CN101251508B - Method for manufacturing gas sensor for testing hydrogen - Google Patents

Method for manufacturing gas sensor for testing hydrogen Download PDF

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CN101251508B
CN101251508B CN2008100695325A CN200810069532A CN101251508B CN 101251508 B CN101251508 B CN 101251508B CN 2008100695325 A CN2008100695325 A CN 2008100695325A CN 200810069532 A CN200810069532 A CN 200810069532A CN 101251508 B CN101251508 B CN 101251508B
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CN101251508A (en
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刘天模
甘浩宇
利佳
赵先瑞
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Chongqing University
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Abstract

The invention relates to a preparation method for a gas sensor for detecting hydrogen, wherein, ultrasonic wave and low-temperature aging technologies are applied to the complex effect of zinc salts and stannum salts and chemical coprecipitation for preparation of nano ZnSnO3. The invention prepares the novel PdO-ZnSnO3 heater type semiconductor gas sensor by isomerisation of noble metal salts PdCl2, adhesives (ethyl orthosilicate) and deionized water through technologies like grinding, ultrasonic vibration, coating, sintering, etc. on the basis of the nano ZnSnO3, wherein, nano ZnSnO3 bases are prepared by adoption of an improved coprecipitation method. The preparation method for the gas sensor for detecting hydrogen has the advantages of high sensitivity of gas sensitive materials, strong selectivity, low operation temperature, simple preparation technology and so on.

Description

Detect the method for manufacturing gas sensor of hydrogen
Technical field
The invention belongs to semiconductor transducer gas sensor manufacturing process technology field, particularly a kind of method for manufacturing gas sensor that detects hydrogen.
Background technology
The Metal Oxide Semiconductor Gas Sensing sensor kind that is used for the warning of gas and monitoring at present is more, the SnO that is doped with commonly used 2, ZnO, Fe 2O 3, WO 3With and other metal oxide modified of mixing after various air-sensitive propagated sensation sensors.In all kinds of gas sensors, the semiconductor gas sensitive sensor has than great share on market with advantage such as simple in structure, cheap, that volume is little, power is little, response is fast.But gas sensitization performances such as the sensitivity of the metal oxide gas sensitive element that these are single, selectivity, stability are desirable not enough, so people have researched and developed the composite metal oxide gas sensor.
ZnSnO 3Be a kind of N type composite oxide semiconductor with perovskite structure, because its unique electronic structure, the surface easily forms alms giver's surface state, helps gas absorption, more and more is subject to people's attention as the gas sensitive that has a high potential.At document [1] Sensors and Actuators B, 120,2007, among the 694-699, people such as Jiaqiang Xu utilize Hydrothermal Preparation to obtain the ZnO/ZnSnO of doping Au 3The gas sensitive of base, the result shows that the adding of Au and ZnO has significant effects for formaldehyde steam good sensitivity and selectivity; At document [2] Solid-State Electronics, 46,2002, among the 715-719, human wet methods such as XingHui Wu have been synthesized slug type ZnSnO 3, and studied its sensitlzing effect to combustible gas such as coal gas, butane; At document [3] Journal of the Ceramic Society of Japan, 104,1212, among the 1158-1159, people such as Hiratsuka N find that the compound mixed oxide of zinc-tin also has good sensitlzing effect to isobutane; In document [4] Sensors and Actuators B, 12,1993,5-9 and document [5] Applied Physics Letters, 86,2005, in 233101, people such as people such as Yu-sheng Shen and Xue XY prepare micron and nano level ZnSnO with chemical co-precipitation method and vapour deposition process respectively 3Gas sensitive tests out its sensitive property to the ethanol excellence.
From above-mentioned document as can be known, ZnSnO 3Carry out compound or mixing and doping with other metal oxides, can improve compound substance catalysis air-sensitive perception can, be on the pure type organic and reducibility gas of representative but mainly concentrate on ethanol for the test of gas.
Along with industrial development, hydrogen has been widely used in fields such as petrochemical complex, medical treatment, electronics, space flight and aviation as reducibility gas with as the carrier of liquid hydrogen.In addition, generate water behind the combustion of hydrogen, environment is not polluted, so hydrogen is as good pollution-free clean reproducible energy, the inexorable trend and the tremendous potential that replace oil to act as a fuel have caused people's very big concern.But simultaneously, when density of hydrogen reached 4% in the air, hydrogen exploded easily, and it is also increasing that therefore this inflammable gas is revealed the blast and the fire failure that cause.Because the hydrogen colorless and odorless is difficult for after the leakage discovering, therefore the detection to hydrogen leak just seems very important.The chemical sensitisation device that is generally used for the hydrogen detection is based on single metal oxides such as tin oxide, zinc paste, tungsten oxides, and sensitivity and selectivity are all relatively poor, can not satisfy the needs that in commercial production and the people's lives hydrogen leak detected in real time.In addition, the detection to the inflammable and explosive hydrogen of colorless and odorless also rarely has research and report.
Summary of the invention
Order of the present invention provides a kind of method for manufacturing gas sensor that detects hydrogen, gas sensor with the detection hydrogen of the inventive method preparation, detect that hydrogen gas is highly sensitive, selectivity good, have easy to operate, preparation technology is simple, with low cost, the advantage that has wide range of applications.
Technical scheme of the present invention has following steps:
A. preparation is doped with PdCl 2ZnSnO with tetraethoxysilance 3Powder;
B.ZnSnO 3Powder is through after 3～6 hours ground and mixed, ultrasonic dispersing;
C. with deionized water with ZnSnO 3Behind the powder furnishing pasty state, be coated on the ceramic pipe that has platinum electrode, coating thickness is 0.5～1.5mm;
D. with above-mentioned ceramic pipe under 80～120 ℃ of temperature dry 1.5～2 hours, 600～800 ℃ of thermal treatment sintering were connected on the base that has the nickel limb after 8 hours, promptly got the gas sensor that is used to detect hydrogen.
Further technical scheme of the present invention is: ZnSnO 3Powder consist of nanometer ZnS nO 3Base-material, PdCl 2And bonding agent, wherein PdCl 2Doping is nanometer ZnS nO 31%～10% of base-material gross mass, bonding agent are nanometer ZnS nO 30.1% of base-material gross mass.
Nanometer ZnS nO 3The preparation method of base-material is:
A. press kation Zn 2+/ Sn 4+Be 1: 1 etc. mol ratio prepare Zn (SnO respectively 4) 27H 2O and SnCl 45H 2Each 2～5 liters of O solution respectively dilute twice with strong aqua and become 4～10 liters;
B. to soluble zinc salt Zn (SnO 4) 27H 2Splashing into ammoniacal liquor to the pH value of solution in the O solution is 9～12;
C. under the continuous magnetic agitation, to the solubility pink salt SnCl that has diluted 45H 2Dropping concentrated hydrochloric acid to the pH value of solution is 5～7 in the O solution;
D. with above-mentioned solubility pink salt Zn (SnO 4) 27H 2O solution slowly joins soluble zinc salt SnCl 45H 2In the O solution, dropping ammonia or hydrochloric acid, constantly stirring the acidity of adjusting solution down is PH=7, ZnSnO occurs 3Precipitation is 50KHz in ultrasonic frequency, and power is ultrasonic dispersing 3～5 hours under the 200W condition, gained ZnSnO 3Be deposited in-15～-10 ℃ of ageings 10 hours, behind the absolute ethyl alcohol flushing suction filtration, 100 ℃ of dryings 2～3 hours, sintering promptly got nanometer ZnS nO in 5 hours in 600～800 ℃ of air 3Base-material.
The present invention is at ZnSnO 3PdCl has mixed in the matrix 2, PdCl 2Chemical reaction takes place in the doping process obtain generating PdO, because the dispersion effect of PdO is good, doped P dO is high dispersion state, makes PdO extensively be distributed in ZnSnO 3Intercrystalline in the matrix, ZnSnO 3Crystal growth and reunion are difficult again, so the doping of PdO has suppressed ZnSnO 3Grow up, caused high specific surface, more oxygen vacancy and nanometer pore appear, increased effective adsorption area, help the absorption of micromolecular hydrogen, thereby make material excellent structural stability and selectivity be arranged hydrogen.
Referring to Fig. 3, simultaneously, be evenly distributed on the PdO in the matrix, has stronger catalytic activation ability, for more hydrogen molecule and a large amount of oxonium ions that are adsorbed on matrix surface provide the possibility of redox reaction rapidly, detect of the sensitivity of the gas sensor of hydrogen thereby improved greatly to hydrogen, in addition, PdO closely is distributed in the surface of matrix, and that the hydrogen molecule amount is compared other gas molecules is much smaller, hydrogen molecule is easy to see through in the reaction that PdO participates in hydrogen and a large amount of adsorb oxygen ion, PdO plays filtration and isolates the effect of other gas molecules, so relative other gases of sensitivity of gas sensor detection hydrogen have good selectivity (referring to table 2).
The gas sensor of detection hydrogen of the present invention can be applied to the safety detection of big-and-middle-sized mine, the safety detection of natural gas in home gas piping, the safe storage of combustible and explosive articles in the commercial production, fields such as the safety detection of the gas analysis in the environment etc., the safe storage of combustible and explosive articles and gas analysis, higher sensitivity and selectivity are arranged, the advantage that has wide range of applications.
Adopt the PdCl that is doped with of the inventive method preparation 2ZnSnO 3Composite metal oxide powder, with the grain size and the sensitive layer pattern of transmission electron microscope (TEM) and scanning electron microscope (SEM) measuring powder, its result shows: the ZnSnO3 powder granule that makes is tiny, and mean grain size is about 30-60nm, Pd 2+Be dispersed in ZnSnO 3In the body.
The inventive method is produced ZnSnO with Complex effect and chemical coprecipitation that ultrasound wave and low temperature maturation technology apply to zinc salt, pink salt 3, again at nanometer ZnS nO 3The basis on, doped precious metal salt PdCl 2, tetraethoxysilance bonding agent and deionized water, prepare PdO-ZnSnO by technologies such as grinding, ultrasonic oscillation, coating, sintering 3The heater-type semiconductor gas sensor, it is easy to have manufacturing process, simple in structure, cheap advantage.
Description of drawings
Fig. 1 is a semiconductor transducer gas-sensitive element structure synoptic diagram of the present invention;
Wherein: 1-resin material base, 2-platinum electrode, 3-alumina ceramic tube, 4-Ni-Cr heater strip;
Fig. 2 represents the TEM figure of the ZnSnO3 composite metal oxide powder of embodiment 1 preparation;
Fig. 3 represents the SEM figure of the PdO doped ZnS nO3 composite metal oxide powder of embodiment 1 preparation.Bulk is ZnSnO3 crystal grain among the figure, and fritter is a PdO crystal grain.
Embodiment
Reagent in the present embodiment:
SnCl 45H 2O analyzes pure; Zn (SnO 4) 27H 2O analyzes pure; Ammoniacal liquor is analyzed pure; PdCl 2, analyze pure; Tetraethoxysilance, chemical pure; Mentioned reagent all adopts the commercially available prod.
Embodiment 1
Preparation nanometer ZnS nO 3Base-material:
Press kation Zn 2+/ Sn 4+Be 1: 1 etc. mol ratio prepare Zn (SnO respectively 4) 27H 2O and SnCl 45H 2O solution 3L, with strong aqua with Zn (SnO 4) 27H 2The O solution dilution becomes twice, with SnCl 45H 2The O solution dilution becomes twice.Soluble zinc salt Zn (SnO after dilution 4) 27H 2Slowly splash into the ammoniacal liquor that concentration is 1mol/L in the O solution, the pH value of adjusting solution is 11; SnCl after dilution 45H 2Drip the PH=6 that concentrated hydrochloric acid is adjusted solution in the O solution, and continuous magnetic agitation.Adjusting acidity SnCl 45H 2O solution slowly joins adjusts acidity Zn (SnO 4) 27H 2In the O solution, dropping ammonia constantly stirs until solution PH=7 again, obtains sediment ZnSnO 3ZnSnO 3Precipitation adopts water bath with thermostatic control magnetic stirring apparatus (production of mayor of Beijing bearing instruments and meters company) to carry out ultrasonic dispersing, and ultrasonic frequency is 50KHz, and power is 200W, and ultrasonic dispersing 4 hours makes ZnSnO 3Precipitation is complete, and deposit seed is uniformly dispersed, and particle is tiny.Sediment ZnSnO 3-15 ℃ of ageings 10 hours, wash suction filtration with absolute ethyl alcohol, drying is 2 hours in muffle furnace.Sintering promptly got nanometer ZnS nO in 5 hours in 600 ℃ of air 3Base-material.
Above-mentioned nanometer ZnS nO 3The PdCl that adds its gross mass 5% in the base-material 2, be both and add nanometer ZnS nO 3The tetraethoxysilance bonding agent of base-material gross mass 0.1%, the common grinding evenly; Adopted water bath with thermostatic control magnetic stirring apparatus (production of mayor of Beijing bearing instruments and meters company) ultrasonic oscillation 3 hours, and made Pd 2+Ion is evenly dispersed in nanometer ZnS nO more 3Matrix on, increase nanometer ZnS nO 3Matrix and Pd 2+The cementability of ion.Ultrasonic frequency is 50KHz, and power is 200W.Gained is doped with PdCl 2ZnSnO 3The composite metal oxide powder is tested with transmission electron microscope (TEM) and scanning electron microscope (SEM), measures the grain size and the sensitive layer pattern of powder.The ZnSnO3 powder granule that makes from TEM (Fig. 2) expression is tiny, and mean grain size is about 30nm, and SEM (Fig. 3) represents Pd 2+Be dispersed in ZnSnO 3In the body.
Doping Pd Cl 2ZnSnO 3Press ZnSnO in the composite metal oxide powder 3Powder and deionized water add deionized water by 1: 5 mol ratio, grind to form pasty state, are coated in writing brush on the alumina ceramic tube that has platinum electrode, and coating thickness is 1mm, and under 100 ℃ of conditions after dry 2 hours, sintering is 8 hours in 700 ℃ of air in muffle furnace.
The resin base that will have the nickel limb immerses in the absolute ethyl alcohol, takes out after 10 minutes, and the hair dryer oven dry repeats immersions-drying course 10-20 time, then 350 ℃ in muffle furnace drying obtained the pretreated base of process in 3 hours.
Be connected on a pair of nickel pin on the good resin material base of pre-service penetrating Ni-Cr heater strip and soldering in the middle of the above-mentioned alumina ceramic tube; Be welded on successively on the residue nickel limb on the base being connected four Pt electrodes on the alumina ceramic tube, promptly get the PdO-ZnSnO that is used to detect hydrogen of the present invention 3Heater-type semiconductor hydrogen-sensitive element.
Referring to Fig. 1, described resin material base 1, its two ends are provided with platinum electrode 2, and alumina ceramic tube 3 is set between the platinum electrode, connect Ni-Cr heater strip 4 applying to such an extent that nanometer ZnS nO arranged by soldering 3The alumina ceramic tube of oar material is fixed on the platinum electrode 2.Finally make the PdO-ZnSnO that detects hydrogen 3The heater-type semiconductor gas sensor.Gained particle mean grain size is about 30nm, Pd 2+Be dispersed in ZnSnO 3In the body.
Embodiment two: the PdCl of present embodiment 2Addition be nanometer ZnS nO 38% of base-material gross mass, other steps are identical with embodiment one, and gained particle mean grain size is about 45nm, Pd 2+The even ZnSnO that is dispersed in 3In the body.
Embodiment three: the PdCl of present embodiment 2Addition be nanometer ZnS nO 3The 10t% of base-material gross mass, other steps are identical with embodiment one, and gained particle mean grain size is about 55nm, Pd 2+The inhomogeneous ZnSnO that is dispersed in 3In the body.
Embodiment four: the PdCl of present embodiment 2Addition be nanometer ZnS nO 31% of base-material gross mass, other steps are identical with embodiment one, and gained particle mean grain size is about 65nm, Pd 2+The inhomogeneous ZnSnO that is dispersed in 3In the body.
Embodiment five: the PdCl of present embodiment 2Addition be nanometer ZnS nO 33% of base-material gross mass, other steps are identical with embodiment one, and gained particle mean grain size is about 40nm, Pd 2+Be dispersed in ZnSnO 3In the body
Sensitivity test
To implement 1～5 made gas sensitive respectively and be determined at sensitivity under the different hydrogen concentration, the result is as shown in table 1:
Table 1
Selectivity test
The ZnSnO3 that obtains with embodiment 1 carries out selectivity test, under 150 ℃ of working temperatures, measures it respectively to LPG, C 2H 2, NH 3, CH 3OH, C 2H 5OH, H 2Sensitivity, the result is as shown in table 2:
Table 2
Figure S2008100695325D00071
Conclusion:
A. mix PdCl 2The PdO-ZnSnO that makes 3Heater-type semiconductor hydrogen-sensitive element under 200～1600ppm hydrogen atmosphere, has higher sensitivity to hydrogen.Sensitivity changes along with the variation of doping, and experiment shows, PdCl 2Optimum doping amount is nanometer ZnS nO 35% o'clock of base-material gross mass, the highest to the sensitivity of hydrogen.Under 1600ppm, to the sensitivity of hydrogen up to 66.147.
B. LPG, C are being arranged 2H 2, NH 3, CH 3OH, C 2H 5Under the interference that other gases such as OH exist, with the PdO-ZnSnO of the inventive method preparation 3Heater-type semiconductor hydrogen-sensitive element still can keep higher sensitivity to hydrogen, demonstrates good selectivity.

Claims (2)

1. method for manufacturing gas sensor that detects hydrogen is characterized in that following steps are arranged:
A. preparation is doped with PdCl 2ZnSnO with tetraethoxysilance 3Powder, ZnSnO 3Powder consist of nanometer ZnS nO 3Base-material, PdCl 2And tetraethoxysilance, wherein nanometer ZnS nO 3The preparation method of base-material is:
1). press kation Zn 2+/ Sn 4+Be 1: 1 etc. mol ratio prepare Zn (SnO respectively 4) 27H 2O and SnCl 45H 2Each 2～5 liters of O solution respectively dilute twice with strong aqua and become 4～10 liters;
2). to soluble zinc salt Zn (SnO 4) 27H 2Splashing into ammoniacal liquor to the pH value of solution in the O solution is 9～12;
3). constantly under the magnetic agitation, to the solubility pink salt SnCl that has diluted 45H 2Dropping concentrated hydrochloric acid to the pH value of solution is 5～7 in the O solution;
4). with above-mentioned solubility pink salt Zn (SnO 4) 27H 2O solution slowly joins soluble zinc salt SnCl 45H 2In the O solution, dropping ammonia or hydrochloric acid, constantly stirring the acidity of adjusting solution down is PH=7, ZnSnO occurs 3Precipitation is 50KHz in ultrasonic frequency, and power is ultrasonic dispersing 3～5 hours under the 200W condition, gained ZnSnO 3Be deposited in-15～-10 ℃ of ageings 10 hours, behind the absolute ethyl alcohol flushing suction filtration, 100 ℃ of dryings 2～3 hours, sintering promptly got nanometer ZnS nO in 5 hours in 600～800 ℃ of air 3Base-material;
B.ZnSnO 3Powder is through after 3～6 hours ground and mixed, ultrasonic dispersing;
C. with deionized water with ZnSnO 3Behind the powder furnishing pasty state, be coated on the ceramic pipe that has platinum electrode, coating thickness is 0.5～1.5mm;
D. with above-mentioned ceramic pipe under 80～120 ℃ of temperature dry 1.5～2 hours, 600～800 ℃ of thermal treatment sintering were connected on the base that has the nickel limb after 8 hours, promptly got the gas sensor that is used to detect hydrogen.
2. preparation method according to claim 1 is characterized in that: ZnSnO 3PdCl in the powder 2Doping is nanometer ZnS nO 31%～10% of base-material gross mass, tetraethoxysilance are nanometer ZnS nO 30.1% of base-material gross mass.
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