CN106770546A - For the preparation method of the catalysis type gas sensor of methane gas detection - Google Patents

For the preparation method of the catalysis type gas sensor of methane gas detection Download PDF

Info

Publication number
CN106770546A
CN106770546A CN201611102335.XA CN201611102335A CN106770546A CN 106770546 A CN106770546 A CN 106770546A CN 201611102335 A CN201611102335 A CN 201611102335A CN 106770546 A CN106770546 A CN 106770546A
Authority
CN
China
Prior art keywords
catalysis
sensing element
powder
hours
methane gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201611102335.XA
Other languages
Chinese (zh)
Other versions
CN106770546B (en
Inventor
花中秋
王天赐
曾艳
李彦
杨瑞霞
武一
田学民
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hebei University of Technology
Original Assignee
Hebei University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hebei University of Technology filed Critical Hebei University of Technology
Priority to CN201611102335.XA priority Critical patent/CN106770546B/en
Publication of CN106770546A publication Critical patent/CN106770546A/en
Application granted granted Critical
Publication of CN106770546B publication Critical patent/CN106770546B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells

Abstract

The present invention is related to carry out test material by means of the chemical property for determining material for the preparation method of the catalysis type gas sensor of methane gas detection, and the method is a kind of method that use silk-screen printing technique technology prepares catalysis sensing element, and step is:The catalysis sensitive material slurry of preparation to be printed in using silk-screen printing technique be made up of platinum zone of heating and ceramic substrate and is made to be catalyzed sensing element in potsherd plane electrode;Silk-screen printing technique is used in addition by Al2O3Powder slurry is printed in potsherd plane electrode and is made to the white element of reference;Catalysis sensing element and the white element of reference are carried out into high-temperature activation treatment;Sensing element will be catalyzed afterwards and the white unit of reference will be assembled into the catalysis type gas sensor detected for methane gas.Preparation method instant invention overcomes the catalysis sensing element of prior art still suffers from that automaticity is low and cost of manufacture is high, the defect of the unstable properties of the obtained catalysis type gas sensor for detecting methane gas.

Description

For the preparation method of the catalysis type gas sensor of methane gas detection
Technical field
Technical scheme is related to carry out test material by means of the chemical property for determining material, is particularly used for The preparation method of the catalysis type gas sensor of methane gas detection.
Background technology
With the adjustment and optimization of China's energy resource structure, a kind of ratio of the natural gas as clean energy resource in the industrial production Improve constantly, while resident's natural gas user and consumption are also increasing year by year.But methane (the CH in natural gas main component4) Diffusion coefficient is big, colorless and odorless, inflammable and explosive property, danger can be brought to daily production and living.It is natural in recent years Gas leakage Frequent Accidents, cause great casualties and economic loss.Therefore, the leak detection and warning device of methane gas It is that industrial production and resident living safe handling natural gas when institute are prerequisite.
The catalysis type gas sensing of methane gas detection is the characteristic using the catalysis combustion heat release amount of methane gas, is led to The resistance variations of measurement heating element heater platinum coil are crossed, the detection of methane gas is realized.The type sensor has to methane gas Stronger sensitivity and compared with high selectivity, even if while can also maintain excellent methane air-sensitive special under water vapour environment higher Property.Therefore, the catalysis type gas sensing of methane gas detection is presently the most conventional methane gas detection sensor part, in work Industry is produced and played an important role with resident living.
Processing system for the catalysis sensing element of the catalysis type gas sensing of methane gas detection is in early days manual coiling Heating platinum coil and manual application sensing material, prior art then spray the system of sensitive material automatically using silicon semiconductor technique Make method.For the Manufacturing Techniques of catalysis sensing element, although researcher is in wet coating, micro drop method and spraying both at home and abroad The preparation methods such as method aspect has done substantial amounts of research work, but due to the limitation using platinum coil and miniature silicon substrate, it is existing The preparation method of the catalysis sensing element of technology still suffers from that automaticity is low and cost of manufacture is high, obtained for detecting by it The defect of the unstable properties of the catalysis type gas sensor of methane gas.Therefore, urgently develop at present obtained for examining Survey the catalysis sensing element of the stable performance, low manufacture cost and high degree of automation of the catalysis type gas sensor of methane gas Preparation method, with improve for detect methane gas catalysis type gas sensor performance, lifting preparation method it is automatic Change degree simultaneously reduces production cost.
The content of the invention
The technical problems to be solved by the invention are:The system of the catalysis type gas sensor for methane gas detection is provided Make method, be a kind of method that use silk-screen printing technique technology prepares catalysis sensing element, overcome the catalysis of prior art The preparation method of sensing element still suffers from that automaticity is low and cost of manufacture is high, obtained for detecting urging for methane gas The defect of the unstable properties of change formula gas sensor.
The present invention solves the technical scheme that is used of the technical problem:Catalysis type air-sensitive for methane gas detection is passed The preparation method of sensor, is that a kind of use silk-screen printing technique technology prepares the method for being catalyzed sensing element, is comprised the following steps that:
The first step, makes ceramic flat surface electrode:
Required platinum slurry is weighed, is 1 by the weight ratio of platinum slurry and terpinol:10, add terpinol to platinum to starch In material, state is stirred until homogeneous repeatedly, then will be coated on the half tone for being printed on electrode pattern added with the platinum slurry of terpinol, The electrode pattern for being coated with the platinum slurry added with terpinol on half tone is printed on alumina ceramic substrate again, and dry Dried 2 hours for 150 DEG C in dry case, further the alumina ceramic substrate is placed in Muffle furnace under air conditionses in 900 DEG C of burnings Knot 2 hours, is thus obtained the potsherd plane electrode being made up of platinum zone of heating and ceramic substrate, for the screen printing of below step Brush catalysis sensing element is used;
Second step, prepares catalysis sensitive material slurry:
By weight it is Pd: Al2O3Weigh porous Al that required purity Coriolis mass percentage be 99.9% at=5: 1002O3Powder End and purity Coriolis mass percentage are 99.9% Pd salt powders, and by every gram of porous Al2O3Powder adds 100mL deionized waters Ratio adds deionized water, is configured to Pd salt plus Al2O3Suspension, the suspension is heated to 80 DEG C, use magnetic stirrer Stirring 4 hours, rotating speed is 450 rev/min, and the suspension after stirring is extremely turned into powder in 120 DEG C of dryings in an oven, then Gained powder is placed in Muffle furnace and is sintered 4 hours in 700 DEG C, catalysis sensitive material powder is obtained, weighed the desired amount of this and urge Change sensitive dusty material to be ground 10 minutes in agate grinding, the weight ratio by the sensitive powder of organic bond and catalysis is 1:5 Organic bond is added, continues to grind 10 minutes to the uniform jelly as the sensitive dusty material of catalysis, and stand 30 minutes, Catalysis sensitive material slurry is obtained, it is stand-by;
3rd step, makes catalysis sensing element:
Sensitivity therein is catalyzed material by the catalysis sensitive material slurry obtained by above-mentioned second step using screen process press Material is printed in the potsherd plane electrode obtained by the first step, is then dried 2 hours in 120 DEG C in an oven, then will printing The potsherd plane electrode for having sensitive material is sintered 2 hours in batch-type furnace in 700 DEG C of degree, is obtained by catalysis sensitive layer and ceramics The catalysis sensing element that plate plane electrode is constituted;
4th step, makes the white element of reference:
Weigh the porous Al that the desired amount of purity Coriolis mass percentage is 99.9%2O3Powder grinds 10 points in agate grinding Zhong Hou, by organic bond and Al2O3The weight ratio of powder is 1:5 add organic bonds, continue to grind 10 minutes to turning into Al2O3The uniform jelly of powder, after standing 30 minutes, using screen process press by the Al2O3Powder slurry is printed in the first step In obtained potsherd plane electrode, and sintered 2 hours in 700 DEG C of degree in batch-type furnace, the white element of reference is obtained;
5th step, high-temperature activation treatment:
Sensing element will be catalyzed obtained in above-mentioned 3rd step and the 4th step and the white element of reference is put into tube furnace, be passed through body Product is processed 2 hours than being hydrogen: nitrogen=1: 100 mixed gas in 600 DEG C of high-temperature activations;
6th step, assembles the catalysis type gas sensor for methane gas detection:
By above-mentioned 6th step the catalysis sensing element after obtained activation and the white element of reference after activation pass through platinum Wire and tube chamber welds with base, then the composition bridge circuit that is connected with two resistors, connect 5 volts of DC voltages after aging 12 hours, Assembling is obtained the catalysis type gas sensor for methane gas detection.
The preparation method of the above-mentioned catalysis type gas sensor for methane gas detection, the organic bond is the third three Alcohol, macrogol, terpinol or glycerine.
The preparation method of the above-mentioned catalysis type gas sensor for methane gas detection, the Pd salt is PdCl2、Pd (NO3)2Or Pd (C2H3O2)2
The preparation method of the above-mentioned catalysis type gas sensor for methane gas detection, involved raw material and equipment is equal Obtained by known approach, involved technique is that those skilled in the art can grasp.
The beneficial effects of the invention are as follows:Compared with prior art, the present invention has the substantive distinguishing features of protrusion and significantly Progress is as follows:
(1) screen printing technique is used for the present invention making of the catalysis type gas sensor of methane gas detection, the party Method has the advantages that strong homogeneity high, process is simple, cycle is short, stability, low production cost and high degree of automation, wherein, The uniform ceramic plate plane for being available for the silk-screen printing catalysis sensitive material slurry for using and making heating properties stabilization is prepared in design Electrode is the key for obtaining catalysis sensing element in high-performance catalytic sensor.
(2) the potsherd plane electrode that the present invention is prepared using silk-screen printing technique, the platinum for preparing compared to existing technology Coiled heating elements, process more simple, and stability is more preferable, and is catalyzed the adding thermal resistance in sensing element and the white element of reference Resistance value matching is more prone to, and is highly suitable as the heating element heater of the catalysis type gas sensor of methane gas detection.
(3) present invention has obtained Tianjin Natural Science Fund In The Light committee research project (breath analysis medical diagnosis on disease high-performance NH3Semiconductor gas sensor is studied, bullets:15JCYBJC52100) (it is based on state natural sciences fund committee project Molecular screen membrane/WO under high humidity3Compound acetone gas sensor research, bullets:61501167) subsidy.
By the further substantive distinguishing features of the protrusion that the display present invention has and marked improvement in following examples.
Brief description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is the operating process schematic block diagram of the inventive method.
Fig. 2 is the structural representation of the obtained catalysis sensing element of the inventive method.
Fig. 3 is the scanning electron microscope (SEM) photograph of the catalysis sensitive layer in the obtained catalysis sensing element of the inventive method.
Fig. 4 be the obtained catalysis type gas sensor for methane gas detection of the inventive method Gas-sensing measurment with The curve map of concentration of methane gas relation.
Fig. 5 be the obtained catalysis type gas sensor for methane gas detection of the inventive method Gas-sensing measurment with The curve map of operating voltage relation.
In figure, sensitive layer is 1. catalyzed, 2. platinum zone of heating, 3. platinum wire, 4. ceramic substrate.
Specific embodiment
Fig. 1 shows that the inventive method operating process is:Making potsherd plane electrode+preparation catalysis sensitive material slurry → Make catalysis sensing element → high-temperature activation and process → assemble the catalysis type gas sensor detected for methane gas;Make pottery White element → the high-temperature activation of ceramics plane electrode → making reference processes → assembles the catalysis type air-sensitive for methane gas detection Sensor;This be used for methane gas detection catalysis type gas sensor be by high-temperature activation process after catalysis sensing element and The white element of reference after high-temperature activation treatment assembles.
Fig. 1 is further illustrated:The catalysis sensitive material slurry of preparation is printed in making using silk-screen printing technique Potsherd plane electrode on be made to be catalyzed sensing element;Silk-screen printing technique is used in addition by Al2O3Powder slurry is printed in The white element of reference is made in potsherd plane electrode;Catalysis sensing element and the white element of reference are carried out into high-temperature activation treatment; The white element of reference after the treatment of catalysis sensing element and high-temperature activation after high-temperature activation is processed again is assembled into for methane gas The catalysis type gas sensor that physical examination is surveyed.
Fig. 2 shows the structure of obtained catalysis sensing element in the inventive method, and its composition includes being catalyzed sensitive layer 1, platinum Golden zone of heating 2 and ceramic substrate 4.Wherein, potsherd plane electrode is constituted by platinum zone of heating 2 and ceramic substrate 4, it is quick by being catalyzed Sense layer 1 and potsherd plane electrode constitute catalysis sensing element, catalysis sensing element platinum wire 3 and the tube chamber welds with base.
Fig. 3 shows the microstructure scanning electron microscope (SEM) photograph of obtained catalysis sensitive layer in the inventive method, using ESEM Analyze the obtained catalysis sensitive layer of visible the inventive method to be made up of numerous spherical nanoparticles, Size Distribution is equal, soilless sticking Phenomenon, average grain diameter is 10 rans.
Fig. 4 shows that the methane air-sensitive of the obtained catalysis type gas sensor for methane gas detection of the inventive method is rung Answer characteristic curve.The curve of the figure shows that the present invention is with the catalysis type detected for methane gas of silk-screen printing technique making Methane gas sensor has sensitivity higher and faster response speed to methane gas.
Fig. 5 shows the Gas-sensing measurment of the obtained catalysis type gas sensor for methane gas detection of the inventive method With the curve map of operating voltage relation.The curve of the figure shows, the made methane gas sensing for methane gas detection The operating voltage range of device is wider, improves operating voltage and is conducive to improving responding ability of the gas sensor to methane.
Embodiment 1
The first step, makes ceramic flat surface electrode:
Platinum slurry 0.1g is weighed, is 1 by the weight ratio of platinum slurry and terpinol:10, add terpinol 0.01g to platinum In Gold conductor, state is stirred until homogeneous repeatedly, the net for being printed on electrode pattern then will be coated on added with the platinum slurry of terpinol In version, then the electrode pattern for being coated with the platinum slurry added with terpinol on half tone is printed on alumina ceramic substrate, And in drying box 150 DEG C dry 2 hours, further by the alumina ceramic substrate be placed in Muffle furnace under air conditionses in 900 DEG C sinter 2 hours, the potsherd plane electrode being made up of platinum zone of heating and ceramic substrate are thus obtained, for below step Silk-screen printing catalysis sensing element use;
Second step, prepares catalysis sensitive material slurry:
By weight it is Pd: Al2O3=5: the 100 purity Coriolis mass percentages for weighing 1g are 99.9% porous Al2O3Powder With the PdCl that the purity Coriolis mass percentage of 0.08g is 99.99%2Powder, adds 100mL deionized waters, is configured to PdCl2Plus Al2O3Suspension, the suspension is heated to 80 DEG C, using magnetic stirrer stir 4 hours, rotating speed be 450 rev/min, Suspension after stirring is extremely turned into powder in 120 DEG C of dryings in an oven, then gained powder is placed in Muffle furnace in 700 DEG C Sintering 4 hours, is obtained catalysis sensitive material powder, weighs 0.5g catalysis sensitivity dusty material and grinds 10 points in agate grinding Clock, adds organic bond glycerine 0.1g, continues to grind 10 minutes to the uniform jelly for turning into the sensitive dusty material of catalysis, And 30 minutes are stood, and catalysis sensitive material slurry is obtained, it is stand-by;
3rd step, makes catalysis sensing element:
Sensitivity therein is catalyzed material by the catalysis sensitive material slurry obtained by above-mentioned second step using screen process press Material is printed in the potsherd plane electrode obtained by the first step, is then dried 2 hours in 120 DEG C in an oven, then will printing The potsherd plane electrode for having sensitive material is sintered 2 hours in batch-type furnace in 700 DEG C of degree, is obtained by catalysis sensitive layer and ceramics The catalysis sensing element that plate plane electrode is constituted;
4th step, makes the white element of reference:
The purity Coriolis mass percentage for weighing 0.5g is 99.9% porous Al2O3After powder grinds 10 minutes in agate grinding, Organic bond glycerine 0.1g is added, continues to grind 10 minutes to as Al2O3The uniform jelly of powder, stands 30 minutes Afterwards, using screen process press by the Al2O3Powder slurry is printed in the potsherd plane electrode obtained by the first step, and in case Sintered 2 hours in 700 DEG C of degree in formula stove, the white element of reference is obtained;
5th step, high-temperature activation treatment:
Sensing element will be catalyzed obtained in above-mentioned 3rd step and the 4th step and the white element of reference is put into tube furnace, be passed through body Product is processed 2 hours than being hydrogen: nitrogen=1: 100 mixed gas in 600 DEG C of high-temperature activations;
6th step, assembles the catalysis type gas sensor for methane gas detection:
By above-mentioned 5th step the catalysis sensing element after obtained activation and the white element of reference after activation pass through platinum Wire and tube chamber welds with base, then the composition bridge circuit that is connected with 2 resistors, connect 5 volts of DC voltages after aging 12 hours, group Dress is obtained the catalysis type gas sensor for methane gas detection.
The methane air-sensitive performance test methods of the obtained catalytic gas transducer for CH_4 detection of the present embodiment are such as Under:
Distribution, i.e., the compressed gas for being mixed with air using methane and synthesis compressed air are carried out using dynamic air-distributing method Mixing, the tested methane gas of 1000ppm to 20000ppm, flow rate set are configured to by quality control flow control gas flow It is 100mL/min;Test condition:Working sensor voltage is respectively set to 5V to 12V, and test environment temperature is room temperature, environment Relative humidity is less than 3%.
The air-sensitive response data that specific methane air-sensitive performance test is obtained is shown in Table 1.As seen from the data in Table 1, the present embodiment The catalytic gas transducer for CH_4 detection for making is fast to the speed of response of methane, and restorative good, responsiveness is high.Separately Outward, compared with the manufacturing technology for making catalytic sensor part with existing platinum coil, the catalysis that the present embodiment method makes The adding thermal resistance matching of formula sensor is good, and air-sensitive performance is obviously improved.
Air-sensitive response performance of the obtained catalytic gas transducer for CH_4 detection of 1. embodiment of table 1 to methane
Concentration (ppm) Sensitivity (mV) The speed of response (S) Regeneration rate (S)
2000 22.1 29 66
5000 28.8 39 67
10000 49 39 71
20000 70.5 45 76.8
Embodiment 2
The first step, makes ceramic flat surface electrode:
With embodiment 1;
Second step, prepares catalysis sensitive material slurry:
By weight it is Pd: Al2O3=5: the 100 purity Coriolis mass percentages for weighing 1g are 99.9% porous Al2O3Powder With the Pd (NO that the purity Coriolis mass percentage of 0.122g is 99.99%3)2Powder, adds 100mL deionized waters, is configured to Pd (NO3)2Plus Al2O3Suspension, the suspension is heated to 80 DEG C, using magnetic stirrer stir 4 hours, rotating speed is 450 Rev/min, extremely turns into powder, then gained powder is placed in into Muffle in 120 DEG C of dryings in an oven by the suspension after stirring Sintered 4 hours in 700 DEG C in stove, catalysis sensitive material powder is obtained, weighed 0.5g catalysis sensitivity dusty materials and ground in agate Ground 10 minutes in mill, add organic bond macrogol 0.1g, continuing to grind extremely turns into the sensitive powder of catalysis for 10 minutes The uniform jelly of material, and 30 minutes are stood, catalysis sensitive material slurry is obtained, it is stand-by;
3rd step, makes catalysis sensing element:
Sensitivity therein is catalyzed material by the catalysis sensitive material slurry obtained by above-mentioned second step using screen process press Material is printed in the potsherd plane electrode obtained by the first step, is then dried 2 hours in 120 DEG C in an oven, then will printing The potsherd plane electrode for having sensitive material is sintered 2 hours in batch-type furnace in 700 DEG C of degree, is obtained by catalysis sensitive layer and ceramics The catalysis sensing element that plate plane electrode is constituted;
4th step, makes the white element of reference:
With embodiment 1;
5th step, high-temperature activation treatment:
Sensing element will be catalyzed obtained in above-mentioned 3rd step and the 4th step and the white element of reference is put into tube furnace, be passed through body Product is processed 2 hours than being hydrogen: nitrogen=1: 100 mixed gas in 600 DEG C of high-temperature activations;
6th step, assembles the catalysis type gas sensor for methane gas detection:
By above-mentioned 6th step the catalysis sensing element after obtained activation and the white element of reference after activation pass through platinum Line and tube chamber welds with base, then the composition bridge circuit that is connected with 2 resistors, connect 5 volts of DC voltages after aging 12 hours, assemble The catalysis type gas sensor for methane gas detection is obtained.
Embodiment 3
The first step, makes ceramic flat surface electrode:
With embodiment 1;
Second step, prepares catalysis sensitive material slurry:
By weight it is Pd: Al2O3=5: the 100 purity Coriolis mass percentages for weighing 1g are 99.9% porous Al2O3Powder With the Pd (C that the purity Coriolis mass percentage of 0.105g is 99.99%2H3O2)2Powder, adds 100mL deionized waters, is configured to Pd (C2H3O2)2Plus Al2O3Suspension, the suspension is heated to 80 DEG C, using magnetic stirrer stir 4 hours, rotating speed is 450 Rpm, the suspension after stirring is extremely turned into powder in 120 DEG C of dryings in an oven, then gained powder is placed in Muffle furnace In sintered 4 hours in 700 DEG C, catalysis sensitive material powder is obtained, weigh 0.5g catalysis sensitivity dusty material and ground in agate Middle grinding 10 minutes, adds organic bond terpinol 1mL, and continuing to grind extremely turns into the equal of the sensitive dusty material of catalysis for 10 minutes Even jelly, and 30 minutes are stood, catalysis sensitive material slurry is obtained, it is stand-by;
3rd step, makes catalysis sensing element:
Sensitivity therein is catalyzed material by the catalysis sensitive material slurry obtained by above-mentioned second step using screen process press Material is printed in the potsherd plane electrode obtained by the first step, is then dried 2 hours in 120 DEG C in an oven, then will printing The potsherd plane electrode for having sensitive material is sintered 2 hours in batch-type furnace in 700 DEG C of degree, is obtained by catalysis sensitive layer and ceramics The catalysis sensing element that plate plane electrode is constituted;
4th step, makes the white element of reference:
With embodiment 1;
6th step, high-temperature activation treatment:
Sensing element will be catalyzed obtained in above-mentioned 3rd step and the 4th step and the white element of reference is put into tube furnace, be passed through body Product is processed 2 hours than being hydrogen: nitrogen=1: 100 mixed gas in 600 DEG C of high-temperature activations;
7th step, assembles the catalysis type gas sensor for methane gas detection:
By above-mentioned 6th step the catalysis sensing element after obtained activation and the white element of reference after activation pass through platinum Line and tube chamber welds with base, then the composition bridge circuit that is connected with 2 resistors, connect 5 volts of DC voltages after aging 12 hours, assemble The catalysis type gas sensor for methane gas detection is obtained.
Embodiment 4
In addition to the organic bond added in the preparation catalysis sensitive material slurry of second step is for glycerine 0.1g, other are same Embodiment 1.
In above-described embodiment, involved raw material and equipment are obtained by known approach, and involved technique is ability What the technical staff in domain can grasp.

Claims (3)

1. the preparation method of the catalysis type gas sensor of methane gas detection is used for, it is characterised in that:It is that one kind uses silk screen The method that printing technology prepares catalysis sensing element, comprises the following steps that:
The first step, makes ceramic flat surface electrode:
Required platinum slurry is weighed, is 1 by the weight ratio of platinum slurry and terpinol:10, in addition terpinol to platinum slurry, State is stirred until homogeneous repeatedly, then will be coated on the half tone for being printed on electrode pattern added with the platinum slurry of terpinol, then will The electrode pattern for being coated with the platinum slurry added with terpinol on half tone is printed on alumina ceramic substrate, and in drying box In 150 DEG C dry 2 hours, further the alumina ceramic substrate is placed in Muffle furnace under air conditionses 2 small in 900 DEG C of sintering When, the potsherd plane electrode being made up of platinum zone of heating and ceramic substrate is thus obtained, the silk-screen printing for below step is urged Change sensing element to use;
Second step, prepares catalysis sensitive material slurry:
By weight it is Pd: Al2O3Weigh porous Al that required purity Coriolis mass percentage be 99.9% at=5: 1002O3Powder and Purity Coriolis mass percentage is 99.9% Pd salt powders, and by every gram of porous Al2O3Powder adds the ratio of 100mL deionized waters Deionized water is added, Pd salt plus Al is configured to2O3Suspension, the suspension is heated to 80 DEG C, stirred using magnetic stirrer 4 hours, rotating speed was 450 rev/min, by the suspension after stirring in an oven in 120 DEG C of dryings to turning into powder, then by institute Powder be placed in Muffle furnace in 700 DEG C sinter 4 hours, be obtained catalysis sensitive material powder, weigh the desired amount of catalysis quick Sense dusty material grinds 10 minutes in agate grinding, and the weight ratio by the sensitive powder of organic bond and catalysis is 1:5 add Organic bond, continues to grind 10 minutes to the uniform jelly as the sensitive dusty material of catalysis, and stands 30 minutes, is obtained Catalysis sensitive material slurry, it is stand-by;
3rd step, makes catalysis sensing element:
Catalysis sensitive material slurry obtained by above-mentioned second step is printed sensitive catalysis material therein using screen process press Brush in the potsherd plane electrode obtained by the first step, then dried 2 hours in 120 DEG C in an oven, then will be printed with quick The potsherd plane electrode for feeling material is sintered 2 hours in batch-type furnace in 700 DEG C of degree, is obtained and is put down by catalysis sensitive layer and potsherd The catalysis sensing element that face electrode is constituted;
4th step, makes the white element of reference:
Weigh the porous Al that the desired amount of purity Coriolis mass percentage is 99.9%2O3After powder grinds 10 minutes in agate grinding, By organic bond and Al2O3The weight ratio of powder is 1:5 add organic bond, continue to grind 10 minutes to as Al2O3Powder The uniform jelly at end, after standing 30 minutes, using screen process press by the Al2O3Powder slurry is printed in obtained by the first step Potsherd plane electrode on, and reference white element is obtained in 700 DEG C of degree sintering 2 hours in batch-type furnace;
5th step, high-temperature activation treatment:
Sensing element will be catalyzed obtained in above-mentioned 3rd step and the 4th step and the white element of reference is put into tube furnace, be passed through volume ratio It is hydrogen: nitrogen=1: 100 mixed gas, and processed 2 hours in 600 DEG C of high-temperature activations;
6th step, assembles the catalysis type gas sensor for methane gas detection:
By above-mentioned 6th step the catalysis sensing element after obtained activation and the white element of reference after activation pass through platinum wire With tube chamber welds with base, then the composition bridge circuit that is connected with 2 resistors, 5 volts of DC voltages are connected after aging 12 hours, assembling is made The catalysis type gas sensor of methane gas detection must be used for.
2. the preparation method of the catalysis type gas sensor of methane gas detection is used for according to claim 1, and its feature exists In:The organic bond is glycerine, macrogol, terpinol or glycerine.
3. the preparation method of the catalysis type gas sensor of methane gas detection is used for according to claim 1, and its feature exists In:The Pd salt is PdCl2、Pd(NO3)2Or Pd (C2H3O2)2
CN201611102335.XA 2016-12-05 2016-12-05 The production method of catalysis type gas sensor for methane gas detection Active CN106770546B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201611102335.XA CN106770546B (en) 2016-12-05 2016-12-05 The production method of catalysis type gas sensor for methane gas detection

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201611102335.XA CN106770546B (en) 2016-12-05 2016-12-05 The production method of catalysis type gas sensor for methane gas detection

Publications (2)

Publication Number Publication Date
CN106770546A true CN106770546A (en) 2017-05-31
CN106770546B CN106770546B (en) 2019-02-19

Family

ID=58883791

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201611102335.XA Active CN106770546B (en) 2016-12-05 2016-12-05 The production method of catalysis type gas sensor for methane gas detection

Country Status (1)

Country Link
CN (1) CN106770546B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107449798A (en) * 2017-08-14 2017-12-08 河北工业大学 Preparation method for the gas sensor of methane gas detection
CN108760831A (en) * 2018-03-29 2018-11-06 宁波大学 A kind of preparation method of indium oxide gas sensor
CN110658238A (en) * 2018-06-29 2020-01-07 上海汽车集团股份有限公司 Catalytic combustion gas sensor based on ceramic-based micro-hotplate and preparation method thereof
CN110702752A (en) * 2019-10-24 2020-01-17 河北工业大学 Manufacturing method of gas sensor for ammonia gas detection

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1041454A (en) * 1988-09-23 1990-04-18 淮南矿业学院 Low current or low-power consumption heat catalytic element and manufacture method thereof
CN203164151U (en) * 2013-04-24 2013-08-28 山东三大博安测控技术有限公司 Methane sensor
KR101489891B1 (en) * 2013-10-16 2015-02-04 한국해양대학교 산학협력단 Marine HNS spill detector using Indium-tin-oxide film sensor
CN104792645A (en) * 2015-03-27 2015-07-22 上海大学 Normal temperature methane sensor and preparation method thereof
CN205538787U (en) * 2016-03-28 2016-08-31 南通理工学院 Multi -functional gas concentration detection appearance

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1041454A (en) * 1988-09-23 1990-04-18 淮南矿业学院 Low current or low-power consumption heat catalytic element and manufacture method thereof
CN203164151U (en) * 2013-04-24 2013-08-28 山东三大博安测控技术有限公司 Methane sensor
KR101489891B1 (en) * 2013-10-16 2015-02-04 한국해양대학교 산학협력단 Marine HNS spill detector using Indium-tin-oxide film sensor
CN104792645A (en) * 2015-03-27 2015-07-22 上海大学 Normal temperature methane sensor and preparation method thereof
CN205538787U (en) * 2016-03-28 2016-08-31 南通理工学院 Multi -functional gas concentration detection appearance

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107449798A (en) * 2017-08-14 2017-12-08 河北工业大学 Preparation method for the gas sensor of methane gas detection
CN107449798B (en) * 2017-08-14 2019-07-26 河北工业大学 The production method of gas sensor for methane gas detection
CN108760831A (en) * 2018-03-29 2018-11-06 宁波大学 A kind of preparation method of indium oxide gas sensor
CN110658238A (en) * 2018-06-29 2020-01-07 上海汽车集团股份有限公司 Catalytic combustion gas sensor based on ceramic-based micro-hotplate and preparation method thereof
CN110702752A (en) * 2019-10-24 2020-01-17 河北工业大学 Manufacturing method of gas sensor for ammonia gas detection

Also Published As

Publication number Publication date
CN106770546B (en) 2019-02-19

Similar Documents

Publication Publication Date Title
CN106770546B (en) The production method of catalysis type gas sensor for methane gas detection
CN108956715B (en) Au @ WO3Core-shell structure nanosphere and preparation method and application thereof
CN102809634B (en) Gas-sensitive sensor made of palladium hybridization ferroferric oxide nanometer material
CN101281159B (en) Nanometer zinc oxide multifunctional gas-sensitive sensor device and making method thereof
TWI410625B (en) Gas sensing material and gas sensor employing the same
CN107655948B (en) With La2NiO4YSZ-based mixed potential type H as sensitive electrode2S sensor and preparation method thereof
CN102680540B (en) Formaldehyde gas-sensing material, corresponding formaldehyde gas-sensing element and preparation method of element
CN106093137A (en) A kind of based on α Fe2o3acetone gas sensor of multi-pore micron flower sensitive material and preparation method thereof
CN109946358A (en) One kind is with MTiO3Electric potential type SO is blended together for the YSZ base of sensitive electrode2Sensor, preparation method and applications
CN108872325A (en) One kind being based on SnSe2/SnO2Nitrogen dioxide gas sensor, preparation process and the application of hetero-junctions
CN105806899A (en) Production and application of Pt-SnO2 oxide semiconductor carbon monoxide sensor
CN105911105B (en) SnO2CO sensing materials of doped catalyst and its preparation method and application
CN105784813A (en) Stable zirconia-based mixed-potential-type SO2 sensor taking MnNb2O6 as sensitive electrode and preparation method and application of stable zirconia-based mixed-potential-type SO2 sensor
CN107966479A (en) A kind of Pd/W for improving hydrogen gas sensor performance18O49The preparation method of composite material
CN108956708A (en) A kind of alcohol gas sensor and preparation method thereof based on zinc ferrite nano sensitive material
CN106395888B (en) The graphene phase carbon nitride oxidation tin composite material and preparation method of a kind of nearly room temperature air-sensitive selective enumeration method of organic pollution and application
Sasahara et al. Highly sensitive detection of volatile organic compounds by an adsorption/combustion-type sensor based on mesoporous silica
CN206114577U (en) Air -sensitive material performance test room
CN106365204A (en) Preparation method of tungsten trioxide sensitive material for ammonia gas sensitive sensor
CN108844999A (en) For detecting the utilization g-C of VOCs3N4The synthetic method of the porous zinc bloom nanometer sheet composite air-sensitive material of modification
CN111781249A (en) Hydrogen sulfide gas detection method and sensor based on composite membrane material
Abe et al. Influences of ball-milling time on gas-sensing properties of Co3O4–SnO2 composites
CN107449798B (en) The production method of gas sensor for methane gas detection
CN109521064B (en) Room temperature NO2 sensor based on WO3 hollow sphere and preparation method thereof
CN107884454A (en) A kind of integrated form carbon monoxide and nitrogen dioxide gas detector

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant