CN110483036A - A kind of B omission Fe strontium titanate doping and preparation method thereof - Google Patents
A kind of B omission Fe strontium titanate doping and preparation method thereof Download PDFInfo
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- CN110483036A CN110483036A CN201910783165.3A CN201910783165A CN110483036A CN 110483036 A CN110483036 A CN 110483036A CN 201910783165 A CN201910783165 A CN 201910783165A CN 110483036 A CN110483036 A CN 110483036A
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- omission
- strontium titanate
- titanate doping
- precursor powder
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- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000003980 solgel method Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 55
- 239000000463 material Substances 0.000 abstract description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 abstract description 10
- 229910002370 SrTiO3 Inorganic materials 0.000 abstract description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 5
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000001035 drying Methods 0.000 abstract description 5
- 238000000227 grinding Methods 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 5
- 238000003760 magnetic stirring Methods 0.000 abstract description 5
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 abstract description 5
- 229910052719 titanium Inorganic materials 0.000 abstract description 5
- 239000011240 wet gel Substances 0.000 abstract description 5
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 16
- 229910052697 platinum Inorganic materials 0.000 description 8
- 239000011195 cermet Substances 0.000 description 5
- 239000000446 fuel Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910052712 strontium Inorganic materials 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910002367 SrTiO Inorganic materials 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- KJNGJIPPQOFCSK-UHFFFAOYSA-N [H][Sr][H] Chemical compound [H][Sr][H] KJNGJIPPQOFCSK-UHFFFAOYSA-N 0.000 description 1
- -1 at low cost Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/465—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates
- C04B35/47—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on strontium titanates
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Abstract
The present invention relates to a kind of B omission Fe strontium titanate dopings and preparation method thereof, belong to technical field of function materials.The B omission Fe strontium titanate doping, molecular formula are Sr (Ti0.6Fe0.4)1‑x O3‑δ, B omissions, which are measured, isx, A/B > 1, wherein A is Sr mole, and B is the integral molar quantity of Ti and Fe.Precursor powder is synthesized using sol-gel method: using strontium acetate, iron oxide and butyl titanate as raw material according to molecular formula molar ratio, being dissolved in isopropanol and dehydrated alcohol, 40min is sufficiently stirred on magnetic stirring apparatus, forms colloidal sol；12h is stood, layering forms wet gel；It is put into drying box and is dried in 60 DEG C, form it into fluffy xerogel, then grinding obtains precursor powder；By obtained precursor powder in 1100 DEG C of calcining 10h, B omission Fe strontium titanate doping powder are obtained.The purpose of the present invention is by pure SrTiO3It is doped to improve the electric conductivity of material and catalytic activity.
Description
Technical field
The present invention relates to a kind of B omission Fe strontium titanate dopings and preparation method thereof, belong to technical field of function materials.
Background technique
Solid oxide fuel cell (SOFC) is a kind of energy conversion device for directly converting chemical energy to electric energy.Make
For complete ceramic electricity generation system solid oxide fuel cell (SOFC) since it is in transfer efficiency, fuel tolerance and environment are dirty
Dye aspect has the advantages that more and receives significant attention than conventional power generation systems.Ni/YSZ cermet is common tradition
SOFC anode material has excellent combustion catalytic activity, good ionic conductivity and electronic conductivity.But it is hydrocarbon when using
For compound as fuel, Ni/YSZ cermet is low to the patience of sulphur and carbon.The oxidation of Ni will lead to Ni/YSZ cermet
Thermal cycle is unstable when redox.Due to the presence of these problems, the SOFC of Ni/YSZ cermet anode will be hindered
Commercialized development.Therefore, it is necessary to find one kind more suitable material as SOFC anode material.
Perovskite (ABO3) there is metal composite oxide good electric conductivity, oxygen diffusivity, oxygen permeability and Surface Oxygen to hand over
The features such as transsexual, while there is Mixed electronic- ionic conduction.Strontium titanates (SrTiO with perovskite structure3) show to tie
The advantages that structure is superior, chemical stability is good and doping ability is stronger also has stronger anti-product compared with Ni/YSZ cermet
Carbon and resistance to SO_2.Therefore, SrTiO3It is most potential one of the candidate material of SOFC anode.But pure SrTiO3Conduction
Property and catalytic activity are poor.
In order to improve SrTiO3Electric conductivity and catalytic activity, can by aliovalent transition metal element introduce SrTiO3Ti
Position.Such as Fe.Fe3+Ionic radius be 0.064nm, with Ti4+Ionic radius (0.068nm) it is close, introduce Fe element and B
Position is vacant, Lai Gaishan SrTiO3The electric conductivity of material.J. S. Yoon, M. Y. Yoon, C. Kwak C et al.
Y0.08Sr0.92Fe x Ti1-x O3-δ perovskite for solid oxide fuel cell anodes, Materials
Science & Engineering B, 2012,177 (2): the optimum doping proportion that 151-156 reports Fe is 0.4.F.
Gao, H. Zhao, X. Li, Y. Cheng, X. Zhou and F. Cui, Preparation and electrical
properties of yttrium-doped strontium titanate with B-site deficiency, J.
Power Sources, 2008,185 (1): 26-31 reports B vacant influences.But the prior art still has
The problems such as electric conductivity and poor catalytic activity, and any element is not adulterated on B.It is lacked so the technology introduces B
Position Fe strontium titanate doping, by increasing the concentration of Lacking oxygen, the electric conductivity of Lai Gaishan material.
Summary of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provide a kind of B omission Fe strontium titanate doping and
Preparation method.The purpose of the present invention is by pure SrTiO3It is doped to improve the electric conductivity of material and catalysis and live
Property.The invention is realized by the following technical scheme.
A kind of B omission Fe strontium titanate doping, molecular formula are Sr (Ti0.6Fe0.4)1-x O3-δ, B omissions, which are measured, isx, A/B >
1, wherein A is Sr, and B is Ti and Fe.
Described B vacant amountxIt is 0.04,0.05 or 0.07.
A kind of preparation method of B omission Fe strontium titanate doping, step include:
Step 1 synthesizes precursor powder using sol-gel method:
Using strontium acetate, iron oxide and butyl titanate as raw material according to molecular formula molar ratio, it is dissolved in isopropanol and anhydrous second
In alcohol, 40min is sufficiently stirred on magnetic stirring apparatus, forms colloidal sol；12h is stood, layering forms wet gel；It is put into drying box
It is dried in 60 DEG C, forms it into fluffy xerogel, then grinding obtains precursor powder；
Step 2, the precursor powder for obtaining step 1 obtain B omission Fe strontium titanate doping powder in 1100 DEG C of calcining 10h.
The position the B omission Fe strontium titanate doping powder that the step 2 obtains is pressed into disk, burns at 1350 DEG C in Muffle furnace
5h is tied, ceramics sample is formed.
The two sides of above-mentioned ceramics sample apply platinum slurry, and fix platinum filament, burn 1h at 1100 DEG C, electrode is prepared；Electricity
Pole is by (AC) AC impedence method, and in the frequency range 1MHz-0.01Hz of AC impedance, AC amplitude is under 5mV air conditions
Measure total conductivity.
The beneficial effects of the present invention are:
(1) present invention prepares Sr (Ti using sol-gel method0.6Fe0.4)1-x O3-δComposite granule, at low cost, particle diameter distribution is equal
It is even.
(2) Fe adulterates SrTiO in the present invention3X-ray diffraction analysis find that no impurity occurs, show not change calcium titanium
The single cubic phase structure of mine.
(3) present invention is to perovskite-type material (SrTiO3) the position B be doped, and introduce B omission, increase Lacking oxygens
The ionic conductivity of material is significantly increased in concentration, so as to improve the electric conductivity of material.
Detailed description of the invention
Fig. 1 is the Sr (Ti that example 1 is prepared in the present invention0.6Fe0.4)0.96O3-δCeramics sample XRD diagram；
Fig. 2 is the Sr (Ti of example 1 in the present invention0.6Fe0.4)0.96O3-δCeramics sample SEM figure；
Fig. 3 is the Sr (Ti that the embodiment of the present invention 1 is prepared0.6Fe0.4)0.96O3-δCeramics sample, embodiment 2 are prepared
Sr(Ti0.6Fe0.4)0.95O3-δSr (the Ti that ceramics sample and embodiment 3 are prepared0.6Fe0.4)0.93O3-δCeramics sample conductance
Rate figure.
Specific embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
The B omission Fe strontium titanate doping, molecular formula are Sr (Ti0.6Fe0.4)1-x O3-δ, B omissions, which are measured, isx, A/B > 1, wherein A
It is Ti and Fe for Sr, B；B vacant amountsxIt is 0.04.
The preparation method of the B omission Fe strontium titanate doping, step include:
Step 1 synthesizes precursor powder using sol-gel method:
1.0286g strontium acetate is dissolved in the deionized water of 4mL, and 0.1533g iron oxide and 0.9801g butyl titanate dissolve
In 34mL isopropanol and 4mL dehydrated alcohol, 40min is sufficiently stirred on magnetic stirring apparatus, forms colloidal sol；Stand 12h, layering
Form wet gel；It is put into drying box and is dried in 60 DEG C, form it into fluffy xerogel, then grinding obtains precursor powder；
Step 2, the precursor powder for obtaining step 1 obtain B omission Fe strontium titanate doping powder in 1100 DEG C of calcining 10h
(Sr (Ti0.6Fe0.4)0.96O3-δComposite granule).
The position the B omission Fe strontium titanate doping powder that the step 2 obtains is pressed into disk (diameter 8mm × thickness 2mm), In
5h is sintered in Muffle furnace at 1350 DEG C, forms ceramics sample.
Sr (the Ti that the present embodiment is prepared0.6Fe0.4)0.96O3-δCeramics sample XRD diagram is as shown in Figure 1, can from Fig. 1
With find out B vacant amounts (x) when being 0.04, impurity phase do not occur in the XRD diagram of Fe strontium titanate doping ceramics sample, still keep
Single cubic phase perovskite structure.Sr(Ti0.6Fe0.4)0.96O3-δCeramics sample SEM schemes as shown in Fig. 2, as can be seen from Figure 2
B vacant amounts (x) be 0.04 when, the compactness of Fe strontium titanate doping ceramics sample is higher, illustrates B omission Fe strontium titanate dopings
With preferable catalytic activity.
The two sides of above-mentioned ceramics sample are applied into platinum slurry, and fix platinum filament, 1h is burnt at 1100 DEG C, electrode is prepared；
Electrode is by (AC) AC impedence method, and in the frequency range 1MHz-0.01Hz of AC impedance, AC amplitude is 5mV air conditions
Lower measurement total conductivity figure is as shown in Figure 3.As can be seen from Figure 3 B vacant amounts (x) be 0.04 when, Fe strontium titanate doping pottery
The total conductivity of porcelain sample increases with increasing temperature, and the conductivity at 800 DEG C reaches most preferably, is 0.08021S/cm.
Embodiment 2
The B omission Fe strontium titanate doping, molecular formula are Sr (Ti0.6Fe0.4)1-x O3-δ, B omissions, which are measured, isx, A/B > 1, wherein A
It is Ti and Fe for Sr, B；B vacant amountsxIt is 0.05.
The preparation method of the B omission Fe strontium titanate doping, step include:
Step 1 synthesizes precursor powder using sol-gel method:
1.0286g strontium acetate is dissolved in the deionized water of 4mL, and 0.1517g iron oxide and 0.9699g butyl titanate dissolve
In 34mL isopropanol and 4mL dehydrated alcohol, 40min is sufficiently stirred on magnetic stirring apparatus, forms colloidal sol；Stand 12h, layering
Form wet gel；It is put into drying box and is dried in 60 DEG C, form it into fluffy xerogel, then grinding obtains precursor powder；
Step 2, the precursor powder for obtaining step 1 obtain B omission Fe strontium titanate doping powder in 1100 DEG C of calcining 10h
(Sr (Ti0.6Fe0.4)0.95O3-δComposite granule).
The position the B omission Fe strontium titanate doping powder that the step 2 obtains is pressed into disk (diameter 8mm × thickness 2mm), In
5h is sintered in Muffle furnace at 1350 DEG C, forms ceramics sample.
The two sides of above-mentioned ceramics sample are applied into platinum slurry, and fix platinum filament, 1h is burnt at 1100 DEG C, electrode is prepared；
Electrode is by (AC) AC impedence method, and in the frequency range 1MHz-0.01Hz of AC impedance, AC amplitude is 5mV air conditions
Lower measurement total conductivity figure is as shown in Figure 3.As can be seen from Figure 3 B vacant amounts (x) be 0.05 when, Fe strontium titanate doping pottery
The total conductivity of porcelain sample increases with increasing temperature, and the conductivity at 800 DEG C reaches most preferably, is 0.237S/cm.
Embodiment 3
The B omission Fe strontium titanate doping, molecular formula are Sr (Ti0.6Fe0.4)1-x O3-δ, B omissions, which are measured, isx, A/B > 1, wherein A
It is Ti and Fe for Sr, B；B vacant amountsxIt is 0.07.
The preparation method of the B omission Fe strontium titanate doping, step include:
Step 1 synthesizes precursor powder using sol-gel method:
1.0286g strontium acetate is dissolved in the deionized water of 4mL, and 0.1485g iron oxide and 0.9495g butyl titanate dissolve
In 34mL isopropanol and 4mL dehydrated alcohol, 40min is sufficiently stirred on magnetic stirring apparatus, forms colloidal sol；Stand 12h, layering
Form wet gel；It is put into drying box and is dried in 60 DEG C, form it into fluffy xerogel, then grinding obtains precursor powder；
Step 2, the precursor powder for obtaining step 1 obtain B omission Fe strontium titanate doping powder in 1100 DEG C of calcining 10h
(Sr (Ti0.6Fe0.4)0.93O3-δComposite granule).
The position the B omission Fe strontium titanate doping powder that the step 2 obtains is pressed into disk (diameter 8mm × thickness 2mm), In
5h is sintered in Muffle furnace at 1350 DEG C, forms ceramics sample.
The two sides of above-mentioned ceramics sample are applied into platinum slurry, and fix platinum filament, 1h is burnt at 1100 DEG C, electrode is prepared；
Electrode is by (AC) AC impedence method, and in the frequency range 1MHz-0.01Hz of AC impedance, AC amplitude is 5mV air conditions
Lower measurement total conductivity figure is as shown in Figure 3.As can be seen from Figure 3 B vacant amounts (x) be 0.05 when, Fe strontium titanate doping pottery
The total conductivity of porcelain sample increases with increasing temperature, and the conductivity at 800 DEG C reaches most preferably, is 0.3445S/cm.
In conjunction with attached drawing, the embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned
Embodiment within the knowledge of a person skilled in the art can also be before not departing from present inventive concept
Put that various changes can be made.
Claims (4)
1. a kind of B omission Fe strontium titanate doping, it is characterised in that: molecular formula is Sr (Ti0.6Fe0.4)1-x O3-δ, B vacant amounts
Forx。
2. B omission Fe strontium titanate doping according to claim 1, it is characterised in that: described B vacant amountxFor 0.04,
0.05 or 0.07.
3. a kind of preparation method of B according to claim 1 or 2 omissions Fe strontium titanate doping, it is characterised in that step
Include:
Step 1 synthesizes precursor powder using sol-gel method；
Step 2, the precursor powder for obtaining step 1 obtain B omission Fe strontium titanate doping powder in 1100 DEG C of calcining 10h.
4. the preparation method of B omission Fe strontium titanate doping according to claim 3, it is characterised in that: the step 2
To the position B omission Fe strontium titanate doping powder be pressed into disk, be sintered 5h at 1350 DEG C in Muffle furnace, form ceramics sample.
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| CN112569948A (en) * | 2020-12-29 | 2021-03-30 | 华中科技大学 | Perovskite nanoparticle catalyst and preparation method and application thereof |
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