CN101532976A - SmFeO3-based conductance acetone gas sensitive material, preparation method and application thereof - Google Patents
SmFeO3-based conductance acetone gas sensitive material, preparation method and application thereof Download PDFInfo
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- CN101532976A CN101532976A CN200910068068A CN200910068068A CN101532976A CN 101532976 A CN101532976 A CN 101532976A CN 200910068068 A CN200910068068 A CN 200910068068A CN 200910068068 A CN200910068068 A CN 200910068068A CN 101532976 A CN101532976 A CN 101532976A
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- smfeo
- sensitive material
- base
- solution
- smfeo3
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Abstract
The invention relates to a SmFeO3-based conductance acetone gas sensitive material, a preparation method and an application thereof. The SmFeO3-based conductance acetone gas sensitive material is a composite oxide with a general form being (Sm1-xLax)(Fe1-yBy)O3, wherein, B represents Cu, Ni, 0<=x<=0.5 and 0.05<=y<=0.2. A SmFeO3 based chemical composition sensitive material is formed for designing formulation by critic acid complexation-polymerizing liquid phase chemical method, and then the material is used for forming thin film type directly-heated sensor or sintering type indirectly heated sensor. The thin film type and sintering type gas sensors prepared by the SmFeO3 based sensitive material can realize the detection of acetone gas with light concentration, has the characteristics of high sensitivity, wide operation temperature range, good selectivity, rapid response and recovery time and excellent stability, and is applicable in fields of respiration detection of diabetic, food quality detection, animal husbandry detection and the like.
Description
Technical field
The invention belongs to semi-conductor gas sensitive material engineering field, be specifically related to SmFe0
3Based conductance acetone gas sensitive material, preparation method and application.
Background technology
Along with the development of society, daily life contacts all kinds of gases with people in the commercial production situation also gets more and more.Acetone gas wherein both can be used as the good solvent of organic substance in industry, be again simultaneously the important source material in the chemosynthesis, can be used for synthesize methyl-isobutyl ketone, diketoalcohol etc.In addition, acetone still is a kind of product of animal body metabolism, be to be caused by increasing of serum ketoboidies in the blood as the ketoacidosis of diabetes, and acetone is the final product of ketoboidies metabolism.In food quality detects, by the detection of acetone concentration in the gas of meat product volatilization being estimated the fresh-keeping situation of food.
Quantitative detecting method to acetone gas mainly contains gas phase or liquid phase chromatography, spectrophotometer method, quartz crystal micro-balance method, Light Addressable Potentiometric Sensor (LAPS) method and Fiber Optical Sensor Based etc. before this.It is relatively more expensive that these detection methods detect cost, and the preparation method is also very complicated.
Use new material, the new gas sensor of new technology research and development, all gases gas is analyzed and detected is one of current important research and application.At present, conductivity type gas sensitive material and element are the main products in using, and its performance not only depends on the chemical composition of material, also depends on the micromechanism and the manufacturing process of material to a great extent.Perovskite composite oxide (ABO wherein
3) having flexibly can " chemical tailoring " design feature, this class gas sensitive had both had very high composition susceptibility, and very high process sensitivity is arranged again.ABO
3Just be studied in a lot of fields and develop as a kind of gas sensitive, wide application prospect is arranged.
Ferrous acid samarium base (SmFeO of the present invention
3) the composite oxide semiconductor gas sensor, have highly sensitive to the low concentration acetone gas, response is fast, volume is little, energy consumption and characteristics such as cost is low, simple to operate, can be widely used in the various application to the acetone gas detection.
Summary of the invention
The invention provides a class with SmFeO
3Conductance acetone gas sensitive material and preparation method for base.This material is by SmFeO
3Composite oxides are formed, according to sensitivity to the acetone air-sensitive, and selectivity, the different request for utilizations of working temperature, application background etc. can realize its sensitivity characteristic by different transition metal and rare earth doped in gas sensory material of the present invention.Wherein at Sm position doped chemical La, at Fe position difference doped chemical Cu, Ni, can form as chemical composition like this is (Sm
1-xLa
x) (Fe
1-yB
y) O
3The composite oxides sensitive material.
By liquid chemical method above-mentioned composite oxides sensitive material is made the colloidal sol form, form film-type directly-heated type and slug type heater-type semiconductor transducer by technology again, realize acetone gas is detected.Material of the present invention and preparation method are highly sensitive to acetone gas, and operating temperature range is wide, and selectivity is good, and response, release time is fast, good stability.
Technology of the present invention is achieved in that
A kind of SmFeO
3Be the conductance acetone gas sensitive material of base, it is characterized in that general formula is (Sm
1-xLa
x) (Fe
1-yB
y) O
3Composite oxides, wherein B represents Cu, Ni, 0≤x≤0.5,0.05≤y≤0.2.
SmFeO of the present invention
3Be the preparation method of the conductance acetone gas sensitive material of base, step is as follows:
A) Sm (NO of configuration 0.5mol/L
3)
3Solution; Fe (the NO of configuration 0.5mol/L
3)
3Solution; The citric acid solution of configuration 1.0mol/L; Take by weighing respectively and contain wherein a kind of nitrate powder of La, Cu, Ni, place in the different separately containers, be dissolved in water, mix, form the solution of 0.5mol/L;
B) by (Sm
1-xLa
x) (Fe
1-yB
y) O
3The metering ratio of composite oxides makes SmFeO
3Based sols is pressed SmFeO again
3Base: the mol ratio of citric acid=1:1 is with SmFeO
3Base mixes with aqueous citric acid solution, forms the SmFeO of component design
3The basic chemical composition solution of base sensitive material.
C) with (Sm
1-xLa
x) (Fe
1-yB
y) O
3Composite oxides solution place heating environment, temperature is controlled at 40-60 ℃, adds ethylene glycol, and its mol ratio is ethylene glycol: citric acid=0.1:1, under agitation mix, the metallic ion formed polyester network of esterified reaction institute huge legendary turtle in citric acid-ethylene glycol complex compound is closed; Add weak aqua ammonia and be adjusted to pH=5, carry out concentration correction, continue stirring and obtain even, stable concentration, finish citric acid complex-polymerization colloidal sol overall process, form the SmFeO of colloidal sol form at the 0.2-0.4mol/L precursor sol by adding entry
3The base sensitive material.
SmFeO of the present invention
3Being the application of the conductance acetone gas sensitive material of base, is to use to form film-type directly-heated type sensor or slug type heater-type sensor.
Film-type directly-heated type sensor and slug type heater-type sensor can adopt any method preparation.Also can adopt following method:
The preparation method of film-type directly-heated type sensor:
1) with SmFeO
3The base sensitive material film heats up with the speed of 3-5 ℃/min, at 600-800 ℃ of thermal treatment 60-120 minute, obtains SmFeO
3Base crystallinity film; The crystallinity film was immersed in rare platinum acid chloride solution 20 minutes, dry back obtains SmFeO 500 ℃ of thermal treatments 30 minutes again
3The based sensor film; The preparation method of slug type heater-type sensor:
(1) with the SmFeO for preparing
3It is fully dry earlier that base sensitive material colloidal sol 0.4mol/L puts into container, forms xerogel; Put into the speed intensification of sintering furnace again, be prepared into SmFeO at 700-850 ℃ of sintering 60-120 minute with 3-5 ℃/min
3Base crystallinity powder;
(2) put into mortar with absolute ethyl alcohol as the medium wet-milling, after oven dry is sieved powder is added inorganic and organic sticking hybrid junctions agent furnishing slurry, slurry is coated on the alumina ceramic tube that has gold electrode equably, cover whole electrodes, the thickness that select to need, drying be placed in the sintering furnace 500-700 ℃ sintering 1-3 hour, again sintered body was immersed in rare platinum acid chloride solution 20 minutes, dry back obtains SmFeO 500 ℃ of thermal treatments 30 minutes
3The based sensor sintered material.
Adopt the present invention with SmFeO
3Base is a sensitive material, by the film-type and the sintering-type gas sensor of citric acid complex-polymer fluid phase chemistry method preparation, can realize the detection to acetone gas, it has highly sensitive, and operating temperature range is wide, and selectivity is good, response, release time is fast, characteristics such as good stability.At SmFeO
3In the base sensitive material, remove above-mentioned mention at Sm position doping La, doped with Cu, Ni respectively in the Fe position form (Sm
1-xLa
x) (Fe
1-yB
y) O
3The combined oxidation beyond the region of objective existence also can at Fe position difference doped with Mn, Mo etc., all can form the sensitive material with identical function at Sm position doping Sr, Zn, Ca.The susceptibility that the present invention is preferable to the low concentration acetone gas is particularly suitable for the breathing detection in diabetes, and food quality detects, fields such as animal husbandry detection, and research is remarkable with using value.
Embodiment
Embodiment 1:
(1) takes by weighing 5.0g powder stock Sm (NO
3)
36H
2O puts into beaker, adds an amount of dissolved in distilled water, mixes, and forms the solution of 0.5mol/L; Take by weighing 5.0g powder stock Fe (NO
3)
39H
2O puts into beaker, adds an amount of dissolved in distilled water, mixes, and forms the solution of 0.5mol/L; Take by weighing 10.0g citric acid powder, add an amount of dissolved in distilled water, mix, form the aqueous citric acid solution of 1.0mol/L concentration.Take by weighing 2.0g powder stock La (NO
3)
33H
2O puts into beaker, adds an amount of dissolved in distilled water, mixes, and forms the solution of 0.5mol/L.Take by weighing 2.0g powder stock Cu (NO
3)
26H
2O puts into beaker, adds an amount of dissolved in distilled water, mixes, and forms the solution of 0.5mol/L.
(2) by (Sm
0.5La
0.5) (Fe
0.8Cu
0.2) O
3The metering ratio of composite oxides makes SmFeO
3Based sols is pressed SmFeO again
3Base: the mol ratio of citric acid=1:1 is with SmFeO
3Base mixes with aqueous citric acid solution, forms composite solution.
(3) the above-mentioned container for preparing solution is placed heating environment, temperature is controlled at 40 ℃, is that the amount of ethylene glycol: citric acid=0.1:1 adds ethylene glycol in molar ratio, stirs to mix down to continue 3 hours, promotes to take place esterification.Add suitable weak aqua ammonia and be adjusted to pH=5, and add entry again and carry out concentration correction, mixed again 3 hours, obtain uniform and stable concentration at the 0.2mol/L precursor sol.
Embodiment 2:
Step of preparation process is identical with embodiment 1, and different is by (Sm in above-mentioned (2)
0.75La
0.25) (Fe
0.9Cu
0.1) O
3The metering ratio of composite oxides makes SmFeO
3Based sols; The container that will prepare solution in above-mentioned (3) places heating environment, and temperature is controlled at 50 ℃, obtains uniform and stable concentration at last at the 0.3mol/L precursor sol.
Embodiment 3:
Step of preparation process is identical with embodiment 1, and different is to press Sm (Fe in above-mentioned (2)
0.95Cu
0.05) O
3The metering ratio of composite oxides makes SmFeO
3Based sols; The container that will prepare solution in above-mentioned (3) places heating environment, and temperature is controlled at 60 ℃, obtains uniform and stable concentration at last at the 0.4mol/L precursor sol.
Embodiment 4:
Step of preparation process is identical with embodiment 1, and different is will take by weighing 2.0g powder stock Cu (NO in above-mentioned (1)
3)
26H
2O changes into and takes by weighing 2.0g powder stock Ni (NO
3)
26H
2O puts into beaker, adds an amount of dissolved in distilled water, mixes, and forms the solution of 0.5mol/L.
(2) among the embodiment 1 are changed into (the Fe by Sm
0.8Ni
0.2) O
3The metering ratio of composite oxides makes SmFeO
3Based sols.Other step is with embodiment 1.
Embodiment 5:
Step of preparation process is identical with embodiment 4, and different is changes (the Fe by Sm into above-mentioned
0.9Ni
0.1) O
3The metering ratio of composite oxides makes SmFeO
3Based sols.Other step is with embodiment 4.
Embodiment 6:
Step of preparation process is identical with embodiment 4, and different is changes (the Fe by Sm into above-mentioned
0.95Ni
0.05) O
3The metering ratio of composite oxides makes SmFeO
3Based sols.Other step is with embodiment 4.
Embodiment 7:
(1) one side is coated with interdigital gold electrode, reverse side has the Al of heating electrode
2O
3The substrate ultrasonic cleaning, oven dry.Immerse then in the precursor sol of the foregoing description 1, with speed slowly it is vertically lifted out liquid level, obtain sol pellicle, the drying polymerization obtains gel mould.
(2) repeat method 3 times in above-mentioned (1), the speed of dried film with 3 ℃/min is heated up, 600 ℃ of thermal treatments 60 minutes.The film that burns till was immersed in rare platinum acid chloride solution 20 minutes, dry back obtains SmFeO 500 ℃ of thermal treatments 30 minutes again
3The based sensor film.
(3) with SmFeO
3Base film in the base of sensor, through burin-in process, forms film-type directly-heated type sensor together with substrate welds, carries out the test of gas-sensitive property.
Embodiment 8:
Step of preparation process is identical with embodiment 7, and different is the precursor sol that immerses embodiment 2 in above-mentioned (1); In above-mentioned (2), the speed of dried film with 4 ℃/min is heated up, 700 ℃ of thermal treatments 90 minutes.Other step is with embodiment 7.
Embodiment 9:
Step of preparation process is identical with embodiment 7, and different is the precursor sol that immerses embodiment 3 in above-mentioned (1); In above-mentioned (2), the speed of dried film with 5 ℃/min is heated up, 800 ℃ of thermal treatments 120 minutes.Other step is with embodiment 7.
Embodiment 10:
(1) the 0.4mol/L precursor sol that the foregoing description 3 is prepared is put into the abundant earlier drying of container, forms xerogel.Put into the speed intensification of sintering furnace again, be prepared into SmFeO in 60 minutes at 700 ℃ of sintering with 3 ℃/min
3Base crystallinity powder.(2) with the powder that is prepared into, put into mortar with absolute ethyl alcohol as the medium wet-milling.After oven dry is sieved powder added 1% porcelain earth and terpinol furnishing slurry.Slurry is coated on the alumina ceramic tube that has gold electrode equably, and drying was placed in the sintering furnace 500 ℃ of sintering 1 hour.Sintered body was immersed in rare platinum acid chloride solution 20 minutes, dry back obtains SmFeO 500 ℃ of thermal treatments 30 minutes again
3The based sensor sintered material.
(3) heater strip that will have an appropriate resistance penetrates in the burned tube core, then contact conductor and heater strip lead-in wire is welded on the base of element, and it is aging to be placed on the agingtable energising.Form slug type heater-type sensor, carry out the test of gas-sensitive property.
Embodiment 11:
Step of preparation process is identical with embodiment 10, and different is in above-mentioned (1), and the 0.4mol/L precursor sol that the foregoing description 4 prepares is put into the abundant earlier drying of container, forms xerogel.Put into the speed intensification of sintering furnace again, be prepared into SmFeO in 90 minutes at 800 ℃ of sintering with 4 ℃/min
3Base crystallinity powder.In above-mentioned (2), drying was placed in the sintering furnace 600 ℃ of sintering 2 hours.Other step is with embodiment 10.
Embodiment 12:
Step of preparation process is identical with embodiment 10, and different is in above-mentioned (1), and the 0.4mol/L precursor sol that the foregoing description 5 prepares is put into the abundant earlier drying of container, forms xerogel.Put into the speed intensification of sintering furnace again, be prepared into SmFeO in 120 minutes at 850 ℃ of sintering with 5 ℃/min
3Base crystallinity powder.In above-mentioned (2), drying was placed in the sintering furnace 700 ℃ of sintering 3 hours.Other step is with embodiment 10.
The example 7 that is obtained is as shown in table 1 to the experimental result of example 12.
The different embodiments of table 1 obtain the performance of sample
Annotate: in the sensitivity, Rg: sensor is resistance in 5ppm acetone atmosphere, and Ra: sensor is resistance in air atmosphere; The response time/time release time is meant 90% required time of recovering respectively to arrive end point values by acetone gas response and bubbling air, with unit's of doing second; Selectivity, middle no unit refers to that sensor (comprises H in acetone gas sensitivity and other gas
2O, CO
2, CO, NH
3) in the ratio of a maximum sensitivity; The stability fluctuation refers to the percent of sensitivity fluctuation in 10 days.
All material, method and technology of preparing that the present invention discloses and proposes, those skilled in the art can be by using for reference this paper content, links such as appropriate change raw material and process route realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change or reconfigure method as herein described and technology path in not break away from content of the present invention, spirit and scope, realizes final film technique.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (5)
1. SmFeO
3Be the conductance acetone gas sensitive material of base, it is characterized in that the chemical composition general formula is (Sm
1-xLa
x) (Fe
1-yB
y) O
3Composite oxides, wherein B represents Cu, Ni, 0≤x≤0.5,0.05≤y≤0.2.
2. the SmFeO of claim 1
3Preparation method for the conductance acetone gas sensitive material of base is characterized in that step is as follows:
A) Sm (NO of configuration 0.5mol/L
3)
3Solution; Fe (the NO of configuration 0.5mol/L
3)
3Solution; The citric acid solution of configuration 1.0mol/L; Take by weighing respectively and contain wherein a kind of nitrate powder of La, Cu, Ni, place in the different separately containers, be dissolved in water, mix, form the solution of 0.5mol/L;
B) by (Sm
1-xLa
x) (Fe
1-yB
y) O
3The metering ratio of composite oxides makes SmFeO
3Based sols is pressed SmFeO again
3Base: the mol ratio of citric acid=1:1 is with SmFeO
3Base mixes with aqueous citric acid solution, forms the SmFeO of component design
3The basic chemical composition solution of base sensitive material.
C) with (Sm
1-xLa
x) (Fe
1-yB
y) O
3Composite oxides solution place heating environment, temperature is controlled at 40-60 ℃, adds ethylene glycol, and its mol ratio is ethylene glycol: citric acid=0.1:1, under agitation mix, the metallic ion formed polyester network of esterified reaction institute huge legendary turtle in citric acid-ethylene glycol complex compound is closed; Add weak aqua ammonia and be adjusted to pH=5, carry out concentration correction, continue stirring and obtain even, stable concentration, finish citric acid complex-polymerization colloidal sol overall process, form colloidal sol form SmFeO at the 0.2-0.4mol/L precursor sol by adding entry
3The base sensitive material.
3. the SmFeO of claim 2
3Be the application of the conductance acetone gas sensitive material of base, it is characterized in that using to form film-type directly-heated type sensor or slug type heater-type sensor.
4. application as claimed in claim 3 is characterized in that the preparation method of film-type directly-heated type sensor:
1) with SmFeO
3The base sensitive material film heats up with the speed of 3-5 ℃/min, at 600-800 ℃ of thermal treatment 60-120 minute, obtains SmFeO
3Base crystallinity film; The crystallinity film was immersed in rare platinum acid chloride solution 20 minutes, dry back obtains SmFeO 500 ℃ of thermal treatments 30 minutes again
3The based sensor film.
5. application as claimed in claim 3 is characterized in that the preparation method of slug type heater-type sensor:
(1) with the SmFeO for preparing
3It is fully dry earlier that the colloidal sol 0.4mol/L of base sensitive material puts into container, forms xerogel; Put into the speed intensification of sintering furnace again, be prepared into SmFeO at 700-850 ℃ of sintering 60-120 minute with 3-5 ℃/min
3Base crystallinity powder;
(2) put into mortar with absolute ethyl alcohol as the medium wet-milling, after oven dry is sieved powder is added inorganic and organic hybrid adhesive furnishing slurry, slurry is coated on the alumina ceramic tube that has gold electrode equably, cover whole electrodes, the thickness that select to need, drying be placed in the sintering furnace 500-700 ℃ sintering 1-3 hour, again sintered body was immersed in rare platinum acid chloride solution 20 minutes, dry back obtains SmFeO 500 ℃ of thermal treatments 30 minutes
3The based sensor sintered material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910068068A CN101532976A (en) | 2009-03-06 | 2009-03-06 | SmFeO3-based conductance acetone gas sensitive material, preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910068068A CN101532976A (en) | 2009-03-06 | 2009-03-06 | SmFeO3-based conductance acetone gas sensitive material, preparation method and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101532976A true CN101532976A (en) | 2009-09-16 |
Family
ID=41103706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910068068A Pending CN101532976A (en) | 2009-03-06 | 2009-03-06 | SmFeO3-based conductance acetone gas sensitive material, preparation method and application thereof |
Country Status (1)
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|---|---|
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Cited By (3)
| 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 |
| CN109490386A (en) * | 2019-01-10 | 2019-03-19 | 福州大学 | It is a kind of using brownmillerite structure oxide as the current mode NH of sensitive electrode material3Sensor |
| CN111579616A (en) * | 2020-05-29 | 2020-08-25 | 吉林大学 | Based on YSZ and Fe2TiO5-TiO2Acetone sensor of sensitive electrode, preparation method and application thereof |
-
2009
- 2009-03-06 CN CN200910068068A patent/CN101532976A/en active Pending
Cited By (5)
| 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 |
| CN101852754B (en) * | 2010-05-14 | 2013-06-19 | 云南大学 | Lanthanum-ferrite-doping formaldehyde gas sensitive material and preparation method thereof |
| CN109490386A (en) * | 2019-01-10 | 2019-03-19 | 福州大学 | It is a kind of using brownmillerite structure oxide as the current mode NH of sensitive electrode material3Sensor |
| CN111579616A (en) * | 2020-05-29 | 2020-08-25 | 吉林大学 | Based on YSZ and Fe2TiO5-TiO2Acetone sensor of sensitive electrode, preparation method and application thereof |
| CN111579616B (en) * | 2020-05-29 | 2022-11-08 | 吉林大学 | Based on YSZ and Fe 2 TiO 5 -TiO 2 Acetone sensor of sensitive electrode, preparation method and application thereof |
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Application publication date: 20090916 |