CN104634824A - Preparation method of gas-sensitive sensor with porous-silicon-based tungsten-oxide nano-rod composite structure - Google Patents
Preparation method of gas-sensitive sensor with porous-silicon-based tungsten-oxide nano-rod composite structure Download PDFInfo
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- CN104634824A CN104634824A CN201510043589.8A CN201510043589A CN104634824A CN 104634824 A CN104634824 A CN 104634824A CN 201510043589 A CN201510043589 A CN 201510043589A CN 104634824 A CN104634824 A CN 104634824A
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Abstract
The invention discloses a preparation method of a gas-sensitive sensor with a porous-silicon-based tungsten-oxide nano-rod composite structure, adopts a hydrothermal method to grow tungsten-oxide nano rods on ordered porous silicon and provides a method capable of controlling the morphology and the gas-sensitive performance of the porous-silicon-based tungsten-oxide nano rods in situ by low cost. The hydrothermal method is simpler in operation and fewer in process conditions needing to be controlled and has no pollution to the environment. In addition, the prepared gas-sensitive sensor with the porous-silicon-based tungsten-oxide nano-rod composite structure has larger specific surface area and the surface activity, can provide more gas absorbing positions and gas diffusing channels, can be used for detecting nitric oxide gas with ultra-low concentration under the room temperature and has the advantages of high sensitivity and good selectivity. Simultaneously, the gas-sensitive element is small in volume and convenient in use and has important practice and research significance.
Description
Technical field
The present invention relates to a kind of preparation of gas sensor element, particularly a kind of working and room temperature and be applicable to the preparation method of the porous silicon-base tungsten oxide nanometer rod composite structure gas sensor detecting oxides of nitrogen gas.
Background technology
Along with the develop rapidly of modern industrial technology, the various harmful gases brought in production run are (as NO
2, CO, NH
3, SO
2deng) constantly increase.Wherein oxides of nitrogen (NO
x) gas is the main cause causing acid rain and photo-chemical smog, its while contaminated environment also serious threat the health and safety of the mankind.Therefore the high-performance gas sensor material and device studied for detecting oxides of nitrogen gas are significant, and become study hotspot in recent years.
Tungsten oxide, as a kind of semiconductor sensitive material having research and apply prospect, has been widely used in and has detected various poisonous and dangerous gas (as NO
2, NH
3deng).But tungsten oxide working temperature higher (150 DEG C ~ 250 DEG C), work under the high temperature conditions for a long time and not only greatly can increase the power consumption of sensor, the bad stability of sensor can be caused simultaneously.Therefore scientific and technical personnel are devoted to the research reducing tungsten oxide working temperature always, and find that one dimension tungsten oxide has larger specific surface area and stronger gas sorption ability, these features can accelerate the reaction between gas, have great importance to raising sensitivity and reduction working temperature.
Porous silicon is a kind of novel gas sensitive of the aperture size, the duct degree of depth and the adjustable porosity that are formed by etching at silicon chip surface, has higher chemical mobility of the surface at ambient temperature, can be used for detecting NO
2, NH
3, H
2s, CO
xand multiple organic gas (ethanol, acetone etc.).In addition, the manufacture craft of porous silicon easily with microelectronic process engineering compatibility.But porous silicon also also exists the low shortcoming of sensitivity, this is by its practical application of restriction.
Summary of the invention
In order to solve problems of the prior art, the invention provides the preparation method of a kind of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor, overcoming harmful gas in prior art and detect the higher problem of tungsten oxide working temperature used.
Technical scheme of the present invention is:
(1) cleaning of silicon chip
The mixed liquor that the monocrystalline silicon substrate of P type single-sided polishing puts into the concentrated sulphuric acid and hydrogen peroxide is soaked 30 ~ 50min, 20 ~ 40min is soaked with in the mixed liquor being placed on hydrofluorite and deionized water, then ultrasonic cleaning 5 ~ 20min in acetone and ethanol respectively, to remove the greasy dirt of silicon substrate surface, organism magazine and surface oxide layer, finally silicon chip is put into absolute ethyl alcohol for subsequent use; The resistivity of the monocrystalline silicon piece of described P type single-sided polishing is 10 ~ 15 Ω cm, and thickness is 400 μm, and crystal orientation is (100), and silicon chip substrate is of a size of 2.2 ~ 2.4cm × 0.8 ~ 0.9cm.
(2) porous silicon is prepared
Double-cell electrochemical etching is adopted to prepare porous silicon layer in the polished surface of the monocrystalline silicon piece of step (1), electrolytic solution used by mass concentration be 40% hydrofluorite and mass concentration be that 40% dimethyl formamide forms, volume ratio is 1:2, in room temperature and not by the average pore size and the thickness that change porous silicon under the environment of illumination by changing current density and etching time, the current density of applying is 50 ~ 100mA/cm
2, etching time is 5 ~ 20min; The average pore size of the porous silicon of preparation is 1.5 μm, and average thickness is 19 μm.
(3) seed solution is prepared
Sodium tungstate is dissolved in the deionized water of 100ml, magnetic stirrer is utilized to make it whole dissolving, dropwise add watery hydrochloric acid subsequently, until no longer produce white precipitate, then mixed liquor is left standstill 30 ~ 60min, supernatant liquor is outwelled the precipitation of the centrifugal bottom of rear recycling low speed centrifuge, then form precipitating to dissolve in the hydrogen peroxide of 10 ~ 30ml the seed solution that concentration is the yellow transparent of 0.5 ~ 1M;
(4) Seed Layer is prepared
The seed solution of preparation in step (3) is spun on porous silicon prepared in step (2), then be placed in muffle furnace and carry out annealing in process, annealing temperature is 550 ~ 700 DEG C, and temperature retention time is 2h, and heating rate is 2 ~ 5 DEG C/min; After Seed Layer annealing, can form equally distributed diameter in the surface and hole of porous silicon is 40 ~ 150nm, and length is the nanometer rods of 80 ~ 240nm.Meanwhile, along with the rising of temperature there will be a small amount of nano wire or nanometer sheet.
(5) hydro-thermal method prepares porous silicon-base tungsten oxide nanometer rod composite structure gas sensor
First reactant liquor is configured, take 4.13 ~ 8.25g sodium tungstate, magnetic stirrer is utilized it to be all dissolved in the deionized water of 25ml, recycling watery hydrochloric acid regulates reacting liquid pH value to 1.5 ~ 2.0, subsequently by above-mentioned solution dilution to 250ml, add appropriate oxalic acid again, the pH value of solution is made to control 1.5 ~ 3.0, then reactant liquor that 60ml configures is pipetted in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, then the level on specimen holder that is inserted in by the porous substrate being attached with Seed Layer in (4) is soared and is placed in liner, finally reactor is placed in thermostatic drying chamber in 180 DEG C of isothermal reaction 2h, prepared porous silicon-base tungsten oxide nanometer rod mean diameter is 50nm, and length is 900nm, and grows a large amount of nanometer rods in the hole of porous silicon.
(6) cleaning of porous silicon substrate after hydro-thermal reaction
By the porous silicon substrate after hydro-thermal reaction in step (5) repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8 ~ 10h in the vacuum drying chamber of 60 ~ 80 DEG C;
(7) porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is prepared
The porous silicon-base tungsten oxide nanometer obtained in step (6) rod is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, argon gas flow is 23 ~ 25sccm, and body vacuum tightness is (4 ~ 5) × 10
-4it is 2 ~ 4Pa that Pa sputters operating pressure, and sputtering power is 80 ~ 100W, and sputtering time is 8 ~ 10min, at porous silicon-base tungsten oxide nanometer rod surface deposition a pair platinum electrode, makes and can be used for the gas sensor element that room temperature detects oxides of nitrogen;
(8) thermal treatment of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element
Porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared by step (7) is placed in muffle furnace and carries out annealing in process, heat treatment temperature is 300 ~ 450 DEG C, temperature retention time is 2h, heating rate is 2 ~ 5 DEG C/min, in order to the crystallinity that increases tungsten oxide nanometer rod with strengthen contacting of tungsten oxide nanometer rod and electrode and porous silicon.
The invention has the beneficial effects as follows: provide and a kind ofly low cost can control the method for porous silicon-base tungsten oxide nanometer clavate looks and air-sensitive performance.Hydro-thermal method operation is comparatively simple, and the process conditions of required control are few, and environmentally safe.The heat treatment temperature of primary study of the present invention Seed Layer is on the impact of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element air-sensitive performance.And, porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared at optimum conditions has larger specific surface area and surfactivity, more gas absorption position and gas diffusion paths can be provided, at room temperature can detect the oxides of nitrogen gas of super low concentration, there is the advantage of high sensitivity, good selectivity.Meanwhile, this gas sensor volume is little, easy to use, has important practice and Research Significance.
Accompanying drawing explanation
Fig. 1 is the porous silicon surface electron scanning micrograph prepared by embodiment 1;
Fig. 2 is the porous silicon cross-sectional scanning electron microphotograph prepared by embodiment 1;
Fig. 3 is the Seed Layer surface Scanning Electron microphotograph prepared by embodiment 1;
Fig. 4 is the porous silicon-base tungsten oxide nanometer rod surface Scanning Electron microphotograph prepared by embodiment 1;
Fig. 5 is the porous silicon-base tungsten oxide nanometer rod cross-sectional scanning electron microphotograph prepared by embodiment 1;
Fig. 6 is that porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared by embodiment 1 is to 0.1 ~ 3ppm NO
2the dynamic response curve of gas;
Fig. 7 is sensitivity and the NO of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared by embodiment 1
2the corresponding relation figure of gas concentration;
Fig. 8 is that porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared by embodiment 1 is to the selectivity schematic diagram of multiple gases.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
The present invention is raw materials used all adopts commercially available chemically pure reagent.
Embodiment 1
(1) cleaning of silicon chip
Be 10 ~ 15 Ω cm by 2 cun of P type resistivity, thickness is 400 μm, crystal orientation is the monocrystalline silicon substrate of the single-sided polishing of (100), cut into the rectangular silicon substrate being of a size of 2.4cm × 0.9cm, silicon chip is put into the concentrated sulphuric acid that volume ratio is 3:1 and hydrogen peroxide solution soaks 40min, soaking 30min with being placed in hydrofluorite and deionized water mixed liquor that volume ratio is 1:1, then ultrasonic cleaning 5min in acetone and ethanol respectively, finally silicon chip being put into absolute ethyl alcohol for subsequent use.
(2) porous silicon is prepared
Double-cell electrochemical etching is adopted to prepare porous silicon layer in the polished surface of the monocrystalline silicon piece of step (1), electrolytic solution used by mass concentration be 40% hydrofluorite and mass concentration be that 40% dimethyl formamide forms, volume ratio is 1:2, is not in room temperature and not 64mA/cm by the current density applied under the environment of illumination
2, etching time is 8min, and the forming region of porous silicon is 1.6cm × 0.4cm.As depicted in figs. 1 and 2, recording average pore size is 1.5 μm for porous silicon surface pattern prepared by embodiment 1 and section structure scanning electron microscope analysis result, and the thickness of porous silicon layer is 19 μm.
(3) seed solution is prepared
1.65g sodium tungstate is dissolved in the deionized water of 100ml, magnetic stirrer is utilized to make it whole dissolving, dropwise add watery hydrochloric acid subsequently, until no longer produce white precipitate, then mixed liquor is left standstill 30min, supernatant liquor is outwelled the precipitation of the centrifugal bottom of rear recycling low speed centrifuge, then form precipitating to dissolve in appropriate hydrogen peroxide the seed solution that concentration is the yellow transparent of 1M.
(4) Seed Layer is prepared
The seed solution of preparation in step (3) is spun on porous silicon prepared in step (2), spin coating 5 layers, is then placed in muffle furnace and carries out annealing in process, and annealing temperature is 650 DEG C, temperature retention time is 2h, and heating rate is 2.5 DEG C/min.Seed Layer surface topography scanning electron microscope analysis result prepared by embodiment 1 is as Fig. 3.
(5) hydro-thermal method prepares porous silicon-base tungsten oxide nanometer rod composite structure gas sensor
First reactant liquor is configured, take 8.25g sodium tungstate, magnetic stirrer is utilized it to be all dissolved in the deionized water of 25ml, recycling watery hydrochloric acid regulates reacting liquid pH value to 2.0, subsequently by above-mentioned solution dilution to 250ml, add appropriate oxalic acid again, the pH value of solution is made to control 2.5, then reactant liquor that 60ml configures is pipetted in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, then the level on specimen holder that is inserted in by the porous substrate being attached with Seed Layer in (4) is soared and is placed in liner, finally reactor is placed in thermostatic drying chamber in 180 DEG C of isothermal reaction 2h.
(6) cleaning of porous silicon substrate after hydro-thermal reaction
By the porous silicon substrate after hydro-thermal reaction in step (5) repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 10h in the vacuum drying chamber of 80 DEG C.Porous silicon-base tungsten oxide nanometer rod surface prepared by embodiment 1 and cross-section morphology scanning electron microscope analysis result as shown in Figure 4 and Figure 5, illustrate that to have a large amount of tungsten oxide nanometers in the bottom of porous hole also length excellent.
(7) porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is prepared
The porous silicon-base tungsten oxide nanometer obtained in step (6) rod is placed in the vacuum chamber of ultrahigh vacuum facing-target magnetron sputtering system equipment, adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, argon gas flow is 24sccm, and body vacuum tightness is 4.0 × 10
-4pa, sputtering operating pressure is 2Pa, and sputtering power is 90W, and sputtering time is 8min, and be of a size of the platinum electrode of 0.2cm × 0.2cm for a pair at porous silicon-base tungsten oxide nanometer rod surface deposition, electrode separation is 8mm.
(8) thermal treatment of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element
Porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared by step (7) is placed in muffle furnace and carries out annealing in process, heat treatment temperature is 400 DEG C, and temperature retention time is 2h, and heating rate is 2.5 DEG C/min.
The porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element that embodiment 1 obtains is at room temperature to the NO of 0.1 ~ 3ppm
2the dynamic response curve of gas as shown in Figure 6.Its sensitivity at room temperature and NO
2the corresponding relation schematic diagram of gas concentration as shown in Figure 7, wherein to 0.1,0.5,1,2,3ppm NO
2the sensitivity of gas is respectively 1.17,2.83,3.38,3.96 and 5.04.
Porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element obtained by embodiment 1 is at room temperature respectively 1.34,1.23,1.18,1.15 to the sensitivity of 50ppm ammonia and 100ppm ethanol, acetone, IPA vapor, and to 3ppm NO
2the sensitivity of gas is 5.04, as shown in Figure 8.This shows that this porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is to NO
2gas has good selectivity.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: in step (4), the heat treatment temperature of Seed Layer is 550 DEG C, and obtained porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is at room temperature to 1ppm NO
2the sensitivity of gas is 2.25.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: in step (4), the heat treatment temperature of Seed Layer is 600 DEG C, and obtained porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is at room temperature to 1ppm NO
2the sensitivity of gas is 2.53.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: in step (4), the heat treatment temperature of Seed Layer is 700 DEG C, and obtained porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is at room temperature to 1ppm NO
2the sensitivity of gas is 1.34.
Above with reference to drawings and Examples, to invention has been schematic description, this description is not restricted.Those of ordinary skill in the art will be understood that in actual applications, and in the present invention, some change all may occur the set-up mode of each parts, and other staff also may make the similar Design of various ways under its enlightenment.It is pointed out that only otherwise depart from design aim of the present invention, all apparent changes and similar Design thereof, be all included within protection scope of the present invention.
Claims (9)
1. a preparation method for porous silicon-base tungsten oxide nanometer rod composite structure gas sensor, is characterized in that, comprise the following steps:
(1) cleaning of silicon chip:
The mixed liquor that the monocrystalline silicon substrate of P type single-sided polishing puts into the concentrated sulphuric acid and hydrogen peroxide is soaked 30 ~ 50min, 20 ~ 40min is soaked with in the mixed liquor being placed on hydrofluorite and deionized water, then ultrasonic cleaning 5 ~ 20min in acetone and ethanol respectively, finally puts into absolute ethyl alcohol by silicon chip for subsequent use;
(2) porous silicon is prepared:
Double-cell electrochemical etching is adopted to prepare porous silicon layer in the polished surface of the monocrystalline silicon piece of step (1);
(3) seed solution is prepared:
Sodium tungstate is all dissolved in deionized water, dropwise add watery hydrochloric acid subsequently, until no longer produce white precipitate, then mixed liquor is left standstill 30 ~ 60min, supernatant liquor is outwelled the precipitation of the centrifugal bottom of rear recycling low speed centrifuge, then form precipitating to dissolve in the hydrogen peroxide of 10 ~ 30ml the seed solution that concentration is the yellow transparent of 0.5 ~ 1M;
(4) Seed Layer is prepared:
The seed solution of preparation in step (3) is spun on porous silicon prepared in step (2), then carries out annealing in process;
(5) hydro-thermal method prepares porous silicon-base tungsten oxide nanometer rod composite structure gas sensor:
First reactant liquor is configured, take 4.13 ~ 8.25g sodium tungstate, it is all dissolved in 25ml deionized water, regulate pH to acid, then the reactant liquor that configures is pipetted in the polytetrafluoroethyllining lining of hydrothermal reaction kettle, then the level on specimen holder that is inserted in by the porous substrate being attached with Seed Layer in (4) is soared and is placed in liner, finally reactor is placed in thermostatic drying chamber isothermal reaction;
(6) cleaning of porous silicon substrate and drying after hydro-thermal reaction;
(7) porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element is prepared:
The porous silicon-base tungsten oxide nanometer rod obtained in step (6) is carried out ultrahigh vacuum facing-target magnetron sputtering system, obtains porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element;
(8) thermal treatment of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element:
Porous silicon-base tungsten oxide nanometer rod composite structure gas sensor element prepared by step (7) is carried out annealing in process.
2. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, the resistivity of the monocrystalline silicon piece of the P type single-sided polishing of described step (1) is 10 ~ 15 Ω cm, thickness is 400 μm, crystal orientation is (100), and silicon chip substrate is of a size of 2.2 ~ 2.4cm × 0.8 ~ 0.9cm.
3. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, described step (2) double-cell electrochemical etching electrolytic solution used by mass concentration be 40% hydrofluorite and mass concentration be that 40% dimethyl formamide forms, volume ratio is 1:2, in room temperature and not by the average pore size and the thickness that change porous silicon under the environment of illumination by changing current density and etching time, the current density of applying is 50 ~ 100mA/cm
2, etching time is 5 ~ 20min.
4. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, the number of times of the Seed Layer spin coating of described step (4) is 5 times, be placed in muffle furnace and carry out annealing in process, annealing temperature is 550 ~ 700 DEG C, temperature retention time is 2h, and heating rate is 2 ~ 5 DEG C/min.
5. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, in described step (5), the pH value of reaction regulates in two steps, first utilize watery hydrochloric acid that solution ph is adjusted to 1.5 ~ 2.0, the pH of the solution after dilution is adjusted to 1.5 ~ 3.0 by recycling oxalic acid.
6. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, in described step (5), hydrothermal reaction condition is isothermal reaction 2h at 180 DEG C.
7. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, described step (6) refers to the porous silicon substrate after by hydro-thermal reaction in step (5) repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8 ~ 10h in the vacuum drying chamber of 60 ~ 80 DEG C.
8. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, described step (7) ultrahigh vacuum facing-target magnetron sputtering system condition is: adopt the metal platinum of quality purity 99.99% as target, using the argon gas of quality purity 99.999% as working gas, argon gas flow is 23 ~ 25sccm, and body vacuum tightness is (4 ~ 5) × 10
-4it is 2 ~ 4Pa that Pa sputters operating pressure, and sputtering power is 80 ~ 100W, and sputtering time is 8 ~ 10min, at porous silicon-base tungsten oxide nanometer rod surface deposition a pair platinum electrode, makes and can be used for the gas sensor element that room temperature detects oxides of nitrogen.
9. the preparation method of porous silicon-base tungsten oxide nanometer rod composite structure gas sensor according to claim 1, it is characterized in that, in described step (8) heat treated condition be at 300 ~ 450 DEG C in muffle furnace constant temperature 2h, heating rate is 2 ~ 5 DEG C/min.
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Application publication date: 20150520 |