CN105695317A - Fermentation tank capable of quick detection - Google Patents
Fermentation tank capable of quick detection Download PDFInfo
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- CN105695317A CN105695317A CN201610070314.8A CN201610070314A CN105695317A CN 105695317 A CN105695317 A CN 105695317A CN 201610070314 A CN201610070314 A CN 201610070314A CN 105695317 A CN105695317 A CN 105695317A
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- fermentation tank
- polyvinyl alcohol
- zinc oxide
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12M—APPARATUS FOR ENZYMOLOGY OR MICROBIOLOGY; APPARATUS FOR CULTURING MICROORGANISMS FOR PRODUCING BIOMASS, FOR GROWING CELLS OR FOR OBTAINING FERMENTATION OR METABOLIC PRODUCTS, i.e. BIOREACTORS OR FERMENTERS
- C12M41/00—Means for regulation, monitoring, measurement or control, e.g. flow regulation
- C12M41/30—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration
- C12M41/34—Means for regulation, monitoring, measurement or control, e.g. flow regulation of concentration of gas
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/22—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
- G01N27/223—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity
- G01N27/225—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance for determining moisture content, e.g. humidity by using hygroscopic materials
Abstract
The invention discloses a fermentation tank capable of quick detection. The inside of the tank body of the fermentation tank is provided with a ZnO-base humidity-sensitive sensor module, and can be used for quickly detecting humidity in the tank body. The humidity-sensitive sensing element part of the humidity-sensitive sensor module is prepared by using a silicon nanoporous pillar material as a substrate and a zinc oxide nanowire combined graphene material as a sensitive material; the device is in an interdigital electrode structure, and the structure has large specific area and favorable gas diffusion channels; besides, the moisture-removal polyvinyl alcohol-ethylenediamine tetramethylenephosphoric acid-polysulfone-base-membrane hollow fiber composite membrane assembly arranged on the surface layer of the tank body of the fermentation tank greatly increases the humidity sensitivity of the fermentation tank and enhances the moisture absorption and corrosion resistance functions.
Description
Technical field
The present invention relates to fermentation arts, be specifically related to a kind of fermentation tank possessing quickly detection。
Background technology
Fermentation tank refers to the device for carrying out fermentable, is generally corrosion resistant plate and is made the cylindrical shape of specific volume。Fermentation tank is widely used in the fields such as milk product, beverage, biological engineering, pharmacy。Tank body is provided with interlayer, can heat, is incubated, cooling etc.。
Owing to sweat requires aseptic, pollution-free, and the humidity requirement of yeasting is higher。
Summary of the invention
It is an object of the invention to avoid above-mentioned weak point of the prior art to provide a kind of fermentation tank possessing quickly detection。
The purpose of the present invention is achieved through the following technical solutions:
The invention provides a kind of fermentation tank possessing quickly detection, it is characterized in that: the internally installed of described fermentation tank tank body (1) has zno-based moisture sensor module (2), it can quickly detect the humidity in tank body, and the normal operation of fermentation tank is provided safeguard。
Described zno-based moisture sensor module (2) is mainly made up of wet sensitive sensing element and data read element, described wet sensitive sensing element is interdigital electrode type, including silicon chip substrate (10), Si NPA (20), zinc oxide nanowire (30) and graphene layer (40)；Described fermentation tank tank body (1) is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module (2), described ZnO moisture sensor module (2) detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module (2) can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body (1) is provided with a polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane assembly for dehumidification, polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire (30) length about 30 μm。
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate (10) of 3cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm；Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
The preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
There is advantages that
1. configuration aspects, the present invention adopts Si-NPA (silicon nano hole column) material to be substrate, ZnONWs (zinc oxide nanowire) is sensitive material in conjunction with Graphene, this structure has great specific surface area and good gas diffusion paths, substantially increases the sensitivity of sensitive material in this fermentation tank；
2. adopting grapheme material can increase the conductivity of material greatly, hydrone primary attachment is on the surface of nano wire Yu Graphene simultaneously, it is easy to desorption so that the repeatability that interior humidity is responded by this fermentation tank is good；
3. preparation process material consumption is few, and the controllable degree of technique is high, device small volume and less weight, it is easy to batch production。
Accompanying drawing explanation
Utilize accompanying drawing that invention is described further, but the embodiment in accompanying drawing does not constitute any limitation of the invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to the following drawings。
Fig. 1 is the schematic diagram of fermentation tank of the present invention。
Fig. 2 is sensor sensing componentry schematic diagram。
Detailed description of the invention
Sensor technology is able to obtain main path and the means of various information in nature, production field。It is the cutting edge technology of a kind of modern science and technology, and it is one of three big pillars of modern information technologies, is the important benchmark weighing a national science and technology level of development。According to definition, sensor is: " can experience the measured of regulation and convert device or the device of usable output signal according to certain rule to, being generally made up of sensing element, conversion element and measuring circuit。" to be able to direct feeling measured and be converted into and the measured element of physical quantity having the electricity determining relation or easily becoming electricity for sensing element。Conversion element is able to the measured element being converted directly into the electricity determining relation experienced by sensing element。Measuring circuit is that the signal of telecommunication that conversion element exports is converted to the circuit of easy-to-handle capable telecommunications number。
Humidity refers to the content of water vapor in air。Along with the development of modern science and technology, the Detection & Controling of humidity in productive life being had very important meaning, the application of moisture sensor is also more and more extensive, and such as moisture sensor has a wide range of applications in the such as field such as household electrical appliance, automobile, industrial or agricultural。
Dew cell refers to that ambient humidity has response maybe can be converted to the element that can measure signal accordingly by ambient humidity, and it has a wide range of applications in fields such as industrial and agricultural production, environment measuring and Engineering Control。The core of humidity sensor is humidity-sensitive material, and it is the hydrone utilizing adsorption effect directly to adsorb in air, makes the electrology characteristic etc. of material change, thus detecting the change of humidity。Zinc oxide is a kind of semiconductor material with wide forbidden band, and it is all widely used in fields such as sensor, solaode, lithium battery, catalysis。And zinc oxide material to have preparation cost low, chemical stability, Heat stability is good, prepare the advantages such as controlled and pattern is abundant, be a kind of desirably humidity sensor material。The advantage of the aspects such as the pattern that has additionally, due to nano material itself, structure, nano zinc oxide material is very sensitive to humidity of external environment condition etc., has obvious Unordered system。
Humidity sensor refers to after utilizing humidity-sensitive material adsorbed water molecule, and the principle that measured amount changes is made。Generally accepted theory be the Water Molecular Adsorption in air when sensitive material surface and grain boundaries, reduce surface and the grain boundary resistance of material。
The problem such as not high, response recovery time length for existing moisture sensor sensitivity, this programme, based on nano zinc oxide material, is prepared for the zinc oxide nanowire with large specific surface area, and in conjunction with the high grapheme material of conductivity, makes moisture sensor。
Moisture sensor of the present invention is made up of wet sensitive sensing element part and data read element part。Wherein, wet sensitive sensing element is based on zinc oxide nanowire, make in conjunction with grapheme material, device architecture is interdigital electrode type, when moisture sensor periphery humidity changes, Water Molecular Adsorption can change in the speed of sensitive material surface and crystal boundary, causes the conductivity of sensitive material to change, and then reflects its capacitance variations from read element part；Digital independent element is with microprocessor, and it is the voltage applying characteristic frequency to sensing element, reads different numerical value according to the change of sensing element electric capacity at this voltage and carrys out the change of display environment humidity。
The invention provides a kind of fermentation tank possessing quickly detection, the internally installed of described fermentation tank tank body has zno-based moisture sensor module, and it can quickly detect the humidity in tank body, and the normal operation of fermentation tank is provided safeguard。
Illustrate that the present invention is further described below in conjunction with accompanying drawing。
Fig. 1 is the schematic diagram of fermentation tank of the present invention。The internally installed of fermentation tank tank body (1) has zno-based moisture sensor module (2)。
Fig. 2 is sensor sensing componentry schematic diagram。Wherein: 10-silicon chip substrate, 20-Si-NPA, 30-zinc oxide nanowire, 40-graphene layer。
The invention will be further described with the following Examples。
Embodiment 1:
A kind of fermentation tank possessing quickly detection as shown in Figure 1, the internally installed of described fermentation tank tank body 1 has zno-based moisture sensor module 2；Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element。As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40；Described fermentation tank tank body 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body is provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire 30 length about 30 μm。
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 20nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm；Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity。Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%～95%, reads the electric capacity of sensing element with humidity situation of change；
The sensitivity definition of dew cell is: CRH-C11/ C11× 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity。Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,39,154,897 and 2371, response and respectively 8s and 11s recovery time, test result shows that this fermentation tank has good wet sensitive performance, the detection of tank body humidity is quick, accurate, ensure the normal humidity environment of fermentation tank。
Embodiment 2
A kind of fermentation tank possessing quickly detection as shown in Figure 1, the internally installed of described fermentation tank tank body 1 has zno-based moisture sensor module 2；Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element。As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40；Described fermentation tank tank body 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body is provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire 30 length about 31 μm。
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 250V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 30nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm；Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity。Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%～95%, reads the electric capacity of sensing element with humidity situation of change；
The sensitivity definition of dew cell is: CRH-C11/ C11× 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity。Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,25,142,943 and 3081, response and respectively 10s and 12s recovery time, test result shows that this fermentation tank has good wet sensitive performance, the detection of tank body humidity is quick, accurate, ensure the normal humidity environment of fermentation tank。
Embodiment 3:
A kind of fermentation tank possessing quickly detection as shown in Figure 1, the internally installed of described fermentation tank tank body 1 has zno-based moisture sensor module 2；Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element。As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40；Described fermentation tank tank body 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body is provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire 30 length about 32 μm。
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:3, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 60ml70% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 150V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 2h, obtains diameter and is about the zinc oxide nanowire of 60nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm；Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1950 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity。Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%～95%, reads the electric capacity of sensing element with humidity situation of change；
The sensitivity definition of dew cell is: CRH-C11/ C11× 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity。Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,31,368,853 and 1952, response and respectively 12s and 13s recovery time, test result shows that this fermentation tank has good wet sensitive performance, the detection of tank body humidity is quick, accurate, ensure the normal humidity environment of fermentation tank。
Embodiment 4
A kind of fermentation tank possessing quickly detection as shown in Figure 1, the internally installed of described fermentation tank tank body 1 has zno-based moisture sensor module 2；Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element。As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40；Described fermentation tank tank body 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body is provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire 30 length about 5 μm。
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 3cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=1:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.9A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 300 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 9nm；Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity。Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%～95%, reads the electric capacity of sensing element with humidity situation of change；
The sensitivity definition of dew cell is: CRH-C11/ C11× 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity。Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,28,128,898 and 15632, response and respectively 12s and 13s recovery time, test result shows that this fermentation tank has good wet sensitive performance, the detection of tank body humidity is quick, accurate, ensure the normal humidity environment of fermentation tank。
Embodiment 5
A kind of fermentation tank possessing quickly detection as shown in Figure 1, the internally installed of described fermentation tank tank body 1 has zno-based moisture sensor module 2；Described zno-based moisture sensor module 2 is mainly made up of wet sensitive sensing element and data read element。As in figure 2 it is shown, described wet sensitive sensing element is interdigital electrode type, it includes silicon chip substrate 10, Si-NPA20, zinc oxide nanowire 30 and graphene layer 40；Described fermentation tank tank body 1 is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module, described ZnO moisture sensor module detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body is provided with a polyvinyl alcohol for dehumidification-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly, polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire 30 length about 5 μm。
Preferably, the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si-NPA substrate: the silicon chip substrate of 4cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si-NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si-NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml60% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si-NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 260V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm；Secondly, putting in tube furnace by this substrate, be warming up to 700 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
Wherein, the preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.5mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
Wet sensitive is tested:
Zinc oxide-base moisture sensor is put in control appliance of temperature and humidity。Test temperature is set as 20 DEG C, then controls relative humidity variations and ranges for 10%～95%, reads the electric capacity of sensing element with humidity situation of change；
The sensitivity definition of dew cell is: CRH-C11/ C11× 100%, wherein CRHFor the component capacitance value obtained under test environment humidity, C11Capacitance for 11% time element of relative humidity。Are defined as the response of dew cell or recovery time testing capacitor value and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
When testing frequency and being 100Hz, under the relative humidity of 15%, 35%, 55%, 75%, 95%, the sensitivity of sensing element respectively 4,21,143,7898 and 1932, response and respectively 15s and 17s recovery time, test result shows that this fermentation tank has good wet sensitive performance, the detection of tank body humidity is quick, accurate, ensure the normal humidity environment of fermentation tank。
Finally should be noted that; above example is only in order to illustrate technical scheme; but not limiting the scope of the invention; although having made to explain to the present invention with reference to preferred embodiment; it will be understood by those within the art that; technical scheme can be modified or equivalent replacement, without deviating from the spirit and scope of technical solution of the present invention。
Claims (2)
1. the fermentation tank possessing quickly detection, it is characterised in that: the internally installed of described fermentation tank tank body (1) has zno-based moisture sensor module (2)；Described zno-based moisture sensor module (2) is mainly made up of wet sensitive sensing element and data read element, described wet sensitive sensing element is interdigital electrode type, including silicon chip substrate (10), Si NPA (20), zinc oxide nanowire (30) and graphene layer (40)；Described fermentation tank tank body (1) is additionally provided with microprocessor, LED display lamp bar and wireless communication module；The input of described microprocessor is connected with the outfan of described ZnO moisture sensor module (2), described ZnO moisture sensor module (2) detected value reaches preset value, described microprocessor controls LED display lamp bar and flashes, described LED display lamp bar is connected to a buzzer, touches buzzer and send alarm while the flicker of LED display lamp bar；Described wireless communication module is CC2420 wireless communication module, described ZnO moisture sensor module (2) can by described CC2420 wireless communication module transmission detection data to data basestation, by the Internet, mobile subscriber terminal can check that detection data are maybe uploaded to cloud storage center by testing result, form detection and monitoring network；The output electric wire sidewall of described fermentation tank tank body (1) is provided with a polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane assembly for dehumidification, polyvinyl alcohol ethylenediamine tetraacetic methene phosphoric acid polysulfones basement membrane hollow fiber composite membrane is fixed in glass electrode by this membrane module, and glass electrode is connected with moisture sensor；Described zinc oxide nanowire (30) length about 30 μm。
2. fermentation tank according to claim 1, it is characterised in that the preparation method of described wet sensitive sensing element is as follows:
Step one, prepares Si NPA substrate: the silicon chip substrate (10) of 3cm × 3cm is included clean dirt, hydro-thermal method corrosion preparation Si NPA substrate；1. taking the silicon chip of 3cm × 3cm, be placed in by silicon chip in the mixed solution of sulphuric acid and hydrogen peroxide volume ratio 4:1, supersound process 20min, taking-up deionized water cleans, to remove the organic impurities of silicon chip surface；It is H that silicon chip is positioned over volume ratio2O:H2O2: NH4In the mixed solution of OH=5:2:1, ultrasonic cleaning 20min, the deionized water of taking-up subsequently cleans, to remove Organic substance and the metal complex of silicon chip surface；2. hydro-thermal method corrosion is utilized to prepare Si NPA: to weigh the Fe (NO of 1.0g3)·9H2O pours in politef, is added thereto to the HF solution of 20ml deionized water and 30ml40% subsequently；Putting in solution by the silicon chip that upper step is cleaned, add a cover and put in water heating kettle, put in drying baker by water heating kettle subsequently, 180 DEG C of constant temperature keep 30min, after natural cooling, take out Wafer Cleaning and namely obtain Si NPA substrate；
Step 2, growth of zinc oxide nano line: adopt magnetron sputtering to prepare zinc oxide nanowire in conjunction with thermal oxidation method；Silicon nano hole column substrate is put in magnetic control sputtering device, when sputtering voltage 220V, sputtering current 0.8A, magnetron sputtering Zn film, thickness is 50nm, putting it into subsequently in batch-type furnace, at 400 DEG C, thermal oxidation method processes 4h, obtains diameter and is about the zinc oxide nanowire of 30nm；
Step 3, grows graphene layer: adopt process for preparing graphenes by chemical vapour deposition；First magnetron sputtering layer of metal Ni film on the substrate that upper step obtains, thickness is about 5nm；Secondly, putting in tube furnace by this substrate, be warming up to 900 DEG C, pass into hydrogen as protection reducing gas by given pace, stablize 30min, then, pass into methane 2h according to a certain percentage simultaneously, stopping starts Temperature fall after passing into methane；Under Ni catalyst action, methane molecule at high temperature can be cracked into carbon atom and hydrogen atom, and at temperature-fall period and under the protection of hydrogen, carbon atom can formation of deposits one layer graphene thin film；
Step 4, is deposited with interdigital electrode: after obtaining growing the silicon nano hole column substrate having zinc oxide nanowire and Graphene, covers interdigital electrode mask at substrate surface, utilizes magnetron sputtering method to be deposited with Au thin film thick for one layer of 500nm on its surface as electrode；
Step 5, assembles sensing element and reads data element: the both positive and negative polarity wire reading data element is connected in interdigital electrode, two parts composition Zinc oxide-base moisture sensor device；
The preparation method of described polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfones basement membrane hollow fiber composite membrane assembly is as follows:
Step one, polysulfone hollow fibre basement membrane pretreatment: polysulfone hollow fibre basement membrane to carry out pretreatment before coating, after soaking 12h with deionized water, with the soak with hydrochloric acid 60min of 1.0mol/l, remove glycerin layer and other organic solvents on film surface；Then use in the sodium hydroxide solution of 1.0mol/l and excessive hydrochloric acid, finally repeatedly rinse with deionized water, make film surface in neutrality, dry in the shade standby；
Step 2, prepare polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane: add in deionized water by the polyvinyl alcohol that the average degree of polymerization of certain mass is 1750 ± 50, it is about 3h 50 DEG C of stirred in water bath to be completely dissolved to polyvinyl alcohol, obtains 5wt% polyvinyl alcohol homogeneous phase aqueous solution；Adding a certain amount of ethylenediamine tetraacetic methene phosphoric acid after solution is cooled to room temperature, and at room temperature stir 1.5h, namely standing and defoaming obtains casting solution；Polysulfones basement membrane (molecular cut off 30000) through pretreatment is taken out after casting solution soaks 20min, is vertically fixed on the guide frame that dries in the air and dries in the shade；After the film of primary coating soaks 20min again in casting solution, will reversely be fixed on and dry in the air on guide frame, dry at room temperature over night, prepare required PVA-EDTMPA/PS hollow fiber composite membrane。
Step 3, fixing: polyvinyl alcohol-ethylenediamine tetraacetic methene phosphoric acid-polysulfone hollow fibre composite membrane is fixed in glass electrode。
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| CN112525975A (en) * | 2020-12-10 | 2021-03-19 | 重庆锟铻电子科技有限公司 | Humidity sensor special for biodegradable toilet bowl |
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Application publication date: 20160622 |