CN106495217A - A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method - Google Patents

A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method Download PDF

Info

Publication number
CN106495217A
CN106495217A CN201610906097.1A CN201610906097A CN106495217A CN 106495217 A CN106495217 A CN 106495217A CN 201610906097 A CN201610906097 A CN 201610906097A CN 106495217 A CN106495217 A CN 106495217A
Authority
CN
China
Prior art keywords
microwave
nanocrystalline
hydrothermal
solution
feature exist
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610906097.1A
Other languages
Chinese (zh)
Inventor
曹丽云
罗艺佳
黄剑锋
周磊
吴建鹏
冯亮亮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shaanxi University of Science and Technology
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201610906097.1A priority Critical patent/CN106495217A/en
Publication of CN106495217A publication Critical patent/CN106495217A/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G29/00—Compounds of bismuth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Materials Engineering (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method, by Bi (NO3)3·5H2O solution and Zr (NO3)4·5H2O mixes, and adjusts pH value to 7～11, stirs, obtains precipitated liquid B；Precipitated liquid B is transferred in microwave hydrothermal tank, after 30～60min of microwave reaction at 200～220 DEG C, white precipitate C is obtained；White precipitate C is dried, powder body D is obtained；By powder body D at 300～750 DEG C 0.5～3h of heat treatment, obtain granular Bi2Zr2O7Nanocrystalline.The present invention gives predecessor energy using microwave hydrothermal process, can reduce the generation temperature of reactant.This method adopts simple microwave-hydrothermal method preparation technology, and reaction time is short, and synthesis temperature is low, obtained Bi2Zr2O7Nanocrystalline for graininess pattern, particle size is little, and good dispersion, photocatalysis performance are excellent.

Description

A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method
Technical field
The invention belongs to field of material preparation, and in particular to a kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline Method.
Background technology
Zirconic acid bismuth (Bi2Zr2O7) as a kind of metal composite oxide, in solid-state physics, materials chemistry and catalytic chemistry etc. Field has potential using value.At present, for the research of zirconic acid bismuth is scarcely out of swaddling-clothes.Isomorphous zirconates such as zirconium Sour samarium (Sm2Zr2O7), it is applied to corrosion and heat resistant field [L.Guo, et al.Comparison of hot corrosion resistance of Sm2Zr2O7and(Sm0.5Sc0.5)2Zr2O7ceramics in Na2SO4+V2O5molten salt[J] .Ceramics International (2016)].Zirconic acid yttrium (Y2Zr2O7), it is applied to photocatalysis field [Y.Tong et al.Preparation and characterization of Y2Zr2O7nanocrystals and their Photocatalytic properties [J] .Materials Science and Engineering B, 150 (2008)： 194 198.] and thermal barrier coating field [Julie M.Drexler, et al.Composition effects of thermal barrier coating ceramics on their interaction with molten Ca–Mg–Al– silicate(CMAS)glass[J].Acta Materialia,60(2012):5437–5447.].It is contemplated that, zirconic acid bismuth (Bi2Zr2O7) also necessarily there is huge researching value in these fields.
At present, it has been reported that zirconic acid bismuth preparation method for precipitation calcination method.Such as Deyong Wu etc. [D.Wu, T.He, J.Xia,Y.Tan.Preparation and photocatalytic properties of Bi2Zr2O7photocatalyst [J].Material Letters,156(2015):195-197.] and S.L.Sorokina etc. [S.L.Sorokina, A.W.Sleight.NEW PHASES IN THE ZrO2-Bi2O3AND HfO2-Bi2O3SYSTEMS[J].Materials Research Bulletin,1998,33(7):1077-1081.] Bi is successfully prepared using precipitation calcination method all2Zr2O7.So And, there is long preparation period in above method, power consumption is high, the uneven problem of product grain.
Content of the invention
It is an object of the invention to proposing a kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method, this side Method can prepare graininess Bi of uniform nano-scale at a lower temperature2Zr2O7Material；Reaction process equipment is simple, conjunction Low into temperature, synthesis cycle is short, and synthetic product size is little, is evenly distributed, with vast potential for future development.
For achieving the above object, the technical solution used in the present invention is as follows：
A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method, comprises the following steps：
1) by Bi (NO3)3·5H2O is dissolved in nitric acid, obtains Bi (NO3)3·5H2O solution, by Zr (NO3)4·5H2O is dissolved in In water, Zr (NO are obtained3)4·5H2O solution, by Bi (NO3)3·5H2O solution and Zr (NO3)4·5H2O mixes, and is configured to forerunner Liquid A；Wherein, Bi is 1 with Zr mol ratios:1；
2) pH value of precursor liquid A is adjusted to 7～11, constantly have white precipitate to produce, stir, obtain during regulation Obtain precipitated liquid B；
3) precipitated liquid B is transferred in microwave hydrothermal tank, after 30～60min of microwave reaction at 200～220 DEG C, is obtained White precipitate C；
4) white precipitate C is dried, obtains powder body D；
5) by powder body D at 300～750 DEG C 0.5～3h of heat treatment, obtain granular Bi2Zr2O7Nanocrystalline.
The present invention is further improved by, Bi (NO3)3·5H2O and Zr (NO3)4·5H2O is pure for analysis.
The present invention is further improved by, Bi (NO in solution A3)3·5H2The concentration of O is 0.05～0.5mol/L.
The present invention is further improved by, and the concentration of concentrated nitric acid is 2mol/L.
The present invention is further improved by, Bi (NO in solution A3)3·5H2The concentration of O is 0.05～0.5mol/L.
The present invention is further improved by, and adjusting pH value is carried out to 7～11 using strong aqua ammonia, the matter of the strong aqua ammonia Amount percentage concentration is 25%-28%.
The present invention is further improved by, and the time of stirring is 2h.
The present invention is further improved by, and the volume packing ratio of microwave hydrothermal tank is 30～50%.
The present invention is further improved by, and drying is carried out in vacuum drying oven, and dry temperature is 60 DEG C～80 DEG C, the dry time is 120～240min.
Compared with prior art, the device have the advantages that：
The invention provides the new method microwave hydrothermal that a kind of building-up process is simple, synthesis temperature is low, synthesis cycle is short Method prepares Bi2Zr2O7Nanocrystalline, microwave-hydrothermal method has the superior of uniqueness in preparation small particle, the uniform nanoparticle of form Property.Microwave-hydrothermal method of the present invention prepares Bi2Zr2O7Nanocrystalline advantage is：(1) can rapidly to reaction using microwave-hydrothermal method System is heated, and promotes reactant rapid crystallization, so as to reach the purpose of energy-conservation；(2) microwave is adopted at 200～220 DEG C Hydro-thermal method can carry out selectivity heating to each component in mixed material, can prepare superfines and be avoided that tradition The reunion that heating causes；(3) by reaction temperature and time during change microwave hydrothermal, different-grain diameter scope can be obtained and is existed The Bi of 17-35nm2Zr2O7Nanocrystalline；(4) predecessor energy is given using microwave hydrothermal process, can reduce the generation of reactant Temperature.This method adopts simple microwave-hydrothermal method preparation technology, and reaction time is short, and synthesis temperature is low, obtained Bi2Zr2O7Receive Meter Jing Wei graininess patterns, particle size are little, and good dispersion, photocatalysis performance are excellent.
Description of the drawings
Fig. 1 obtained Bi under conditions of embodiment 2 for the present invention2Zr2O7X-ray diffraction (XRD) figure of nano material Spectrum.
Fig. 2 is the prepared Bi under the conditions of embodiment 2 of the present invention2Zr2O7Scan under 50,000 enlargement ratios of nano material Electronic Speculum (SEM) photo.
Fig. 3 is the prepared Bi under the conditions of embodiment 2 of the present invention2Zr2O7Scan under 100,000 enlargement ratios of nano material Electronic Speculum (SEM) photo.
Fig. 4 is the prepared block Bi under the conditions of embodiment 2 of the present invention2Zr2O7Nanocrystalline 1000W xenon lamps irradiation under The photocatalysis performance figure of rhodamine B degradation.
Specific embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
Embodiment 1
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 0.05mol/L；Wherein, Bi with Zr mole Than for 1:1；
2) precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=10, adjusted Constantly there is white precipitate to produce during section, drop stirs 2h after finishing, and obtains precipitated liquid B.Wherein, ammonia (NH contained by the strong aqua ammonia3) Mass percentage concentration be 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 40% to control volume packing ratio, microwave reaction temperature is set and is 200 DEG C, the response time is 30min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 120min under conditions of 60 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 0.5h under the conditions of 550 DEG C, you can obtain granular Bi2Zr2O7Nanocrystalline.
Embodiment 2
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 0.1mol/L；Wherein, Bi with Zr mole Than for 1:1；
2) gained precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=10, During regulation, constantly there is white precipitate to produce, stir 2h, obtain precipitated liquid B.Wherein, ammonia (NH contained by the strong aqua ammonia3) Mass percentage concentration is 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 40% to control volume packing ratio, microwave reaction temperature is set and is 220 DEG C, the response time is 30min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 180min under conditions of 60 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 1h under the conditions of 450 DEG C, you can obtain granular Bi2Zr2O7 Nanocrystalline.
Occurred without impurity peaks by can be seen that in sample in XRD spectrum in Fig. 1, it was demonstrated that the product of pure phase is succeeded Prepare.From figures 2 and 3, it will be seen that preparing Bi using microwave-hydrothermal method2Zr2O7Particle size minimum is between 18～40nm.
From fig. 4, it can be seen that sample exist visible light-responded.After 1000W xenon lamps irradiation 240min, sample degradation concentration Rhodamine B efficiency for 10mg/L can reach 81%.
Embodiment 3
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 0.2mol/L；Wherein, Bi with Zr mole Than for 1:1；
2) gained precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=7, During regulation, constantly there is white precipitate to produce, stir 2h, obtain precipitated liquid B.Wherein, ammonia (NH contained by the strong aqua ammonia3) Mass percentage concentration is 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 40% to control volume packing ratio, microwave reaction temperature is set and is 220 DEG C, the response time is 60min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 240min under conditions of 60 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 2h under the conditions of 400 DEG C, you can obtain granular Bi2Zr2O7 Nanocrystalline.
Embodiment 4
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 0.5mol/L；Wherein, Bi with Zr mole Than for 1:1；
2) gained precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=7, During regulation, constantly there is white precipitate to produce, stir 2h, obtain precipitated liquid B.Wherein, ammonia (NH contained by the strong aqua ammonia3) Mass percentage concentration is 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 40% to control volume packing ratio, microwave reaction temperature is set and is 200 DEG C, the response time is 60min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 240min under conditions of 60 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 3h under the conditions of 350 DEG C, you can obtain granular Bi2Zr2O7 Nanocrystalline.
Embodiment 5
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 1mol/L；Wherein, Bi and Zr mol ratios For 1:1；
2) gained precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=7, During regulation, constantly there is white precipitate to produce, drop stirs 2h after finishing, and obtains precipitated liquid B.Wherein, ammonia contained by the strong aqua ammonia (NH3) mass percentage concentration be 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 40% to control volume packing ratio, microwave reaction temperature is set and is 220 DEG C, the response time is 60min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 180min under conditions of 80 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 0.5h under the conditions of 650 DEG C, you can obtain granular Bi2Zr2O7Nanocrystalline.
Embodiment 6
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 0.3mol/L；Wherein, Bi with Zr mole Than for 1:1；
2) gained precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=11, During regulation, constantly there is white precipitate to produce, drop stirs 2h after finishing, and obtains precipitated liquid B.Wherein, ammonia contained by the strong aqua ammonia (NH3) mass percentage concentration be 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 50% to control volume packing ratio, microwave reaction temperature is set and is 210 DEG C, the response time is 60min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 200min under conditions of 70 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 3h under the conditions of 300 DEG C, you can obtain granular Bi2Zr2O7 Nanocrystalline.
Embodiment 7
1) by analytically pure Bi (NO3)3·5H2O is dissolved in the nitric acid of 2mol/L, obtains Bi (NO3)3·5H2O solution； In beaker, by Zr (NO3)4·5H2O is soluble in water, obtains Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution with Zr(NO3)4·5H2O mixes, and is configured to Bi (NO3)3·5H2Precursor liquid A of the O concentration for 0.4mol/L；Wherein, Bi with Zr mole Than for 1:1；
2) gained precursor liquid A is placed on magnetic stirring apparatuss and is sufficiently mixed, then be slowly added dropwise strong aqua ammonia and adjust its pH=9, During regulation, constantly there is white precipitate to produce, drop stirs 2h after finishing, and obtains precipitated liquid B.Wherein, ammonia contained by the strong aqua ammonia (NH3) mass percentage concentration be 25%-28%.
3) precipitated liquid B is transferred in microwave hydrothermal tank, it is 30% to control volume packing ratio, microwave reaction temperature is set and is 205 DEG C, the response time is 40min, after reaction terminates, is cleaned multiple times using deionized water and dehydrated alcohol, white is collected by centrifugation Precipitate C.
4) the white precipitate C of gained is placed in vacuum drying oven, control temperature dries 150min under conditions of 75 DEG C, Obtain powder body D.
5) the powder body D of acquisition is placed in Muffle furnace, heat treatment 0.5h under the conditions of 750 DEG C, you can obtain granular Bi2Zr2O7Nanocrystalline.

Claims (9)

1. a kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method, it is characterised in that comprise the following steps：
1) by Bi (NO3)3·5H2O is dissolved in nitric acid, obtains Bi (NO3)3·5H2O solution, by Zr (NO3)4·5H2O is dissolved in water In, obtain Zr (NO3)4·5H2O solution, by Bi (NO3)3·5H2O solution and Zr (NO3)4·5H2O mixes, and is configured to precursor liquid A；Wherein, Bi is 1 with Zr mol ratios:1；
2) pH value of precursor liquid A is adjusted to 7～11, constantly have white precipitate to produce, stir, sunk during regulation Shallow lake liquid B；
3) precipitated liquid B is transferred in microwave hydrothermal tank, after 30～60min of microwave reaction at 200～220 DEG C, obtains white Precipitate C；
4) white precipitate C is dried, obtains powder body D；
5) by powder body D at 300～750 DEG C 0.5～3h of heat treatment, obtain granular Bi2Zr2O7Nanocrystalline.
2. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In Bi (NO3)3·5H2O and Zr (NO3)4·5H2O is pure for analysis.
3. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In Bi (NO in solution A3)3·5H2The concentration of O is 0.05～0.5mol/L.
4. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In the concentration of concentrated nitric acid is 2mol/L.
5. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In Bi (NO in solution A3)3·5H2The concentration of O is 0.05～0.5mol/L.
6. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In adjusting pH value is carried out to 7～11 using strong aqua ammonia, and the mass percentage concentration of the strong aqua ammonia is 25%-28%.
7. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In the time of stirring is 2h.
8. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In the volume packing ratio of microwave hydrothermal tank is 30～50%.
9. a kind of microwave-hydrothermal method according to claim 1 prepares graininess Bi2Zr2O7Nanocrystalline method, its feature exist In drying is carried out in vacuum drying oven, and dry temperature is 60 DEG C～80 DEG C, and the dry time is 120～240min.
CN201610906097.1A 2016-10-18 2016-10-18 A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method Pending CN106495217A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610906097.1A CN106495217A (en) 2016-10-18 2016-10-18 A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610906097.1A CN106495217A (en) 2016-10-18 2016-10-18 A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method

Publications (1)

Publication Number Publication Date
CN106495217A true CN106495217A (en) 2017-03-15

Family

ID=58293806

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610906097.1A Pending CN106495217A (en) 2016-10-18 2016-10-18 A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method

Country Status (1)

Country Link
CN (1) CN106495217A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104556213A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm2Sn2O7-SnO2 nano composite by microwave hydrothermal-water bath process
CN105905944A (en) * 2016-04-20 2016-08-31 陕西科技大学 Method of preparing Bi2Zr2O7 nano material through non-hydrolytic sol-gel method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104556213A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm2Sn2O7-SnO2 nano composite by microwave hydrothermal-water bath process
CN105905944A (en) * 2016-04-20 2016-08-31 陕西科技大学 Method of preparing Bi2Zr2O7 nano material through non-hydrolytic sol-gel method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
DEYONG WU等: "Preparation and photocatalytic properties of Bi2Zr2O7 photocatalyst", 《MATERIALS LETTERS》 *
庄建东等: "Bi2Sn2O7的不同水热法制备及其可见光光催化除As(III)性能分析", 《物理化学学报》 *
徐存英等: "纳米粉体材料的制备", 《云南民族学院学报》 *

Similar Documents

Publication Publication Date Title
CN101890354B (en) Method for preparing bismuth ferrite photocatalyst
CN107129304B (en) -step synthesis method of lanthanum molybdate based electrolyte material by microwave combustion-supporting methods
CN111908922A (en) Low-temperature synthesized rare earth hafnate high-entropy ceramic powder and preparation method thereof
CN101113010A (en) Method for preparing cerium oxide nano particle by auxiliary microwave
CN105170157A (en) Neodymium-doped bismuth ferrite nanometer photocatalyst and preparation method thereof
CN104973615A (en) Microwave burning preparation method of nano gadolinium oxide powder
CN103301832A (en) Preparation of tungsten trioxide photocatalyst in porous structure, and application of tungsten trioxide photocatalyst to sewage treatment
CN109942012A (en) A kind of nano-grade boehmite and preparation method thereof
CN107055597A (en) A kind of quick method for preparing cubic bismuth titanate sodium powder body under low temperature
CN102659154A (en) Method for preparing nano alpha-Al2O3 powder
CN102951686A (en) Preparation method for granular manganese tungstate nanocrystals
RU2404125C2 (en) Method of preparing zirconium dioxide nanopowder
CN106882842A (en) A kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials
Sun et al. Coordination mechanism, characterization, and photoluminescence properties of spinel ZnAl 2 O 4 nanoparticles prepared by a modified polyacrylamide gel route
CN106316386A (en) Preparation method of rare earth-doped bismuth system layered perovskite oxide ferroelectric up-conversion material
CN105923650B (en) One kind prepares nanometer Bi using precipitation calcination method2Zr2O7The method of powder
CN109384262B (en) Flaky Li4Mn5O12Ion sieve precursor and preparation method of ion sieve
CN109126769B (en) Method for preparing tungsten trioxide/zinc tungstate composite photocatalytic material by in-situ self-growth
CN106495217A (en) A kind of microwave-hydrothermal method prepares graininess Bi2Zr2O7Nanocrystalline method
CN107930636B (en) Preparation method and application of Ce-containing visible light catalytic nano material
CN102963925A (en) Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor
CN105692697A (en) Method for preparing nanometer Bi2Zr2O7 powder by sedimentation-calcination method assisted with molten salt method
CN104843792A (en) Method for preparing nano needle-shaped purple tungsten powder
CN101660204A (en) Preparation method of hexagonal piece aluminum oxide whisker material
CN105858707B (en) Preparing method for Sm2O3 nanocrystalline

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170315

RJ01 Rejection of invention patent application after publication