CN104569051A - Method for manufacturing hydrogen sensor - Google Patents
Method for manufacturing hydrogen sensor Download PDFInfo
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- CN104569051A CN104569051A CN201410639624.8A CN201410639624A CN104569051A CN 104569051 A CN104569051 A CN 104569051A CN 201410639624 A CN201410639624 A CN 201410639624A CN 104569051 A CN104569051 A CN 104569051A
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Abstract
The invention relates to the technical field of electronic materials and in particular relates to a method for manufacturing a hydrogen sensor. The method comprises the following steps: 1, annealing a metal oxide; 2, simultaneously adding a chloride, polyvinylpyrrolidone, NaI.2H2O and deionized water into a beaker filled with dimethyl formamide; and 3, ultrasonically dispersing a metal oxide room temperature hydrogen sensitive material obtained in the step 2 into absolute ethyl alcohol, dropwise adding the dispersed turbid liquid into a cleaned interdigital electrode, obtaining a gas sensitive chip after the ethyl alcohol is completely volatilized, connecting the gas sensitive chip with a peripheral circuit, thereby obtaining the hydrogen sensor. The room temperature hydrogen sensor manufactured by the method is high in response speed, high in sensitivity, high in uniformity, easy to manufacture and low in cost, can be widely applied to the condition that hydrogen leakage needs to be detected and is particularly suitable for the occasions in which the hydrogen concentration is high and an accident is easily caused by using a traditional high-temperature sensor.
Description
Technical field
The present invention relates to technical field of electronic materials, especially relate to a kind of making method of hydrogen gas sensor.
Background technology
Along with socioeconomic fast development, the enforcement of raising and the strategy of sustainable development day by day of industrialization degree, energy problem and the own thing through becoming urgent need solution of environmental problem.A large amount of consumption of Nonrenewable energy resources (such as oil, Sweet natural gas etc.) and incident Greenhouse effect, day by day severe global environment, day by day serious pollution level etc. make in the urgent need to finding ideal, efficient, clean novel energy, thus effectively complete the Sustainable development of the energy, environment.
Hydrogen, as a kind of ideal novel energy, because it is pollution-free, rich reserves and the multiple advantage such as combustion heat release is many, is subject to the favor of people, and obtains developing more and more widely.Hydrogen is widely used in various industrial production occasion, as the reduction and metallurgy etc. of the synthesis of ammonia, methyl alcohol and other chemical preparations, refining of petroleum, semiconductor fabrication, chemical preparations.Meanwhile, as the important raw and processed materials of chemistry, food, electronic industry etc., also have a wide range of applications in industrial and agricultural production.
But, also there are some shortcomings significantly in hydrogen itself: hydrogen is a kind of flammable explosive gas, easily blast with after air mixed, its explosive range is 4.65%-93.9%(volumetric concentration), and hydrogen has larger spread coefficient and lower combustion heat energy.Therefore, in order to ensure the use of hydrogen as energy source in various hydrogeneous Industrial processes, the security of the application aspect such as transfer and storage, the highly sensitive hydrogen gas sensor of development for detecting density of hydrogen in hydrogen gas leakage and environment, become the problem of people's growing interest, study the important research direction that high performance hydrogen gas sensor has also become sensor field.
At present, the sensor for monitoring hydrogen richness mainly comprises metal-oxide semiconductor (MOS) hydrogen gas sensor, the quick material of electrothermic type hydrogen and sensor, optical type hydrogen gas sensor and electrochemistry type hydrogen gas sensor etc.
Metal oxide semiconductor sensor is made for main with metal oxide materials such as stannic oxide, zinc oxide, Tungsten oxide 99.999s, and stability is high, structure is simple, low price, be easy to compound, and nearly decades obtain to be studied widely.But, the response sensitivity of the single quick material of metal oxide hydrogen is difficult to meet actual requirement, simultaneously because metal oxide has general response to reducing gas, to hydrogen without special responsiveness, so the selectivity of metal-oxide semiconductor (MOS) hydrogen gas sensor is poor.
Electrothermic type hydrogen gas sensor is the detection that the heat reacting discharged under the catalyst action mainly comprised in detector by hydrogen in measurement environment and oxygen carries out hydrogen.Generally, the catalytic metal selected in the quick material of electrothermic type hydrogen has specificity to hydrogen, and therefore electrothermic type hydrogen gas sensor has good selectivity.But the performance due to electrothermic type hydrogen gas sensor depends on the activity of catalyzer, poisoning of catalyst phenomenon can affect its performance.
Optical type hydrogen gas sensor adopts palladium as sensitive material usually.Palladium metal, after absorption hydrogen, can undergo phase transition, and then its optical property changes thereupon, and changing value is the function of density of hydrogen, and optical type hydrogen gas sensor is exactly according to the monitoring of this principle realization to density of hydrogen.Up to the present, also there are some shortcomings in optical type hydrogen gas sensor, and as easily there is delamination, foaming after repeatedly circulating, thus work-ing life is shorter.How to extend the work-ing life of the quick material of optical type hydrogen, become the focal issue in the research of optical type hydrogen gas sensor.
Electrochemical hydrogen gas sensor has nothing to do due to the size of its electromotive force produced and sensor, easily microminiaturized, therefore obtains application.But the life-span of electrochemical hydrogen gas sensor still has much room for improvement.
Summary of the invention
The invention provides that a kind of response speed is faster, selectivity good, the manufacture method of the hydrogen gas sensor of long service life.
Technical scheme of the present invention is:
A making method for hydrogen gas sensor, described hydrogen gas sensor comprises anodic alumina support layer;
Nano metal palladium layers, described nano metal palladium layers is arranged on described anodic alumina support layer; Protecting film layer; Described protecting film layer is covered on nano metal target layer; Interdigital electrode, described interdigital electrode is arranged in described nano metal palladium layers; Comprise the following steps:
The first step, anneal is carried out to metal oxide;
Second step, by muriate, polyvinylpyrrolidone, NaI2H
2o and deionized water add simultaneously and fill in the beaker of dimethyl formamide, described muriate is Palladous chloride or platinum chloride, obtain dark brown solution, dark brown solution is transferred in reactor, then by step 1) in metal oxide after anneal to join in reactor and to carry out ultrasonic disperse, after dispersion completely, reactor sealed and place under the growth temperature of setting, react complete be cooled to room temperature after, products therefrom is centrifugal and with absolute ethanol washing, in a solvent by product dispersion finally, obtain the metal oxide room temperature hydrogen sensitive material having palladium or Pt nanoparticle at surface deposition,
3rd step, the metal oxide room temperature hydrogen sensitive material ultrasonic disperse that obtained by second step are in dehydrated alcohol, then the suspension liquid after dispersion is dropped in cleaned interdigital electrode, air-sensitive chip is obtained after ethanol volatilization completely, then air-sensitive chip is connected with peripheral circuit, obtains hydrogen gas sensor.
Described protecting film layer is Pb, Pt or Au film.
The material of described interdigital electrode is gold and silver, aluminium or nickel-cadmium.
Anodic alumina support layer preparation process comprises the following steps:
A, annealing aluminum sheet and cleaning
Metallic aluminum material is carried out high temperature annealing, anneals under air, nitrogen or ar gas environment;
B, electrochemical etching
Using the metallic aluminum material after step a process as anode, be placed in polishing fluid and carry out polishing;
C, alumilite process
Using the aluminum after step b process as anode, immerse in electrolytic solution and carry out anodic oxidation.
Annealing temperature is chosen as 500 DEG C, and the time can be chosen as 5-10 hour, and the aluminum after annealing is ultrasonic cleaning in acetone soln and ethanolic soln respectively.
The hydrogen gas sensor obtained according to making method of the present invention has following beneficial effect:
The first, with thermal evaporation, be sputtered to representative physical method compared with, production efficiency significantly promotes, and cost declines to a great extent, and is applicable to synthesis in enormous quantities.
Second, compared with other wet chemistry synthetic methods, one is by selecting suitable solvent (dimethyl formamide) to enable palladium or platinum directly grow on oxide-base bottom material, granules of catalyst be combined with base material than mechanical mix techniques obtain tightr, be conducive to the electronics in the response process of hydrogen between catalyzer and base material and ion transport, two is the crystal faces utilizing the synergy of polyvinylpyrrolidone and iodide ion to control product, the crystal face major part that palladium or Pt catalyst granule are finally exposed is { 100} crystal face, catalytic performance is more all even stable.
Three, the room-temperature hydrogen sensor fast response time made of the present invention, highly sensitive, homogeneity is good, and make simple, cost is low.The situation needing to detect hydrogen leak can be widely used in, be particularly suitable for the place that density of hydrogen is higher, easily cause security incident with traditional pyrostat.
Embodiment
Below by embodiment, the technical scheme of invention is described in further detail.
embodiment one:
The preparation method of hydrogen gas sensor described in the present embodiment, comprises the following steps:
Step one, WO to routine
3nanometer sheet carries out pre-treatment, at ambient temperature by 1g WO
3nanometer sheet loads in quartz crucible, then puts it in retort furnace.Start the heating schedule of retort furnace, be heated to 500 DEG C with the heating rate of 5 DEG C/min from room temperature, keep 2h at 500 DEG C, then close retort furnace heating schedule, make its Temperature fall, after being down to room temperature, by WO
3nanometer sheet loads in sample bottle stand-by.
Described conventional tungstic trioxide nano-slice is average side length is 150nm, and mean thickness is the thin slice of 30nm.Can synthesize with simple hydrothermal method in the lab, also can buy business-like similar clause.
Step 2,0.12g Palladous chloride, 1.6g polyvinylpyrrolidone, 3.6g sodium iodide and 20 ml deionized water are added in the beaker containing 100 milliliters of dimethyl formamides, at room temperature use magnetic stirrer 10min, obtain the mixture of brownish black, in the reactor then said mixture being transferred to 250ml and by the 1g WO of step one gained
3nanometer sheet adds, and is supersound process 30min in the supersonic cleaning machine of 100W at rated output.Then reactor is sealed, in the air dry oven of 150 DEG C, place 8h.After room temperature is down to by reactor, the solid product dimethyl formamide obtained and dehydrated alcohol are washed three times respectively.Obtain the WO being modified with palladium nano-particles
3nanometer sheet (namely surface deposition has the metal oxide room temperature hydrogen sensitive material of palladium nano-particles).
Described Palladous chloride, polyvinylpyrrolidone, sodium iodide and dimethyl formamide are general analysis pure reagent.
Step 3, get the WO being modified with palladium nano-particles that 10mg step 2 obtains
3nanometer sheet is scattered in 5ml dehydrated alcohol, then the suspension liquid after 2.5 microlitre dispersions is dropped in interdigital electrode cleaned in advance, after ethanol volatilization completely, obtain air-sensitive chip, then air-sensitive chip is connected with peripheral circuit, obtains room-temperature hydrogen sensor.
Step 4, be modified with the WO of palladium nano-particles with the measurement of NS-4003 type sense instrument
3nanometer sheet is to the response of hydrogen.
Test condition is normal temperature and pressure, and measurement atmosphere is air, hydrogen is expelled to the test gas obtaining respective concentration in the glass air chamber of 10L.The quick conductance of hydrogen increases with the increase of density of hydrogen.
embodiment two:
The preparation method of room-temperature hydrogen sensor described in the present embodiment, comprises the following steps:
Step one, WO to routine
3nanometer sheet carries out pre-treatment, at ambient temperature by 1g WO
3nanometer sheet loads in quartz crucible, then puts it in retort furnace.Start the heating schedule of retort furnace, be heated to 600 DEG C with the heating rate of 5 DEG C/min from room temperature, keep 2h at 600 DEG C, then close retort furnace heating schedule, make its Temperature fall, after being down to room temperature, by WO
3nanometer sheet loads in sample bottle stand-by.
Described conventional tungstic trioxide nano-slice is average side length is 150nm, and mean thickness is the thin slice of 30nm.Can synthesize with simple hydrothermal method in the lab, also can buy business-like similar clause.
Step 2,0.15g platinum chloride, 2.0g polyvinylpyrrolidone, 4.5g sodium iodide and 20 ml deionized water are added in the beaker containing 100 milliliters of dimethyl formamides, at room temperature use magnetic stirrer 10min, obtain the mixture of total black, in the reactor then said mixture being transferred to 250ml and by the 1g WO of step one gained
3nanometer sheet adds, and is supersound process 30min in the supersonic cleaning machine of 100W at rated output.Then reactor is sealed, in the air dry oven of 120 DEG C, place 6h.After room temperature is down to by reactor, the solid product dimethyl formamide obtained and dehydrated alcohol are washed three times respectively.Obtain the WO being modified with Pt nanoparticle
3nanometer sheet.
Described platinum chloride, polyvinylpyrrolidone, sodium iodide and dimethyl formamide are general analysis pure reagent.
Step 3, get the WO being modified with Pt nanoparticle that 10mg step 2 obtains
3nanometer sheet is scattered in 5ml dehydrated alcohol, then the suspension liquid after 2.5 microlitre dispersions is dropped in golden interdigital electrode cleaned in advance, after ethanol volatilization completely, obtain air-sensitive chip, then air-sensitive chip is connected with peripheral circuit, obtains room-temperature hydrogen sensor.
Step 4, be modified with the WO of Pt nanoparticle with the measurement of NS-4003 type sense instrument
3nanometer sheet is to the response of hydrogen.
Test condition is normal temperature and pressure, and measurement atmosphere is air, a certain amount of hydrogen is expelled to the test gas obtaining respective concentration in the glass air chamber of 10L.The quick conductance of hydrogen increases with the increase of density of hydrogen.
embodiment three:
The preparation method of room-temperature hydrogen sensor described in the present embodiment, comprises the following steps:
Step one, In2O to routine
3nanocubes carries out pre-treatment, at ambient temperature by 1g In2O
3nanocubes loads in quartz crucible, then puts it in retort furnace.Start the heating schedule of retort furnace, be heated to 400 DEG C with the heating rate of 5 DEG C/min from room temperature, keep 2h at 400 DEG C, then close retort furnace heating schedule, make its Temperature fall, after being down to room temperature, by In2O
3nanocubes loads in sample bottle stand-by.
Described conventional In2O
3the Indium sesquioxide nanocubes of nanocubes to be average side length be 200nm.In the lab with simple solvent structure, also can buy business-like similar clause.
Step 2,0.15g platinum chloride, 1.6g polyvinylpyrrolidone, 3.2g sodium iodide and 20 ml deionized water are added in the beaker containing 100 milliliters of dimethyl formamides, at room temperature use magnetic stirrer 10min, obtain the mixture of total black, in the reactor then said mixture being transferred to 250ml and by the In2O of step one gained
3nanocubes adds, and is supersound process 30min in the supersonic cleaning machine of 100W at rated output.Then reactor is sealed, in the air dry oven of 160 DEG C, place 10h.After room temperature is down to by reactor, the solid product dimethyl formamide obtained and dehydrated alcohol are washed three times respectively.Finally product is dispersed in 100 milliliters of dehydrated alcohols.Obtain the In2O being modified with Pt nanoparticle
3nanocubes.
Described platinum chloride, polyvinylpyrrolidone, sodium iodide and dimethyl formamide are general analysis pure reagent.
Step 3, get the In2O being modified with Pt nanoparticle that 10mg step 2 obtains
3nanocubes is scattered in 5ml dehydrated alcohol, then the suspension liquid after 2.5 microlitre dispersions is dropped in golden interdigital electrode cleaned in advance, after ethanol volatilization completely, obtain air-sensitive chip, then air-sensitive chip is connected with peripheral circuit, obtains room-temperature hydrogen sensor.
Step 4, be modified with the In2O of Pt nanoparticle with the measurement of NS-4003 type sense instrument
3nanocubes is to the response of hydrogen.
Test condition is normal temperature and pressure, and measurement atmosphere is air, a certain amount of hydrogen is expelled to the test gas obtaining respective concentration in the glass air chamber of 10L.The quick conductance of hydrogen increases with the increase of density of hydrogen.
Claims (5)
1. a making method for hydrogen gas sensor, described hydrogen gas sensor comprises anodic alumina support layer;
Nano metal palladium layers, described nano metal palladium layers is arranged on described anodic alumina support layer; Protecting film layer; Described protecting film layer is covered on nano metal target layer; Interdigital electrode, described interdigital electrode is arranged in described nano metal palladium layers; It is characterized in that comprising the following steps:
The first step, anneal is carried out to metal oxide;
Second step, by muriate, polyvinylpyrrolidone, NaI2H
2o and deionized water add simultaneously and fill in the beaker of dimethyl formamide, described muriate is Palladous chloride or platinum chloride, obtain dark brown solution, dark brown solution is transferred in reactor, then by step 1) in metal oxide after anneal to join in reactor and to carry out ultrasonic disperse, after dispersion completely, reactor sealed and place under the growth temperature of setting, react complete be cooled to room temperature after, products therefrom is centrifugal and with absolute ethanol washing, in a solvent by product dispersion finally, obtain the metal oxide room temperature hydrogen sensitive material having palladium or Pt nanoparticle at surface deposition,
3rd step, the metal oxide room temperature hydrogen sensitive material ultrasonic disperse that obtained by second step are in dehydrated alcohol, then the suspension liquid after dispersion is dropped in cleaned interdigital electrode, air-sensitive chip is obtained after ethanol volatilization completely, then air-sensitive chip is connected with peripheral circuit, obtains hydrogen gas sensor.
2. the making method of a kind of hydrogen gas sensor according to claim 1, is characterized in that described protecting film layer is Pb, Pt or Au film.
3. the making method of a kind of hydrogen gas sensor according to claim 1, is characterized in that the material of described interdigital electrode is gold and silver, aluminium or nickel-cadmium.
4. the making method of hydrogen gas sensor described in claim any one of claims 1 to 3, is characterized in that: anodic alumina support layer preparation process comprises the following steps:
A, annealing aluminum sheet and cleaning
Metallic aluminum material is carried out high temperature annealing, anneals under air, nitrogen or ar gas environment;
B, electrochemical etching
Using the metallic aluminum material after step a process as anode, be placed in polishing fluid and carry out polishing;
C, alumilite process
Using the aluminum after step b process as anode, immerse in electrolytic solution and carry out anodic oxidation.
5. the making method of hydrogen gas sensor according to claim 4, is characterized in that: annealing temperature is chosen as 500 DEG C, and the time can be chosen as 5-10 hour, and the aluminum after annealing is ultrasonic cleaning in acetone soln and ethanolic soln respectively.
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| CN201410639624.8A CN104569051A (en) | 2014-11-13 | 2014-11-13 | Method for manufacturing hydrogen sensor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891126A (en) * | 2015-06-30 | 2016-08-24 | 四川智立方博导科技有限责任公司 | Low-cost portable hydrogen optical sensor |
| CN106198648A (en) * | 2016-09-14 | 2016-12-07 | 扬州大学 | A kind of preparation method of room-temperature hydrogen sensor |
| CN106483120A (en) * | 2015-09-01 | 2017-03-08 | 现代自动车株式会社 | Chemical stain nano-particle, its manufacture method and the hydrogen sensor including it |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100108529A1 (en) * | 2008-10-30 | 2010-05-06 | University Of Louisville Research Foundation, Inc. | Sensors and switches for detecting hydrogen |
| CN102297881A (en) * | 2011-05-26 | 2011-12-28 | 东南大学 | Preparation method of titanium dioxide nanotube based hydrogen sensor |
| CN103558261A (en) * | 2013-11-20 | 2014-02-05 | 厦门大学 | Preparation method of room-temperature hydrogen sensor |
-
2014
- 2014-11-13 CN CN201410639624.8A patent/CN104569051A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100108529A1 (en) * | 2008-10-30 | 2010-05-06 | University Of Louisville Research Foundation, Inc. | Sensors and switches for detecting hydrogen |
| CN102297881A (en) * | 2011-05-26 | 2011-12-28 | 东南大学 | Preparation method of titanium dioxide nanotube based hydrogen sensor |
| CN103558261A (en) * | 2013-11-20 | 2014-02-05 | 厦门大学 | Preparation method of room-temperature hydrogen sensor |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891126A (en) * | 2015-06-30 | 2016-08-24 | 四川智立方博导科技有限责任公司 | Low-cost portable hydrogen optical sensor |
| CN106483120A (en) * | 2015-09-01 | 2017-03-08 | 现代自动车株式会社 | Chemical stain nano-particle, its manufacture method and the hydrogen sensor including it |
| CN106198648A (en) * | 2016-09-14 | 2016-12-07 | 扬州大学 | A kind of preparation method of room-temperature hydrogen sensor |
| CN106198648B (en) * | 2016-09-14 | 2020-12-01 | 扬州大学 | Preparation method of room temperature hydrogen sensor |
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