CN104891574A - Preparation method of gold-doped porous silicon-based tungsten oxide nano rod with composite structure - Google Patents
Preparation method of gold-doped porous silicon-based tungsten oxide nano rod with composite structure Download PDFInfo
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- CN104891574A CN104891574A CN201510227472.5A CN201510227472A CN104891574A CN 104891574 A CN104891574 A CN 104891574A CN 201510227472 A CN201510227472 A CN 201510227472A CN 104891574 A CN104891574 A CN 104891574A
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Abstract
The invention discloses a preparation method of a gold-doped porous silicon-based tungsten oxide nano rod with a composite structure. According to the invention, porous silicon and tungsten oxide nano rod are composited to form a gas-sensitive material with the composite structure by a hydrothermal method, a gold sputtering step is added, the prepared tungsten oxide nano rod has large specific surface area and a gas diffusion channel and large surface active, massive adsorption position and diffusion channels are provided, defect of high work temperature of the gas-sensitive material based on the tungsten oxide nanostructure can be overcome, and the material has important research value for increasing the gas-sensitive performance of a gas-sensitive sensor. The method has the advantages of simple equipment, convenient operation, good repeatability and low cost. The material has large research space for reducing the work temperature of the gas-sensitive sensor and increasing the sensitivity of the sensor.
Description
Technical field
The present invention relates to a kind of preparation method of composite structure gas sensitive, particularly a kind of preparation method of porous silicon-base tungsten oxide nanometer rod composite structure.
Background technology
In the past few decades, great technological revolution not only facilitates the fast development of human civilization, and improve the standard of living of people, but along with constantly discharging toxic and harmful in air, the ecotope that the mankind depend on for existence has suffered havoc.NO
xgas is exactly wherein a kind of, and every day ceaselessly discharges NO in air
xgas, causes have a strong impact on comprising aquatic animals and plants and terrestrial organism to the healthy of the mankind and animals and plants.According to medical data textual criticism, short burst is exposed to NO
xunder gas, may respiratory system disease be caused, healthy population such as can be made to suffer from air flue inflammation, make originally have the crowd of asthma to increase the weight of the state of an illness.And if long-term exposure is in NO
xunder gas, then crowd may be caused to suffer from pulmonary edema even dead.Under heating or sunlight, oxides of nitrogen gas will react with ammonia, water molecules, hydrocarbon polymer and other compounds and form fine particle, penetrate into lung thus cause or worsen the respiratory system disease such as pulmonary emphysema and bronchitis, even increasing the weight of heart trouble.In Urban areas, the main release source of oxynitride is the aspect such as burning, Energy production, transport of fossil oil respectively.In order to toxic and harmful protection environment for human survival can be monitored in real time and effectively, we be badly in need of a kind of can the gas sensor of probe gas kind and concentration.
Nanostructured metal oxides gas sensor is because of its reduce power consumption, high-performance and obtain the concern of vast academia and commercial and industrial circles.Wherein, Tungsten oxide 99.999 is a kind of N-type metal-oxide semiconductor (MOS) of broad stopband, has had report to mention it to NO, NO
2detection Deng oxides of nitrogen gas has good selectivity and sensitivity.But similar with most metals oxide semiconductor, the working temperature of Tungsten oxide 99.999 is higher, which greatly increases the power consumption of sensor.In addition, based on the gas sensor still gas-sensitive property problem such as ubiquity long reaction time, gas-selectively difference of Tungsten oxide 99.999, this microminiaturization to gas sensing techniques, integrated development add many complicacy and unstable.Scientific and technical personnel are devoted to the research reducing gas sensitive working temperature always for this reason.Research shows, one dimension tungsten oxide nanometer structure has larger specific surface area, surfactivity and stronger gas sorption ability, thus can accelerate the reaction between gas, effective lower working temperature carrying highly sensitive further while.
Silica-based porous silicon is a kind of novel gas sensitive forming the great potential of aperture size, the duct degree of depth and adjustable porosity at silicon chip surface.In addition, because manufacture craft is easy and microelectronic process engineering is compatible, silica-based porous silicon becomes one of research field of most magnetism.Its special microtexture can obtain huge specific surface area, and can provide effective passage for the diffusion of gas, makes it have good air-sensitive performance.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of preparation method of gold doping porous silicon-base tungsten oxide nanometer rod composite structure, overcoming problem higher based on tungsten oxide nanometer structure gas sensitive working temperature in prior art.
Technical scheme of the present invention is:
. a kind of preparation method of gold doping porous silicon-base tungsten oxide nanometer rod composite structure, comprises the following steps:
(1) cleaning of silicon substrate
The mixed solution that the monocrystalline silicon substrate of P type single-sided polishing puts into the vitriol oil and hydrogen peroxide is soaked 30 ~ 50min, 20 ~ 40min is soaked with in the mixed solution being placed on hydrofluoric acid and deionized water, then ultrasonic cleaning 10 ~ 20min in acetone and ethanol respectively, to remove the greasy dirt of silicon substrate surface, organic impurities and surface oxide layer, finally silicon substrate is put into dehydrated alcohol for subsequent use;
(2) porous silicon is prepared
Double-cell electrochemical etching is adopted to prepare porous silicon layer in the glazed surface of the monocrystalline silicon piece of step (1), electrolytic solution used by mass concentration be 40% hydrofluoric acid and mass concentration be that 40% dimethyl formamide forms, volume ratio is 1:2, in room temperature and not by the mean 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 ~ 80mA/cm
2, etching time is 5 ~ 10min;
(3) gold doping
Porous silicon prepared by step (2) is carried out gold sputtering, at porous silicon surface deposited gold film;
(4) seed solution is prepared
Sodium wolframate is dissolved in the deionized water of 100ml, magnetic stirrer is utilized to make it whole dissolving, dropwise add dilute hydrochloric acid subsequently, until no longer produce white precipitate, then mixed solution is left standstill 1 ~ 3h, supernatant liquid is outwelled the precipitation of the centrifugal bottom of rear recycling low speed centrifuge, then form precipitating to dissolve in hydrogen peroxide the seed solution that concentration is the yellow transparent of 0.5 ~ 1M;
(5) Seed Layer is prepared
The seed solution of preparation in step (4) is spun on the porous silicon of gold doping prepared in step (3), then be placed in retort furnace and carry out anneal, annealing temperature is 600 ~ 700 DEG C, and soaking time is 2h, and temperature rise rate is 2 ~ 10 DEG C/min; (6) hydrothermal method prepares porous silicon-base tungsten oxide nanometer rod composite structure
First reaction solution is configured, take 4.13 ~ 8.25g sodium wolframate, magnetic stirrer is utilized it to be all dissolved in the deionized water of 25ml, recycling dilute hydrochloric acid regulates reacting liquid pH value, subsequently by above-mentioned solution dilution to 250ml, add appropriate oxalic acid regulator solution pH value again, then reaction solution that 60ml configures is pipetted in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, and add the NaCl of 0.45 ~ 0.9g, then the level on specimen holder that is inserted in by the porous substrate being attached with Seed Layer in (5) is soared and is placed in liner, finally reactor is placed in thermostatic drying chamber in 180 DEG C of isothermal reaction 2h,
(7) cleaning of porous silicon substrate after hydro-thermal reaction
By the porous silicon substrate after hydro-thermal reaction in step (6) repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8 ~ 10h in the vacuum drying oven of 60 ~ 80 DEG C.
The resistivity of the monocrystalline silicon piece of the P type single-sided polishing of described step (1) is 10 ~ 15 Ω cm, and thickness is 300 ~ 400 μm, and crystal orientation is (100), and silicon substrate substrate is of a size of 2.1 ~ 2.4cm × 0.8 ~ 0.9cm.
The mean pore size of porous silicon prepared by described step (2) is 1.3 ~ 1.8 μm, and mean thickness is 15 ~ 20 μm.
Described step (3) adopts the gold target material of SBC-12 small ion sputtering instrument quality purity 99.99% to carry out gold sputtering, and operating pressure is 5 ~ 6Pa, and sputtering time is 10 ~ 60s.
Solution ph is first adjusted to 1.5 ~ 2.0 with dilute hydrochloric acid by described step (6), and the pH of the solution after dilution is adjusted to 1.0 ~ 3.0 by recycling oxalic acid.
Beneficial effect of the present invention is: the preparation method of the present invention's gold doping porous silicon-base tungsten oxide nanometer rod composite structure, there is huge specific surface area and gas diffusion paths and larger surfactivity, a large amount of absorption positions and diffusion admittance can be provided, thus be conducive to overcoming based on the higher defect of tungsten oxide nanometer structure gas sensitive working temperature, in the air-sensitive performance improving gas sensor, there is important researching value.The method has that equipment is simple, easy to operate, favorable repeatability, the advantage such as with low cost, simultaneously this material by reducing gas sensor working temperature, improve in the sensitivity of sensor very large research space be provided.
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 surface Scanning Electron microphotograph of the gold doping porous silicon-base tungsten oxide nanometer rod composite structure prepared by embodiment 1;
Fig. 4 is the high power electron scanning micrograph of the gold doping porous silicon-base tungsten oxide nanometer rod composite structure prepared by embodiment 1;
Fig. 5 is the surface Scanning Electron microphotograph of the porous silicon-base tungsten oxide nanometer rod composite structure prepared by embodiment 2;
Fig. 6 is the surface Scanning Electron microphotograph of the gold doping porous silicon-base tungsten oxide nanometer rod composite structure prepared by embodiment 3;
Fig. 7 is the surface Scanning Electron microphotograph of the gold doping porous silicon-base tungsten oxide nanometer rod composite structure prepared by embodiment 4.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in more detail.
The present invention is raw materials used all adopts commercially available chemically pure reagent.
Embodiment 1
(1) cleaning of silicon substrate
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 × 0.8cm, silicon chip is put into the vitriol oil that volume ratio is 3:1 and hydrogen peroxide solution soaks 40min, 30min is soaked with being placed in hydrofluoric acid and deionized water mixed solution that volume ratio is 1:1, then ultrasonic cleaning 20min in acetone and ethanol respectively, finally puts into dehydrated alcohol by silicon substrate for subsequent use.
(2) porous silicon is prepared
Double-cell electrochemical etching is adopted to prepare porous silicon layer in the glazed surface of the monocrystalline silicon piece of step (1), electrolytic solution used by mass concentration be 40% hydrofluoric acid 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 mean 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 18 μm.
(3) gold doping
Porous silicon prepared by step (2) is placed in the vacuum chamber of SBC-12 small ion sputtering instrument, adopt the gold target material of quality purity 99.99%, sputtering operating pressure is 5Pa, and sputtering time is 10s, at porous silicon surface deposited gold film.
(4) seed solution is prepared
1.65g sodium wolframate is dissolved in the deionized water of 100ml, magnetic stirrer is utilized to make it whole dissolving, dropwise add dilute hydrochloric acid subsequently, until no longer produce white precipitate, then mixed solution is left standstill 1h, supernatant liquid 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.
(5) Seed Layer is prepared
The seed solution of preparation in step (4) is spun on and preparedly in step (3) is attached with on the porous silicon of gold thin film, spin coating 5 layers, is then placed in retort furnace and carries out anneal, and annealing temperature is 650 DEG C, soaking time is 2h, and temperature rise rate is 2.5 DEG C/min.
(6) hydrothermal method prepares porous silicon-base orderly tungsten oxide nanometer rod composite structure
First reaction solution is configured, take 8.25g sodium wolframate, magnetic stirrer is utilized it to be all dissolved in the deionized water of 25ml, recycling dilute 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 reaction solution that 60ml configures is pipetted in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, add the NaCl of 0.9g, then the level on specimen holder that is inserted in by the porous substrate being attached with Seed Layer in (5) is soared and is placed in liner, finally reactor is placed in thermostatic drying chamber in 180 DEG C of isothermal reaction 2h.
(7) cleaning of porous silicon substrate after hydro-thermal reaction
By the porous silicon substrate after hydro-thermal reaction in step (6) repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 10h in the vacuum drying oven of 80 DEG C.
Tungsten oxide 99.999 mainly monodimension nano stick prepared by embodiment 1, porous silicon-base tungsten oxide nanometer rod composite structure surface topography scan electron microscopic analysis result as shown in Figure 3 and Figure 4, wherein Fig. 4 is partial enlarged drawing, can be observed prepared tungsten oxide nanometer rod almost perpendicular to porous silicon surface growth, the specific surface area of porous silicon-base tungsten oxide nanometer rod composite structure can be significantly improved.
Embodiment 2
The difference of the present embodiment and embodiment 1 is: in step (3), sputtering time is 0s, and directly spin coating Seed Layer on porous silicon, as shown in Figure 5, obtained Tungsten oxide 99.999 is monodimension nano stick to the scanning electron microscope analysis result of surface topography.
Embodiment 3
The difference of the present embodiment and embodiment 1 is: in step (3), sputtering time is 30s, and as shown in Figure 6, obtained tungsten oxide nanometer rod density reduces the scanning electron microscope analysis result of surface topography to some extent.
Embodiment 4
The difference of the present embodiment and embodiment 1 is: in step (3), sputtering time is 50s, the scanning electron microscope analysis result of surface topography as shown in Figure 7, the density of tungsten oxide nanometer rod reduces further, is attended by a large amount of fusiform tungsten oxide nanometer clusters simultaneously and produces.
Claims (4)
1. a preparation method for gold doping porous silicon-base tungsten oxide nanometer rod composite structure, is characterized in that, comprise the following steps:
(1) cleaning of silicon substrate
The mixed solution that the monocrystalline silicon substrate of P type single-sided polishing puts into the vitriol oil and hydrogen peroxide is soaked 30 ~ 50min, 20 ~ 40min is soaked with in the mixed solution being placed on hydrofluoric acid and deionized water, then ultrasonic cleaning 10 ~ 20min in acetone and ethanol respectively, to remove the greasy dirt of silicon substrate surface, organic impurities and surface oxide layer, finally silicon substrate is put into dehydrated alcohol for subsequent use;
(2) porous silicon is prepared
Double-cell electrochemical etching is adopted to prepare porous silicon layer in the glazed surface of the monocrystalline silicon piece of step (1), electrolytic solution used by mass concentration be 40% hydrofluoric acid and mass concentration be that 40% dimethyl formamide forms, volume ratio is 1:2, in room temperature and not by the mean 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 ~ 80mA/cm
2, etching time is 5 ~ 10min;
(3) gold doping
Porous silicon prepared by step (2) is carried out gold sputtering, at porous silicon surface deposited gold film;
(4) seed solution is prepared
Sodium wolframate is dissolved in the deionized water of 100ml, magnetic stirrer is utilized to make it whole dissolving, dropwise add dilute hydrochloric acid subsequently, until no longer produce white precipitate, then mixed solution is left standstill 1 ~ 3h, supernatant liquid is outwelled the precipitation of the centrifugal bottom of rear recycling low speed centrifuge, then form precipitating to dissolve in hydrogen peroxide the seed solution that concentration is the yellow transparent of 0.5 ~ 1M;
(5) Seed Layer is prepared
The seed solution of preparation in step (4) is spun on the porous silicon of gold doping prepared in step (3), then be placed in retort furnace and carry out anneal, annealing temperature is 600 ~ 700 DEG C, and soaking time is 2h, and temperature rise rate is 2 ~ 10 DEG C/min; (6) hydrothermal method prepares porous silicon-base tungsten oxide nanometer rod composite structure
First reaction solution is configured, take 4.13 ~ 8.25g sodium wolframate, magnetic stirrer is utilized it to be all dissolved in the deionized water of 25ml, recycling dilute hydrochloric acid regulates reacting liquid pH value, subsequently by above-mentioned solution dilution to 250ml, add appropriate oxalic acid regulator solution pH value again, then reaction solution that 60ml configures is pipetted in the polytetrafluoroethyllining lining of 100ml hydrothermal reaction kettle, and add the NaCl of 0.45 ~ 0.9g, then the level on specimen holder that is inserted in by the porous substrate being attached with Seed Layer in (5) is soared and is placed in liner, finally reactor is placed in thermostatic drying chamber in 180 DEG C of isothermal reaction 2h,
(7) cleaning of porous silicon substrate after hydro-thermal reaction
By the porous silicon substrate after hydro-thermal reaction in step (6) repeatedly through deionized water and soaked in absolute ethyl alcohol cleaning, then dry 8 ~ 10h in the vacuum drying oven of 60 ~ 80 DEG C.
2. the preparation method of gold doping porous silicon-base tungsten oxide nanometer rod composite structure 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 300 ~ 400 μm, crystal orientation is (100), and silicon substrate substrate is of a size of 2.1 ~ 2.4cm × 0.8 ~ 0.9cm.
3. the preparation method of gold doping porous silicon-base tungsten oxide nanometer rod composite structure according to claim 1, it is characterized in that, described step (3) adopts the gold target material of SBC-12 small ion sputtering instrument quality purity 99.99% to carry out gold sputtering, operating pressure is 5 ~ 6Pa, and sputtering time is 10 ~ 60s.
4. the preparation method of gold doping porous silicon-base tungsten oxide nanometer rod composite structure according to claim 1, it is characterized in that, solution ph is first adjusted to 1.5 ~ 2.0 with dilute hydrochloric acid by described step (6), and the pH of the solution after dilution is adjusted to 1.0 ~ 3.0 by recycling oxalic acid.
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Cited By (4)
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| CN106442878A (en) * | 2016-09-08 | 2017-02-22 | 天津大学 | Preparation method of gold-doped silicon nanocone array gas-sensitive sensor |
| CN106949912A (en) * | 2017-03-17 | 2017-07-14 | 苏州大学 | A kind of self-driven sensor-based system based on friction nanometer power generator |
| CN107561133A (en) * | 2017-08-28 | 2018-01-09 | 东北大学 | A kind of preparation method and application of precious metal doping WO3 base formaldehyde gas sensitive materials |
| CN111204766A (en) * | 2020-02-04 | 2020-05-29 | 河南理工大学 | Method for preparing luminous porous silicon powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106442878A (en) * | 2016-09-08 | 2017-02-22 | 天津大学 | Preparation method of gold-doped silicon nanocone array gas-sensitive sensor |
| CN106949912A (en) * | 2017-03-17 | 2017-07-14 | 苏州大学 | A kind of self-driven sensor-based system based on friction nanometer power generator |
| CN106949912B (en) * | 2017-03-17 | 2019-08-30 | 苏州大学 | A kind of driving sensor-based system certainly based on friction nanometer power generator |
| CN107561133A (en) * | 2017-08-28 | 2018-01-09 | 东北大学 | A kind of preparation method and application of precious metal doping WO3 base formaldehyde gas sensitive materials |
| CN107561133B (en) * | 2017-08-28 | 2019-09-27 | 东北大学 | A kind of preparation method and application of precious metal doping WO3 base formaldehyde gas sensitive material |
| CN111204766A (en) * | 2020-02-04 | 2020-05-29 | 河南理工大学 | Method for preparing luminous porous silicon powder |
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Application publication date: 20150909 |