CN105136870A - Hydrogen gas sensor and production method thereof - Google Patents
Hydrogen gas sensor and production method thereof Download PDFInfo
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- CN105136870A CN105136870A CN201510605927.2A CN201510605927A CN105136870A CN 105136870 A CN105136870 A CN 105136870A CN 201510605927 A CN201510605927 A CN 201510605927A CN 105136870 A CN105136870 A CN 105136870A
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Abstract
The embodiment of the invention discloses a method for producing hydrogen gas sensors and a hydrogen gas sensor produced through the method. The method comprises the following steps: forming an aluminium layer on a first surface of a silicon substrate; carrying out anodic oxidation treatment on the aluminium layer, so as to form an aluminium oxide layer with a plurality of small holes; forming carbon atom layers on the inner walls of the small holes; forming an upper electrode on the aluminium oxide layer; forming a lower electrode on a second surface of the silicon substrate. The hydrogen gas sensor provided by the embodiment of the invention has the advantages of being high in response speed, good in repeatability, low in working temperature, simple in structure, small in size, and the like, and is sensitive to hydrogen gas with the volume concentration of 0.05%-2% at room temperature; besides, the method for producing hydrogen gas sensors provided by the embodiment of the invention is simple in technology and good in repeatability.
Description
Technical field
The present invention relates to nano material gas sensor technical field, especially relate to a kind of hydrogen gas sensor and manufacture method thereof.
Background technology
Hydrogen advantage that is efficient with it, renewable and environmental protection is considered to the most attractive energy resources in future.At present, hydrogen is for internal combustion engine and fuel cell, and very fast by relying on potentiality of its clean discharge to become the ubiquitous energy, is applied to automobile, house etc.But because hydrogen is colourless, tasteless, in dry air, concentration is very easily exploded between 4% to 70% time, therefore stores and uses the danger of hydrogen to be problem demanding prompt solution.Therefore, to the detection of the detection of hydrogen leak, particularly low concentration under room temperature, be very important for safety.
The critical aspects meeting hydric safe utilization is hydrogen gas sensor.Safety hydrogen sensor is the key being acknowledged as successful Application hydrogen.USDOE has delivered the target call specification of a safety hydrogen sensor, and propose the parameter request of hydrogen gas sensor and the candidate scheme of hydrogen gas sensor, precision prescribed is high, and the response time fast (being less than 1 second), measurement range is 1% to 10%.
There is the hydrogen gas sensor of a variety of different principle at present, comprise combustion-type hydrogen gas sensor, electrochemical hydrogen gas sensor, conductor oxidate hydrogen gas sensor, thermal conductance type hydrogen gas sensor etc.But these hydrogen gas sensors existing all have respective shortcoming in response speed, repeatability, working temperature etc., there is the space of improving further.
Summary of the invention
An object of the present invention is to provide that a kind of technique is simple, the method for the manufacture hydrogen gas sensor of favorable repeatability.
An object of the present invention is to provide a kind of fast response time, reproducible, working temperature is low, the simple hydrogen gas sensor of structure.
Technical scheme disclosed by the invention comprises:
Provide a kind of method manufacturing hydrogen gas sensor, it is characterized in that, comprising: provide silicon substrate, described silicon substrate comprises first surface and the second surface relative with described first surface; Form aluminium lamination on the first surface; Anodized is carried out to described aluminium lamination, described aluminium lamination is formed the alumina layer with multiple aperture, and described aperture runs through described alumina layer; Deposit carbon atomic layer on described aperture inwall, wherein inwall deposited the keyhole formation carbon nano-tube of carbon atomic layer; Described alumina layer forms top electrode; The second surface of described silicon substrate forms bottom electrode.
In some embodiments of the present invention, form aluminium lamination on the first surface and comprise: deposited by electron beam evaporation sedimentation, thermal evaporation deposition method or magnetron sputtering deposition method form aluminium lamination in described first surface deposition.
In some embodiments of the present invention, anodized is carried out to described aluminium lamination and comprises: first time anodized is carried out to described aluminium lamination, described aluminium lamination is formed first alumina layer with multiple aperture; Remove described first alumina layer; Second time anodized is carried out to the described aluminium lamination after eliminating described first alumina layer, described aluminium lamination is formed second alumina layer with multiple aperture, and expanding treatment is carried out to the aperture in the second alumina layer.
In some embodiments of the present invention, first time anodized is carried out to described aluminium lamination and comprises: sulfuric acid or oxalic acid are dissolved in deionized water, obtain the first acid solution; The silicon substrate defining aluminium lamination be placed in described first acid solution and receive DC power anode, being energized for first schedule time.
In some embodiments of the present invention, remove described first alumina layer and comprise: the mixed solution of preparation phosphoric acid and chromic acid, obtains the second acid solution; The silicon substrate defining the first alumina layer is placed in described second acid solution, water-bath second schedule time, removes described first alumina layer.。
In some embodiments of the present invention, second time anodized is carried out to the described aluminium lamination after eliminating described first alumina layer and expanding treatment comprises: the silicon substrate after eliminating described first alumina layer is placed in described first acid solution and receives DC power anode, be energized for the 3rd schedule time, described aluminium lamination is formed second alumina layer with multiple aperture; Phosphoric acid is dissolved in deionized water, obtains the 3rd acid solution; The substrate defining the second alumina layer is placed in described 3rd acid solution, the 4th schedule time of corrosion.
In some embodiments of the present invention, on described aperture inwall, deposit carbon atomic layer comprises: with chemical vapour deposition technique at described aperture inwall deposit carbon atomic layer.
In some embodiments of the present invention, the diameter of described aperture is 40 to 100 nanometers, and the degree of depth of described aperture is 1 to 1.5 micron.
Additionally provide a kind of hydrogen gas sensor in embodiments of the invention, it is characterized in that, comprising: silicon substrate, described silicon substrate comprises first surface and the second surface relative with described first surface; Aluminium lamination, described aluminium lamination is formed on the first surface; Alumina layer, described alumina layer is formed on described aluminium lamination, forms multiple aperture in described alumina layer, and described aperture runs through described alumina layer, and the inwall of described aperture is formed with carbon atomic layer; Top electrode, described top electrode is formed on described alumina layer; Bottom electrode, described bottom electrode is formed on the second surface of described silicon substrate.
In some embodiments of the present invention, the diameter of described aperture is 40 to 100 nanometers, and the degree of depth of described aperture is 1 to 1.5 micron.
In embodiments of the invention, form the alumina layer with multiple aperture, and there is the alumina layer of multiple aperture for template with this, deposit carbon atom on the inwall of aperture, form carbon atomic layer.Like this, namely the aperture that each inwall deposited carbon atomic layer becomes a carbon nano-tube, and namely the array of so multiple apertures defines carbon nano pipe array.The surface of alumina layer forms top electrode, and this top electrode is connected with bottom electrode by the carbon nano pipe array formed like this.Utilize upper/lower electrode can measure the resistance of carbon nano-tube.This carbon nano-tube has very large specific surface area, and has high physical strength and good electrology characteristic, can detect the multiple gases such as ammonia, water vapour, nitrogen dioxide, oxygen.Therefore, the hydrogen gas sensor in embodiments of the invention has the advantages such as fast response time, reproducible, working temperature is low, structure is simple, volume is little, at room temperature to the hydrogen sensitive of 0.05%-2% volumetric concentration.In addition, the method technique of the manufacture hydrogen gas sensor of the embodiment of the present invention is simple, favorable repeatability.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the method for the manufacture hydrogen gas sensor of one embodiment of the invention.
Fig. 2 is the schematic diagram of the elevational sectional view of the hydrogen gas sensor of one embodiment of the invention.
Fig. 3 is the schematic top plan view of the hydrogen gas sensor of one embodiment of the invention.
Embodiment
The concrete steps of method of manufacture hydrogen gas sensor and the concrete structure of the hydrogen gas sensor of manufacture thereof of embodiments of the invention is described in detail below in conjunction with accompanying drawing.
Fig. 1 is the schematic flow sheet of the method for the manufacture hydrogen gas sensor of some embodiments of the invention.
As shown in Figure 1, in some embodiments of the present invention, in step 10, aluminium lamination can be formed on the first surface of silicon substrate.
In embodiments of the invention, in step 10, can provide silicon substrate, this silicon substrate can be that (such as, doping content is 1 × 10 in heavy doping
18-10
20cm
-3) N-type silicon chip.This silicon substrate can be sheet, can comprise two major surfaces (surface that namely area is large) respect to one another, be referred to as the first performance and the second surface relative with first surface herein.Then, aluminium lamination can be formed on the first surface of silicon substrate.This aluminium lamination can by being formed metallic aluminium deposition by multiple applicable method on the first surface.Such as, in some embodiments, electron beam vapor deposition method can be used, thermal evaporation deposition method or magnetron sputtering deposition method etc. method deposits formation aluminium lamination on the first surface.Electron beam vapor deposition method, thermal evaporation deposition method and magnetron sputtering deposition method can be deposition processs conventional in this area, are not described in detail in this.
In some embodiments, the thickness of this aluminium lamination can be 2.5 to 3 microns.If this aluminium lamination is too thin, then just easily all oxidized during anodic oxidation hereinafter described, thus cause easily coming off; And if this aluminium lamination is too thick, can need long in the time of silicon substrate deposited aluminum layer.Inventor finds, preferably thickness range scope for this reason.
After defining aluminium lamination on a silicon substrate, in step 20, anodized can be carried out to this aluminium lamination, thus a part for this aluminium lamination is oxidized, formed and there is the alumina layer of multiple aperture, and these apertures run through aluminium lamination that alumina layer contacts with alumina layer to top (also i.e. the aluminium lamination of not oxidized one-tenth aluminium oxide in anodized).In some embodiments, twice anodised method can be used to form the alumina layer that this has multiple aperture.
Such as, in some embodiments, first can carry out first anode oxidation processes to aluminium lamination.Such as, in some embodiments, can sulfuric acid, phosphoric acid or oxalic acid be dissolved in deionized water, obtain the first acid solution.Then, the silicon substrate defining aluminium lamination be placed in this first acid solution and receive the positive pole of direct supply, with the metal material be applicable to (such as, platinum) as negative pole, be energized for first schedule time, in this process, aluminium lamination will produce nanoassemble process, thus on aluminium lamination, form the alumina layer with multiple aperture.
In these embodiments, the concentration of the first acid solution can be 0.3-0.5 mol/L (mol/L).The anode voltage (i.e. the voltage at aluminium lamination place on a silicon substrate) used can be 30 to 40 volts.This first schedule time (time be namely energized also is the time that electrochemical oxidation carries out) can be 1-2 hour.
Then, this first alumina layer can be removed.
Such as, in some embodiments, the mixed solution of phosphoric acid and chromic acid can be prepared, obtain the second acid solution, then the silicon substrate defining the first alumina layer is placed in this second acid solution, at a predetermined temperature water-bath second schedule time, thus erosion removal first alumina layer.Because the bottom shape of the aperture in the first alumina layer is normally hemispheric, after therefore removing the first alumina layer, the aluminium lamination that the little pit corresponding with the bottom shape of aperture can be stayed on the surface.The high systematicness of aperture that these regularly arranged pits will be conducive in the second alumina layer that hereinafter described second time anodized formed.
In these embodiments, the concentration of the second acid solution can be phosphoric acid quality mark 5-7%, chromic acid massfraction 1.5-1.8%.Aforesaid predetermined temperature can be 60-70 DEG C.Aforesaid second schedule time can be 1.5-2 hour.
Then, second time anodized can be carried out to the aluminium lamination eliminated after the first alumina layer, aluminium lamination be formed second alumina layer with multiple apertures of high-sequential, and expanding treatment is carried out to the aperture in the second alumina layer.
In some embodiments, the method for second time anodized can use the electrochemical anodic oxidation method similar with first time anode oxidative treatment method.Such as, in some embodiments, silicon substrate after eliminating the first alumina layer can be placed in aforesaid first acid solution and receive DC power anode, the 3rd schedule time of energising, thus on aluminium lamination, forming second alumina layer with multiple apertures of high-sequential.Then, can phosphoric acid be dissolved in deionized water, obtain the 3rd acid solution, and the substrate defining the second alumina layer is placed in the 3rd acid solution, the 4th schedule time of corrosion, thus make aperture reaming.
In some embodiments of the present invention, aforesaid 3rd schedule time can be 0.5-1 hour, and the concentration of aforesaid 3rd acid solution can be the massfraction of phosphoric acid is 2-5%, and aforesaid 4th schedule time can be 10-30 minute.
Like this, by aforesaid twice anodised process, the alumina layer of multiple apertures (such as, array of orifices) with high-sequential can be formed.
In some embodiments of the present invention, the diameter of the aperture of formation can be 40 to 100 nanometers, and the degree of depth of aperture can be 1 to 1.5 micron.In some embodiments, the shape of cross section of the aperture of formation can be circular, and such as can arrange by hexagonal cell shape between these apertures.
Define these apertures in alumina layer after, in step 40, formation carbon atomic layer can be deposited on the inwall of these apertures.Such as, in some embodiments, can deposit on these aperture inwalls with chemical vapour deposition technique and form carbon atomic layer.
In some embodiments, single injection or bi-injection method can be adopted, utilize ethanol for carbon source, ferrocene is catalyst precursor, using the aforesaid alumina layer defining multiple aperture as template, in quartz ampoule at 800 DEG C reactive deposition, now, alcohol catalysis is cracked into carbon atom, is deposited on hole wall, thus deposition forms carbon atomic layer on aperture inwall.The aperture that each inwall deposited carbon atomic layer can be formed as a carbon nano-tube.In multiple aperture inwalls in alumina layer, deposition forms carbon atomic layer, namely defines multiple carbon nano-tube, thus obtains the array of carbon nano-tube.
Such as, in some embodiments, ferrocene and the alcohol mixed solution (ethanol is solvent) of 0.0125g/ml can be prepared, ultrasonic process makes to mix, then the alumina layer (i.e. aforesaid silicon substrate) defining multiple aperture is placed on the quartzy thin slice in quartz ampoule, after furnace temperature rises to 800 DEG C, by syringe under the control of computer micro-injection pump, continuously carbon source (ethanol) and catalyzer (ferrocene) note are reacted in quartz ampoule reaction chamber with rate of injection 10ml/h, argon flow amount 1000sccm.
In some embodiments of the present invention, in step 50, top electrode and bottom electrode can be formed.Such as, bottom electrode can be formed on the second surface of silicon substrate, and form carbon nano pipe array one-tenth in step 40 on aperture inwall after, alumina layer form top electrode.
In some embodiments of the present invention, can deposit on alumina layer with magnetron sputtering method and form palladium layers, this palladium layers is top electrode.In some embodiments, the thickness of palladium layers can be 3-to 60 nanometer.
In some embodiments of the present invention, deposited by electron beam evaporation deposition process, thermal evaporation deposition method or magnetron sputtering deposition method etc. can deposit on a second surface and form metal level, then anneal in a nitrogen atmosphere, form Ohmic contact.This metal level is bottom electrode.In some embodiments, this metal level can be aluminium lamination, molybdenum layer or titanium layer etc.
Like this, through aforesaid step, namely make hydrogen gas sensor of the present invention.
Fig. 2 and Fig. 3 show schematically show the hydrogen gas sensor that method according to some embodiments of the invention manufactures.As shown in Figures 2 and 3, in some embodiments, hydrogen gas sensor comprises silicon substrate 2, aluminium lamination 3, alumina layer 4, top electrode 6 and bottom electrode 1.
Silicon substrate 2 comprises first surface (surface on the upside of in Fig. 2) and the second surface relative with first surface (surface on the downside of in Fig. 2).Aluminium lamination 3 is formed on the first surface of silicon substrate 2.Alumina layer 4 is formed on aluminium lamination 3.Form multiple aperture 7 in alumina layer 4, the inwall of these apertures 7 is formed with carbon atomic layer 5.
Top electrode 6 is formed on alumina layer 4.Bottom electrode 1 is formed on the second surface of silicon substrate 2.
As mentioned before, in some embodiments, the diameter of these apertures can be 40 to 100 nanometers, and the degree of depth of these apertures can be 1 to 1.5 micron.These apertures can be arranged in the hexagonal cell shape of rule.
In embodiments of the invention, form the alumina layer surface with multiple aperture and form top electrode, and there is the alumina layer of multiple aperture for template with this, deposit carbon atom on the inwall of aperture, form carbon atomic layer.Like this, namely the aperture that each inwall deposited carbon atomic layer becomes a carbon nano-tube, and namely the array of so multiple apertures defines carbon nano pipe array.The top electrode of alumina layer is connected with bottom electrode by the carbon nano pipe array layer formed like this.Utilize upper/lower electrode can measure the resistance of carbon nano-tube.This carbon nano-tube has very large specific surface area, and has high physical strength and good electrology characteristic, can detect the multiple gases such as ammonia, water vapour, nitrogen dioxide, oxygen.Therefore, the hydrogen gas sensor in embodiments of the invention has the advantages such as fast response time, reproducible, working temperature is low, volume is little, at room temperature to the hydrogen sensitive of 0.05%-2% volumetric concentration.In addition, the method technique of the manufacture hydrogen gas sensor of the embodiment of the present invention is simple, favorable repeatability.
Described the present invention by specific embodiment above, but the present invention is not limited to these specific embodiments.It will be understood by those skilled in the art that and can also make various amendment, equivalent replacement, change etc. to the present invention, as long as these conversion do not deviate from spirit of the present invention, all should within protection scope of the present invention.In addition, " embodiment " described in above many places represents different embodiments, can certainly by its all or part of combination in one embodiment.
Claims (10)
1. manufacture a method for hydrogen gas sensor, it is characterized in that, comprising:
There is provided silicon substrate, described silicon substrate comprises first surface and the second surface relative with described first surface;
Form aluminium lamination on the first surface;
Anodized is carried out to described aluminium lamination, described aluminium lamination is formed the alumina layer with multiple aperture, and described aperture runs through described alumina layer;
Deposit carbon atomic layer on described aperture inwall, wherein inwall deposited the keyhole formation carbon nano-tube of carbon atomic layer;
Described alumina layer forms top electrode;
The second surface of described silicon substrate forms bottom electrode.
2. the method for claim 1, is characterized in that, forms aluminium lamination on the first surface and comprises: deposited by electron beam evaporation sedimentation, thermal evaporation deposition method or magnetron sputtering deposition method form aluminium lamination in described first surface deposition.
3. method as described in claim 1 or 2, is characterized in that, carry out anodized comprise described aluminium lamination:
First time anodized is carried out to described aluminium lamination, described aluminium lamination is formed first alumina layer with multiple aperture;
Remove described first alumina layer;
Second time anodized is carried out to the described aluminium lamination after eliminating described first alumina layer, described aluminium lamination is formed second alumina layer with multiple aperture, and expanding treatment is carried out to the aperture in the second alumina layer.
4. method as claimed in claim 3, is characterized in that, carries out first time anodized comprise described aluminium lamination:
Sulfuric acid, phosphoric acid or oxalic acid are dissolved in deionized water, obtain the first acid solution;
The silicon substrate defining aluminium lamination be placed in described first acid solution and receive DC power anode, being energized for first schedule time.
5. the method as described in claim 3 or 4, is characterized in that, removes described first alumina layer and comprises:
The mixed solution of preparation phosphoric acid and chromic acid, obtains the second acid solution;
The silicon substrate defining the first alumina layer is placed in described second acid solution, water-bath second schedule time, removes described first alumina layer.
6. method as claimed in claim 4, is characterized in that, carries out second time anodized and expanding treatment comprises to the described aluminium lamination after eliminating described first alumina layer:
Silicon substrate after eliminating described first alumina layer is placed in described first acid solution and receives DC power anode, the 3rd schedule time of energising, described aluminium lamination is formed second alumina layer with multiple aperture;
Phosphoric acid is dissolved in deionized water, obtains the 3rd acid solution;
The substrate defining the second alumina layer is placed in described 3rd acid solution, the 4th schedule time of corrosion.
7. as the method in claim 1 to 6 as described in any one, it is characterized in that, on described aperture inwall, deposit carbon atomic layer comprises: with chemical vapour deposition technique deposit carbon atomic layer on described aperture inwall.
8. method as claimed in any of claims 1 to 7 in one of claims, is characterized in that: the diameter of described aperture is 40 to 100 nanometers, and the degree of depth of described aperture is 1 to 1.5 micron.
9. a hydrogen gas sensor, is characterized in that, comprising:
Silicon substrate, described silicon substrate comprises first surface and the second surface relative with described first surface;
Aluminium lamination, described aluminium lamination is formed on the first surface;
Alumina layer, described alumina layer is formed on described aluminium lamination, forms multiple aperture in described alumina layer, and described aperture runs through described alumina layer, and the inwall of described aperture is formed with carbon atomic layer;
Top electrode, described top electrode is formed on described alumina layer;
Bottom electrode, described bottom electrode is formed on the second surface of described silicon substrate.
10. hydrogen gas sensor as claimed in claim 9, is characterized in that: the diameter of described aperture is 40 to 100 nanometers, and the degree of depth of described aperture is 1 to 1.5 micron.
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| CN107748188A (en) * | 2017-09-12 | 2018-03-02 | 电子科技大学 | The flexible hydrogen sensor of dense uniform nano-micro structure based on Pd films |
| CN109187660A (en) * | 2018-08-23 | 2019-01-11 | 电子科技大学 | A kind of semi-conductor type hydrogen gas sensor based on graphene reticular structure |
| CN111208059A (en) * | 2020-02-11 | 2020-05-29 | 南京信息工程大学 | Optical fiber hydrogen sensor based on core/shell nano periodic line array plasma metamaterial |
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