CN104374810A - 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 semiconductor material and gas sensitization technical field, particularly relate to a kind of hydrogen sensitive part making method based on orthorhombic phase molybdena nanobelt.
Background technology
The advantages such as hydrogen is described as the clean energy resource of 21 century, has burning efficiency high, and product is pollution-free.Simultaneously as a kind of reducibility gas and carrier gas, be widely used in the numerous areas such as chemical industry, medicine, medical treatment, aviation, metal smelt, particularly also had very important using value in modern national defense field.But because hydrogen molecule is very little, hydrogen colorless and odorless, very easily leaks in actual production, transport and use procedure, and is not easily therefore easily perceived by humans.When the hydrogen content in air reaches 4%, meeting naked light will blast, therefore utilizes hydrogen gas sensor to carry out on-line checkingi to the content of hydrogen in environment and leak it and carry out monitoring, alarming and seem extremely important.
The many class hydrogen gas sensor of current research is metal-oxide semiconductor (MOS) (TiO
2with ZnO etc.) hydrogen gas sensor, this kind of sensor utilizes the resistance value of Sensitive Apparatus in the hydrogen gas atmosphere to change to realize the monitoring to density of hydrogen.But the room temperature hydrogen sensitivity of the hydrogen sensor of report can be unsatisfactory at present, response time is long (>60s) generally, overwhelming majority hydrogen gas sensor just will can show at higher temperature (>200 DEG C) and respond preferably hydrogen, which greatly limits the range of application of sensors with auxiliary electrode, and also improve cost to a certain extent.Molybdenum trioxide (MoO
3) be the important functional material of a class, all show greatly using value in a series of fields such as electrochromic device, gas sensor, photocatalysis, Flied emission, lithium ion battery and solar cells.It is reported, semiconductor oxide molybdenum film is to NO, NO
2, CO, H
2and NH
3in the environment of 300-600 DEG C, show good hydrogen sensitive characteristic, but higher working temperature adds the loss of the energy, also limit applying of molybdena Sensitive Apparatus simultaneously.The synthesis MoO of current bibliographical information
3the method of nanobelt is less, mainly comprises hydro-thermal method, direct oxidation method and thermal evaporation.2002, the people such as Lou Xiongwen for raw material, synthesized at the Water Under thermal response 30-40h of 170-180 DEG C the nanobelt that length is tens microns with ammonium heptamolybdate and nitric acid.2006, the people such as a civilian bell-shaped percussion instrument, used in ancient time by troops on march took molybdenum foil as raw material, prepare MoO at 850 DEG C by thermal oxidation process
3nanobelt.2013, the people such as Bai Shouli for raw material with molybdenum salt, reacted 1-3h and prepare the nanobelt that length is about 1.5-2.0 micron under the electromagnetic agitation condition of 80-120 DEG C.But forefathers prepare MoO
3appearance of nano material is more coarse, and process repeatability is poor, and some preparation method's cost compares are high, are not suitable for a large amount of production.Therefore find a kind of practical, and simple to operate, and stable preparation process, is applicable to controllable growth MoO simultaneously
3the method of nanobelt is necessary.Utilize MoO simultaneously
3the electronics radial migration performance of nanobelt high-ratio surface sum excellence, be expected to the hydrogen sensitivity energy improving room temperature lower semiconductor type hydrogen element, the size avoiding heating element complicated in device to bring and power problems, effectively reduce and produce and testing cost.
Summary of the invention
Object of the present invention aims to provide a kind of hydrogen sensitive part making method based on orthorhombic phase molybdena nanobelt.
The step of this hydrogen sensitive part making method is as follows:
Steps A: the preparation of molybdena nanobelt
1) in 25-500ml reaction vessel, by Na
2moO
42H
2o joins in deionized water, and the concentration of molybdenum element is about 0.1-2.5mol/L, slowly stirs and molybdenum salt is fully dissolved;
2) under electromagnetic agitation, be slowly poured into by the red fuming nitric acid (RFNA) of 65% in above-mentioned solution, form acid solution, concentration of nitric acid is 0.01-5mol/L;
3) after fully mixing, above-mentioned solution is transferred in hydrothermal reaction kettle, at 120-300 DEG C of temperature, reacts 1-72h;
4) after question response terminates, by reactor air cooling to room temperature, isolated by filtration, can obtain orthorhombic phase molybdenum trioxide nanobelt powder at 40-80 DEG C of dry 5-24h.
Step B: the preparation of electrode
1) mask blank makes: adopt L-edit Software for Design interdigital electrode predetermined pattern, and with Nanjing clear microelectric technique Ltd customized Cr layer photoetching mask plate, wherein single interdigital electrode pattern dimension is 1cm × 1cm, its interdigital width of fringe 10-50 μm and spacing 1-10 μm, its interdigital striped quantity 10-50, described interdigital electrode pattern repeats to be arranged in the square scope of length of side 70mm equably.
2) substrate cleaning: the SiO by oxidated layer thickness being 10nm single-sided polishing
2/ Si sheet is cut into the small pieces of 1.5cm × 1.5cm, successively uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning 10-30min, then in the air of temperature 40-60 DEG C, dries 20-30min.
3) spin coating photoresist: in step 2) spin coating one deck photoresist on the oven dry substrate that obtains, then at temperature 98-102 DEG C, 1-3min is dried, put step 1 again) mask blank that makes, by described interdigital electrode pattern and described substrate alignment.
According to the present invention, described photoresist is the type photoresists such as AZ5214-E, A21500, A26112, and they are all product solds in the market.
4) mask exposure: step 3) the spin coating photoresist substrate that obtains is at litho machine enterprising line mask exposure 2-6s, then at temperature 98-102 DEG C, 1-3min is dried, at room temperature cool 2-4min again, then maskless lithography 5-10s is carried out, then develop 15-40s after double exposure in developer solution, thereafter wash down with ultrapure water, dry up rear stand-by.
Described developer solution model is
400K,
300 developer solutions such as grade, adopt 0.26N/2.38%TMAH (Tetramethylammonium hydroxide) standard recipe.
Described ultrapure water should be appreciated that it is meet China national use for laboratory water specification GB6682-92.
5) adopt standard direct current magnetron sputtering technique, priority sputtered with Ti and Pt under the condition of Ar atmosphere with 70W sputtering power, their deposit thickness is 10-50nm Ti and 40-200nm Pt respectively.
Step C: constructing of hydrogen sensitive element
1) using liquid-transfering gun to measure 2-10l absolute ethyl alcohol joins in centrifuge tube, takes 10-100mg molybdena powder and joins in aforesaid liquid;
2) ultrasonic process 2-20min, ultrasonic frequency is 40-100Hz;
3) ultrasonic be disposed after, use liquid-transfering gun to measure the above-mentioned mixed liquor of 1-3l and be added drop-wise to interdigital electrode centre;
4) by obtained device in vacuum tightness be 0.0001-0.01Pa condition under anneal
Process, annealing temperature is 100-300 DEG C, and annealing time is 1-10h.
The present invention is with Na
2moO
42H
2o is raw material, adopts simple hydrothermal method to prepare pattern uniform orthorhombic phase molybdena nanobelt, and use equipment fairly simple, manufacturing cycle is short, and output is high, with low cost.By a kind of simple method, the nanobelt after ultrasonic disperse is coated in interdigital electrode, obtains the hydrogen sensitive element of excellent properties.Under room temperature, this element shows the feature of highly sensitive and quick response to low-concentration hydrogen, has good repeatability and selectivity to hydrogen simultaneously, can meet the requirement detecting low-concentration hydrogen fast.
Accompanying drawing explanation
Fig. 1 is the X ray diffracting spectrum of example 1,2,3,4 gained molybdena nanobelt, and wherein a, b, c, d are the XRD collection of illustrative plates that hydrothermal temperature is respectively 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C gained molybdena nanobelts;
Fig. 2 is the SEM figure of example 1,2,3,4 gained molybdena nanobelt; Wherein a, b, c, d are the SEM figure that hydrothermal temperature is respectively 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C gained molybdena nanobelts;
Fig. 3 is the single MoO of example 4 gained
3the microstructure tem analysis result of nanobelt;
Fig. 4 be example 1,2,3,4 gained molybdena nanobelt network to the response curve of 500ppm hydrogen, wherein a, b, c, d are that hydrothermal temperature is respectively 120 DEG C, 160 DEG C, 180 DEG C, 200 DEG C gained molybdena nanobelts to the response diagram of 500ppm hydrogen;
Fig. 5 is that embodiment 4 gained nanometer line network is to the response curve of variable concentrations hydrogen;
Fig. 6 be embodiment 4 gained nanometer line network to the repeatability of hydrogen and selectivity test result, wherein a is the reperformance test result of gas sensor to hydrogen; B is the selectivity test result of gas sensor.
Embodiment
Below in conjunction with instantiation, further illustrate the present invention, but described embodiment is only the present invention's part embodiment, instead of whole embodiments.
Embodiment 1:
The preparation A of molybdena nanobelt
1) in 50ml reaction vessel, by 2.4195g Na
2moO
42H
2o joins in 32.75ml deionized water, and the concentration of molybdenum element is about 0.305mol/L, slowly stirs and molybdenum salt is fully dissolved;
2) under electromagnetic agitation, be slowly poured into by the red fuming nitric acid (RFNA) of 65% of 6.25ml in above-mentioned solution, form acid solution, concentration of nitric acid is 2.5mol/L;
3) after fully mixing, above-mentioned solution is transferred in hydrothermal reaction kettle, at 120 DEG C of temperature, reacts 12h;
4) after question response terminates, by reactor air cooling to room temperature, isolated by filtration, can obtain orthorhombic phase molybdenum trioxide nanobelt powder at 70 DEG C of dry 10h.
Embodiment 2:
The preparation B of molybdena nanobelt
1) in 50ml reaction vessel, by 2.4195g Na
2moO
42H
2o joins in 32.75ml deionized water, and the concentration of molybdenum element is about 0.305mol/L, slowly stirs and molybdenum salt is fully dissolved;
2) under electromagnetic agitation, be slowly poured into by the red fuming nitric acid (RFNA) of 65% of 6.25ml in above-mentioned solution, form acid solution, concentration of nitric acid is 2.5mol/L;
3) after fully mixing, above-mentioned solution is transferred in hydrothermal reaction kettle, at 160 DEG C of DEG C of temperature, reacts 12h;
4) after question response terminates, by reactor air cooling to room temperature, isolated by filtration, can obtain orthorhombic phase molybdenum trioxide nanobelt powder at 70 DEG C of dry 10h.
Embodiment 3:
The preparation C of molybdena nanobelt
1) in 50ml reaction vessel, by 2.4195g Na
2moO
42H
2o joins in 32.75ml deionized water, and the concentration of molybdenum element is about 0.305mol/L, slowly stirs and molybdenum salt is fully dissolved;
2) under electromagnetic agitation, be slowly poured into by the red fuming nitric acid (RFNA) of 65% of 6.25ml in above-mentioned solution, form acid solution, concentration of nitric acid is 2.5mol/L;
3) after fully mixing, above-mentioned solution is transferred in hydrothermal reaction kettle, at 180 DEG C of temperature, reacts 12h;
4) after question response terminates, by reactor air cooling to room temperature, isolated by filtration, can obtain orthorhombic phase molybdenum trioxide nanobelt powder at 70 DEG C of dry 10h.
Embodiment 4:
The preparation D of molybdena nanobelt
1) in 50ml reaction vessel, by 2.4195g Na
2moO
42H
2o joins in 32.75ml deionized water, and the concentration of molybdenum element is about 0.305mol/L, slowly stirs and molybdenum salt is fully dissolved;
2) under electromagnetic agitation, be slowly poured into by the red fuming nitric acid (RFNA) of 65% of 6.25ml in above-mentioned solution, form acid solution, concentration of nitric acid is 2.5mol/L;
3) after fully mixing, above-mentioned solution is transferred in hydrothermal reaction kettle, at 200 DEG C of temperature, reacts 12h;
4) after question response terminates, by reactor air cooling to room temperature, isolated by filtration, can obtain orthorhombic phase molybdenum trioxide nanobelt powder at 70 DEG C of dry 10h.
The X ray diffracting spectrum of gained powder is shown in Fig. 1, and analysis result shows that products therefrom is the orthorhombic phase molybdena of high-crystallinity; As shown in Figures 2 and 3, the length > 10m of molybdena nanobelt, width is about 100-500nm to its scanning electron microscope result, and thickness is 30-80nm.
Embodiment 5
A: the preparation of electrode
1) mask blank makes: adopt L-edit Software for Design interdigital electrode predetermined pattern, and with Nanjing clear microelectric technique Ltd customized Cr layer photoetching mask plate, wherein single interdigital electrode pattern dimension is 1cm × 1cm, its interdigital width of fringe 10m and spacing 5m, its interdigital striped quantity 20, described interdigital electrode pattern repeats to be arranged in the square scope of length of side 70mm equably.
2) substrate cleaning: the SiO by oxidated layer thickness being 10nm twin polishing
2/ Si sheet is cut into the small pieces of 1.5cm × 1.5cm, successively uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning 15min, then in the air of temperature 40 DEG C, dries 30min.
3) spin coating photoresist: the KW-4A type sol evenning machine using Microelectronic Institute of the Chinese Chinese Academy of Sciences to produce, in step 2) the oven dry substrate that obtains drips the photoresist that volume is 100L, then at temperature 100 DEG C, 2min is dried, put step 1 again) mask blank that makes, by described interdigital electrode pattern and described substrate alignment.
4) mask exposure: step 3) the spin coating photoresist substrate that obtains ABM.lnc (China branch office) produce dark/medium ultraviolet litho machine enterprising line mask exposure 3s, then at temperature 100 DEG C, 1.5min is dried, at room temperature cool 3min again, then maskless lithography 10s is carried out, then develop 25s after double exposure in developer solution, thereafter wash down with ultrapure water, dry up rear stand-by.5) standard direct current magnetron sputtering technique is adopted, use the JGPH50 type high vacuum magnetic control sputtering device that Shenyang Scientific Instrument Research & Mfg. Center Co., Ltd., C.A.S produces, at Ar atmosphere and 70W sputtering power, priority sputtered with Ti and Pt under the condition of successively spattering under the condition of background vacuum 4 × 10-4Pa, sputtering pressure 0.5Pa, target-substrate distance 4cm, their deposit thickness is 30nm Ti and 100nm Pt respectively.
B: constructing of hydrogen sensitive element
1) preparing 4 volumes is the centrifuge tube of 2.5ml, uses liquid-transfering gun to measure 5l absolute ethyl alcohol and join in centrifuge tube, takes 50mg example 1 respectively, example 2, example 3, example 4 gained molybdena powder join in aforesaid liquid;
2) ultrasonic process 5min, ultrasonic frequency is 100Hz;
3) ultrasonic be disposed after, use liquid-transfering gun measure the centre that the above-mentioned mixed liquor of 2l is added drop-wise to 4 interdigital electrodes respectively;
4) by obtained device in vacuum tightness be 0.001Pa condition under carry out annealing in process, annealing temperature is 200 DEG C, and annealing time is 2h, and heating rate is 5 DEG C/min.Just hydrogen sensitive element can be obtained when its cool to room temperature.
By the element for preparing as in test cavity, setting constant operating voltage is 1V, weighs its hydrogen sensitivity energy by testing its resistance in gas to be measured and air.For reducibility gas (CO, C
2h
5oH, CH
3cOCH
3), sensitivity definition is the ratio of the difference of element in atmosphere with element in gas to be measured and element resistance in atmosphere.
Claims (1)
1., based on a hydrogen sensitive part making method for orthorhombic phase molybdena nanobelt, it is characterized in that step is as follows:
Steps A: the preparation of molybdena nanobelt
1) in 25-500ml reaction vessel, by Na
2moO
42H
2o joins in deionized water, and the concentration of molybdenum element is about 0.1-2.5mol/L, slowly stirs and molybdenum salt is fully dissolved;
2) under electromagnetic agitation, be slowly poured into by the red fuming nitric acid (RFNA) of 65% in above-mentioned solution, form acid solution, concentration of nitric acid is 0.01-5mol/L;
3) after fully mixing, above-mentioned solution is transferred in hydrothermal reaction kettle, at 120-300 DEG C of temperature, reacts 1-72h;
4) after question response terminates, by reactor air cooling to room temperature, isolated by filtration, can obtain orthorhombic phase molybdenum trioxide nanobelt powder at 40-80 DEG C of dry 5-24h.
Step B: the preparation of electrode
1) mask blank makes: adopt L-edit Software for Design interdigital electrode predetermined pattern, wherein single interdigital electrode pattern dimension is 1cm × 1cm, its interdigital width of fringe 10-50 μm and spacing 1-10 μm, its interdigital striped quantity 10-50, described interdigital electrode pattern repeats to be arranged in the square scope of length of side 70mm equably;
2) substrate cleaning: the SiO by oxidated layer thickness being 10nm single-sided polishing
2/ Si sheet is cut into the small pieces of 1.5cm × 1.5cm, successively uses acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning 10-30min, then in the air of temperature 40-60 DEG C, dries 20-30min;
3) spin coating photoresist: in step 2) spin coating one deck photoresist on the oven dry substrate that obtains, then at temperature 98-102 DEG C, 1-3min is dried, put step 1 again) mask blank that makes, by described interdigital electrode pattern and described substrate alignment; Product sold in the market used by described photoresist;
4) mask exposure: step 3) the spin coating photoresist substrate that obtains is at litho machine enterprising line mask exposure 2-6s, then at temperature 98-102 DEG C, 1-3min is dried, at room temperature cool 2-4min again, then maskless lithography 5-10s is carried out, then develop 15-40s after double exposure in developer solution, thereafter wash down with ultrapure water, dry up rear stand-by;
5) adopt standard direct current magnetron sputtering technique, priority sputtered with Ti and Pt under the condition of Ar atmosphere with 70W sputtering power, their deposit thickness is 10-50nm Ti and 40-200nm Pt respectively;
Step C: constructing of hydrogen sensitive element
1) using liquid-transfering gun to measure 2-10l absolute ethyl alcohol joins in centrifuge tube, takes 10-100mg molybdena powder and joins in aforesaid liquid;
2) ultrasonic process 2-20min, ultrasonic frequency is 40-100Hz;
3) ultrasonic be disposed after, use liquid-transfering gun to measure the above-mentioned mixed liquor of 1-3l and be added drop-wise to interdigital electrode centre;
4) by obtained device in vacuum tightness be 0.0001-0.01Pa condition under carry out annealing in process, annealing temperature is 100-300 DEG C, and annealing time is 1-10h.
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| CN111735856B (en) * | 2020-06-29 | 2024-01-26 | 黄冈师范学院 | Doped MoO 3 Nanobelt, preparation method and application thereof |
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