CN106290273B - A kind of equipment of the dangerous solid waste analyte detection for building field - Google Patents
A kind of equipment of the dangerous solid waste analyte detection for building field Download PDFInfo
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- CN106290273B CN106290273B CN201610594959.1A CN201610594959A CN106290273B CN 106290273 B CN106290273 B CN 106290273B CN 201610594959 A CN201610594959 A CN 201610594959A CN 106290273 B CN106290273 B CN 106290273B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/02—Mechanical
Abstract
The invention discloses a kind of equipment of dangerous solid waste analyte detection for building field, including detection device ontology；The inside of the detection device ontology is disposed with heat-resistant layer, insulating layer and heat preservation channel from inside to outside；The side of the detection device ontology is provided with an air inlet, and the other side is provided with an exhaust outlet；The air inlet is provided with the first temperature control device, and the second temperature control device and detector are provided at the exhaust outlet；The center of inside position of the detection device ontology is provided with filter device.
Description
Technical field
The present invention relates to building fields, are more particularly to a kind of setting for dangerous solid waste analyte detection for building field
It is standby.
Background technique
In building construction process, excavate the processes such as landfill due to being frequently necessary to carry out, in the process, it is often in need
Solid waste landfill carries out excavating the operation such as construction, and some solid waste contain toxic, flammability, explosivity, put
The pernicious gas of penetrating property, corrosivity etc. can generate such hazardous gas, to the testing requirements sensitivity of such hazardous gas,
Stability etc. is higher.
Summary of the invention
A kind of danger for building field is provided it is an object of the invention to avoid shortcoming in the prior art
The equipment of solid waste analyte detection.
The purpose of the present invention is achieved through the following technical solutions：A kind of dangerous solid waste analyte detection for building field
Equipment, including detection device ontology；The inside of the detection device ontology is disposed with heat-resistant layer, insulating layer from inside to outside
And heat preservation channel；The side of the detection device ontology is provided with an air inlet, and the other side is provided with an exhaust outlet；It is described
Air inlet is provided with the first temperature control device, and the second temperature control device and detector are provided at the exhaust outlet；The inspection
The center of inside position of measurement equipment ontology is provided with filter device.
Embodiment provided by the invention solves above-mentioned technical problem.
Detailed description of the invention
The drawings herein are incorporated into the specification and forms part of this specification, and shows and meets implementation of the invention
Example, and be used to explain the principle of the present invention together with specification.
Fig. 1 is structural schematic diagram of the invention.
Fig. 2 is the structural schematic diagram for the detector that the present invention shown according to an exemplary embodiment uses.
The structural schematic diagram for the sensitive blocks that Fig. 3 present invention shown according to an exemplary embodiment uses.
Fig. 4 is the preparation process flow block diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses.
Wherein：1- silicon wafer, 2- silicon nitride layer, 3-Cr film layer, 4-PANI film, 5-Ni film, 6-HKUST-1 film, 7-BSP film,
8- detection device ontology, 9- heat-resistant layer, 10- sensitive blocks, 11- insulating layer, 12- heat preservation channel, 13,19- solenoid valve, 14- into
Air port, the first temperature control device of 15-, 16- filter device, 17- detector, 18- exhaust outlet, 20- data read module, 21-
Second temperature control device.
Specific embodiment
Example embodiments are described in detail here, and the example is illustrated in the accompanying drawings.Following description is related to
When attached drawing, unless otherwise indicated, the same numbers in different drawings indicate the same or similar elements.Following exemplary embodiment
Described in embodiment do not represent all embodiments consistented with the present invention.On the contrary, they be only with it is such as appended
The example of device and method being described in detail in claims, some aspects of the invention are consistent.
In the description of the present application, it should be noted that unless otherwise specified and limited, term " installation ", " connected ",
" connection " shall be understood in a broad sense, for example, it may be mechanical connection or electrical connection, the connection being also possible to inside two elements can
, can also indirectly connected through an intermediary, for the ordinary skill in the art to be to be connected directly, it can basis
Concrete condition understands the concrete meaning of above-mentioned term.
With economic fast development and industrial expansion, can not only be generated in industry manufacture production process various
The exhaust gas of various kinds can also generate various gases in manufactured various instruments in use, and the generation of these gases not only can
The use of instrument itself is influenced, and the potential threat of environmental pollution can be become.
Therefore, it is necessary to look for a kind of equipment that can monitor the gas that various instruments generate in use, and can
With the gas sensor of timely feedback monitoring to gas data.
The method of conventional detection gas is to acquire gas at the scene, is stored in clean sample devices, is then sent to
Laboratory, using in the detection gas such as various instruments, such as GC, GC/MS or LC/MS ingredient and it is quantitative the problems such as, however,
Above-mentioned detection method not only needs a large amount of sample collector to carry out spot sampling, consumes a large amount of manpower and material resources, and in sample
In product transportational process, it is frequently present of contaminated problem, the gaseous sample to laboratory is sent to be unable to existing for reactor tool at all
Problem or its harmfulness to environmental functional unable to monitor.
In existing report, has existed and gas detection sensor is made come detection gas using inorganic material film, but
It is that above-mentioned gas sensor has the following problems：The membrane material service life of use is short, and when humidity is biggish in the environment
It waits, is easy failure, its effect cannot be played well.Therefore, need to find one kind can on a large scale it is sensitive to hydrone and
It can monitor and separate in time the material of measured target gas station.
Metal-organic framework materials (MOFs) are the bonding modes and one for passing through coordinate bond by metal ion or metal cluster
What a little organic ligands combinations were formed, due to the difference of metal ion or organic ligand, various topological structures can be shown.
MOFs itself has many advantages, such as that pore size is adjustable, specific surface area is high, in gas-liquid separation, catalysis, light, electricity, gas sensing etc.
Aspect has potential using value.Wherein HKUST-1 is a kind of typical metal-organic framework materials, very quick to hydrogen
Sense, when it is contacted with hydrogen, the skeleton flexibility of HKUST-1 can become due to sucking different guest molecules in duct
Change, this variation can cause the variation of its unit cell again, and the variation of unit cell eventually results in the change of HKUST-1 film resistance, lead to
The concentration variation of hydrogen to be measured can sensitively be reacted by crossing measurement resistance.
The present invention is based on resistor-type HKUST-1 membrane materials, design hydrogen gas sensor, the fork using Cr film as sensitive blocks
Refer to electrode layer, the catalyst that Ni film forms a film as HKUST-1.
In conjunction with following application scenarios, the invention will be further described.
Application scenarios 1
Fig. 1 is a kind of dangerous solid waste analyte detection for building field shown according to an exemplary application scene
The structural schematic diagram of equipment, as shown in Figure 1, the detection device includes detection device ontology 8；The detection device ontology 8
Inside is disposed with heat-resistant layer 9, insulating layer 11 and heat preservation channel 12 from inside to outside；The side of the detection device ontology 8 is set
It is equipped with an air inlet 14, the other side is provided with an exhaust outlet 18；The first temperature control device 15 is provided at the air inlet 14,
The second temperature control device 21 and detector 17 are provided at the exhaust outlet 18；The center of inside of the detection device ontology 8
Position is provided with filter device 16.
Embodiment provided by the invention solves above-mentioned technical problem.
Preferably, the air inlet 14 is located at the bottom of the detection device ontology 8.
Preferably, the exhaust outlet 18 is located at the top of the detection device ontology 8.
Preferably, the air inlet 14 is located at the left side of the detection device ontology 8, and the exhaust outlet 18 is located at the inspection
The right side of measurement equipment ontology 8.
Preferably, the cross section of the detection device ontology 8 is one of cylinder, rectangle, square.
Fig. 2 is the structural schematic diagram of the detector 17 used according to the present invention shown in an exemplary application scene.
As shown in Fig. 2, the detector 17 includes sensitive blocks 10 and data read module 20, the sensitive blocks 10 are placed on
Hollow structure is in the shell of air hole.
The structural schematic diagram for the sensitive blocks that Fig. 3 is used according to the present invention shown in an exemplary application scene, such as Fig. 3 institute
Show, which includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；The silicon chip substrate includes
Silicon wafer 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 are used as insulating layer, and Cr film layer 3 is used as interdigital electrode layer；The Ni film 5
It is prepared using magnetron sputtering method, with a thickness of 10nm；The thickness of the HKUST-1 film 6 is about 2~60 μm；The Cr film layer 3 and number
It is conductively connected according to read module 20.
Fig. 4 is the preparation process flow frame of the sensitive blocks used according to the present invention shown in an exemplary application scene
Figure, as shown in figure 4, the production of the sensitive blocks 10 includes the following steps：
Step 1 prepares silicon chip substrate：
N-type silicon chip is taken, cut size is 5cm × 1cm, successively by acetone, ethyl alcohol, deionized water ultrasonic cleaning, ultrasound
Time is 30min, is then dried up with nitrogen gun；The silicon wafer cleaned is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 200nm；By Wafer Cleaning, one layer photoresist of spin coating, photoresist parameter is low speed 900rpm spin coating 13s, high speed
4500rpm spin coating 50s；Then interdigital electrode mask is covered, 7s is exposed, develop 65s；It is put into magnetic control sputtering device, magnetic control splashes
Cr film is penetrated, as interdigital electrode layer, with a thickness of 500nm, then washes silicon chip surface photoresist；
Step 2 prepares microcavity：
The silicon chip substrate that will be handled through step 1, it is first with 75% ethanol solution that its surface wipes are clean, using flame plus
Silicon chip substrate is placed on flame by thermal method, since one end, is drawn once at interval of 1cm, to form the microcavity of 2 cone cells；It is micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the detectability of the detection device is enhanced, and makes its suction to hydrogen
It is attached very competent；
Step 3 prepares PANI film：
It takes a certain amount of polyaniline to be dissolved in dimethylformamide and forms saturated solution, will be satisfied using spin coating-czochralski method
It is spun to the surface through the processed silicon chip substrate of step 2 with solution, the speed of spin coating is 3000rpm, then spin coating 10s exists
It is dried overnight in 100 DEG C of baking oven, obtains PANI film on silicon chip substrate surface；
The type gas sense module of use is due to being based on resistive type metal-organic framework materials, and metal-organic framework materials
It forms a film on polyaniline film, since polyaniline has strong electric conductivity, further enhance the spirit of type gas sense module
Sensitivity, and then reinforce the detection device significantly the sensitivity of gas；
Step 4 prepares HKUST-1 film：
1) silicon chip substrate is put into magnetron sputtering, base vacuum is lower than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 10nm
5, silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g is completely dissolved colorless and transparent molten in another small beaker with 19.2mL ethyl alcohol
Liquid weighs Cu (NO3)2·3H2O 0.7g is in small beaker, with 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour into Cu (NO3)2·3H2Half an hour is stirred in O solution, obtains HKUST-1 mother liquor azury；Prepared HKUST-1 is female
Liquid and silicon chip substrate are placed in the reaction kettle of 50mL, synthesize MOF film using hydrothermal synthesis method, reaction temperature is 135 DEG C, reaction 2
After it, after being taken out silicon chip substrate with tweezers several times with methanol repeated flushing, dried 1 hour in 100 DEG C, in silicon chip substrate
To the HKUST-1 film of blue, the thickness of HKUST-1 film is about 2~60 μm；
Due to using the Ni layers of catalyst as metal-organic framework materials film forming, the Ni film meeting on the surface PANI and HKUST-
Therefore on the one hand 1 film reaction promotes the film forming of HKUST-1, on the other hand improve the combination of PANI film and HKUST-1 film
Performance makes that film layer is combined to have stronger stability, so that the sensing performance for the type gas sense module being thus prepared
It is more stable；
Step 5 prepares BSP film：
1) BSP sub-micrometer rod is grown：In(NO3)3·x H2O (0.08g) and H3BTC (0.068g) is added to mixed solvent
H2O/DMF(1:1,10mL) in, 10min is stirred at room temperature, solution A is made, by photochromic compounds BSP
(0.057mmol) is added in solution A, and dark place is stirred 1 hour；
2) it forms a film：BSP solution is revolved and is formed a film on Tu silicon wafer/PANI/HKUST-1 film, the speed for revolving Tu is 5000rpm, rotation
The Tu time is 5 seconds；
Due to joined on its surface with fluorescence property in the preparation process for the gas sensitization module that it is used
BSP photochromic molecule, the photochromic molecule can issue fluorescence in there are inflammable and explosive hazardous environment, make this under electromagnetism excitation
Detection device can be realized the flammable explosive gas in qualitative and quantitative detection environment including hydrogen, can make to cause danger
A possibility that situation, reduces；
Step 5, sensitive blocks assembling：
Silicon chip substrate is put into hollow structure shell, wafer sections downward, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon wafer.Since the manufacturing process of the sensitive blocks is very simple and convenient and
Fast, a large amount of man power and material can be saved, the potentiality with large-scale industrial production.
Experiment test：
(1) experiments Hydrogen：25 ± 2 DEG C of conditions each lead into the nitrogen of air, hydrogen and hydrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 1ppm hydrogen, gas sensor signal
Value changes to rapidly 1.0mV in 10s, and tends towards stability in signal value in 20s；Air is passed through after 1min, signal value is in 5s
Return to 0 value and in tending towards stability in 30s；By 2000 stability tests, data variation rate is less than 10%；Test result is aobvious
Show that the solid waste detection device has good response performance to hydrogen.
(2) ammonia is tested：25 ± 2 DEG C of conditions each lead into air ammonia and the nitrogen containing ammonia, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 100ppm ammonia, gas sensor letter
Number value changes to rapidly 5.0mV in 10s, and tends towards stability in signal value in 1min；Be passed through air after 5min, signal value in
0 value is returned in 10s and in tending towards stability in 0.5min；By 2000 stability tests, data variation rate is less than 10%；It surveys
Test result shows that the solid waste detection device has good response performance to ammonia.
(3) hydrogen sulfide is tested：25 ± 2 DEG C of conditions each lead into air and hydrogen sulfide containing nitrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 0.05ppm hydrogen sulfide gas, gas passes
Sensor signal value changes to rapidly 3.0mV in 10s, and tends towards stability in signal value in 30s；Air, signal are passed through after 5min
It is worth in returning to 0 value in 5s and in tending towards stability in 10s；By 2000 stability tests, data variation rate is less than 10%；It surveys
Test result shows that the solid waste detection device has good response performance to hydrogen sulfide gas.
The experimental results showed that：The sensitive blocks poisonous and hazardous gas also this to ammonia and hydrogen sulfide has very strong quick
Sense and selection performance, are improved the detection device all to the susceptibility of toxic and harmful gas and selectivity, reduce production
Risk.
Application scenarios 2：
Fig. 1 is a kind of dangerous solid waste analyte detection for building field shown according to an exemplary application scene
The structural schematic diagram of equipment, as shown in Figure 1, the detection device includes detection device ontology 8；The detection device ontology 8
Inside is disposed with heat-resistant layer 9, insulating layer 11 and heat preservation channel 12 from inside to outside；The side of the detection device ontology 8 is set
It is equipped with an air inlet 14, the other side is provided with an exhaust outlet 18；The first temperature control device 15 is provided at the air inlet 14,
The second temperature control device 21 and detector 17 are provided at the exhaust outlet 18；The center of inside of the detection device ontology 8
Position is provided with filter device 16.
Embodiment provided by the invention solves above-mentioned technical problem.
Preferably, the air inlet 14 is located at the bottom of the detection device ontology 8.
Preferably, the exhaust outlet 18 is located at the top of the detection device ontology 8.
Preferably, the air inlet 14 is located at the left side of the detection device ontology 8, and the exhaust outlet 18 is located at the inspection
The right side of measurement equipment ontology 8.
Preferably, the cross section of the detection device ontology 8 is one of cylinder, rectangle, square.
Fig. 2 is the structural schematic diagram of the detector used according to the present invention shown in an exemplary application scene.Such as
Shown in Fig. 2, the detector 17 includes sensitive blocks 10 and data read module 20, during the sensitive blocks 10 are placed on
Hollow structure is in the shell of air hole.
Fig. 3 is the structural schematic diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses, such as Fig. 3 institute
Show, which includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；The silicon chip substrate includes
Silicon wafer 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 are used as insulating layer, and Cr film layer 3 is used as interdigital electrode layer；The Ni film 5
It is prepared using magnetron sputtering method, with a thickness of 8nm；The thickness of the HKUST-1 film 6 is about 10 μm；The Cr film layer 3 is read with data
Modulus block 20 is conductively connected.
Fig. 4 is the preparation process flow block diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses,
As shown in figure 4, the production of the sensitive blocks 10 includes the following steps：
Step 1 prepares silicon chip substrate：
N-type silicon chip is taken, cut size is 5cm × 1cm, successively by acetone, ethyl alcohol, deionized water ultrasonic cleaning, ultrasound
Time is 30min, is then dried up with nitrogen gun；The silicon wafer cleaned is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 210nm；By Wafer Cleaning, one layer photoresist of spin coating, photoresist parameter is low speed 900rpm spin coating 13s, high speed
4500rpm spin coating 50s；Then interdigital electrode mask is covered, 7s is exposed, develop 65s；It is put into magnetic control sputtering device, magnetic control splashes
Cr film is penetrated, as interdigital electrode layer, with a thickness of 510nm, then washes silicon chip surface photoresist；
Step 2 prepares microcavity：
The silicon chip substrate that will be handled through step 1, it is first with 75% ethanol solution that its surface wipes are clean, using flame plus
Silicon chip substrate is placed on flame by thermal method, since one end, is drawn once at interval of 1cm, to form the microcavity of 2 cone cells；It is micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the detectability of the detection device is enhanced, and makes its suction to hydrogen
It is attached very competent；
Step 3 prepares PANI film：
It takes a certain amount of polyaniline to be dissolved in dimethylformamide and forms saturated solution, will be satisfied using spin coating-czochralski method
It is spun to the surface through the processed silicon chip substrate of step 2 with solution, the speed of spin coating is 3000rpm, then spin coating 10s exists
It is dried overnight in 100 DEG C of baking oven, obtains PANI film on silicon chip substrate surface；Step 4 prepares HKUST-1 film：
1) silicon chip substrate is put into magnetron sputtering, base vacuum is lower than 1.5 × 10-3The Ni film 5 of Pa, magnetron sputtering 8nm,
Silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g is completely dissolved colorless and transparent molten in another small beaker with 19.2mL ethyl alcohol
Liquid weighs Cu (NO3)2·3H2O 0.7g is in small beaker, with 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour into Cu (NO3)2·3H2Half an hour is stirred in O solution, obtains HKUST-1 mother liquor azury；Prepared HKUST-1 is female
Liquid and silicon chip substrate are placed in the reaction kettle of 50mL, synthesize MOF film using hydrothermal synthesis method, reaction temperature is 135 DEG C, reaction 2
After it, after being taken out silicon chip substrate with tweezers several times with methanol repeated flushing, dried 1 hour in 100 DEG C, in silicon chip substrate
To the HKUST-1 film of blue, the thickness of HKUST-1 film is about 2~60 μm；Due to being used as metal-organic framework materials using Ni layers
The Ni film of the catalyst of film forming, the surface PANI can be with HKUST-1 film reaction, and therefore, the rate of film build of one side HKUST-1 improves
10%, another aspect PANI film and the binding performance of HKUST-1 film improve 5%, make that film layer is combined to have stronger stability,
So that the sensing performance for the type gas sense module being thus prepared is more stable；
Step 5 prepares BSP film：
1) BSP sub-micrometer rod is grown：In(NO3)3·x H2O (0.08g) and H3BTC (0.068g) is added to mixed solvent
H2O/DMF(1:1,10mL) in, 10min is stirred at room temperature, solution A is made, by photochromic compounds BSP
(0.057mmol) is added in solution A, and dark place is stirred 1 hour；
2) it forms a film：BSP solution is revolved and is formed a film on Tu silicon wafer/PANI/HKUST-1 film, the speed for revolving Tu is 5000rpm, rotation
The Tu time is 5 seconds；
Due to joined on its surface with fluorescence property in the preparation process for the gas sensitization module that it is used
BSP photochromic molecule, the photochromic molecule can issue fluorescence in there are inflammable and explosive hazardous environment, make this under electromagnetism excitation
Detection device can be realized the flammable explosive gas in qualitative and quantitative detection environment including hydrogen, can make to cause danger
A possibility that situation, reduces 10%；
Step 5, sensitive blocks assembling：
Silicon chip substrate is put into hollow structure shell, wafer sections downward, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon wafer.Since the manufacturing process of the sensitive blocks is very simple and convenient and
Fast, a large amount of man power and material can be saved, the potentiality with large-scale industrial production.
Experiment test：
(1) hydrogen is tested：25 ± 2 DEG C of conditions, each lead into the nitrogen of air and hydrogen, flow velocity 1000ml/min,
Load resistance is 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 10ppm hydrogen, gas sensor signal value exists
3.0mV is changed in 8s rapidly, and is tended towards stability in signal value in 30s；It is passed through air after 1min, signal value is in returning to 0 in 10s
Value and in tending towards stability in 1min；By 2000 stability tests, data variation rate is less than 10%.Test result shows this
Solid waste detection device has good response performance to hydrogen.
(2) ammonia is tested：25 ± 2 DEG C of conditions each lead into air ammonia and the nitrogen containing ammonia, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 200ppm ammonia, gas sensor letter
Number value changes to rapidly 10.0mV in 5s, and tends towards stability in signal value in 1min；Be passed through air after 5min, signal value in
0 value is returned in 10s and in tending towards stability in 0.5min；By 2000 stability tests, data variation rate is less than 10%.It surveys
Test result shows that the solid waste detection device has good response performance to ammonia.
(3) hydrogen sulfide is tested：25 ± 2 DEG C of conditions each lead into air and hydrogen sulfide containing nitrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 0.1ppm ammonia, gas sensor letter
Number value changes to rapidly 5.0mV in 7s, and tends towards stability in signal value in 30s；Air is passed through after 5min, signal value is in 5s
Return to 0 value and in tending towards stability in 0.5min；By 2000 stability tests, data variation rate is less than 10%.Test knot
Fruit shows that the solid waste detection device has good response performance to hydrogen sulfide gas.
The experimental results showed that：The sensitive property of the sensitive blocks poisonous and hazardous gas also this to ammonia and hydrogen sulfide increases
Strong 5% and selection performance improve 8%, mention the detection device all to the susceptibility of toxic and harmful gas and selectivity
Height reduces the risk of production.
Application scenarios 3：
Fig. 1 is a kind of dangerous solid waste analyte detection for building field shown according to an exemplary application scene
The structural schematic diagram of equipment, as shown in Figure 1, the detection device includes detection device ontology 8；The detection device ontology 8
Inside is disposed with heat-resistant layer 9, insulating layer 11 and heat preservation channel 12 from inside to outside；The side of the detection device ontology 8 is set
It is equipped with an air inlet 14, the other side is provided with an exhaust outlet 18；The first temperature control device 15 is provided at the air inlet 14,
The second temperature control device 21 and detector 17 are provided at the exhaust outlet 18；The center of inside of the detection device ontology 8
Position is provided with filter device 16.
Embodiment provided by the invention solves above-mentioned technical problem.
Preferably, the air inlet 14 is located at the bottom of the detection device ontology 8.
Preferably, the exhaust outlet 18 is located at the top of the detection device ontology 8.
Preferably, the air inlet 14 is located at the left side of the detection device ontology 8, and the exhaust outlet 18 is located at the inspection
The right side of measurement equipment ontology 8.
Preferably, the cross section of the detection device ontology 8 is one of cylinder, rectangle, square.
Fig. 2 is the structural schematic diagram of the detector used according to the present invention shown in an exemplary application scene.Such as
Shown in Fig. 2, the detector 17 includes sensitive blocks 10 and data read module 20, during the sensitive blocks 10 are placed on
Hollow structure is in the shell of air hole.
Fig. 3 is the structural schematic diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses, such as Fig. 3 institute
Show, which includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；The silicon chip substrate includes
Silicon wafer 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 are used as insulating layer, and Cr film layer 3 is used as interdigital electrode layer；The Ni film 5
It is prepared using magnetron sputtering method, with a thickness of 12nm；The thickness of the HKUST-1 film 6 is about 20 μm；The Cr film layer 3 and data
Read module 20 is conductively connected.
Fig. 4 is the preparation process flow block diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses,
As shown in figure 4, the production of the sensitive blocks 10 includes the following steps：
Step 1 prepares silicon chip substrate：
N-type silicon chip is taken, cut size is 5cm × 1cm, successively by acetone, ethyl alcohol, deionized water ultrasonic cleaning, ultrasound
Time is 30min, is then dried up with nitrogen gun；The silicon wafer cleaned is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 220nm；By Wafer Cleaning, one layer photoresist of spin coating, photoresist parameter is low speed 900rpm spin coating 13s, high speed
4500rpm spin coating 50s；Then interdigital electrode mask is covered, 7s is exposed, develop 65s；It is put into magnetic control sputtering device, magnetic control splashes
Cr film is penetrated, as interdigital electrode layer, with a thickness of 550nm, then washes silicon chip surface photoresist；
Step 2 prepares microcavity：
The silicon chip substrate that will be handled through step 1, it is first with 75% ethanol solution that its surface wipes are clean, using flame plus
Silicon chip substrate is placed on flame by thermal method, since one end, is drawn once at interval of 1cm, to form the microcavity of 2 cone cells；It is micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the detectability of the detection device is enhanced, and makes its suction to hydrogen
It is attached very competent；
Step 3 prepares PANI film：
It takes a certain amount of polyaniline to be dissolved in dimethylformamide and forms saturated solution, will be satisfied using spin coating-czochralski method
It is spun to the surface through the processed silicon chip substrate of step 2 with solution, the speed of spin coating is 3000rpm, then spin coating 10s exists
It is dried overnight in 100 DEG C of baking oven, obtains PANI film on silicon chip substrate surface；Step 4 prepares HKUST-1 film：
1) silicon chip substrate is put into magnetron sputtering, base vacuum is lower than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 12nm
5, silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g is completely dissolved colorless and transparent molten in another small beaker with 19.2mL ethyl alcohol
Liquid weighs Cu (NO3)2·3H2O 0.7g is in small beaker, with 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour into Cu (NO3)2·3H2Half an hour is stirred in O solution, obtains HKUST-1 mother liquor azury；Prepared HKUST-1 is female
Liquid and silicon chip substrate are placed in the reaction kettle of 50mL, synthesize MOF film using hydrothermal synthesis method, reaction temperature is 135 DEG C, reaction 2
After it, after being taken out silicon chip substrate with tweezers several times with methanol repeated flushing, dried 1 hour in 100 DEG C, in silicon chip substrate
To the HKUST-1 film of blue, the thickness of HKUST-1 film is about 2~60 μm；Due to being used as metal-organic framework materials using Ni layers
The Ni film of the catalyst of film forming, the surface PANI can be with HKUST-1 film reaction, and therefore, the rate of film build of one side HKUST-1 improves
20%, another aspect PANI film and the binding performance of HKUST-1 film improve 10%, make that film layer is combined to have stronger stabilization
Property, so that the sensing performance for the type gas sense module being thus prepared is more stable；
Step 5 prepares BSP film：
1) BSP sub-micrometer rod is grown：In(NO3)3·x H2O (0.08g) and H3BTC (0.068g) is added to mixed solvent
H2O/DMF(1:1,10mL) in, 10min is stirred at room temperature, solution A is made, by photochromic compounds BSP
(0.057mmol) is added in solution A, and dark place is stirred 1 hour；
2) it forms a film：BSP solution is revolved and is formed a film on Tu silicon wafer/PANI/HKUST-1 film, the speed for revolving Tu is 5000rpm, rotation
The Tu time is 5 seconds；Due to joined on its surface with fluorescence property in the preparation process for the gas sensitization module that it is used
BSP photochromic molecule, which can issue fluorescence in there are inflammable and explosive hazardous environment, make under electromagnetism excitation
The detection device can be realized the flammable explosive gas in qualitative and quantitative detection environment including hydrogen, can make to endanger
A possibility that dangerous situation condition, reduces 15%；
Step 5, sensitive blocks assembling：
Silicon chip substrate is put into hollow structure shell, wafer sections downward, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon wafer.Since the manufacturing process of the sensitive blocks is very simple and convenient and
Fast, a large amount of man power and material can be saved, the potentiality with large-scale industrial production.
Experiment test：
(1) hydrogen is tested：25 ± 2 DEG C of conditions each lead into the nitrogen of air, hydrogen and hydrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 50ppm hydrogen, gas sensor signal
Value changes to rapidly 10.0mV in 5s, and tends towards stability in signal value in 1min；Air is passed through after 5min, signal value is in 40s
Inside return to 0 value and in tending towards stability in 1min；By 2000 stability tests, data variation rate is less than 10%.Test knot
Fruit shows that the solid waste detection device has good response performance to hydrogen.
(2) ammonia is tested：25 ± 2 DEG C of conditions each lead into air ammonia and the nitrogen containing ammonia, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 500ppm ammonia, gas sensor letter
Number value changes to rapidly 15.0mV in 2s, and tends towards stability in signal value in 1min；Be passed through air after 5min, signal value in
0 value is returned in 10s and in tending towards stability in 1.5min；By 2000 stability tests, data variation rate is less than 10%.It surveys
Test result shows that the solid waste detection device has good response performance to ammonia.
(3) hydrogen sulfide is tested：25 ± 2 DEG C of conditions each lead into air and hydrogen sulfide containing nitrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 1ppm ammonia, gas sensor signal
Value changes to rapidly 20.0mV in 3s, and tends towards stability in signal value in 1min；Air is passed through after 5min, signal value is in 10s
Inside return to 0 value and in tending towards stability in 1min；By 2000 stability tests, data variation rate is less than 10%.Test knot
Fruit shows that the solid waste detection device has good response performance to hydrogen sulfide gas.
The experimental results showed that：The sensitive property of the sensitive blocks poisonous and hazardous gas also this to ammonia and hydrogen sulfide increases
Strong 10% and selection performance improve 16%, obtain the detection device all to the susceptibility of toxic and harmful gas and selectivity
It improves, reduces the risk of production.
Application scenarios 4
Fig. 1 is a kind of dangerous solid waste analyte detection for building field shown according to an exemplary application scene
The structural schematic diagram of equipment, as shown in Figure 1, the detection device includes detection device ontology 8；The detection device ontology 8
Inside is disposed with heat-resistant layer 9, insulating layer 11 and heat preservation channel 12 from inside to outside；The side of the detection device ontology 8 is set
It is equipped with an air inlet 14, the other side is provided with an exhaust outlet 18；The first temperature control device 15 is provided at the air inlet 14,
The second temperature control device 21 and detector 17 are provided at the exhaust outlet 18；The center of inside of the detection device ontology 8
Position is provided with filter device 16.
Embodiment provided by the invention solves above-mentioned technical problem.
Preferably, the air inlet 14 is located at the bottom of the detection device ontology 8.
Preferably, the exhaust outlet 18 is located at the top of the detection device ontology 8.
Preferably, the air inlet 14 is located at the left side of the detection device ontology 8, and the exhaust outlet 18 is located at the inspection
The right side of measurement equipment ontology 8.
Preferably, the cross section of the detection device ontology 8 is one of cylinder, rectangle, square.
Fig. 2 is the structural schematic diagram of the detector used according to the present invention shown in an exemplary application scene.Such as
Shown in Fig. 2, the detector 17 includes sensitive blocks 10 and data read module 20, during the sensitive blocks 10 are placed on
Hollow structure is in the shell of air hole.
Fig. 3 is the structural schematic diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses, such as Fig. 3 institute
Show, which includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；The silicon chip substrate includes
Silicon wafer 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 are used as insulating layer, and Cr film layer 3 is used as interdigital electrode layer；The Ni film 5
It is prepared using magnetron sputtering method, with a thickness of 20nm；The thickness of the HKUST-1 film 6 is about 40 μm；The Cr film layer 3 and data
Read module 20 is conductively connected.
Fig. 4 is the preparation process flow block diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses,
As shown in figure 4, the production of the sensitive blocks 10 includes the following steps：
Step 1 prepares silicon chip substrate：
N-type silicon chip is taken, cut size is 5cm × 1cm, successively by acetone, ethyl alcohol, deionized water ultrasonic cleaning, ultrasound
Time is 30min, is then dried up with nitrogen gun；The silicon wafer cleaned is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 300nm；By Wafer Cleaning, one layer photoresist of spin coating, photoresist parameter is low speed 900rpm spin coating 13s, high speed
4500rpm spin coating 50s；Then interdigital electrode mask is covered, 7s is exposed, develop 65s；It is put into magnetic control sputtering device, magnetic control splashes
Cr film is penetrated, as interdigital electrode layer, with a thickness of 600nm, then washes silicon chip surface photoresist；
Step 2 prepares microcavity：
The silicon chip substrate that will be handled through step 1, it is first with 75% ethanol solution that its surface wipes are clean, using flame plus
Silicon chip substrate is placed on flame by thermal method, since one end, is drawn once at interval of 1cm, to form the microcavity of 2 cone cells；It is micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the detectability of the detection device is enhanced, and makes its suction to hydrogen
It is attached very competent；
Step 3 prepares PANI film：
It takes a certain amount of polyaniline to be dissolved in dimethylformamide and forms saturated solution, will be satisfied using spin coating-czochralski method
It is spun to the surface through the processed silicon chip substrate of step 2 with solution, the speed of spin coating is 3000rpm, then spin coating 10s exists
It is dried overnight in 100 DEG C of baking oven, obtains PANI film on silicon chip substrate surface；Step 4 prepares HKUST-1 film：
1) silicon chip substrate is put into magnetron sputtering, base vacuum is lower than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 10nm
5, silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g is completely dissolved colorless and transparent molten in another small beaker with 19.2mL ethyl alcohol
Liquid weighs Cu (NO3)2·3H2O 0.7g is in small beaker, with 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour into Cu (NO3)2·3H2Half an hour is stirred in O solution, obtains HKUST-1 mother liquor azury；Prepared HKUST-1 is female
Liquid and silicon chip substrate are placed in the reaction kettle of 50mL, synthesize MOF film using hydrothermal synthesis method, reaction temperature is 135 DEG C, reaction 2
After it, after being taken out silicon chip substrate with tweezers several times with methanol repeated flushing, dried 1 hour in 100 DEG C, in silicon chip substrate
To the HKUST-1 film of blue, the thickness of HKUST-1 film is about 2~60 μm；Due to being used as metal-organic framework materials using Ni layers
The Ni film of the catalyst of film forming, the surface PANI can be with HKUST-1 film reaction, and therefore, the rate of film build of one side HKUST-1 improves
30%, another aspect PANI film and the binding performance of HKUST-1 film improve 20%, make that film layer is combined to have stronger stabilization
Property, so that the sensing performance for the type gas sense module being thus prepared is more stable；
Step 5 prepares BSP film：
1) BSP sub-micrometer rod is grown：In(NO3)3·x H2O (0.08g) and H3BTC (0.068g) is added to mixed solvent
H2O/DMF(1:1,10mL) in, 10min is stirred at room temperature, solution A is made, by photochromic compounds BSP
(0.057mmol) is added in solution A, and dark place is stirred 1 hour；
2) it forms a film：BSP solution is revolved and is formed a film on Tu silicon wafer/PANI/HKUST-1 film, the speed for revolving Tu is 5000rpm, rotation
The Tu time is 5 seconds；Due to joined on its surface with fluorescence property in the preparation process for the gas sensitization module that it is used
BSP photochromic molecule, which can issue fluorescence in there are inflammable and explosive hazardous environment, make under electromagnetism excitation
The detection device can be realized the flammable explosive gas in qualitative and quantitative detection environment including hydrogen, can make to endanger
A possibility that dangerous situation condition, reduces 35%；
Step 5, sensitive blocks assembling：
Silicon chip substrate is put into hollow structure shell, wafer sections downward, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon wafer.Since the manufacturing process of the sensitive blocks is very simple and convenient and
Fast, a large amount of man power and material can be saved, the potentiality with large-scale industrial production.
Experiment test：
(1) hydrogen is tested：25 ± 2 DEG C of conditions each lead into the nitrogen of air, hydrogen and hydrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 1 00ppm hydrogen, gas sensor letter
Number value changes to rapidly 30.0mV in 3s, and tends towards stability in signal value in 20s；Air is passed through after 5min, signal value is in 20s
Inside return to 0 value and in tending towards stability in 2min；By 2000 stability tests, data variation rate is less than 10%.Test knot
Fruit shows that the solid waste detection device has good response performance to hydrogen.
(2) ammonia is tested：25 ± 2 DEG C of conditions each lead into air ammonia and the nitrogen containing ammonia, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 1000ppm ammonia, sensor signal value
It changes to 10.0mV rapidly in 2s, and tends towards stability in signal value in 2min；Air is passed through after 5min, signal value is in 10s
Return to 0 value and in tending towards stability in 2min；By 2000 stability tests, data variation rate is less than 10%.Test result
Show that the solid waste detection device has good response performance to ammonia.
(3) hydrogen sulfide is tested：25 ± 2 DEG C of conditions each lead into air and hydrogen sulfide containing nitrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 10ppm ammonia, sensor signal value exists
25.0mV is changed in 2s rapidly, and is tended towards stability in signal value in 2min；Air is passed through after 5min, signal value is in 40s times
To 0 value and in tending towards stability in 2min；By 2000 stability tests, data variation rate is less than 10%.Test result is aobvious
Show that the solid waste detection device has good response performance to hydrogen sulfide gas.
The experimental results showed that：The sensitive property of the sensitive blocks poisonous and hazardous gas also this to ammonia and hydrogen sulfide increases
Strong 20% and selection performance improve 30%, obtain the detection device all to the susceptibility of toxic and harmful gas and selectivity
It improves, reduces the risk of production.
Application scenarios 5
Fig. 1 is a kind of dangerous solid waste analyte detection for building field shown according to an exemplary application scene
The structural schematic diagram of equipment, as shown in Figure 1, the detection device includes detection device ontology 8；The detection device ontology 8
Inside is disposed with heat-resistant layer 9, insulating layer 11 and heat preservation channel 12 from inside to outside；The side of the detection device ontology 8 is set
It is equipped with an air inlet 14, the other side is provided with an exhaust outlet 18；The first temperature control device 15 is provided at the air inlet 14,
The second temperature control device 21 and detector 17 are provided at the exhaust outlet 18；The center of inside of the detection device ontology 8
Position is provided with filter device 16.
Embodiment provided by the invention solves above-mentioned technical problem.
Preferably, the air inlet 14 is located at the bottom of the detection device ontology 8.
Preferably, the exhaust outlet 18 is located at the top of the detection device ontology 8.
Preferably, the air inlet 14 is located at the left side of the detection device ontology 8, and the exhaust outlet 18 is located at the inspection
The right side of measurement equipment ontology 8.
Preferably, the cross section of the detection device ontology 8 is one of cylinder, rectangle, square.
Fig. 2 is the structural schematic diagram of the detector used according to the present invention shown in an exemplary application scene.Such as
Shown in Fig. 2, the detector 17 includes sensitive blocks 10 and data read module 20, during the sensitive blocks 10 are placed on
Hollow structure is in the shell of air hole.
Fig. 3 is the structural schematic diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses, such as Fig. 3 institute
Show, which includes silicon chip substrate, PANI film 4, Ni film 5, HKUST-1 film 6 and BSP film 7；The silicon chip substrate includes
Silicon wafer 1, silicon nitride film 2 and Cr film layer 3, silicon nitride film 2 are used as insulating layer, and Cr film layer 3 is used as interdigital electrode layer；The Ni film 5
It is prepared using magnetron sputtering method, with a thickness of 30nm；The thickness of the HKUST-1 film 6 is about 60 μm；The Cr film layer 3 and data
Read module 20 is conductively connected.
Fig. 4 is the preparation process flow block diagram for the sensitive blocks that the present invention shown according to an exemplary embodiment uses,
As shown in figure 4, the production of the sensitive blocks 10 includes the following steps：
Step 1 prepares silicon chip substrate：
N-type silicon chip is taken, cut size is 5cm × 1cm, successively by acetone, ethyl alcohol, deionized water ultrasonic cleaning, ultrasound
Time is 30min, is then dried up with nitrogen gun；The silicon wafer cleaned is put into PECVD device, deposits one layer of silicon nitride film,
Thickness about 400nm；By Wafer Cleaning, one layer photoresist of spin coating, photoresist parameter is low speed 900rpm spin coating 13s, high speed
4500rpm spin coating 50s；Then interdigital electrode mask is covered, 7s is exposed, develop 65s；It is put into magnetic control sputtering device, magnetic control splashes
Cr film is penetrated, as interdigital electrode layer, with a thickness of 700nm, then washes silicon chip surface photoresist；
Step 2 prepares microcavity：
The silicon chip substrate that will be handled through step 1, it is first with 75% ethanol solution that its surface wipes are clean, using flame plus
Silicon chip substrate is placed on flame by thermal method, since one end, is drawn once at interval of 1cm, to form the microcavity of 2 cone cells；It is micro-
Cavity configuration enhances the sensitivity of sensitive blocks, and then the detectability of the detection device is enhanced, and makes its suction to hydrogen
It is attached very competent；
Step 3 prepares PANI film：
It takes a certain amount of polyaniline to be dissolved in dimethylformamide and forms saturated solution, will be satisfied using spin coating-czochralski method
It is spun to the surface through the processed silicon chip substrate of step 2 with solution, the speed of spin coating is 3000rpm, then spin coating 10s exists
It is dried overnight in 100 DEG C of baking oven, obtains PANI film on silicon chip substrate surface；Step 4 prepares HKUST-1 film：
1) silicon chip substrate is put into magnetron sputtering, base vacuum is lower than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 30nm
5, silicon chip extracting is stand-by；
2) H is weighed3BTC 0.336g is completely dissolved colorless and transparent molten in another small beaker with 19.2mL ethyl alcohol
Liquid weighs Cu (NO3)2·3H2O 0.7g is in small beaker, with 19.2mL deionized water dissolving, by H3BTC solution is along walls of beaker
Pour into Cu (NO3)2·3H2Half an hour is stirred in O solution, obtains HKUST-1 mother liquor azury；Prepared HKUST-1 is female
Liquid and silicon chip substrate are placed in the reaction kettle of 50mL, synthesize MOF film using hydrothermal synthesis method, reaction temperature is 135 DEG C, reaction 2
After it, after being taken out silicon chip substrate with tweezers several times with methanol repeated flushing, dried 1 hour in 100 DEG C, in silicon chip substrate
To the HKUST-1 film of blue, the thickness of HKUST-1 film is about 2~60 μm；Due to being used as metal-organic framework materials using Ni layers
The Ni film of the catalyst of film forming, the surface PANI can be with HKUST-1 film reaction, and therefore, the rate of film build of one side HKUST-1 improves
30%, another aspect PANI film and the binding performance of HKUST-1 film improve 20%, make that film layer is combined to have stronger stabilization
Property, so that the sensing performance for the type gas sense module being thus prepared is more stable；
Step 5 prepares BSP film：
1) BSP sub-micrometer rod is grown：In(NO3)3·x H2O (0.08g) and H3BTC (0.068g) is added to mixed solvent
H2O/DMF(1:1,10mL) in, 10min is stirred at room temperature, solution A is made, by photochromic compounds BSP
(0.057mmol) is added in solution A, and dark place is stirred 1 hour；
2) it forms a film：BSP solution is revolved and is formed a film on Tu silicon wafer/PANI/HKUST-1 film, the speed for revolving Tu is 5000rpm, rotation
The Tu time is 5 seconds；Due to joined on its surface with fluorescence property in the preparation process for the gas sensitization module that it is used
BSP photochromic molecule, which can issue fluorescence in there are inflammable and explosive hazardous environment, make under electromagnetism excitation
The detection device can be realized the flammable explosive gas in qualitative and quantitative detection environment including hydrogen, can make to endanger
A possibility that dangerous situation condition, reduces 50%；
Step 5, sensitive blocks assembling：
Silicon chip substrate is put into hollow structure shell, wafer sections downward, place towards small ventilating holes by sensitive thin film part,
Metal wire connects interdigital electrode and data read module on silicon wafer.Since the manufacturing process of the sensitive blocks is very simple and convenient and
Fast, a large amount of man power and material can be saved, the potentiality with large-scale industrial production.
Experiment test：
(1) hydrogen is tested：25 ± 2 DEG C of conditions each lead into the nitrogen of air, hydrogen and hydrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 500ppm hydrogen, gas sensor letter
Number value changes to rapidly 50.0mV in 2s, and tends towards stability in signal value in 2min；Be passed through air after 5min, signal value in
0 value is returned in 1min and in tending towards stability in 2min；By 2000 stability tests, data variation rate is less than 10%.It surveys
Test result shows that the solid waste detection device has good response performance to hydrogen.
(2) ammonia is tested：25 ± 2 DEG C of conditions each lead into air ammonia and the nitrogen containing ammonia, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 2000ppm ammonia, gas passes through 2000
Secondary stability test, sensor signal value changes to rapidly 15.0mV in 1s, and tends towards stability in signal value in 2min；5min
After be passed through air, signal value is in returning to 0 value and in tending towards stability in 5min in 20s；Its data variation rate is less than 10%.By
2000 stability tests, data variation rate is less than 10%.Test result shows the solid waste detection device to ammonia
With good response performance.
(3) hydrogen sulfide is tested：25 ± 2 DEG C of conditions each lead into air and hydrogen sulfide containing nitrogen, flow velocity 1000ml/
Min, load resistance are 200 Ω；When blowing air, gas sensor signal value is O；It is passed through 100ppm ammonia, sensor signal value
It changes to 30.0mV rapidly in 1s, and tends towards stability in signal value in 3min；Air is passed through after 5min, signal value is in 2min
Return to 0 value and in tending towards stability in 5min；Its data variation rate is less than 10%.By 2000 stability tests, data become
Rate is less than 10%.Test result shows that the solid waste detection device has good response performance to hydrogen sulfide gas.
The experimental results showed that：The sensitive property of the sensitive blocks poisonous and hazardous gas also this to ammonia and hydrogen sulfide increases
It is strong by 40%, it selects performance to improve 50%, obtains the detection device all to the susceptibility of toxic and harmful gas and selectivity
It improves, reduces the risk of production.
From the point of view of the applicable cases of application scenarios 1 to application scenarios 5, provided by the present invention for the mistake of diesel exhaust
Filter and its equipment have the advantage that：
1, a kind of equipment of the dangerous solid waste analyte detection for building field provided by application scenarios of the invention,
The equipment use type gas sense module due to be based on resistive type metal-organic framework materials, and metal-organic framework materials at
Film is on polyaniline film, since polyaniline has strong electric conductivity, further enhance the sensitive of type gas sense module
Degree, and then reinforce the detection device significantly the sensitivity of gas.Further, since being used as metal using Ni layers
Therefore on the one hand the catalyst of organic framework material film forming, the Ni film on the surface PANI can be promoted with HKUST-1 film reaction
On the other hand the film forming of HKUST-1 improves the binding performance of PANI film Yu HKUST-1 film, make to combine film layer with stronger
Stability, so that the sensing performance for the type gas sense module being thus prepared is more stable.
2, a kind of equipment of the dangerous solid waste analyte detection for building field provided by application scenarios of the invention,
Due to joined the discoloration point of the BSP with fluorescence property on its surface in the preparation process for the gas sensitization module that it is used
Son, the photochromic molecule can issue fluorescence in there are inflammable and explosive hazardous environment, enable the detection device under electromagnetism excitation
Enough realize the flammable explosive gas in qualitative and quantitative detection environment including hydrogen, the possibility for the situation that can make to cause danger
Property reduce.
3, a kind of equipment of the dangerous solid waste analyte detection for building field provided by application scenarios of the invention,
Use polyaniline as substrate liquid spin coating silicon chip substrate, during the preparation process due to making silicon chip substrate that the knot of similar microcavity be made
Structure, and joined the material including BSP, micro-cavity structure enhance the sensitivity of sensitive blocks, and then the detection device
Detectability is enhanced, and keeps it extremely strong to the adsorption capacity of hydrogen；In addition, the sensitive blocks are also this to ammonia and hydrogen sulfide
Poisonous and hazardous gas has very strong sensitive and selection performance, makes susceptibility and choosing of the detection device to toxic and harmful gas
Selecting property is all improved, and reduces the risk of production；Finally, due to which the manufacturing process of the sensitive blocks is very simple and convenient and fast
Victory can save a large amount of man power and material, and the potentiality with large-scale industrial production, therefore, the application scenarios of the application are mentioned
A kind of equipment of the dangerous solid waste analyte detection for building field supplied has great promotional value.
Finally it should be noted that use above scene is merely illustrative of the technical solution of the present invention, rather than to the present invention
The limitation of protection scope, although being explained in detail referring to preferred application scene to the present invention, the ordinary skill people of this field
Member is it should be appreciated that can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from technical solution of the present invention
Spirit and scope.
Claims (5)
1. a kind of equipment of the dangerous solid waste analyte detection for building field, which is characterized in that including detection device ontology；
The inside of the detection device ontology is disposed with heat-resistant layer, insulating layer and heat preservation channel from inside to outside；The detection device
The side of ontology is provided with an air inlet, and the other side is provided with an exhaust outlet；The air inlet is provided with the first temperature control
Device is provided with the second temperature control device and detector at the exhaust outlet；The center of inside position of the detection device ontology
It installs and is equipped with filter device；The detector includes sensitive blocks and data read module；The sensitive blocks are placed on
Hollow structure is in the shell of air hole；The sensitive blocks include silicon chip substrate, PANI film, Ni film, HKUST-1 film and
BSP film；The silicon chip substrate includes silicon wafer, silicon nitride film and Cr film layer, and silicon nitride film is used as insulating layer, and Cr film layer is used as interdigital
Electrode layer；The Ni film is prepared using magnetron sputtering method, with a thickness of 10nm；The HKUST-1 film with a thickness of 2~60 μm；Institute
It states Cr film layer and data read module is conductively connected；The production of the sensitive blocks includes the following steps：
Step 1 prepares silicon chip substrate：
N-type silicon chip is taken, cut size is 5cm × 1cm, successively by acetone, ethyl alcohol, deionized water ultrasonic cleaning, ultrasonic time
For 30min, then dried up with nitrogen gun；The silicon wafer cleaned is put into PECVD device, deposits one layer of silicon nitride film, thickness
200nm；By Wafer Cleaning, one layer photoresist of spin coating, photoresist parameter is low speed 900rpm spin coating 13s, high speed 4500rpm spin coating
50s；Then interdigital electrode mask is covered, 7s is exposed, develop 65s；It is put into magnetic control sputtering device, magnetron sputtering C r film, as
Interdigital electrode layer then washes silicon chip surface photoresist with a thickness of 500nm；
Step 2 prepares microcavity：
The silicon chip substrate that will be handled through step 1, it is first with 75% ethanol solution that its surface wipes are clean, using flame heating,
Silicon chip substrate is placed on flame, since one end, is drawn once at interval of 1cm, to form the microcavity of 2 cone cells；Microcavity knot
Structure enhances the sensitivity of sensitive blocks, and then the detectability of the detection device is enhanced, and makes its adsorption energy to hydrogen
Power is extremely strong；
Step 3 prepares PANI film：
It takes a certain amount of polyaniline to be dissolved in dimethylformamide and forms saturated solution, will be saturated using spin coating-czochralski method molten
Liquid is spun to the surface through the processed silicon chip substrate of step 2, and the speed of spin coating is 3000rpm, spin coating 10s, then 100
DEG C baking oven in be dried overnight, obtain PANI film on silicon chip substrate surface；
Step 4 prepares HKUST-1 film：
1) silicon chip substrate is put into magnetron sputtering, base vacuum is lower than 1.5 × 10-3The Ni film of Pa, magnetron sputtering 10nm, silicon wafer
It takes out stand-by；
2) H3BTC 0.336g is weighed in another small beaker, is completely dissolved to obtain colourless transparent solution with 19.2mL ethyl alcohol, is claimed
Take Cu (NO3)2·3H2H3BTC solution, with 19.2mL deionized water dissolving, is poured into Cu along walls of beaker in small beaker by O 0.7g
(NO3)2·3H2Half an hour is stirred in O solution, obtains HKUST-1 mother liquor azury；By prepared HKUST-1 mother liquor and silicon
Piece substrate is placed in the reaction kettle of 50mL, synthesizes MOF film using hydrothermal synthesis method, and reaction temperature is 135 DEG C, after reaction 2 days, is used
Tweezers use methanol repeated flushing several times after taking out silicon chip substrate, dry 1 hour in 100 DEG C, blue is obtained in silicon chip substrate
HKUST-1 film, HKUST-1 film with a thickness of 2~60 μm；
Step 5 prepares BSP film：
1) BSP sub-micrometer rod is grown：It is 1 in 10mL volume ratio:1 H20.08g In is added in O/DMF in the mixed solvent
(NO3)3·x H2O and 0.068g H3BTC stirs 10min and solution A is made, at room temperature by 0.057mmol organic photochromic
It closes object BSP to be added in solution A, dark place is stirred 1 hour；
2) it forms a film：BSP solution is revolved and is formed a film on Tu silicon wafer/PANI/HKUST-1 film, the speed for revolving Tu is 5000rpm, when revolving Tu
Between be 5 seconds；
Step 6, sensitive blocks assembling：
Silicon chip substrate is put into hollow structure shell, wafer sections downward, place towards small ventilating holes, metal by sensitive thin film part
Line connects interdigital electrode and data read module on silicon wafer.
2. a kind of equipment of dangerous solid waste analyte detection for building field according to claim 1, feature exist
In the air inlet is located at the bottom of the detection device ontology.
3. a kind of equipment of dangerous solid waste analyte detection for building field according to claim 1, feature exist
In the exhaust outlet is located at the top of the detection device ontology.
4. a kind of equipment of dangerous solid waste analyte detection for building field according to claim 1, feature exist
In the air inlet is located at the left side of the detection device ontology, and the exhaust outlet is located at the right side of the detection device ontology.
5. a kind of equipment of dangerous solid waste analyte detection for building field according to claim 1, feature exist
In the cross section of the detection device ontology is one of cylinder, rectangle, square.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610594959.1A CN106290273B (en) | 2016-07-25 | 2016-07-25 | A kind of equipment of the dangerous solid waste analyte detection for building field |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610594959.1A CN106290273B (en) | 2016-07-25 | 2016-07-25 | A kind of equipment of the dangerous solid waste analyte detection for building field |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106290273A CN106290273A (en) | 2017-01-04 |
| CN106290273B true CN106290273B (en) | 2018-11-27 |
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| CN201811956U (en) * | 2010-10-21 | 2011-04-27 | 上海科绿特环境科技有限公司 | Artificial board formaldehyde release tester by catharometry |
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| JP2013022525A (en) * | 2011-07-21 | 2013-02-04 | Sumitomo Metal Mining Co Ltd | Filter |
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| CN204767952U (en) * | 2015-05-26 | 2015-11-18 | 南安市金美奋水暖洁具厂 | Too many levels exhaust -gas treatment is recycle device again |
| CN205014055U (en) * | 2015-09-23 | 2016-02-03 | 攀钢集团西昌钢钒有限公司 | Raw coke oven gas contains oxygen analyzer system |
| CN105548503A (en) * | 2016-01-29 | 2016-05-04 | 中绿环保科技股份有限公司 | Integral smoke gas sampling and humidity measuring device |
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