CN101545883A - Nuclear shell structure micro-nano material humidity sensor and preparation method thereof - Google Patents
Nuclear shell structure micro-nano material humidity sensor and preparation method thereof Download PDFInfo
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- CN101545883A CN101545883A CN200910050280A CN200910050280A CN101545883A CN 101545883 A CN101545883 A CN 101545883A CN 200910050280 A CN200910050280 A CN 200910050280A CN 200910050280 A CN200910050280 A CN 200910050280A CN 101545883 A CN101545883 A CN 101545883A
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Abstract
The invention discloses a nuclear shell structure micro-nano material humidity sensor and a preparation method thereof. The preparation method is characterized in that high molecular polymers cover entire metallic nano particles to form micro-nano materials with a nuclear shell structure which are uniformly coated on the surface of a silicon chip; and an electrode is prepared for encapsulation, and the nuclear shell structure micro-nano material humidity sensor is obtained. The preparation method comprises preparation of a metallic nano particle solution and a polymer solution, surface treatment of the silicon chip, and coating and encapsulation. The selectivity on materials which are sensitive to the target quantity of the sensor is wide, and raw materials are easy to obtain. Compared with the prior art, the invention has the advantages of simple method, convenient operation, low production cost, pollution-free environment, great improvement of the electrical properties of the sensor, high integrity and small volume.
Description
Technical field
The present invention relates to technical field of sensor manufacture, specifically a kind of nuclear shell structure micro-nano material humidity sensor and preparation method thereof.
Background technology
Nano particle is meant the particle of yardstick at 1～100nm.Studies show that the physics of nano material and the material that chemical property is different from macroscopic view.Metal and semi-conductor nano particles are subjected to people's attention day by day because of its characteristic in aspect uniquenesses such as light, electricity, catalysis, chemical sensitisation and following nanoscale memory spares, are focuses in the present scientific research to its research in science and application.In the last few years, along with going deep into of research, a lot of technology was established and is used for synthetic and characterizes nano particle, and had a large amount of nanostructureds to be used or realize.How the material of these nanostructureds being synthesized on the device and how adopting these materials in the application of reality will be the next developing stage of nanometer technology, and the application of nano structural material will be following focus.
When adopting nano structural material as sensitive element structure electric sensor, need usually and will arrange or be connected across between two electrodes as the nanostructured of sensing material, so that utilize its characteristic is spread out of with the variation of the measuring object form with electric signal.So selectively specific sensitive material is positioned between the electrode,, be the emphasis of current novel sensor research so that specific detected object is produced electrical reactions.
Traditionally, the sensor production of special gas is difficulty comparatively, and main cause is to be difficult to seek specific sensitive material, and also wayward for sensitive material.The method for making that a large amount of sensors is arranged in the disclosed technical information at present, and the sensor at different detected objects miscellaneous mainly are summarized as follows:
First kind is traditional humidity or gas sensor, traditional specific sensitive material will be coated with or attached on the substrate of carrying out electrode, dry then, has the part material and places between the electrode, and form sensor.This method is widely used, and can commercially produce in a large number.But its main problem is that device size is bigger, and integrated level is low, and the response time is slow, less stable.
Second kind is to be referred to as " novel " sensor, at first form the very sensitive materials of small scale with special chemistry or physical method, generally, on silicon substrate, make other electrode of micro-nano level that coexists with specific method then, thereby form sensor in the micro-nano rank.This sensor bulk is little, the integrated level height, and electrology characteristic is good, and problem is that cost is higher, the skewness of sensitive material between electrode.
Summary of the invention
A kind of nuclear shell structure micro-nano material humidity sensor that provides at the deficiencies in the prior art and preparation method thereof is provided, it adopts a kind of nucleocapsid structure coated materials of metal-polymer between the electrode of sensor, make being more evenly distributed of sensitive material, big or small homogeneous, good stability, solved the problem that traditional material is reunited, the electrology characteristic of sensor can further improve, and the integrated level height, and volume is little, production cost is low, and is pollution-free.
The concrete technical scheme that realizes the object of the invention is: a kind of nuclear shell structure micro-nano material humidity sensor, the characteristics micro-nano material that to be them form a kind of nucleocapsid structure after with the metal nanoparticle integral coating with high molecular polymer evenly is coated on silicon chip surface, do top electrode then and encapsulate, make the micro-nano material humidity sensor of nucleocapsid structure.
Described polymkeric substance is the high molecular polymer of polyvinyl alcohol (PVA), polyvinylpyrrolidone or polystyrene to humidity sensitive.
Described metal nanoparticle is that gold, silver, copper or aluminium adopt pure reducing process, the sodium citrate reducing process, and the potassium borohydride reduction legal system gets metal nanoparticle solution.
A kind of preparation method of nuclear shell structure micro-nano material humidity sensor, characteristics are these methods with the nucleocapsid structure coated materials of metal-polymer in silicon chip surface, do top electrode then and encapsulate and form, and concrete the making may further comprise the steps:
(1) preparation of metal nanoparticle solution
Adopt sodium citrate reducing process, pure reducing process or potassium borohydride reduction method that gold, silver, copper or aluminium reducing are become the solution of metal nanoparticle, with standby as the carrier of amplification electrical quantities;
(2) preparation of polymer solution
It is standby that employing is mixed with corresponding polymer solution to polyvinyl alcohol (PVA), polyvinylpyrrolidone or the polystyrene of humidity sensitive and water by 1: 20 mass ratio;
(3) surface oxidation treatment of silicon chip
A, silicon chip is put into sulfuric acid and hydrogen peroxide by volume for the solution of 3:1 preparation cleans 10min, its sulfuric acid concentration is 98%, and hydrogen peroxide concentration is 30%;
B, above-mentioned silicon chip is taken out, with cleaning in the deionized water;
C, the silicon chip after the above-mentioned cleaning is put into concentration is that 99.7% ethanolic solution soaks 10min;
D, with silane couplent or 1, the 6-ethanthiol joins in 99.7% the ethanolic solution, is configured to the solution of 1mM, is heated to boiling after stirring, and puts into above-mentioned silicon chip then and soaks 45min at the solution of boiling;
E, above-mentioned silicon chip being taken out, is 99.7% alcohol solution dipping 10min with concentration, to remove unnecessary silane couplent or 1, the 6-ethanthiol;
F, with above-mentioned silicon chip washed with de-ionized water, it is stand-by to put on 100 ℃ the dryer oven dry then.
(4) coating of silicon chip and encapsulation
A, above-mentioned polymer solution is joined in the metal nanoparticle solution, under magnetic agitation, reacted 2～3 hours, the volume ratio of polymer solution and metal nanoparticle solution is 1:10, making polymkeric substance form the whole evenly coating of metal nanoparticle back a kind of is nuclear with the metal nanoparticle, and polymkeric substance is the micro-nano material solution of the nucleocapsid structure of shell;
B, with above-mentioned silicon slice placed through oxidation processes on glue spreader, add with the micro-nano material solution of above-mentioned nucleocapsid structure and to drop in silicon chip surface, and start glue spreader with 500 revolutions per seconds of rotational speed 5 seconds, and then with 2000 revolutions per seconds of rotational speed 20～30 seconds, make the micro-nano material of nucleocapsid structure evenly be coated on the surface of silicon chip, make electrode by technological requirement then, the line sensor structural leadthroughs of going forward side by side encapsulates, and makes the micro-nano material humidity sensor of nucleocapsid structure.
The present invention is extensive to the material selectivity of sensor target amount sensitivity, starting material obtain easily, not high to production equipment and environmental requirement yet, it is simple compared with prior art to have method, easy to operate, and production cost is lower, environmentally safe, and the electrology characteristic of sensor can improve integrated level height, the advantage that volume is little greatly.
Description of drawings
Fig. 1～Fig. 7 is the micro-nano material frequency curve chart of gold-polyvinyl alcohol (PVA) nucleocapsid structure
Fig. 8 is the stability curve figure of sensor of the present invention
Fig. 9 is the impedance synoptic diagram of the uncoated nuclear shell structure micro-nano material of silicon chip surface
Figure 10 applies the impedance synoptic diagram of nuclear shell structure micro-nano material for silicon chip surface
Figure 11 is the test circuit figure of sensor of the present invention
Embodiment
Evenly be coated on silicon chip surface below by the nucleocapsid structure material that adopts polyvinyl alcohol (PVA) parcel golden nanometer particle as the sensitive material of sensor, the present invention is described in further detail to prepare a kind of embodiment of nm-humidity sensor:
Embodiment 1
Employing gold-polyvinyl alcohol (PVA) is that the micro-nano material of nucleocapsid structure is coated on silicon chip surface, does top electrode then and encapsulates, and makes nuclear shell structure micro-nano material humidity sensor, and its concrete making is carried out according to the following steps:
(1) preparation of metal nanoparticle solution
A, employing gold are got 1g HAuCl4 (gold chloride) and are mixed with yellow chlorauric acid solution with the 3L deionized water, and be heated to boiling as the carrier that amplifies electrical quantities.Because HAuCl4 (gold chloride) deliquescence in air very easily, thus very rapid during weighing, in order to avoid weight error.
The deionized water of b, the sodium citrate of getting 1.14g and 100ml is mixed with sodium citrate solution, stirs.
Restore the Au nano particle in c, the chlorauric acid solution with the above-mentioned sodium citrate solution adding boiling for preparing, its sodium citrate solution and chlorauric acid solution are 1:10 by volume.Reaction time is 10min.
D, with above-mentioned reacted solution through placing, cooling, can getting the nano-Au solution that particle diameter is 10nm after filtering.
The method of reducing of above metal also can adopt pure reducing process, potassium borohydride (KBH4) reducing process.The sodium citrate reducing process usually with sodium citrate as reductive agent and protective agent.Can suitably regulate the ratio of gold chloride and sodium citrate, prepared gold nanometer particle grain size is different.
(2) preparation of polymer solution
Adopt polyvinyl alcohol (PVA) to adsorb specific detection target as sensitive material, it has good hydroscopicity, can absorb the steam of thousands of times of volumes separately, is good humidity sensor modulator material.
Get 5gPVA and be dissolved in the 200ml water, dissolving at room temperature, it is standby to get clear liquid after filtering.Can suitably heat raising solubleness, but heating-up temperature can not surpass the decomposition temperature of polymkeric substance.
(3) surface oxidation treatment of silicon chip
A, with silicon chip put into by concentration be 98% sulfuric acid 150ml and concentration be 30% hydrogen peroxide 50ml preparation and solution, clean 10min.
B, above-mentioned silicon chip is taken out, with cleaning in the deionized water.
C, the silicon chip after the above-mentioned cleaning is put into concentration is that 99.7% ethanolic solution soaks 10min.
D, silane couplent (APTMS) joined in 99.7% the ethanolic solution, be configured to the solution of 1mM, be heated to boiling after stirring, put into above-mentioned silicon chip then and soak 45min at the solution of boiling.Silicon chip surface is modified with silane coupling agent, can strengthen and the combining of sensitive material, and makes sensitive material not lose easily because of the external force effect.
E, above-mentioned silicon chip being taken out, is 99.7% alcohol solution dipping 10min with concentration, to remove unnecessary silane couplent (APTMS).
F, with above-mentioned silicon chip washed with de-ionized water, it is stand-by to put on 100 ℃ the dryer oven dry then.
(4) coating of silicon chip and encapsulation
A, above-mentioned poly-vinyl alcohol solution is joined in the nano-Au solution, reaction is 2.5 hours under magnetic agitation, making polymkeric substance form the whole evenly coating of metal nanoparticle back a kind of is nuclear with the metal nanoparticle, and polymkeric substance is the micro-nano material solution of the nucleocapsid structure of shell.
B, with above-mentioned silicon slice placed through oxidation processes on glue spreader, add with the micro-nano material solution of above-mentioned gold-polyvinyl alcohol (PVA) nucleocapsid structure and to drop in silicon chip surface, and start glue spreader with 500 revolutions per seconds of rotating speed spin coatings 5 seconds, and then with 2000 revolutions per seconds of rotating speed spin coatings 25 seconds, make the gold-micro-nano material of polyvinyl alcohol (PVA) nucleocapsid structure evenly be coated on the surface of silicon chip, make electrode by technological requirement then, the line sensor structural leadthroughs of going forward side by side encapsulates, and makes the micro-nano material humidity sensor of nucleocapsid structure.
The above-mentioned nuclear shell structure micro-nano material humidity sensor that makes is carried out relative humidity test: two incoming ends of sensing arrangement are connected in the multivibrator circuit of being made up of 555 timers as capacitor element, observe the variation of its frequency by computer program.Needed standard humidity produces by the saturated solution method of salt in the test, depresses at a normal atmosphere, when experimental temperature is 25 ℃, gets CH3COOK, K2CO3, NaBr, KI, NaCl, KCl, 6 kinds of saturated salt solutions such as KNO3.And humidity sensor of the present invention the test of following project and the check of effect have been carried out.
1, the test of recovery
With 25 degrees centigrade of following silica gel (relative humidity 11.3%) is benchmark, respectively to CH3COOK, and K2CO3, NaBr, KI, NaCl, KCl, 6 kinds of saturated salt solutions such as KNO3, rh value is respectively 23%, 43%, 57%, 68%, 75%, 85%, 93% carries out the recovery test.Be specially: humidity sensor was placed in silica gel 10 minutes, put rapidly then to the corresponding salt solusion 10 minutes, and then put rapidly to the silica gel 10 minutes, sensor was put back in the salt solusion 10 minutes again, it was put back at last in the silica gel 10 minutes again.With this,, can obtain the frequency change data of twice repeated test by 555 oscillatory circuits.
Consult accompanying drawing 1～Fig. 7, can be clear that the recovery of nuclear shell structure micro-nano material humidity sensor of the present invention is good, no matter high humidity or low humidity, maximum or minimum frequency basically identical.No matter be high humidity (relative humidity is more than 68%), still under low humidity (relative humidity is below the 53%) condition, the frequency values of sensor all can be returned to initial position, what its medium frequency was higher is benchmark relative humidity, the humidity 11.3% of silica gel under this temperature just, frequency is hanged down when forming ladder, for placing under the condition of saturated salt solution when sensor of the present invention.
2, the test of response time and release time
Consult accompanying drawing 1～Fig. 7, from highest frequency to the low-limit frequency ladder height 66% is fall time, is the rise time with low-limit frequency to 33% of highest frequency ladder height simultaneously.Can be fully aware of find out, the typical rise time is about 40 seconds, and typical fall time is about 110 seconds.Different along with the difference of relative humidity, can find out obviously that the low humidity following reaction time of condition is slower, and reaction is comparatively rapid under the high humidity situation.Also can see, for same humidity measurement point, the always a little higher than measured value in revesal of measured value in humidity incremental impedance change curve, and the response time in humidity incremental impedance change curve always than the impedance variation curve that successively decreases in humidity in the response time short, may be owing to moisture absorption than the easy reason of dehumidification.In same test stroke, no matter be humidity incremental impedance change curve or the humidity impedance variation curve that successively decreases, moisture absorption and dehumidification are all very fast during low humidity, and during high humility, the beginning moisture absorption is very fast, and is slack-off near saturated moisture absorption, this is consistent with the multilayer adsorption theory.
3, the test of sensitivity
Consult accompanying drawing 1～Fig. 7, just humidity is from 23%-93%.Can see fully aware ofly that the ladder that forms between highest frequency and low-limit frequency is more and more obvious, shape is standard more and more also.Ladder seems smaller under low moisture conditions, particularly 23%, still in distinguishable scope, that is to say, and can differentiate the difference of itself and benchmark relative humidity 11.3% fully, so it still has the ability of test low humidity.And at this more than humidity, it is more clear to differentiate.And the stairstepping of different relative humidity formation, that is to say the frequency-splitting difference, so can fully clearly differentiate different damp conditions, consider the variation range of envionmental humidity under the daily life situation, this type of sensor is suitable fully.
4, Wen Dingxing test
As its stability of sensor is crucial technical parameter, whether stablize be directly connected to it can carry out the test that long stability is also referred to as fatigue strength to sensor of the present invention with reference to property.Be specially the saturated salt solution NaCl (relative humidity 75% time) than high humidity the typical case, the test reach 3.9h hour, with respect to its reaction time be tens of seconds, can explain its stability fully.
Consult accompanying drawing 8, sensor of the present invention as can be seen is very stable, specifically calculate and frequency jitter in 5.3%, that is to say that its stability reaches within the acceptable scope of daily use fully.
5, the test of impedance and analysis
Consult accompanying drawing 9, the uncoated nuclear shell structure micro-nano material of silicon chip surface, silicon chip surface is near insulator, and resistance value is high.
Consult accompanying drawing 10, silicon chip surface has applied nuclear shell structure micro-nano material, and the resistance value of silicon chip surface significantly descends, and variation on the order of magnitude is obviously arranged to stable back impedance phase when uncoated, visible apply remarkable for the influence of silicon chip surface impedance.The impedance of clean silicon chip surface and the impedance that applied the silicon chip surface of nuclear shell structure micro-nano material are tested respectively, and its comparative analysis sees Table 1 and table 2.
The impedance of the clean silicon chip surface of table 1
| Frequency | Voltage | Impedance |
| 100HZ | 1V | 335.4M |
| 1KHZ | 1V | 70M |
| 10KHZ | 1V | 6.7M |
Table 2 has applied the impedance of the silicon chip surface of nuclear shell structure micro-nano material
| Frequency | Voltage | Impedance |
| 100HZ | 1V | 2.6M |
| 1KHZ | 1V | 1.6M |
| 10KHZ | 1V | 1.1M |
Consult accompanying drawing 11, R
1, R
2, C is outward element.Work as u
cCharging rises to C because of power connection
The time, comparer A
1Be output as low level, make the output of R-S trigger put 0, the T conducting, capacitor C is discharged by T; Work as u
cBecause of capacitor discharge be reduced to a little less than
The time, comparer A
2Be output as low level, make the output of R-S trigger put 1, T ends, and capacitor C continues charging up to u
cA little more than
The time, trigger is turned to 0 again, thereby finishes the one-period vibration.Can calculate its oscillation period with following formula:
T＝0.7(R
1+2R
2)C
Sensor of the present invention is inserted the C position of circuit shown in the accompanying drawing 11 as probe, can record because humidity changes the sensor capacitance variation that causes, thereby develop into the frequency change of circuit, in theory because frequency F is inversely proportional to capacitor C, and capacitor C becomes big under high humility, so frequency F has the trend that diminishes, the experimental result that this and this sensor records meets fully.
Just the present invention will be further described for above embodiment, is not in order to restriction patent of the present invention, all for the present invention's equivalence enforcement, all should be contained within the claim scope of patent of the present invention.
Claims (4)
1, a kind of nuclear shell structure micro-nano material humidity sensor, it is characterized in that the micro-nano material that forms a kind of nucleocapsid structure with high molecular polymer after with the metal nanoparticle integral coating evenly is coated on silicon chip surface, do top electrode then and encapsulate, make the micro-nano material humidity sensor of nucleocapsid structure.
2,, it is characterized in that described polymkeric substance is the high molecular polymer to polyvinyl alcohol (PVA), polyvinylpyrrolidone or the polystyrene of humidity sensitive according to the described nuclear shell structure micro-nano material humidity sensor of claim 1.
3,, it is characterized in that described metal nanoparticle is that gold, silver, copper or aluminium adopt pure reducing process, sodium citrate reducing process or potassium borohydride reduction legal system to get the solution of metal nanoparticle according to the described nuclear shell structure micro-nano material humidity sensor of claim 1.
4, the preparation method of the described nuclear shell structure micro-nano material humidity sensor of a kind of claim 1, it is characterized in that this method with the nucleocapsid structure coated materials of metal-polymer in silicon chip surface, do top electrode then and encapsulate and form, the concrete making may further comprise the steps:
(1) preparation of metal nanoparticle solution
Adopt pure reducing process, sodium citrate reducing process or potassium borohydride reduction method that gold, silver, copper or aluminium reducing are become the solution of metal nanoparticle, with standby as the carrier that amplifies electrical quantities;
(2) preparation of polymer solution
It is standby that employing is mixed with corresponding polymer solution to polyvinyl alcohol (PVA), polyvinylpyrrolidone or the polystyrene of humidity sensitive and water by 1: 20 mass ratio;
(3) surface oxidation treatment of silicon chip
A, silicon chip is put into sulfuric acid and hydrogen peroxide by volume for the solution of 3:1 preparation cleans 10min, its sulfuric acid concentration is 98%, and hydrogen peroxide concentration is 30%;
B, above-mentioned silicon chip is taken out, with cleaning in the deionized water;
C, the silicon chip after the above-mentioned cleaning is put into concentration is that 99.7% ethanolic solution soaks 10min;
D, with silane couplent or 1, the 6-ethanthiol joins in 99.7% the ethanolic solution, is configured to the solution of 1mM, is heated to boiling after stirring, and puts into above-mentioned silicon chip then and soaks 45min at the solution of boiling;
E, above-mentioned silicon chip being taken out, is 99.7% alcohol solution dipping 10min with concentration, to remove unnecessary silane couplent or 1, the 6-ethanthiol;
F, with above-mentioned silicon chip washed with de-ionized water, it is stand-by to put on 100 ℃ the dryer oven dry then.
(4) coating of silicon chip and encapsulation
A, above-mentioned polymer solution is joined in the metal nanoparticle solution, under magnetic agitation, reacted 2～3 hours, the volume ratio of polymer solution and metal nanoparticle solution is 1:10, making polymkeric substance form the whole evenly coating of metal nanoparticle back a kind of is nuclear with the metal nanoparticle, and polymkeric substance is the micro-nano material solution of the nucleocapsid structure of shell;
B, with above-mentioned silicon slice placed through oxidation processes on glue spreader, add with the micro-nano material solution of above-mentioned nucleocapsid structure and to drop in silicon chip surface, and start glue spreader with 500 revolutions per seconds of rotational speed 5 seconds, and then with 2000 revolutions per seconds of rotational speed 20～30 seconds, make the micro-nano material of nucleocapsid structure evenly be coated on the surface of silicon chip, make electrode by technological requirement then, the line sensor structural leadthroughs of going forward side by side encapsulates, and makes the micro-nano material humidity sensor of nucleocapsid structure.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016041022A1 (en) * | 2014-09-19 | 2016-03-24 | The University Of Queensland | Sensor scaffold |
| CN109085204A (en) * | 2018-08-22 | 2018-12-25 | 成都信息工程大学 | A kind of transparent flexible humidity sensor and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3951181B2 (en) * | 2003-03-31 | 2007-08-01 | 独立行政法人科学技術振興機構 | Preparation method of core-shell structure |
| CN100515614C (en) * | 2007-06-05 | 2009-07-22 | 暨南大学 | Core-shell structure composite nanometer material and preparation method thereof |
| CN101202341B (en) * | 2007-12-13 | 2011-08-31 | 复旦大学 | Carbon cladding alloy nanometer particle material for lithium ion battery and method for making same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016041022A1 (en) * | 2014-09-19 | 2016-03-24 | The University Of Queensland | Sensor scaffold |
| CN109085204A (en) * | 2018-08-22 | 2018-12-25 | 成都信息工程大学 | A kind of transparent flexible humidity sensor and preparation method thereof |
| CN109085204B (en) * | 2018-08-22 | 2023-10-17 | 成都信息工程大学 | Transparent flexible humidity sensor and preparation method thereof |
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