, measure with the open channel of transmitter, can obtain curve as shown in figure 12.Can effectively discern＞5% organic solution water mixing ratio.
Claims (1)
1, the preparation method of the sensitive membrane of acoustic surface wave liquid phase array sensor, it is characterized in that: adopt pulsed laser deposition technique on the SAW (Surface Acoustic Wave) delay line sensor array, to prepare responsive passage, that is: pulsed laser deposition equipment mainly is made up of laser generator (19), lens (12) and vacuum chamber (14), by vacuum pump (13) vacuum chamber is being evacuated, is charging into N by inflation inlet (17) then
2Gas, pressure is 0.2mbar, sensor base (18) is warmed up to 90～120 ℃, preheating 15～25 minutes, produce laser by laser apparatus, scioptics (12) utilize to be radiated at and the target material (15) of different metal ion-sensitive is gone up the plasma atmosphere (16) that the back forms target material (15) are deposited on the piezoelectric substrate (18) of sensing unit, deposition finishes the back and kept 8～15 minutes, cooling naturally in vacuum chamber then.
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|---|---|---|---|
| CN 200510085895 CN1721571A (en) | 2004-01-14 | 2004-01-14 | Method for preparing sensitive membrane on acoustic surface wave liquid phase array sensor |
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| CN 200510085895 CN1721571A (en) | 2004-01-14 | 2004-01-14 | Method for preparing sensitive membrane on acoustic surface wave liquid phase array sensor |
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|---|---|---|---|
| CN 200410015906 Division CN1243977C (en) | 2004-01-14 | 2004-01-14 | Acoustic surface wave liquid phase array transducer and preparation method for sensitive membrane thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101784892B (en) * | 2007-03-23 | 2013-03-27 | 霍尼韦尔国际公司 | Design and deposition of sensing layers for surface acoustic wave chemical sensors based on supra-molecular chemistry |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101784892B (en) * | 2007-03-23 | 2013-03-27 | 霍尼韦尔国际公司 | Design and deposition of sensing layers for surface acoustic wave chemical sensors based on supra-molecular chemistry |
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