CN108722447A - A kind of high activity β-Bi2O3The preparation method of/Bi/BiOCl tri compound catalysis materials - Google Patents
A kind of high activity β-Bi2O3The preparation method of/Bi/BiOCl tri compound catalysis materials Download PDFInfo
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- CN108722447A CN108722447A CN201810645113.5A CN201810645113A CN108722447A CN 108722447 A CN108722447 A CN 108722447A CN 201810645113 A CN201810645113 A CN 201810645113A CN 108722447 A CN108722447 A CN 108722447A
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 17
- 150000001875 compounds Chemical class 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 7
- 230000000694 effects Effects 0.000 title claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 12
- 238000002604 ultrasonography Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 12
- 239000012467 final product Substances 0.000 claims description 6
- RLXDCJUIXHSXQD-UHFFFAOYSA-N oxalic acid;hydrate Chemical class O.OC(=O)C(O)=O.OC(=O)C(O)=O RLXDCJUIXHSXQD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 3
- 239000011218 binary composite Substances 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract description 20
- 239000002243 precursor Substances 0.000 abstract description 15
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical class O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 16
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 8
- 229910052797 bismuth Inorganic materials 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 description 2
- 229940073609 bismuth oxychloride Drugs 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 229910006362 δ-Bi2O3 Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
Abstract
The invention discloses a kind of high activity β-Bi2O3The preparation method of/Bi/BiOCl tri compound catalysis materials.Technical scheme of the present invention main points are：Five water bismuth nitrates are dissolved in dilute nitric acid solution and obtain solution A, in being stirred on magnetic stirring apparatus, it is all dissolved to it, two oxalic acid hydrates are dissolved in deionized water and obtain solution B, it is all dissolved to it in stirring on magnetic stirring apparatus, solution B is added in the solution A stirred, 30 min ultrasounds, 30 min are stirred to be precipitated, it rinses repeatedly to solution and takes out precipitation after being in neutrality, it is dried to obtain precursor powder 1, different time is kept the temperature at 270 DEG C obtains precursor powder, precursor powder is dissolved in absolute ethyl alcohol, 50ul hydrochloric acid is added in whipping process, continue to stir, it is precipitated after ultrasound, precipitation is taken out after being rinsed repeatedly with absolute ethyl alcohol to neutrality, it is dried to obtain precursor powder, the composite photocatalyst material of different content is obtained after keeping the temperature 50 min at 80 DEG C.Preparation process simple possible of the present invention, synthesis cycle are relatively short.
Description
Technical field
The invention belongs to the synthesis technical fields of photoelectric material, and in particular to a kind of high activity β-Bi2O3/ Bi/BiOCl tri-
The preparation method of first composite photocatalyst material.
Background technology
China's bismuth is resourceful, and in recent years, for annual output up to more than 6000 tons, application is very extensive.Bismuth oxide is as bismuth source
A kind of product after deep processing is a kind of advanced functional material, is that one kind being rich in attractive semi-conducting material, is had more
Kind crystal form, such as：α-, β-, γ-, ω-and δ-Bi2O3.It has good electron conductivity and macroscopic property.It is widely used
In many fields, such as microelectronics, sensor technology, optical material, ultracapacitor etc., more and more people begin to focus on oxygen
Change bismuth material.It is reported that can be obtained after bismuth oxide and bismuth metal are compound excellent photoelectric properties [Weng S, Chen B,
Xie L, et al. J. of Mater. Chem. A, 2013, 1: 3068-3075].The present invention relates to a kind of high activities
β-Bi2O3The simple preparation method of/Bi/BiOCl tri compound catalysis materials.
Invention content
The technical problem to be solved by the present invention is to provide the β-that a kind of growth in situ, efficient, photocatalytic activity significantly improve
Bi2O3The preparation method of/Bi/BiOCl tri compound catalysis materials.
The present invention adopts the following technical scheme that, it is characterised in that the specific steps are：
4~6g, five water bismuth nitrates are dissolved in the dilute nitric acid solution of a concentration of 1mol/L~3mol/L, are stirred on magnetic stirring apparatus
It mixes to it and all dissolves, obtain solution A；2~4g, bis- oxalic acid hydrates are dissolved in 50~100ml deionized waters, in magnetic stirring apparatus
Upper stirring is all dissolved to it, is obtained solution B, then solution B is added dropwise in the solution A stirred, and stirring 20~
50min, 20~50 min of ultrasound, is precipitated, is rinsed repeatedly to solution after being in neutrality, and is taken out precipitation, is dried to obtain presoma
Powder（White）, by being layered in surface plate for presoma uniform ground, further it is sintered, obtains binary composite, it will be compound
Material is dissolved in absolute ethyl alcohol, is stirred on magnetic stirring apparatus, and 20~100ul hydrochloric acid is added in whipping process, stirs 3 h, ultrasound 1
H is precipitated, and is rinsed repeatedly to solution after being in neutrality, and is taken out precipitation, is dried to obtain final product trielement composite material.
First time drying condition is 60~100 DEG C of dry 4 h, and sintering condition is 260-280 DEG C of 60~100min of sintering, the
Redrying condition is 60~100 DEG C of dry 50 min.
Preparation process simple possible of the present invention, synthesis cycle is shorter, target product β-Bi obtained2O3/ Bi/BiOCl ternarys
Composite photocatalyst material has potential application in field of photovoltaic materials.
Description of the drawings
Fig. 1 is powder-product β-Bi obtained2O3/Bi/BiOCl、β-Bi2O3/BiOCl、β-Bi2O3Xrd figure.
Powder-product β-Bi made from Fig. 22O3The abosrption spectrogram of/Bi/BiOCl visible light photocatalytic degradation rhodamine B solutions
And versus time curve.
Fig. 3 is the rhodamine B degradation concentration versus time curve figure of 3 examples.
Fig. 4 is powder-product β-Bi obtained2O3The scanning electron microscope (SEM) photograph of/Bi/BiOCl,
Fig. 5 is the partial enlarged view of Fig. 4.
Fig. 6 is powder-product β-Bi obtained2O3The UV-vis absorption spectrum of/Bi/BiOCl.
Specific implementation mode
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on the above of the present invention belong to this hair
Bright range.
Embodiment 1
1) dilute nitric acid solution of the 1.6mol/L of configuration 100ml.
2) it weighs five water bismuth nitrates of 4.00g to be added in above-mentioned solution, in stirring with the rate of 400r/min on magnetic stirring apparatus
It mixes, until it is all dissolved, obtains solution A.
3) bis- oxalic acid hydrates of 2.8g are weighed to be dissolved in 50ml deionized waters, on magnetic stirring apparatus with the rate of 400r/min
Stirring obtains solution B until it is all dissolved.
4) solution B is slow（Dropwise）It is added in the solution A stirred, forms white precipitate, rotating speed is kept to continue to stir
30 min are mixed, then 30 min of ultrasound.
5) beaker is taken out, a moment is stood, surveys supernatant liquor pH (about 2).
6) it rinses to solution and is in neutrality repeatedly.
7) precipitation in step 6) is moved on surface plate, 90 DEG C of 4 h of drying obtain white precursor powder.
8) precursor powder is layered on surface plate, drying box temperature is allowed to rise to 270 DEG C, be put into drug, keep the temperature 90 min,
Obtain precursor powder.
9) precursor powder is placed in 25ml absolute ethyl alcohols, in being stirred with the rate of 400r/min on magnetic stirring apparatus, stirred
20ul hydrochloric acid is added during mixing, keeps rotating speed to continue to stir 3 h, then 1 h of ultrasound.
10) beaker is taken out, a moment is stood.
11) it is rinsed to solution and is in neutrality repeatedly with absolute ethyl alcohol.
12) precipitation in step 11) is moved on surface plate, 80 DEG C of 50 min of drying obtain final product, are product β-
Bi2O3/Bi/BiOCl。
Embodiment 2
1) dilute nitric acid solution of the 1.6mol/L of configuration 100ml.
2) it weighs five water bismuth nitrates of 5.25g to be added in above-mentioned solution, in stirring with the rate of 400r/min on magnetic stirring apparatus
It mixes, until it is all dissolved, obtains solution A.
3) bis- oxalic acid hydrates of 3.6g are weighed to be dissolved in 80ml deionized waters, on magnetic stirring apparatus with the rate of 400r/min
Stirring obtains solution B until it is all dissolved.
4) solution B is slow（Dropwise）It is added in the solution A stirred, forms white precipitate, rotating speed is kept to continue to stir
20 min are mixed, then 50 min of ultrasound.
5) beaker is taken out, a moment is stood, surveys supernatant liquor pH (about 2).
6) it rinses to solution and is in neutrality repeatedly.
7) by step 6）Precipitation moves on surface plate, and 60 DEG C of 4 h of drying obtain white precursor powder.
8) precursor powder is layered on surface plate, drying box temperature is allowed to rise to 280 DEG C, be put into drug, heat preservation 100
Min obtains precursor powder.
9) precursor powder is placed in 25ml absolute ethyl alcohols, in being stirred with the rate of 400r/min on magnetic stirring apparatus, stirred
50ul hydrochloric acid is added during mixing, keeps rotating speed to continue to stir 3 h, then 1 h of ultrasound.
10) beaker, static a moment are taken out.
11) it is rinsed to solution and is in neutrality repeatedly with absolute ethyl alcohol.
12) precipitation in step 11) is moved on surface plate, 60 DEG C of 50 min of drying obtain final product, in following the description
In become product β-Bi2O3。
Embodiment 3
1) dilute nitric acid solution of the 1.6mol/L of configuration 100ml.
2) it weighs five water bismuth nitrates of 6.00g to be added in above-mentioned solution, in stirring with the rate of 400r/min on magnetic stirring apparatus
It mixes, until it is all dissolved, obtains solution A.
3) bis- oxalic acid hydrates of 4.00g are weighed to be dissolved in 100ml deionized waters, on magnetic stirring apparatus with the speed of 400r/min
Rate stirs, until it is all dissolved, obtains solution B.
4) solution B is slow（Dropwise）It is added in the solution A stirred, forms white precipitate, rotating speed is kept to continue to stir
50 min are mixed, then 30 min of ultrasound.
5) beaker is taken out, a moment is stood, surveys supernatant liquor pH (about 2).
6) it rinses to solution and is in neutrality repeatedly.
7) by step 6）Precipitation moves on surface plate, and 90 DEG C of 4 h of drying obtain white precursor powder.
8) precursor powder is layered on surface plate, drying box temperature is allowed to rise to 260 DEG C, be put into drug, heat preservation 80
Min obtains final product, becomes product β-Bi in the following2O3。
9) precursor powder is placed in 25ml absolute ethyl alcohols, in being stirred with the rate of 400r/min on magnetic stirring apparatus, stirred
100ul hydrochloric acid is added during mixing, keeps rotating speed to continue to stir 3 h, then 1 h of ultrasound.
10) beaker, static a moment are taken out.
11) it is rinsed to solution and is in neutrality repeatedly with absolute ethyl alcohol.
Precipitation in step 11) is moved on surface plate, 60 DEG C of 50 min of drying obtain final product, in the following
As product β-Bi2O3/BiOCl。
X-ray diffraction test is carried out to the product obtained in above-mentioned 3 examples respectively（Such as Fig. 1）, product is obtained in example 1
X-ray diffraction peak include pure beta-oxidation bismuth（JCPDS 78-1793）, the corresponding diffraction maximum of bismuth metal（JCPDS 85-1329）With
The corresponding diffraction maximum of bismuth oxychloride（JCPDS 73-2060）, therefore 1 product form ingredient of example is β-Bi2O3/Bi/BiOCl.Together
The analysis method of sample shows that the constituent of product in example 2 is β-Bi2O3/ BiOCl, the constituent of product is β-in example 3
Bi2O3, Fig. 2 is β-Bi2O3The abosrption spectrogram of/Bi/BiOCl visible light photocatalytic degradation rhodamine B solutions；Fig. 3 is 3 examples
Sample degradation rhodamine B concentration versus time curve, wherein β-Bi2O3/ Bi/BiOCl sample efficiencies highests, in 30 min
Inside degrade 99.5%.To product β-Bi2O3/ Bi/BiOCl is scanned Electronic Speculum test, and Fig. 4 is β-Bi2O3/ Bi/BiOCl's sweeps
Electron microscope is retouched, Fig. 5 is that the partial enlarged view of Fig. 4 is dispersed with irregular little particle and flaky crystalline grain, β-on bulk morphologies surface
Bi2O3For bulk morphologies, bismuth metal is irregular particle, and BiOCl is flaky crystalline grain；β-Bi2O3The ultraviolet-visible of/Bi/BiOCl
Light photometer tests absorption spectrum（Such as Fig. 6）Show β-Bi2O3, bismuth metal, after bismuth oxychloride is compound, in 400-550nm light wave models
There is absorption to visible light in enclosing.
Embodiment above describes the basic principles and main features of the present invention, It should be understood by those skilled in the art that this
Invention is not restricted to the described embodiments, and the above embodiments and description only illustrate the principle of the present invention, not
It is detached under the range of the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements each fall within the present invention
In the range of protection.
Claims (2)
1. a kind of β-Bi of high activity2O3The preparation method of/Bi/BiOCl tri compound catalysis materials, it is characterised in that specific
Step is：
（1）4~6g, five water bismuth nitrates are dissolved in the dilute nitric acid solution of a concentration of 1mol/L~3mol/L, on magnetic stirring apparatus
Stirring is all dissolved to it, obtains solution A；2~4g, bis- oxalic acid hydrates are dissolved in 50~100ml deionized waters, in magnetic agitation
Stirring is all dissolved to it on device, is obtained solution B, then solution B is added dropwise in the solution A stirred, and stirring 20~
50min, 20~50 min of ultrasound, is precipitated, is rinsed repeatedly to solution after being in neutrality, and is taken out precipitation, is dried to obtain presoma
Powder（White）, by being layered in surface plate for presoma uniform ground, further it is sintered, obtains binary composite, it will be compound
Material is dissolved in absolute ethyl alcohol, is stirred on magnetic stirring apparatus, and 20~100ul hydrochloric acid is added in whipping process, stirs 3 h, ultrasound 1
H is precipitated, and is rinsed repeatedly to solution after being in neutrality, and is taken out precipitation, is dried to obtain final product trielement composite material.
2. a kind of β-Bi of high activity as described in claim 12O3The preparation side of/Bi/BiOCl tri compound catalysis materials
Method, it is characterised in that：First time drying condition be 60~100 DEG C of dry 4 h, sintering condition be 260-280 DEG C be sintered 60~
100min；Second of drying condition is 60~100 DEG C of dry 50 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107115857A (en) * | 2017-04-18 | 2017-09-01 | 西安交通大学 | A kind of CQDs/ β Bi2O3Composite visible light catalyst and preparation method thereof |
| CN107233902A (en) * | 2017-07-11 | 2017-10-10 | 河南师范大学 | A kind of hollow flower ball-shaped β Bi2O3/ BiOBr heterojunction photocatalysis materials and its preparation method and application |
| CN108031479A (en) * | 2017-10-30 | 2018-05-15 | 哈尔滨理工大学 | A kind of preparation method of beta bismuth oxide-bismoclite |
-
2018
- 2018-06-21 CN CN201810645113.5A patent/CN108722447A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107115857A (en) * | 2017-04-18 | 2017-09-01 | 西安交通大学 | A kind of CQDs/ β Bi2O3Composite visible light catalyst and preparation method thereof |
| CN107233902A (en) * | 2017-07-11 | 2017-10-10 | 河南师范大学 | A kind of hollow flower ball-shaped β Bi2O3/ BiOBr heterojunction photocatalysis materials and its preparation method and application |
| CN108031479A (en) * | 2017-10-30 | 2018-05-15 | 哈尔滨理工大学 | A kind of preparation method of beta bismuth oxide-bismoclite |
Non-Patent Citations (1)
| Title |
|---|
| O. MONNEREAU ET.AL: "Synthesis of Bi2O3 by controlled transformation rate thermal analysis: a new route for this oxide", 《SOLID STATE IONICS》 * |
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