CN105699442A - Plastic mold for fusion plastic water content detection - Google Patents
Plastic mold for fusion plastic water content detection Download PDFInfo
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- CN105699442A CN105699442A CN201610021815.7A CN201610021815A CN105699442A CN 105699442 A CN105699442 A CN 105699442A CN 201610021815 A CN201610021815 A CN 201610021815A CN 105699442 A CN105699442 A CN 105699442A
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- 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
Abstract
The invention discloses a plastic mold for fusion plastic water content detection.A humidity sensitivity sensor module is installed outside a mold fixing part of the plastic mold so that in the use process of the plastic mold, the concentration of steam released in the plastic raw material fusing process can be detected, then, the water content in plastic raw materials can be judged through parameter comparison, and a very good control effect is achieved for the quality of the prepared plastic mold.Creative designs are made on the aspects of sensitive materials, manufacturing conditions, structures and the like of a sensor for the humidity sensitivity sensor module, the sensitivity of the plastic mold is greatly improved, the responding time is greatly prolonged, an extraordinary technical effect is produced, and the plastic mold has very good market application prospects.
Description
Technical field
The invention belongs to mould applications, be more particularly to a kind of mould of plastics for the detection of molten plastic water content。
Background technology
Mould, is used to the instrument of formed article, is made up of various parts, is industrial obtain the various moulds of required product and the general name of instrument in order to methods such as injection moulding, blowing, extrusion, punching presses。Mould of plastics is the instrument in plastics processing industry for the complete configuration of plastic and accurate dimension, generally comprises fixed half and moving half part。
But, there is techniques below problem in the mould of plastics in correlation technique: in use, and in mould of plastics course of normal operation, the steam detection of molten plastic generally gets the brush-off。
Summary of the invention
The present invention is directed to background technology Problems existing, it is provided that a kind of mould of plastics for the detection of molten plastic water content。
The purpose of the present invention is achieved through the following technical solutions:
A kind of mould of plastics for the detection of molten plastic water content, it is characterized in that, the outside of described mould of plastics cover half part is provided with moisture sensor module, this moisture sensor module can detect the concentration of plastic raw materials melting process release steam, and then can be determined that the water content in plastic raw materials is how many by parameter comparison, the quality of made mould is played and well control is acted on, it is possible to well control die quality。
This moisture sensor module includes the heavy doping silicon chip laid successively from top to bottom, the SiO being close to heavy doping silicon chip2Layer, carbon nanotube layer, it is positioned at SiO2The bottom electrode of interlayer and the upper electrode being positioned on carbon nanotube layer, described carbon nanotube layer is grown on SiO2On layer；Described bottom electrode has metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 50nm, 250nm and 500nm；Described carbon nanotube layer adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode and upper electrode are connected to a micro-control processor for connecting with client communication。
Preferably, the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip, puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO at heavy doping silicon chip surface2Layer；
S2: bottom electrode makes: have SiO by what prepare in step S12The heavy doping silicon chip of layer uses acetone, ethanol, deionized water cleaning 15min post-drying successively, at its surface spin coating photoresist, uses bottom electrode mask to its exposure, and development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer, etches 30min, will etch SiO2Heavy doping silicon chip after layer cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. use Fe/Ni nanoparticle as the catalyst of carbon nano tube growth, first, to the heavy doping silicon chip spin coating photoresist with bottom electrode, adopt the localization mask of catalyst that it is exposed, be then passed through development, clean standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 200mg, 50mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip, the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip, obtain the CNT of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 60% acetic acid of 40ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip of Patterned Carbon Nanotube put into, stands 2h；
B. substrate growth being had the heavy doping silicon chip of CNT is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip ozone clean 20min that will obtain in step S1～S5, in covering, the ceramic mask of electrode, then puts in magnetic control sputtering device by heavy doping silicon chip, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode of Au layer, and wherein, the thickness of Au layer is about 200nm；
S7: welding encapsulation: make upper electrode and bottom electrode connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
Preferably, in step S2, the parameter of spin coating photoresist is arranged as follows: low speed 900rpm, 15s；High speed 3500rpm, 50s。
The invention have benefit that:
(1) a kind of mould of plastics for the detection of molten plastic water content that embodiments of the invention provide, the outside of described mould of plastics cover half part is provided with moisture sensor, this moisture sensor is capacity type wet dependent sensor, and bottom electrode is respectively formed Ohmic contact with heavy doping silicon chip, upper electrode with CNT；Bottom electrode is connected with silicon chip and forms two pole plates of electric capacity, SiO with upper electrode2Layer and CNT are the medium between electric capacity, when device local environment humidity changes, water vapour molecule interacts with CNT, causes the change in electrical properties of CNT, the i.e. change in dielectric constant of electric capacity, therefore from output result can monitoring of environmental humidity change。And this moisture sensor is highly sensitive, and response time is short, manufacturing process is simple, the repeatable height of experimental technique, it is easy to batch production。
(2) a kind of mould of plastics for the detection of molten plastic water content that embodiments of the invention provide, the moisture sensor adopted, CNT after growth is carried out Cement Composite Treated by Plasma, make carbon nano tube modified upper oh group, owing to it is to hydrone strong interaction, promote the CNT adsorption to steam, and then increase the wet sensitive performance of CNT, and being glued with the bacterial enzyme rete of sensing bacterial growth on its electrode, this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；This antibacterial enzyme membrane is by sensing bacterial growth amount and then sensing ambient humidity, it is possible to dual sensing humidity, solves conventional wet dependent sensor problem of hydraulic performance decline after metallic film life-time service。
(3) a kind of mould of plastics for the detection of molten plastic water content that embodiments of the invention provide, the electrode of the moisture sensor adopted is connected to a micro-control processor, for connecting mobile client, user can check humidity condition by client。
Accompanying drawing explanation
The invention will be further described to utilize accompanying drawing, 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 the present invention。
The humidity sensor structural representation that Fig. 2 provides for embodiments of the invention。
Detailed description of the invention
CNT is a kind of allotrope of carbon, and its structure is: radial dimension is nanometer scale, and axial dimension is micron dimension, and pipe two ends are substantially all sealing。It is the body of the seamless hollow that the close heap graphite flake layer of the hexagonal formed by carbon atom is rolled into, and is a kind of quasi-One-dimensional Quantum material。Curling and become SWCN (SWNT) by one layer of graphite, multi-walled carbon nano-tubes (MWNT) is made up of the coaxial pipe of several layers to tens of layers。CNT has good mechanical property, and its tensile strength is 100 times of steel, has good pliability, and hardness is suitable with diamond, is desirable high tensile strength fibrous material。CNT is generally adopted arc discharge, laser evaporation and chemical vapor deposition growth method。Research shows, CNT has shown that the response to gases such as steam, ammonia, nitrogen dioxide, hydrogen, methane, sulfur dioxide, hydrogen sulfide and oxygen。
Humidity describes physical quantitys how many containing water content or hydrone in environment, and dew cell refers to that ambient humidity has response maybe can be converted to the element that can measure signal (such as resistance, electric capacity, frequency etc.) accordingly by ambient humidity。Humidity sensor is converted to the device of the signal of telecommunication ambient humidity, and it has a wide range of applications in fields such as industrial and agricultural production, environment measuring, household electrical appliance, meteorology, 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。CNT has very big specific surface area, and has very strong interaction between the medium of surrounding, therefore that the humidity of external environment condition etc. is very sensitive, has obvious Unordered system。
CNT capacitance type sensor is mainly through the change of dielectric layer constant and then causes measurable capacitance variations that gas to be measured is detected。
A kind of mould of plastics for the detection of molten plastic water content, it is characterized in that, the outside of described mould of plastics cover half part is provided with moisture sensor module, this moisture sensor module can detect the concentration of plastic raw materials melting process release steam, and then can be determined that the water content in plastic raw materials is how many by parameter comparison, the quality of made mould is played and well control is acted on, it is possible to well control die quality。
In conjunction with legend the present invention made and further illustrating:
Fig. 1 is the schematic diagram of the present invention。10 is the mould of plastics of the present invention, and 20 is the moisture sensor module being arranged on mould of plastics cover half portion of external。
The humidity sensor structural representation that Fig. 2 provides for embodiments of the invention。Wherein: 1-heavy doping silicon chip, 2-SiO2Layer, 3-bottom electrode, 4-CNT, the upper electrode of 5-。
Provide below 5 embodiments described moisture sensor module is described further:
Embodiment 1
A kind of mould of plastics for the detection of molten plastic water content, the outside of described mould of plastics cover half part is provided with moisture sensor module, and this moisture sensor module includes the heavy doping silicon chip laid successively from top to bottom, the SiO being close to heavy doping silicon chip2Layer, carbon nanotube layer, it is positioned at SiO2The bottom electrode of interlayer and the upper electrode being positioned on carbon nanotube layer, described carbon nanotube layer is grown on SiO2On layer；Described bottom electrode has metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 50nm, 250nm and 500nm；Described carbon nanotube layer adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode and upper electrode are connected to a micro-control processor for connecting with client communication。
Further, the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip, puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO at heavy doping silicon chip surface2Layer；
S2: bottom electrode makes: have SiO by what prepare in step S12The heavy doping silicon chip of layer uses acetone, ethanol, deionized water to clean 15min post-drying successively, at its surface spin coating photoresist (low speed 900rpm, 15s；High speed 3500rpm, 50s), use bottom electrode mask to its exposure, development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer, etches 30min, will etch SiO2Heavy doping silicon chip after layer cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. use Fe/Ni nanoparticle as the catalyst of carbon nano tube growth, first, to the heavy doping silicon chip spin coating photoresist with bottom electrode, adopt the localization mask of catalyst that it is exposed, be then passed through development, clean standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 200mg, 50mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip, the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip, obtain the CNT of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 60% acetic acid of 40ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip of Patterned Carbon Nanotube put into, stands 2h；
B. substrate growth being had the heavy doping silicon chip of CNT is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip ozone clean 20min that will obtain in step S1～S5, in covering, the ceramic mask of electrode, then puts in magnetic control sputtering device by heavy doping silicon chip, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode of Au layer, and wherein, the thickness of Au layer is about 200nm；
S7: welding encapsulation: make upper electrode and bottom electrode connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
Test data: CNT capacity type wet dependent sensor is placed on a metal sealing chamber (1m3) in, metal sealing chamber is with air inlet and gas outlet。During test, digital electric bridge output frequency is 50Hz, and test temperature is 20 DEG C, then controls relative humidity variations and ranges for 5%～95%, reads capacitance with humidity situation of change；
The sensitivity definition of this CNT capacity type wet dependent sensor is: CRH-C11/ C11× 100%, wherein CRHFor the sensor capacitance value obtained under test environment humidity, C11Capacitance for relative humidity 11% lower sensor。The response of this CNT capacity type wet dependent sensor or be defined as testing capacitor value recovery time and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
Test finds, under the relative humidity of 95%, sensitivity up to 3626, optimal response and recovery time respectively 6s and 13s, and through 2000 retests, the pad value of its electric capacity is less than 10%。The electric capacity of this CNT capacitance type sensor is good with envionmental humidity linear change, highly sensitive, fast response time, good stability。
Embodiment 2
A kind of mould of plastics for the detection of molten plastic water content, the outside of described mould of plastics cover half part is provided with moisture sensor module, and this moisture sensor module includes the heavy doping silicon chip laid successively from top to bottom, the SiO being close to heavy doping silicon chip2Layer, carbon nanotube layer, it is positioned at SiO2The bottom electrode of interlayer and the upper electrode being positioned on carbon nanotube layer, described carbon nanotube layer is grown on SiO2On layer；Described bottom electrode has metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 30nm, 125nm and 500nm；Described carbon nanotube layer adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode and upper electrode are connected to a micro-control processor for connecting with client communication。
Further, the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip, puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO at heavy doping silicon chip surface2Layer；
S2: bottom electrode makes: have SiO by what prepare in step S12The heavy doping silicon chip of layer uses acetone, ethanol, deionized water to clean 15min post-drying successively, at its surface spin coating photoresist (low speed 900rpm, 15s；High speed 3500rpm, 50s), use bottom electrode mask to its exposure, development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer, etches 30min, will etch SiO2Heavy doping silicon chip after layer cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. use Fe/Ni nanoparticle as the catalyst of carbon nano tube growth, first, to the heavy doping silicon chip spin coating photoresist with bottom electrode, adopt the localization mask of catalyst that it is exposed, be then passed through development, clean standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 240mg, 50mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip, the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip, obtain the CNT of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 60% acetic acid of 40ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip of Patterned Carbon Nanotube put into, stands 2h；
B. substrate growth being had the heavy doping silicon chip of CNT is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip ozone clean 20min that will obtain in step S1～S5, in covering, the ceramic mask of electrode, then puts in magnetic control sputtering device by heavy doping silicon chip, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode of Au layer, and wherein, the thickness of Au layer is about 150nm；
S7: welding encapsulation: make upper electrode and bottom electrode connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
Test data: CNT capacity type wet dependent sensor is placed on a metal sealing chamber (1m3) in, metal sealing chamber is with air inlet and gas outlet。During test, digital electric bridge output frequency is 50Hz, and test temperature is 20 DEG C, then controls relative humidity variations and ranges for 5%～95%, reads capacitance with humidity situation of change；
The sensitivity definition of this CNT capacity type wet dependent sensor is: CRH-C11/ C11× 100%, wherein CRHFor the sensor capacitance value obtained under test environment humidity, C11Capacitance for relative humidity 11% lower sensor。The response of this CNT capacity type wet dependent sensor or be defined as testing capacitor value recovery time and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
Test finds, under the relative humidity of 95%, sensitivity up to 3154, optimal response and recovery time respectively 9s and 16s, and through 2000 retests, the pad value of its electric capacity is less than 10%。The electric capacity of this CNT capacitance type sensor is good with envionmental humidity linear change, highly sensitive, fast response time, good stability。
Embodiment 3
A kind of mould of plastics for the detection of molten plastic water content, the outside of described mould of plastics cover half part is provided with moisture sensor module, and this moisture sensor module includes the heavy doping silicon chip laid successively from top to bottom, the SiO being close to heavy doping silicon chip2Layer, carbon nanotube layer, it is positioned at SiO2The bottom electrode of interlayer and the upper electrode being positioned on carbon nanotube layer, described carbon nanotube layer is grown on SiO2On layer；Described bottom electrode has metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 60nm, 160nm and 400nm；Described carbon nanotube layer adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode and upper electrode are connected to a micro-control processor for connecting with client communication。
Further, the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip, puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO at heavy doping silicon chip surface2Layer；
S2: bottom electrode makes: have SiO by what prepare in step S12The heavy doping silicon chip of layer uses acetone, ethanol, deionized water to clean 15min post-drying successively, at its surface spin coating photoresist (low speed 900rpm, 15s；High speed 3500rpm, 50s), use bottom electrode mask to its exposure, development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer, etches 30min, will etch SiO2Heavy doping silicon chip after layer cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. use Fe/Ni nanoparticle as the catalyst of carbon nano tube growth, first, to the heavy doping silicon chip spin coating photoresist with bottom electrode, adopt the localization mask of catalyst that it is exposed, be then passed through development, clean standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 100mg, 50mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip, the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip, obtain the CNT of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 60% acetic acid of 40ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip of Patterned Carbon Nanotube put into, stands 2h；
B. substrate growth being had the heavy doping silicon chip of CNT is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip ozone clean 20min that will obtain in step S1～S5, in covering, the ceramic mask of electrode, then puts in magnetic control sputtering device by heavy doping silicon chip, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode of Au layer, and wherein, the thickness of Au layer is about 300nm；
S7: welding encapsulation: make upper electrode and bottom electrode connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
Test data: CNT capacity type wet dependent sensor is placed on a metal sealing chamber (1m3) in, metal sealing chamber is with air inlet and gas outlet。During test, digital electric bridge output frequency is 50Hz, and test temperature is 20 DEG C, then controls relative humidity variations and ranges for 5%～95%, reads capacitance with humidity situation of change；
The sensitivity definition of this CNT capacity type wet dependent sensor is: CRH-C11/ C11× 100%, wherein CRHFor the sensor capacitance value obtained under test environment humidity, C11Capacitance for relative humidity 11% lower sensor。The response of this CNT capacity type wet dependent sensor or be defined as testing capacitor value recovery time and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
Test finds, under the relative humidity of 95%, sensitivity up to 2743, optimal response and recovery time respectively 10s and 19s, and through 2000 retests, the pad value of its electric capacity is less than 10%。The electric capacity of this CNT capacitance type sensor is good with envionmental humidity linear change, highly sensitive, fast response time, good stability。
Embodiment 4
A kind of mould of plastics for the detection of molten plastic water content, the outside of described mould of plastics cover half part is provided with moisture sensor module, and this moisture sensor module includes the heavy doping silicon chip laid successively from top to bottom, the SiO being close to heavy doping silicon chip2Layer, carbon nanotube layer, it is positioned at SiO2The bottom electrode of interlayer and the upper electrode being positioned on carbon nanotube layer, described carbon nanotube layer is grown on SiO2On layer；Described bottom electrode has metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 30nm, 120nm and 400nm；Described carbon nanotube layer adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode and upper electrode are connected to a micro-control processor for connecting with client communication。
Further, the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip, puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO at heavy doping silicon chip surface2Layer；
S2: bottom electrode makes: have SiO by what prepare in step S12The heavy doping silicon chip of layer uses acetone, ethanol, deionized water to clean 15min post-drying successively, at its surface spin coating photoresist (low speed 900rpm, 15s；High speed 3500rpm, 50s), use bottom electrode mask to its exposure, development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer, etches 30min, will etch SiO2Heavy doping silicon chip after layer cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. use Fe/Ni nanoparticle as the catalyst of carbon nano tube growth, first, to the heavy doping silicon chip spin coating photoresist with bottom electrode, adopt the localization mask of catalyst that it is exposed, be then passed through development, clean standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 220mg, 45mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip, the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip, obtain the CNT of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 60% acetic acid of 40ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip of Patterned Carbon Nanotube put into, stands 2h；
B. substrate growth being had the heavy doping silicon chip of CNT is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip ozone clean 20min that will obtain in step S1～S5, in covering, the ceramic mask of electrode, then puts in magnetic control sputtering device by heavy doping silicon chip, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode of Au layer, and wherein, the thickness of Au layer is about 100nm；
S7: welding encapsulation: make upper electrode and bottom electrode connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
Test data:
CNT capacity type wet dependent sensor is placed on a metal sealing chamber (1m3) in, metal sealing chamber is with air inlet and gas outlet。During test, digital electric bridge output frequency is 50Hz, and test temperature is 20 DEG C, then controls relative humidity variations and ranges for 5%～95%, reads capacitance with humidity situation of change；
The sensitivity definition of this CNT capacity type wet dependent sensor is: CRH-C11/ C11× 100%, wherein CRHFor the sensor capacitance value obtained under test environment humidity, C11Capacitance for relative humidity 11% lower sensor。The response of this CNT capacity type wet dependent sensor or be defined as testing capacitor value recovery time and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
Test finds, under the relative humidity of 95%, sensitivity up to 2281, optimal response and recovery time respectively 12s and 29s, and through 2000 retests, the pad value of its electric capacity is less than 10%。The electric capacity of this CNT capacitance type sensor is good with envionmental humidity linear change, highly sensitive, fast response time, good stability。
Embodiment 5
A kind of mould of plastics for the detection of molten plastic water content, the outside of described mould of plastics cover half part is provided with moisture sensor module, and this moisture sensor module includes the heavy doping silicon chip laid successively from top to bottom, the SiO being close to heavy doping silicon chip2Layer, carbon nanotube layer, it is positioned at SiO2The bottom electrode of interlayer and the upper electrode being positioned on carbon nanotube layer, described carbon nanotube layer is grown on SiO2On layer；Described bottom electrode has metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 80nm, 160nm and 600nm；Described carbon nanotube layer adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode and upper electrode are connected to a micro-control processor for connecting with client communication。
Further, the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip, puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO at heavy doping silicon chip surface2Layer；
S2: bottom electrode makes: have SiO by what prepare in step S12The heavy doping silicon chip of layer uses acetone, ethanol, deionized water to clean 15min post-drying successively, at its surface spin coating photoresist (low speed 900rpm, 15s；High speed 3500rpm, 50s), use bottom electrode mask to its exposure, development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer, etches 30min, will etch SiO2Heavy doping silicon chip after layer cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. use Fe/Ni nanoparticle as the catalyst of carbon nano tube growth, first, to the heavy doping silicon chip spin coating photoresist with bottom electrode, adopt the localization mask of catalyst that it is exposed, be then passed through development, clean standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 200mg, 50mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip, the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip, obtain the CNT of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 30% acetic acid of 60ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip of Patterned Carbon Nanotube put into, stands 2h；
B. substrate growth being had the heavy doping silicon chip of CNT is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip ozone clean 20min that will obtain in step S1～S5, in covering, the ceramic mask of electrode, then puts in magnetic control sputtering device by heavy doping silicon chip, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode of Au layer, and wherein, the thickness of Au layer is about 200nm；
S7: welding encapsulation: make upper electrode and bottom electrode connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
Test data: CNT capacity type wet dependent sensor is placed on a metal sealing chamber (1m3) in, metal sealing chamber is with air inlet and gas outlet。During test, digital electric bridge output frequency is 50Hz, and test temperature is 20 DEG C, then controls relative humidity variations and ranges for 5%～95%, reads capacitance with humidity situation of change；
The sensitivity definition of this CNT capacity type wet dependent sensor is: CRH-C11/ C11× 100%, wherein CRHFor the sensor capacitance value obtained under test environment humidity, C11Capacitance for relative humidity 11% lower sensor。The response of this CNT capacity type wet dependent sensor or be defined as testing capacitor value recovery time and reach the time used by total variation 80% at the variable quantity of 11%RH to 75%RH；
Test finds, under the relative humidity of 95%, sensitivity up to 1748, optimal response and recovery time respectively 15s and 27s, and through 2000 retests, the pad value of its electric capacity is less than 10%。The electric capacity of this CNT capacitance type sensor is good with envionmental humidity linear change, highly sensitive, fast response time, good stability。
The above; it is only the present invention preferably detailed description of the invention; but protection scope of the present invention is not limited thereto; any those familiar with the art is in the technical scope that the invention discloses; technological invention and inventive concept thereof according to the present invention are equal to replacement or are changed, and all should be encompassed within protection scope of the present invention。
Claims (3)
1. the mould of plastics for the detection of molten plastic water content, it is characterized in that, the cover half part of described mould of plastics is provided with moisture sensor module, and this moisture sensor module includes the heavy doping silicon chip (1) laid successively from top to bottom, the SiO being close to heavy doping silicon chip (1)2Layer (2), carbon nanotube layer (4), be positioned at SiO2Bottom electrode (3) between layer (2) and the upper electrode (5) that is positioned on carbon nanotube layer (4), described carbon nanotube layer (4) is grown on SiO2On layer (2)；Described bottom electrode (3) is metallic film, described metallic film be followed successively by from inside to outside have the Cr layer of adhesion, conductive and heat-conductive Cu layer and as the Au layer of electrode layer, the thickness of described Cr layer, Cu layer and Au layer is followed successively by 50nm, 250nm and 500nm；Described carbon nanotube layer (4) adopts catalyst and/or photoetching process to realize the growth of its localization, described carbon nanotube layer (4) using plasma after growth makes it produce hydroxyl modified, and carbon nanotube layer (4) have passed through the process of acetic acid and the hydrogen peroxide mixed solution adding trace tungsten powder before plasma hydroxyl modified；The surface of described metallic film is glued with the bacterial enzyme rete of sensing bacterial growth, and this bacterial enzyme rete and metallic film collectively form the antibacterial wet sensitive sensor of sensing moisture；Described bottom electrode (3) and upper electrode (5) are connected to a micro-control processor for connecting with client communication。
2. a kind of mould of plastics for the detection of molten plastic water content according to claim 1, it is characterised in that the making of described moisture sensor comprises the following steps:
S1:SiO2Layer makes: takes described heavy doping silicon chip (1), puts it in tube furnace, according to the ramp to 500 DEG C of 10 DEG C/min, is incubated 12h, then naturally cools to room temperature, can form SiO on heavy doping silicon chip (1) surface2Layer (2)；
S2: bottom electrode makes: have SiO by what prepare in step (1)2The heavy doping silicon chip (1) of layer (2) uses acetone, ethanol, deionized water cleaning 15min post-drying successively, at its surface spin coating photoresist, uses bottom electrode mask to its exposure, and development, drying after 120 DEG C of drying 2min, at CHF3Dry etching SiO under atmosphere2Layer (2), etches 30min, will etch SiO2Heavy doping silicon chip (1) after layer (2) cleaning is put in magnetic control sputtering device, lower than 1.5 × 10-3Magnetron sputtering C r layer, Cu layer and Au layer successively under pa vacuum；By fixing for bottom electrode (1) surface of good for magnetron sputtering Cr layer, Cu layer and Au layer upper antibacterial enzyme membrane, then clean photoresist；The size of described heavy doping silicon chip (1) is 2cm × 2cm；
S3: gas blowout catalyst film, step is as follows:
A. the catalyst that Fe/Ni nanoparticle grows is used as CNT (4), first, to heavy doping silicon chip (1) the spin coating photoresist with bottom electrode (3), adopt the localization mask of catalyst that it is exposed, it is then passed through development, cleans standby；
B. the dispersion liquid of catalyst Fe/Ni is prepared: weigh Fe nanoparticle and the Ni nanoparticle of 200mg, 50mg respectively, be added into the 98%H of 60ml2SO4With the 69% of 40ml HNO3In mixed solution, ultrasonic 3h in 80 DEG C of water-baths, filters after then cleaning with deionized water, obtain the Fe/Ni mix nanoparticles dried, then weigh the Fe/Ni nanoparticle of 100mg, add in the deionized water of 500ml, after being sufficiently stirred for, obtain the dispersion liquid of Fe/Ni mix nanoparticles；
C. use high pure nitrogen as gas blowout carrier, regulate the horizontal and vertical distance between airbrush and heavy doping silicon chip (1), the solvent making dispersion liquid just volatilizees when arriving on substrate and is as the criterion, gas blowout 5 times, each gas blowout 20s, makes the mix nanoparticles thin film of catalyst Fe/Ni that one layer of uniform thickness of formation is about 20nm；
S4:CVD method growth CNT:
CNT (4) reactant gas source is CH4And H2Mixing gas, first the heavy doping silicon chip (1) with patterned catalyst particle is carried out, remove photoresist, put in reaction chamber；Then evacuation, passes into hydrogen after reaching vacuum requirement, apply microwave and make generation plasma in reflection chamber；Heating substrate reaches certain temperature and keeps 40min, passes into methane gas, and now CNT (4) starts growth；In growth course lumen, vacuum remains unchanged；Through about 10min, close microwave source and radio heater, stop passing into methane gas, close hydrogen, pass into argon, take out the substrate of heavy doping silicon chip (1), obtain the CNT (4) of patterning；
S5: Surface Modification of Carbon Nanotube By Plasma:
A. first the hydrogen peroxide of the 10% of 60% acetic acid of 40ml and 20ml is put into beaker, be sufficiently mixed, add trace tungsten powder wherein, then growth has the substrate of the heavy doping silicon chip (1) of Patterned Carbon Nanotube (4) put into, stand 2h；
B. substrate growth being had the heavy doping silicon chip (1) of CNT (4) is sent in plasma generator, is evacuated to 1.0 × 10-1Below pa, then with noble gas N2For carrier gas, by reactant ammonia with N2Air-flow is brought in instrument, makes air-flow velocity stable at 20mL/min, waits 1h, open power source, regulate to 50W, instrument produces aura, under action of plasma, gas molecule valence link be destroyed, great amount of hydroxy group produce, CNT (4) in the environment of acetic acid and hydrogen peroxide through the effect of tungsten powder, the hydroxyl modified that CNT is generated, after Cement Composite Treated by Plasma 30min, close power source, take out substrate；
S6: electrode in preparation: the heavy doping silicon chip (1) obtained in step S1～S5 is used ozone clean 20min, the ceramic mask of electrode (5) in covering, then heavy doping silicon chip (1) is put in magnetic control sputtering device, lower than 1.5 × 10-3Under pa vacuum, sputtering has the upper electrode (5) of Au layer, and wherein, the thickness of Au layer is about 200nm；
S7: welding encapsulation: make upper electrode (5) and bottom electrode (3) connect with lead-in wire respectively, described moisture sensor is packaged, and digital electric bridge is welded with CNT capacity type wet dependent sensor, digital electric bridge is used for reading the capacitance variations of moisture sensor under humidity changing environment, demarcates water vapor concentration with this。
3. a kind of mould of plastics for the detection of molten plastic water content according to claim 2, it is characterised in that in described step S2, the parameter of spin coating photoresist is provided that low speed 900rpm, 15s；High speed 3500rpm, 50s。
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| US20100065190A1 (en) * | 2008-09-12 | 2010-03-18 | Tsinghua University | Method for making composite material having carbon nanotube array |
| CN102103115A (en) * | 2011-01-26 | 2011-06-22 | 山东理工大学 | Method for manufacturing electrochemical acetylcholinesterase biological sensor |
| WO2015012186A1 (en) * | 2013-07-25 | 2015-01-29 | 東レ株式会社 | Carbon nanotube composite, semiconductor device, and sensor using same |
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