CN102507662A - Preparation methods of lanthanum-doped cobalt nickel ferrite gas-sensitive powder and gas sensor - Google Patents

Preparation methods of lanthanum-doped cobalt nickel ferrite gas-sensitive powder and gas sensor Download PDF

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CN102507662A
CN102507662A CN2011103068271A CN201110306827A CN102507662A CN 102507662 A CN102507662 A CN 102507662A CN 2011103068271 A CN2011103068271 A CN 2011103068271A CN 201110306827 A CN201110306827 A CN 201110306827A CN 102507662 A CN102507662 A CN 102507662A
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lanthanum
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ferrite
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李耀刚
唐亚
王宏志
张青红
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Donghua University
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Abstract

The invention relates to preparation methods of lanthanum-doped cobalt nickel ferrite gas-sensitive powder and a gas sensor. The preparation method of the gas-sensitive powder comprises the following steps: (1) soluble cobalt salt, nickel salt, lanthanum salt and ferric salt are mixed and dispersed into ethylene glycol, and sodium acetate anhydrous is added and stirred to form reaction solution; and (2) the reaction solution is heated and reacted, then is cooled to room temperature after the reaction, and washed, centrifugated and dried. The preparation method of the gas sensor comprises the following steps: the gas-sensitive powder and terpilenol solution of ethyl cellulose are mixed and ground to form gas-sensitive slurry; and then the gas-sensitive slurry is uniformly coated to an Al2O3 ceramic tube with an Au electrode, conducted to gas drying and calcination, and installed on a testing base, and then the gas sensor is obtained after ageing. The preparation methods are simple, the requirement on the production equipment is low, the industrial production is easy, and the prepared gas-sensitive powder has good selectivity, good chemical stability and good sensitivity.

Description

The preparation method of a kind of lanthanum doping cobalt Ni ferrite air-sensitive powder and gas sensor
Technical field
The invention belongs to the preparation field of gas sensitive and gas sensor, particularly relate to a kind of lanthanum doping cobalt Ni ferrite (Co 1-xNi xLa yFe 2-yO 4) preparation method of air-sensitive powder and gas sensor.
Background technology
VOC is one type of air pollutants that human being's production, life had material impact; Many building materialss; People's detersive used in everyday, cosmetics and agricultural go up the agricultural chemicals that uses all can produce VOC, and common toxic, harmful VOC comprise ammoniacal liquor, benzene, toluene and methyl alcohol etc.Along with people's is to the pay attention to day by day of environmental protection; In air monitoring, food security and living environment monitoring field monitoring poisonous, harmful gas is had higher requirement; This also makes the research and development of gas sensor more and more come into one's own, and the gas sensitive of especially novel high selectivity has caused scientific circles and the great interest of industry member.
The gas sensitive of being used widely at present comprises conductor oxidates such as indium oxide, tin oxide, gallium oxide and zinc paste; Their advantage is that common toxic, harmful gas are all had higher sensitivity, but their shortcoming also is significantly same: the one, to the poor selectivity of specific harmful gas; The 2nd, poor chemical stability (the general requirement of gas sensor worked under higher temperature).To these two shortcomings of conventional semiconductors gas sensitive, solution commonly used comprises doping, compound and development of new gas sensitive.In recent years, ferrite receives bigger concern as one type of novel gas sensitive, and main cause is that the ferrite gas sensitive has high selectivity and better chemical stability, has well solved the shortcoming of conventional semiconductors type gas sensitive.It is lower that but the disadvantage of ferrite gas sensitive is sensitivity, and this has limited its large-scale application, and the sensitivity that therefore improves the ferrite gas sensitive just becomes the focus of the novel gas sensitive research of this type.
Ferrite Material comprises AB 2O 4Spinel-type and ABO 3Ca-Ti ore type, wherein ABO 3Ca-Ti ore type ferrite gas sensitive has obtained a large amount of research, and AB 2O 4Spinel type ferrite investigation of materials then less.The spinel type ferrite material of bibliographical information mainly contains NiFe 2O 4, CoFe 2O 4, ZnFe 2O 4And Co 1-xNi xFe 2O 4People such as Chu have been reported at Sensors andActuators B 120 (2006) 177-181 and have utilized the solvent-thermal method to have synthesized the nanocrystalline of vectolite and tested its sensitive property to alcohol vapour.People such as Reddy have been reported to through solvent-thermal method at Materials Research Bulletin 39 (2004) 1491-1498 and have synthesized Ni ferrite and tested its sensitive property to liquefied petroleum gas (LPG) (LPG).In order to improve the sensitivity of ferrite gas sensitive, ion doping is a kind of effective method, and Ce, La, REEs such as Nd are introduced in the ferritic lattice to increase its lattice imperfection.People such as Rezlescu can improve its sensitivity greatly last the report after Co and Mn ion doping are gone into Ni ferrite of Sensors and Actuators B 114 (2006) 427-432.People such as Gedam are helpful to the improvement of its sensitivity after introducing vectolite at the last minor N i ion of having reported of Journal of Sol-Gel Science and Technology 50 (2009) 296-300.
Research shows: vectolite and cobalt Ni ferrite become a kind of gas sensitive that gets a good chance of because of high selectivity and the better chemical stability that it had, but lower sensitivity still is to limit its key in application.
Summary of the invention
Technical matters to be solved by this invention provides the preparation method of a kind of lanthanum doping cobalt Ni ferrite air-sensitive powder and gas sensor, and this preparation method is simple, is easy to suitability for industrialized production; Prepared Co 1-xNi xLa yFe 2-yO 4Gas sensitive has higher selectivity and sensitivity to ammonia.
A kind of lanthanum doping cobalt Ni ferrite (Co of the present invention 1-xNi xLayFe 2-yO 4) preparation method of air-sensitive powder, comprising:
(1) at room temperature, press the ratio 1-x of amount of substance: x: y: 2-y mixes cobalt salt, nickel salt, lanthanum salt and the molysite of solubility, be distributed to then in the monoethylene glycol, and after treating to dissolve fully, Fe in the solution 3+The volumetric molar concentration scope is 0.085~0.106mol/L, and then adds anhydrous sodium acetate, stirs, and makes the above-mentioned substance dissolving, forms reactant liquor; Wherein the scope of x is 0.2~0.8, and the scope of y is 0.02~0.5;
(2) above-mentioned reactant liquor is heated to 180~220 ℃ of reaction 8~16h; After reaction finishes, be cooled to room temperature, wash centrifugal, dry at last Co 1-xNi xLa yFe 2-yO 4The air-sensitive powder.
The cobalt salt of the solubility described in the step (1) is nitrate, sulfate and the chlorate of cobalt, the nitrate Co (NO of preferred cobalt 3) 26H 2O; The nickel salt of described solubility is nitrate, sulfate and the chlorate of nickel, the nitrate Ni (NO of preferred nickel 3) 26H 2O; The lanthanum salt of described solubility is nitrate, sulfate and the chlorate of lanthanum, the nitrate La (NO of preferred lanthanum 3) 36H 2O; The molysite of described solubility is nitrate, sulfate and the chlorate of iron, the nitrate Fe (NO of preferred iron 3) 39H 2O.
Monoethylene glycol described in the step (1) is pure for analyzing.
The amount of substance and the La of the anhydrous sodium acetate that is added in the step (1) 3+And Fe 3+The ratio of amount of substance sum be 8: 1~12: 1.
The stirring rate that stirs described in the step (1) is 300~600 commentaries on classics/min, mixing time 20~40min.
Washing described in the step (2) is centrifugal for using distilled water, absolute ethanol washing product successively, and centrifuging is 3~5 times then.
The bake out temperature of oven dry is 40~80 ℃ described in the step (2), and the time is 12~24h.
The preparation method of a kind of lanthanum doping cobalt Ni ferrite gas sensor of the present invention comprises:
The lanthanum doping cobalt Ni ferrite air-sensitive powder of above-mentioned preparation is mixed with the terpineol solution of ethyl cellulose, grind 5~10min, form the air-sensitive slurry; Then the air-sensitive slurry for preparing evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after fully drying, in 450~550 ℃ of calcining 2~4h, attach it to then on the test pedestal, ageing obtained the gas sensor of stable performance after 7~12 days.
The mass volume ratio of the terpineol solution of described lanthanum doping cobalt Ni ferrite air-sensitive powder and ethyl cellulose is 0.1~0.2g/ml.
The massfraction of ethyl cellulose is 5~8% in the terpineol solution of described ethyl cellulose.
Described grinding is to grind in the agate mortar; The described welded and installed that is that adopts on the test pedestal that is installed to.
The present invention adopts solvent-thermal method to prepare La 3+Part replaces Co 1-xNi xLa yFe 2-yO 4The Fe of B position 3+, increase lattice imperfection, improved the sensitivity of cobalt Ni ferrite; The Co that the present invention is prepared 1-xNi xLa yFe 2-yO 4Air-sensitive powder and gas sensor have selectivity and higher sensitivity preferably to ammonia, and the preparation method is easy, are a kind of up-and-coming Ammonia Sensitive Material.
The air-sensitive performance test condition: its air-sensitive performance of static liquid distribution method test is adopted in experiment; Concrete steps are to utilize liquid-transfering gun to pipette certain amount of ammonia water, toluene, ethanol, benzene, methyl alcohol and xylene solution; Drip on the warm table of air-sensitive test macro (Fig. 1 sees in WS-30A, Zhengzhou Wei Sheng Electronic Technology Co., Ltd) fast; Under heating and action of fan, steam is mixed in confined space; The concentration range of chemical vapors is: 500~4000ppm, the WV of gas sensitive is: 5~9V obtains its air-sensitive performance through the resistance variations that detects gas sensitive.
Beneficial effect
(1) preparation method of the present invention is simple, and is low to the production equipment requirement, is easy to suitability for industrialized production;
(2) the prepared Co of the present invention 1-xNi xLa yFe 2-yO 4The gas sensitive selectivity is good, chemical stability is good, sensitivity is better.
Description of drawings
Fig. 1. air-sensitive test macro synoptic diagram;
Fig. 2 .Co 0.8Ni 0.2La 0.2Fe 1.8O 4The X-ray diffractogram of air-sensitive powder;
Fig. 3 .Co 0.8Ni 0.2La 0.2Fe 1.8O 4The sem photograph of air-sensitive powder;
Fig. 4 .Co 0.8Ni 0.2La 0.2Fe 1.8O 4The air-sensitive selectivity comparison diagram of gas sensitive;
Fig. 5 .Co 0.8Ni 0.2Fe 2O 4And Co 0.8Ni 0.2La 0.2Fe 1.8O 4(wherein a is Co to gas sensitive to the sensitivity test figure of ammonia 0.8Ni 0.2Fe 2O 4The sensitivity test curve of gas sensitive under the ammonia atmosphere of 500ppm, b, c, d, e and f are respectively Co 0.8Ni 0.2La 0.2Fe 1.8O 4The sensitivity test curve of gas sensitive under the ammonia atmosphere of 500ppm, 1000ppm, 1500ppm, 2000ppm and 4000ppm).
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing 1.8181g Fe (NO 3) 39H 2O, 0.5821g Co (NO 3) 26H 2O, 0.1454g Ni (NO 3) 26H 2O, 0.2165g La (NO 3) 36H 2O adds there-necked flask, adds the analytically pure ethylene glycol solution of 50ml again, through fully stirring Fe in the solution 3+Volumetric molar concentration is 0.09mol/L; Add the 3.6g anhydrous sodium acetate again, be mechanical raking 25min under the 500 commentaries on classics/min, after treating to dissolve fully, more above-mentioned solution is poured in the agitated reactor, be warming up to 200 ℃, reaction 12h at rotating speed.Reaction finishes, and product is used distilled water and absolute ethanol washing, centrifuging 3 times respectively, then with product at 80 ℃ times dry 12h, obtain Co 0.8Ni 0.2La 0.2Fe 1.8O 4Nano-powder.
Fig. 2 is the X-ray diffractogram of present embodiment synthetic powder, and the diffraction peak among the figure shows: this nano-powder is Co 0.8Ni 0.2La 0.2Fe 1.8O 4, the Scherrer formula calculates and shows that the crystallite dimension of synthetic powder is about 5.4nm; Fig. 3 is the stereoscan photograph of synthetic powder, can find out the Co in this powder 0.8Ni 0.2La 0.2Fe 1.8O 4Particle size greatly about about 100nm, Size Distribution is comparatively even.
Take by weighing the Co of 0.075g 0.8Ni 0.2La 0.2Fe 1.8O 4Air-sensitive powder and 0.75ml massfraction are that the terpineol solution of 5% ethyl cellulose mixes mutually, in agate mortar, grind 10min, form the air-sensitive slurry; The air-sensitive slurry for preparing evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after fully drying, be positioned in the muffle furnace and calcine 4h, then it is welded on the test pedestal, after 12 days, obtain the gas sensor of stable performance through ageing with 450 ℃.
The gas sensor for preparing is placed the steam atmosphere of certain density ammonia, ethanol, toluene, benzene, methyl alcohol and xylene respectively, and the variation through testing software its resistance value of monitoring obtains air-sensitive performance.Fig. 4 is the selectivity comparison diagram of this gas sensitive to six kinds of common chemical vaporses, can obtain this gas sensitive from test result ammonia is had good selectivity; Fig. 5 is the sensitivity test to ammonia under gas with various concentration and different operating voltage of this gas sensitive, can obtain the optimum operating voltage that 8V is this gas sensitive from test result, and its sensitivity reaches 12.8 under the ammonia atmosphere of 4000ppm.
Embodiment 2
Take by weighing 1.9191g Fe (NO 3) 39H 2O, 0.5821g Co (NO 3) 26H 2O, 0.1454g Ni (NO 3) 26H 2O, 0.1083g La (NO 3) 36H 2O adds there-necked flask, adds the analytically pure ethylene glycol solution of 55ml again, through fully stirring Fe in the solution 3+Volumetric molar concentration is 0.085mol/L; Add the 4.42g anhydrous sodium acetate again, be mechanical raking 40min under the 300 commentaries on classics/min, after treating to dissolve fully, more above-mentioned solution is poured in the agitated reactor, be warming up to 220 ℃, reaction 8h at rotating speed; Reaction finishes, and product is used distilled water and absolute ethanol washing, centrifuging 4 times respectively, then with product at 60 ℃ times dry 18h, obtain Co 0.8Ni 0.2La 0.1Fe 1.9O 4Nano-powder.
X-ray diffraction analysis shows: this nano-powder is Co 0.8Ni 0.2La 0.1Fe 1.9O 4Can find out the Co this powder from the stereoscan photograph of synthetic powder 0.8Ni 0.2La 0.1Fe 1.9O 4Particle size greatly about about 100nm.
Take by weighing the Co of 0.08g 0.8Ni 0.2La 0.1Fe 1.9O 4Air-sensitive powder and 0.65ml massfraction are that the terpineol solution of 6% ethyl cellulose mixes mutually, in agate mortar, grind 5min, form the air-sensitive slurry.The air-sensitive slurry for preparing evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after fully drying, be positioned in the muffle furnace and calcine 2h, then it is welded on the test pedestal, after 10 days, obtain the gas sensor of stable performance through ageing with 550 ℃.
Selectivity contrast test result shows that this gas sensitive has good selectivity to ammonia; This gas sensitive of air-sensitive test shows to ammonia under gas with various concentration and different operating voltage has higher sensitivity.
Embodiment 3
Take by weighing 1.5151g Fe (NO 3) 39H 2O, 0.1455g Co (NO 3) 26H 2O, 0.5816g Ni (NO 3) 26H 2O, 0.5413g La (NO 3) 36H 2O adds there-necked flask, adds the analytically pure ethylene glycol solution of 50ml again, through fully stirring Fe in the solution 3+Volumetric molar concentration is 0.094mol/L; Add the 4.62g anhydrous sodium acetate again, be mechanical raking 35min under the 400 commentaries on classics/min, after treating to dissolve fully, more above-mentioned solution is poured in the agitated reactor, be warming up to 190 ℃, reaction 14h at rotating speed.Reaction finishes, and product is used distilled water and absolute ethanol washing, centrifuging 5 times respectively, then with product at 50 ℃ times dry 22h, obtain Co 0.2Ni 0.8La 0.5Fe 1.5O 4Nano-powder.
X-ray diffraction analysis shows: this nano-powder is Co 0.8Ni 0.2La 0.1Fe 1.9O 4Can find out the Co this powder from the stereoscan photograph of synthetic powder 0.2Ni 0.8La 0.5Fe 1.5O 4Particle size greatly about about 100nm.
Take by weighing the Co of 0.09g 0.2Ni 0.8La 0.5Fe 1.5O 4Air-sensitive powder and 0.6ml massfraction are that the terpineol solution of 7% ethyl cellulose mixes mutually, in agate mortar, grind 8min, form the air-sensitive slurry; The air-sensitive slurry for preparing evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after fully drying, be positioned in the muffle furnace and calcine 3h, then it is welded on the test pedestal, after 7 days, obtain the gas sensor of stable performance through ageing with 500 ℃.
Selectivity contrast test result shows that this gas sensitive has good selectivity to ammonia; This gas sensitive of air-sensitive test shows to ammonia under gas with various concentration and different operating voltage has higher sensitivity.
Embodiment 4
Take by weighing 1.9191g Fe (NO 3) 39H 2O, 0.2911g Co (NO 3) 26H 2O, 0.4362g Ni (NO 3) 26H 2O, 0.1083g La (NO 3) 36H 2O adds there-necked flask, adds the analytically pure ethylene glycol solution of 45ml again, through fully stirring Fe in the solution 3+Volumetric molar concentration is 0.106mol/L; Add the 4.8g anhydrous sodium acetate again, be mechanical raking 20min under the 600 commentaries on classics/min, after treating to dissolve fully, more above-mentioned solution is poured in the agitated reactor, be warming up to 210 ℃, reaction 10h at rotating speed.Reaction finishes, and product is used distilled water and absolute ethanol washing, centrifuging 4 times respectively, then with product at 70 ℃ times dry 14h, obtain Co 0.4Ni 0.6La 0.1Fe 1.9O 4Nano-powder.
X-ray diffraction analysis shows: this nano-powder is Co 0.8Ni 0.2La 0.1Fe 1.9O 4Can find out the Co this powder from the stereoscan photograph of synthetic powder 0.4Ni 0.6La 0.1Fe 1.9O 4Particle size greatly about about 100nm.
Take by weighing the Co of 0.095g 0.4Ni 0.6La 0.1Fe 1.9O 4Air-sensitive powder and 0.55ml massfraction are that the terpineol solution of 8% ethyl cellulose mixes mutually, in agate mortar, grind 7min, form the air-sensitive slurry.The air-sensitive slurry for preparing evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after fully drying, be positioned in the muffle furnace and calcine 4h, then it is welded on the test pedestal, after 9 days, obtain the gas sensor of stable performance through ageing with 450 ℃.Selectivity contrast test result shows that this gas sensitive has good selectivity to ammonia; This gas sensitive of air-sensitive test shows to ammonia under gas with various concentration and different operating voltage has higher sensitivity.
Embodiment 5
Take by weighing 2.6031g Fe 2(SO 4) 37H 2O, 0.1406g CoSO 47H 2O, 0.5257g NiSO 46H 2O, 0.0364gLa 2(SO 4) 39H 2O adds there-necked flask, adds the analytically pure ethylene glycol solution of 50ml again, through fully stirring Fe in the solution 3+Volumetric molar concentration is 0.099mol/L.Add the 4.92g anhydrous sodium acetate again, be mechanical raking 30min under the 450 commentaries on classics/min, after treating to dissolve fully, more above-mentioned solution is poured in the agitated reactor, be warming up to 180 ℃, reaction 16h at rotating speed.Reaction finishes, and product is used distilled water and absolute ethanol washing, centrifuging 3 times respectively, then with product at 40 ℃ times dry 24h, obtain Co 0.2Ni 0.8La 0.02Fe 1.98O 4Nano-powder.
X-ray diffraction analysis shows: this nano-powder is Co 0.8Ni 0.2La 0.1Fe 1.9O 4Can find out the Co this powder from the stereoscan photograph of synthetic powder 0.8Ni 0.2La 0.1Fe 1.9O 4Particle size greatly about about 100nm.
Take by weighing the Co of 0.1g 0.8Ni 0.2La 0.1Fe 1.9O 4Air-sensitive powder and 0.5ml massfraction are that the terpineol solution of 6% ethyl cellulose mixes mutually, in agate mortar, grind 9min, form the air-sensitive slurry; The air-sensitive slurry for preparing evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after fully drying, be positioned in the muffle furnace and calcine 3h, then it is welded on the test pedestal, after 8 days, obtain the gas sensor of stable performance through ageing with 500 ℃.
Selectivity contrast test result shows that this gas sensitive has good selectivity to ammonia; This gas sensitive of air-sensitive test shows to ammonia under gas with various concentration and different operating voltage has higher sensitivity.

Claims (10)

1. lanthanum doping cobalt Ni ferrite Co 1-xNi xLayFe 2-yO 4The preparation method of air-sensitive powder comprises:
(1) at room temperature, press the ratio 1-x of amount of substance: x: y: 2-y mixes cobalt salt, nickel salt, lanthanum salt and the molysite of solubility, be distributed to then in the monoethylene glycol, and after treating to dissolve fully, Fe in the solution 3+The volumetric molar concentration scope is 0.085~0.106mol/L, and then adds anhydrous sodium acetate, stirs, and makes the above-mentioned substance dissolving, forms reactant liquor; Wherein the scope of x is 0.2~0.8, and the scope of y is 0.02~0.5;
(2) above-mentioned reactant liquor is heated to 180~220 ℃ of reaction 8~16h; After reaction finishes, be cooled to room temperature, wash centrifugal, dry at last lanthanum doping cobalt Ni ferrite air-sensitive powder.
2. a kind of lanthanum doping cobalt Ni ferrite Co according to claim 1 1-xNi xLa yFe 2-yO 4The preparation method of air-sensitive powder is characterized in that: the cobalt salt of the solubility described in the step (1) is nitrate, sulfate and the chlorate of cobalt; The nickel salt of described solubility is nitrate, sulfate and the chlorate of nickel; The lanthanum salt of described solubility is nitrate, sulfate and the chlorate of lanthanum; The molysite of described solubility is nitrate, sulfate and the chlorate of iron.
3. a kind of lanthanum doping cobalt Ni ferrite Co according to claim 1 1-xNi xLa yFe 2-yO 4The preparation method of air-sensitive powder is characterized in that: the cobalt salt of the solubility described in the step (1), nickel salt, lanthanum salt and molysite are followed successively by the nitrate Co (NO of cobalt 3) 26H 2Nitrate Ni (the NO of O, nickel 3) 26H 2Nitrate La (the NO of O, lanthanum 3) 36H 2Nitrate Fe (the NO of O, iron 3) 39H 2O.
4. a kind of lanthanum doping cobalt Ni ferrite Co according to claim 1 1-xNi xLa yFe 2-yO 4The preparation method of air-sensitive powder is characterized in that: the monoethylene glycol described in the step (1) is pure for analyzing.
5. a kind of lanthanum doping cobalt Ni ferrite Co according to claim 1 1-xNi xLa yFe 2-yO 4The preparation method of air-sensitive powder is characterized in that: the amount of substance and the La of the anhydrous sodium acetate that is added in the step (1) 3+And Fe 3+The ratio of amount of substance sum be 8: 1~12: 1.
6. a kind of lanthanum doping cobalt Ni ferrite Co according to claim 1 1-xNi xLa yFe 2-yO 4The preparation method of air-sensitive powder is characterized in that: the stirring rate that stirs described in the step (1) is 300~600 commentaries on classics/min, mixing time 20~40min.
7. a kind of lanthanum doping cobalt Ni ferrite Co according to claim 1 1-xNi xLa yFe 2-yO 4The preparation method of air-sensitive powder is characterized in that: the washing described in the step (2) is centrifugal for using distilled water, absolute ethanol washing product successively, and centrifuging is 3~5 times then; The bake out temperature of said oven dry is 40~80 ℃, and the time is 12~24h.
8. the preparation method of a lanthanum doping cobalt Ni ferrite gas sensor comprises:
The lanthanum doping cobalt Ni ferrite air-sensitive powder that claim 1 is prepared mixes with the terpineol solution of ethyl cellulose, grinds 5~10min, forms the air-sensitive slurry; Then above-mentioned air-sensitive slurry evenly is coated on the Al that has the Au electrode 2O 3On the ceramic pipe, after drying, in 450~550 ℃ of calcining 2~4h, attach it to then on the test pedestal, ageing promptly got gas sensor after 7~12 days.
9. the preparation method of a kind of lanthanum doping cobalt Ni ferrite gas sensor according to claim 8 is characterized in that: the mass volume ratio of the terpineol solution of described lanthanum doping cobalt Ni ferrite air-sensitive powder and ethyl cellulose is 0.1~0.2g/ml; The massfraction of ethyl cellulose is 5~8% in the terpineol solution of ethyl cellulose.
10. the preparation method of a kind of lanthanum doping cobalt Ni ferrite gas sensor according to claim 8, it is characterized in that: described grinding is to grind in the agate mortar; The described welded and installed that is that adopts on the test pedestal that is installed to.
CN201110306827.1A 2011-10-11 2011-10-11 Preparation methods of lanthanum-doped cobalt nickel ferrite gas-sensitive powder and gas sensor Expired - Fee Related CN102507662B (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012161713A (en) * 2011-02-03 2012-08-30 Agc Seimi Chemical Co Ltd Ammonia decomposition catalyst and decomposition method of ammonia
CN103091369A (en) * 2012-11-30 2013-05-08 郑州轻工业学院 Preparation method of Pd-nanoparticle-modified porous ZnO nanosheet gas-sensitive material and gas sensor
CN103529080A (en) * 2013-10-17 2014-01-22 山东理工大学 Preparation method of film-type gas sensor
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CN105238985A (en) * 2015-07-02 2016-01-13 苏州科技学院 Sulfur-doped iron-nickel oxygen alloy and preparing method thereof
CN109678218A (en) * 2018-12-17 2019-04-26 上海理工大学 A kind of preparation method of cobalt/nickel co-doped zinc oxide composite air-sensitive material
CN113376310A (en) * 2021-06-17 2021-09-10 上海松柏传感技术有限公司 Preparation method of gas-sensitive material for combustible gas sensor and product
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101852754A (en) * 2010-05-14 2010-10-06 云南大学 Lanthanum-ferrite-doping formaldehyde gas sensitive material and preparation method thereof
CN101857275A (en) * 2010-05-19 2010-10-13 北京化工大学 Magnesium doped lanthanum ferrite gas sensitive material and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101852754A (en) * 2010-05-14 2010-10-06 云南大学 Lanthanum-ferrite-doping formaldehyde gas sensitive material and preparation method thereof
CN101857275A (en) * 2010-05-19 2010-10-13 北京化工大学 Magnesium doped lanthanum ferrite gas sensitive material and preparation method and application thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
《Journal of Sol-Gel Science and technology》 20090323 Gedam N.N. et al Ammonia gas sensor based on a spinel semiconductor Co0.8Ni0.2Fe2O4 nanomaterial , *
《功能材料》 19951031 张天舒 等 "镧掺杂对CdO-SnO2系物相及性能的影响 , *
GEDAM N.N. ET AL: "Ammonia gas sensor based on a spinel semiconductor Co0.8Ni0.2Fe2O4 nanomaterial", 《JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY》 *
N. REZLESCU ET.AL: "Semiconducting gas sensor for acetone based on the fine grained nickel ferrite", 《SENSORS AND ACTUATORS B》 *
张天舒 等: ""镧掺杂对CdO-SnO2系物相及性能的影响", 《功能材料》 *

Cited By (10)

* Cited by examiner, † Cited by third party
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JP2012161713A (en) * 2011-02-03 2012-08-30 Agc Seimi Chemical Co Ltd Ammonia decomposition catalyst and decomposition method of ammonia
CN103091369A (en) * 2012-11-30 2013-05-08 郑州轻工业学院 Preparation method of Pd-nanoparticle-modified porous ZnO nanosheet gas-sensitive material and gas sensor
CN103529080A (en) * 2013-10-17 2014-01-22 山东理工大学 Preparation method of film-type gas sensor
CN103529080B (en) * 2013-10-17 2015-07-01 山东理工大学 Preparation method of film-type gas sensor
CN103675033A (en) * 2013-11-29 2014-03-26 中山鼎晟生物科技有限公司 Detecting system for moisture retention of cosmetics
CN105238985A (en) * 2015-07-02 2016-01-13 苏州科技学院 Sulfur-doped iron-nickel oxygen alloy and preparing method thereof
CN105238985B (en) * 2015-07-02 2017-03-22 苏州科技学院 Sulfur-doped iron-nickel oxygen alloy and preparing method thereof
CN109678218A (en) * 2018-12-17 2019-04-26 上海理工大学 A kind of preparation method of cobalt/nickel co-doped zinc oxide composite air-sensitive material
CN113376310A (en) * 2021-06-17 2021-09-10 上海松柏传感技术有限公司 Preparation method of gas-sensitive material for combustible gas sensor and product
CN113433171A (en) * 2021-06-24 2021-09-24 兰州大学 Gas-sensitive material, gas-sensitive sensor, and preparation method and application thereof

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