CN104374810B - Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt - Google Patents
Method for preparing hydrogen sensitive element based on quadrature-phase molybdenum oxide nano-belt Download PDFInfo
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Abstract
The invention provides a method for preparing a hydrogen sensitive element based on a quadrature-phase molybdenum oxide nano-belt. The method comprises the following steps: A, a quadrature-phase molybdenum oxide nano-belt powder by a hydrothermal method; B, preparing an interdigital electrode by a photolithographic mask method; and C assembling a hydrogen sensitive element, namely molybdenum oxide powder and an absolute ethyl alcohol mixed liquid, carrying out ultrasonic treatment, dropwise adding the mixed liquid into the center position of the interdigital electrode, and annealing. According to the method, Na2MoO4.2H20 is used as a raw material, the quadrature-phase molybdenum oxide nano-belt with uniform appearance is prepared by adopting the simple hydrothermal method, the using process is simple, the preparation cycle is short, the sample yield is high, and the cost is low; the nano-belt dispersed by ultrasonics is coated to the interdigital electrode to obtain the hydrogen sensitive element with excellent performance; at room temperature, the element has the characteristics of high sensitivity and quick response on low-concentration hydrogen, has excellent repeatability and selectivity on hydrogen, and can meet the requirement of quickly detecting low-concentration hydrogen.
Description
Technical field
The present invention relates to the preparation of metal oxide 1-dimention nano semi-conducting material and gas sensitization technical field, more particularly, to
A kind of hydrogen sensitive part making method based on orthorhombic phase molybdenum oxide nanobelt.
Background technology
Hydrogen is described as the clean energy resource of 21 century, has high combustion efficiency, the advantages of product is pollution-free.Simultaneously as one
Plant reducibility gas and carrier gas, be widely used in the numerous areas such as chemical industry, medicine, medical treatment, aviation, metal smelt, especially
It is also to have particularly important using value in modern national defense field.But due to hydrogen molecule very little, hydrogen colorless and odorless, in reality
Produce, transport and easily leaked using process, and be difficult to be therefore easily perceived by humans.When the hydrogen content of in the air reaches 4%,
Meet naked light will explode, thus using hydrogen gas sensor the content of hydrogen in environment is carried out on-line checking and it is leaked into
Row monitoring, alarming seems extremely important.
The more class hydrogen gas sensors of research are metal-oxide semiconductor (MOS) (TiO at present2With ZnO etc.) hydrogen sensing
Device, this kind of sensor is to change to realize the prison to density of hydrogen using the resistance value of Sensitive Apparatus in the hydrogen gas atmosphere
Survey.But the room temperature hydrogen sensitivity of the hydrogen sensor of current report can be unsatisfactory, the response time generally long (>60s), absolutely
Most of hydrogen gas sensor will higher temperature (>200 DEG C) just can show to hydrogen preferable response, this is to a great extent
Limit the range of application of sensors with auxiliary electrode, and also improve cost to a certain extent.Molybdenum trioxide (MoO3) it is a class weight
The functional material wanted, in electrochromic device, gas sensor, photocatalysis, Flied emission, lithium ion battery and solar cell etc.
A series of fields have all shown greatly using value.It is reported that, semiconductor oxide molybdenum film is to NO, NO2、CO、H2And NH3
Show good hydrogen sensitive characteristic in 300-600 DEG C of environment, but higher operating temperature increased the damage of the energy
Consumption, also limit the popularization and application of molybdenum oxide Sensitive Apparatus simultaneously.The synthesis MoO of document report at present3The method of nanobelt is relatively
Few, mainly include hydro-thermal method, direct oxidation method and thermal evaporation.2002, Lou Xiongwen et al. was with ammonium heptamolybdate and nitre
Acid is raw material, and under conditions of 170-180 DEG C, hydro-thermal reaction 30-40h has synthesized the nanobelt that length is tens microns.2006
Year, civilian bell-shaped percussion instrument, used in ancient time by troops on march et al., with molybdenum foil as raw material, prepares MoO at 850 DEG C by thermal oxidation process3Nanobelt.2013, Bai Shouli
Et al. with molybdenum salt as raw material, under the conditions of 80-120 DEG C of electromagnetic agitation reaction 1-3h prepare length about 1.5-2.0 micron
Nanobelt.But forefathers prepare MoO3Appearance of nano material is relatively rough, and process repeatability is poor, and the preparation side having
Method cost is higher, is not suitable for producing in a large number.Therefore find a kind of practical and simple to operate, stable preparation process, with
Shi Shihe controllable growth MoO3The method of nanobelt is necessary.Utilize MoO simultaneously3Nanobelt high-specific surface area and excellent electricity
Sub- radial migration performance, is expected to improve the hydrogen sensitivity energy of room temperature lower semiconductor type hydrogen element, it is to avoid complicated heating in device
Size and power problemses that element brings, effectively reduce and produce and testing cost.
Content of the invention
The purpose of the present invention aims to provide a kind of hydrogen sensitive part making method based on orthorhombic phase molybdenum oxide nanobelt.
The step of this hydrogen sensitive part making method is as follows：
Step A：The preparation of molybdenum oxide nanobelt
1) in 25-500ml reaction vessel, by Na2MoO4·2H2O is added in deionized water, and the concentration of molybdenum element is about
For 0.1-2.5mol/L, it is slowly stirred and so that molybdenum salt is fully dissolved；
2) under electromagnetic agitation, 65% red fuming nitric acid (RFNA) is poured slowly in above-mentioned solution, forms acid solution, concentration of nitric acid
For 0.01-5mol/L；
3) after being sufficiently mixed, above-mentioned solution is transferred in hydrothermal reaction kettle, react 1- at a temperature of 120-300 DEG C
72h；
4), after question response terminates, reactor is air cooled to room temperature, filtration separation, 5-24h is dried at 40-80 DEG C and just can get
Hand over phase molybdenum trioxide nano band powder.
Step B：The preparation of electrode
1) mask blank makes：Using L-edit Software for Design interdigital electrode predetermined pattern, and the clear microelectronics with Nanjing
Technology Co., Ltd customized Cr layer photo mask board, wherein single interdigital electrode pattern dimension is 1cm × 1cm, and it is interdigital
10-50 μm of width of fringe and spacing 1-10 μm, its interdigital striped quantity 10-50, described interdigital electrode pattern equably repeats
It is arranged in the square scope of length of side 70mm.
2) substrate cleaning：By oxidated layer thickness for 10nm single-sided polishing SiO2/ Si piece is cut into the little of 1.5cm × 1.5cm
Piece, successively uses acetone, absolute ethyl alcohol and deionized water to be cleaned by ultrasonic 10-30min, then the in the air in temperature 40-60 DEG C is dried
Dry 20-30min.
3) spin coating photoresist：In step 2) one layer of photoresist of spin coating on the drying substrate that obtains, then in temperature 98-102
Dry 1-3min at DEG C, then put step 1) mask blank that makes, by described interdigital electrode pattern and described substrate pair
Together.
According to the present invention, described photoresist is the type photoresist such as AZ5214-E, A21500, A26112, and they are all
The product sold in the market.
4) mask exposure：Step 3) the spin coating photoresist substrate that obtains exposes 2-6s in the enterprising line mask of litho machine, then
Dry 1-3min at temperature 98-102 DEG C, then cool down 2-4min at room temperature, then carry out maskless lithography 5-10s, two
Secondary exposure development 15-40s followed by developer solution, is washed down with ultra-pure water thereafter, stand-by after drying up.
Described developer solution model400K、300 grade developer solutions, using 0.26N/2.38%TMAH (tetramethyl
Base ammonium hydroxide) standard recipe.
Described ultra-pure water is it should be understood that meet China national use for laboratory water specification GB6682-92.
5) adopt standard direct current magnetron sputtering technique, successively sputter under conditions of Ar atmosphere and 70W sputtering power Ti and
Pt, their deposit thickness is 10-50nm Ti and 40-200nm Pt respectively.
Step C：The constructing of hydrogen sensitive element
1) measure 2-10l absolute ethyl alcohol using liquid-transfering gun to be added in centrifuge tube, weigh 10-100mg molybdenum oxide powder and add
Enter in aforesaid liquid；
2) ultrasonically treated 2-20min, supersonic frequency is 40-100Hz；
3) ultrasonically treated finish after, measure the above-mentioned mixed liquor of 1-3l using liquid-transfering gun and be added drop-wise to interdigital electrode centre；
4) obtained device is annealed under conditions of vacuum is for 0.0001-0.01Pa
Process, annealing temperature is 100-300 DEG C, annealing time is 1-10h.
The present invention is with Na2MoO4·2H2O is raw material, has prepared the uniform orthorhombic phase of pattern using simple hydrothermal method
Molybdenum oxide nanobelt, short preparation period fairly simple using equipment, yield is high, with low cost.Will by a kind of simple method
Nanobelt after ultrasonic disperse is coated in interdigital electrode, obtains the hydrogen sensitive element of excellent properties.Under room temperature, this element
Low-concentration hydrogen is shown with highly sensitive and quick response feature, to hydrogen, there is good repeatability and selectivity simultaneously,
The requirement of quick detection low-concentration hydrogen can be met.
Brief description
Fig. 1 is the X ray diffracting spectrum of example 1,2,3,4 gained molybdenum oxide nanobelt, and wherein a, b, c, d is hydro-thermal reaction
Temperature is respectively the XRD spectrum of 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C gained molybdenum oxide nanobelts；
Fig. 2 is the SEM figure of example 1,2,3,4 gained molybdenum oxide nanobelt；Wherein a, b, c, d are hydrothermal temperature difference
SEM figure for 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C gained molybdenum oxide nanobelts；
Fig. 3 is the single MoO of example 4 gained3The micro-structural tem analysis result of nanobelt；
Fig. 4 be the response curve to 500ppm hydrogen for example 1,2,3, the 4 gained molybdenum oxide nanobelt network, wherein a, b,
C, d be hydrothermal temperature be respectively 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C of gained molybdenum oxide nanobelts are to 500ppm hydrogen
Response diagram；
Fig. 5 is the response curve to variable concentrations hydrogen for the embodiment 4 gained nanometer line network；
Fig. 6 be embodiment 4 gained nanometer line network to the repeatability of hydrogen and selectivity test result, wherein a is air-sensitive
The reperformance test result to hydrogen for the element；B is the selectivity test result of gas sensor.
Specific embodiment
With reference to instantiation, further illustrate the present invention, but described embodiment is only that a present invention part is real
Apply example, rather than whole embodiments.
Embodiment 1：
The preparation A of molybdenum oxide nanobelt
1) in 50ml reaction vessel, by 2.4195g Na2MoO4·2H2O is added in 32.75ml deionized water, molybdenum unit
The concentration of element is about 0.305mol/L, is slowly stirred and so that molybdenum salt is fully dissolved；
2) under electromagnetic agitation, the 65% of 6.25ml red fuming nitric acid (RFNA) is poured slowly in above-mentioned solution, forms acid solution,
Concentration of nitric acid is 2.5mol/L；
3) after being sufficiently mixed, above-mentioned solution is transferred in hydrothermal reaction kettle, react 12h at a temperature of 120 DEG C；
4), after question response terminates, reactor is air cooled to room temperature, filtration separation, 10h is dried at 70 DEG C and can get orthorhombic phase
Molybdenum trioxide nano band powder.
Embodiment 2：
The preparation B of molybdenum oxide nanobelt
1) in 50ml reaction vessel, by 2.4195g Na2MoO4·2H2O is added in 32.75ml deionized water, molybdenum unit
The concentration of element is about 0.305mol/L, is slowly stirred and so that molybdenum salt is fully dissolved；
2) under electromagnetic agitation, the 65% of 6.25ml red fuming nitric acid (RFNA) is poured slowly in above-mentioned solution, forms acid solution,
Concentration of nitric acid is 2.5mol/L；
3) after being sufficiently mixed, above-mentioned solution is transferred in hydrothermal reaction kettle, react 12h at a temperature of 160 DEG C DEG C；
4), after question response terminates, reactor is air cooled to room temperature, filtration separation, 10h is dried at 70 DEG C and can get orthorhombic phase
Molybdenum trioxide nano band powder.
Embodiment 3：
The preparation C of molybdenum oxide nanobelt
1) in 50ml reaction vessel, by 2.4195g Na2MoO4·2H2O is added in 32.75ml deionized water, molybdenum unit
The concentration of element is about 0.305mol/L, is slowly stirred and so that molybdenum salt is fully dissolved；
2) under electromagnetic agitation, the 65% of 6.25ml red fuming nitric acid (RFNA) is poured slowly in above-mentioned solution, forms acid solution,
Concentration of nitric acid is 2.5mol/L；
3) after being sufficiently mixed, above-mentioned solution is transferred in hydrothermal reaction kettle, react 12h at a temperature of 180 DEG C；
4), after question response terminates, reactor is air cooled to room temperature, filtration separation, 10h is dried at 70 DEG C and can get orthorhombic phase
Molybdenum trioxide nano band powder.
Embodiment 4：
The preparation D of molybdenum oxide nanobelt
1) in 50ml reaction vessel, by 2.4195g Na2MoO4·2H2O is added in 32.75ml deionized water, molybdenum unit
The concentration of element is about 0.305mol/L, is slowly stirred and so that molybdenum salt is fully dissolved；
2) under electromagnetic agitation, the 65% of 6.25ml red fuming nitric acid (RFNA) is poured slowly in above-mentioned solution, forms acid solution,
Concentration of nitric acid is 2.5mol/L；
3) after being sufficiently mixed, above-mentioned solution is transferred in hydrothermal reaction kettle, react 12h at a temperature of 200 DEG C；
4), after question response terminates, reactor is air cooled to room temperature, filtration separation, 10h is dried at 70 DEG C and can get orthorhombic phase
Molybdenum trioxide nano band powder.
The X ray diffracting spectrum of gained powder is shown in Fig. 1, and analysis result shows the orthorhombic phase oxygen that products therefrom is high-crystallinity
Change molybdenum；Its SEM result as shown in Figures 2 and 3, the length ＞ 10m of molybdenum oxide nanobelt, width is about 100-
500nm, thickness is 30-80nm.
Embodiment 5
A：The preparation of electrode
1) mask blank makes：Using L-edit Software for Design interdigital electrode predetermined pattern, and the clear microelectronics with Nanjing
Technology Co., Ltd customized Cr layer photo mask board, wherein single interdigital electrode pattern dimension is 1cm × 1cm, and it is interdigital
Width of fringe 10m and spacing 5m, its interdigital striped quantity 20, described interdigital electrode pattern equably repeats to be arranged in the length of side
In the square scope of 70mm.
2) substrate cleaning：By oxidated layer thickness for 10nm twin polishing SiO2/ Si piece is cut into the little of 1.5cm × 1.5cm
Piece, successively uses acetone, absolute ethyl alcohol and deionized water to be cleaned by ultrasonic 15min, and then the in the air in 40 DEG C of temperature is dried
30min.
3) spin coating photoresist：The KW-4A type sol evenning machine being produced using Microelectronic Institute of the Chinese Chinese Academy of Sciences, in step 2)
To dropping volume on substrate of drying be the photoresist of 100L, then at 100 DEG C of temperature, dry 2min, then put step 1) make
Mask blank, by described interdigital electrode pattern and described substrate alignment.
4) mask exposure：Step 3) the spin coating photoresist substrate that obtains produce in ABM.lnc (China branch company) depth/
The enterprising line mask of middle ultraviolet photolithographic machine exposes 3s, then dries 1.5min at 100 DEG C of temperature, then cools down 3min at room temperature,
Then carry out maskless lithography 10s, in the 25s that develops followed by developer solution that double exposes, washed down with ultra-pure water thereafter, dry up
Stand-by afterwards.5) adopt standard direct current magnetron sputtering technique, using Shenyang Scientific Instrument Research ＆ Mfg. Center Co., Ltd., C.A.S
The JGPH50 type high vacuum magnetic control sputtering device producing, in Ar atmosphere and 70W sputtering power, background vacuum 4 × 10-4Pa, sputtering
Ti and Pt is successively sputtered, their deposit thickness is respectively under conditions of successively splashing under conditions of air pressure 0.5Pa, target-substrate distance 4cm
30nm Ti and 100nm Pt.
B：The constructing of hydrogen sensitive element
1) prepare the centrifuge tube that 4 volumes are 2.5ml, measure 5l absolute ethyl alcohol using liquid-transfering gun and be added in centrifuge tube,
Weigh 50mg example 1 respectively, example 2, example 3, example 4 gained molybdenum oxide powder are added in aforesaid liquid；
2) ultrasonically treated 5min, supersonic frequency is 100Hz；
3) ultrasonically treated finish after, measure the above-mentioned mixed liquor of 2l using liquid-transfering gun and be added drop-wise to respectively in 4 interdigital electrodes
Center portion position；
4) obtained device is made annealing treatment under conditions of vacuum is for 0.001Pa, annealing temperature is 200 DEG C, moves back
The fiery time is 2h, and heating rate is 5 DEG C/min.Hydrogen sensitive element is just can get when it is cooled to room temperature.
By the element preparing as in test cavity, set constant operating voltage as 1V, by testing it to be measured
The resistance of gas and in the air is weighing its hydrogen sensitivity energy.For reducibility gas (CO, C2H5OH、CH3COCH3), sensitivity is fixed
Justice is the element ratio with difference under test gas for the element and element resistance in atmosphere in atmosphere.
Claims (1)
1. a kind of hydrogen sensitive part making method based on orthorhombic phase molybdenum oxide nanobelt is it is characterised in that step is as follows：
Step A：The preparation of molybdenum oxide nanobelt
1) in 25-500ml reaction vessel, by Na2MoO4·2H2O is added in deionized water, and the concentration of molybdenum element is about
0.1-2.5mol/L, is slowly stirred and so that molybdenum salt is fully dissolved；
2) under electromagnetic agitation, 65% red fuming nitric acid (RFNA) is poured slowly into step A 1) in solution, form acid solution, concentration of nitric acid
For 0.01-5mol/L；
3) after being sufficiently mixed, by step A 2) solution transfers in hydrothermal reaction kettle, reacts 1- at a temperature of 120-300 DEG C
72h；
4), after question response terminates, reactor is air cooled to room temperature, filtration separation, 5-24h is dried at 40-80 DEG C and can get orthorhombic phase
Molybdenum trioxide nano band powder；
Step B：The preparation of electrode
1) mask blank makes：Using L-edit Software for Design interdigital electrode predetermined pattern, wherein single interdigital electrode pattern
A size of 1cm × 1cm, 10-50 μm of its interdigital width of fringe and spacing 1-10 μm, its interdigital striped quantity 10-50, described fork
Refer in the square scope that electrode pattern equably repeats be arranged in length of side 70mm；
2) substrate cleaning：By oxidated layer thickness for 10nm single-sided polishing SiO2/ Si piece is cut into the small pieces of 1.5cm × 1.5cm, first
It is cleaned by ultrasonic 10-30min with acetone, absolute ethyl alcohol and deionized water respectively afterwards, then the in the air in temperature 40-60 DEG C is dried
20-30min；
3) spin coating photoresist：In step B 2) one layer of photoresist of spin coating on the drying substrate that obtains, then in temperature 98-102 DEG C
Lower baking 1-3min, then put step B 1) mask blank that makes, by described interdigital electrode pattern and described substrate pair
Together；
4) mask exposure：Step B 3) the spin coating photoresist substrate that obtains exposes 2-6s in the enterprising line mask of litho machine, then exists
Dry 1-3min at temperature 98-102 DEG C, then cool down 2-4min at room temperature, then carry out maskless lithography 5-10s, twice
Exposure development 15-40s followed by developer solution, is washed down with ultra-pure water thereafter, stand-by after drying up；
5) adopt standard direct current magnetron sputtering technique, under conditions of Ar atmosphere with 70W sputtering power, successively sputter Ti and Pt, it
Deposit thickness be 10-50nm Ti and 40-200nm Pt respectively；
Step C：The constructing of hydrogen sensitive element
1) measure 2-10 μ l absolute ethyl alcohol using liquid-transfering gun to be added in centrifuge tube, weigh the orthorhombic phase three of 10-100mg step A
Molybdenum oxide nanometer powder is added in absolute ethyl alcohol liquid；
2) ultrasonically treated 2-20min, supersonic frequency is 40-100Hz；
3) ultrasonically treated finish after, measure 1-3 μ l step C 1 using liquid-transfering gun) mixed liquor be added drop-wise to the interdigital electrode of step B
Centre；
4) obtained device is made annealing treatment under conditions of vacuum is for 0.0001-0.01Pa, annealing temperature is 100-300
DEG C, annealing time is 1-10h.
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| CN112881476B (en) * | 2021-01-20 | 2022-06-28 | 湖北大学 | Response type adjustable two-dimensional semiconductor room temperature hydrogen sensor and manufacturing method thereof |
| CN115558897A (en) * | 2022-09-13 | 2023-01-03 | 华中科技大学 | Gas sensor and preparation method and application thereof |
| CN116046852A (en) * | 2023-01-17 | 2023-05-02 | 云南民族大学 | High-performance ethanol gas sensor of ZnO nanoparticle modified alpha-molybdenum trioxide heterojunction |
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