CN109437306A - A kind of metal molybdate micro nano structure raw powder's production technology - Google Patents
A kind of metal molybdate micro nano structure raw powder's production technology Download PDFInfo
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- CN109437306A CN109437306A CN201811552846.0A CN201811552846A CN109437306A CN 109437306 A CN109437306 A CN 109437306A CN 201811552846 A CN201811552846 A CN 201811552846A CN 109437306 A CN109437306 A CN 109437306A
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- salt
- molybdate
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- 239000000843 powder Substances 0.000 title claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 title claims abstract description 30
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 23
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 150000003839 salts Chemical class 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- QGAVSDVURUSLQK-UHFFFAOYSA-N ammonium heptamolybdate Chemical compound N.N.N.N.N.N.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Mo].[Mo].[Mo].[Mo].[Mo].[Mo].[Mo] QGAVSDVURUSLQK-UHFFFAOYSA-N 0.000 claims abstract description 20
- -1 amide compound Chemical class 0.000 claims abstract description 14
- 239000012046 mixed solvent Substances 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 8
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 14
- 229910052712 strontium Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000011572 manganese Chemical class 0.000 claims description 12
- 239000011575 calcium Substances 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 9
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical group [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 7
- 239000011701 zinc Chemical class 0.000 claims description 7
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 6
- PMDCZENCAXMSOU-UHFFFAOYSA-N N-ethylacetamide Chemical compound CCNC(C)=O PMDCZENCAXMSOU-UHFFFAOYSA-N 0.000 claims description 4
- OHLUUHNLEMFGTQ-UHFFFAOYSA-N N-methylacetamide Chemical compound CNC(C)=O OHLUUHNLEMFGTQ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001408 amides Chemical class 0.000 claims description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 claims description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical compound CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 claims description 2
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 2
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 2
- 229910001626 barium chloride Inorganic materials 0.000 claims description 2
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 claims description 2
- 239000001639 calcium acetate Substances 0.000 claims description 2
- 229960005147 calcium acetate Drugs 0.000 claims description 2
- 235000011092 calcium acetate Nutrition 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- AJFDBNQQDYLMJN-UHFFFAOYSA-N n,n-diethylacetamide Chemical compound CCN(CC)C(C)=O AJFDBNQQDYLMJN-UHFFFAOYSA-N 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 claims description 2
- 239000004246 zinc acetate Substances 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- UXGNZZKBCMGWAZ-UHFFFAOYSA-N dimethylformamide dmf Chemical compound CN(C)C=O.CN(C)C=O UXGNZZKBCMGWAZ-UHFFFAOYSA-N 0.000 claims 1
- IJRVLVIFMRWJRQ-UHFFFAOYSA-N nitric acid zinc Chemical compound [Zn].O[N+]([O-])=O IJRVLVIFMRWJRQ-UHFFFAOYSA-N 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 19
- 238000000034 method Methods 0.000 abstract description 13
- 239000004530 micro-emulsion Substances 0.000 abstract description 8
- 239000004094 surface-active agent Substances 0.000 abstract description 6
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 29
- BIOOACNPATUQFW-UHFFFAOYSA-N calcium;dioxido(dioxo)molybdenum Chemical compound [Ca+2].[O-][Mo]([O-])(=O)=O BIOOACNPATUQFW-UHFFFAOYSA-N 0.000 description 19
- 238000002604 ultrasonography Methods 0.000 description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- 229910052748 manganese Inorganic materials 0.000 description 10
- 238000001228 spectrum Methods 0.000 description 10
- 238000004140 cleaning Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 9
- 229910052791 calcium Inorganic materials 0.000 description 8
- 238000010586 diagram Methods 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 8
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical class O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 229910052788 barium Inorganic materials 0.000 description 6
- RCMWGBKVFBTLCW-UHFFFAOYSA-N barium(2+);dioxido(dioxo)molybdenum Chemical compound [Ba+2].[O-][Mo]([O-])(=O)=O RCMWGBKVFBTLCW-UHFFFAOYSA-N 0.000 description 6
- 229910052793 cadmium Inorganic materials 0.000 description 6
- 229940113088 dimethylacetamide Drugs 0.000 description 6
- 210000003743 erythrocyte Anatomy 0.000 description 6
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910052750 molybdenum Inorganic materials 0.000 description 4
- 239000011733 molybdenum Substances 0.000 description 4
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229910002412 SrMoO4 Inorganic materials 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000002057 nanoflower Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 230000005622 photoelectricity Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910004647 CaMoO4 Inorganic materials 0.000 description 1
- 235000011511 Diospyros Nutrition 0.000 description 1
- 244000236655 Diospyros kaki Species 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000004064 cosurfactant Substances 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
- ZXOKVTWPEIAYAB-UHFFFAOYSA-N dioxido(oxo)tungsten Chemical compound [O-][W]([O-])=O ZXOKVTWPEIAYAB-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229960000314 zinc acetate Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
-
- 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
- C01P2004/50—Agglomerated particles
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of metal molybdate micro nano structure raw powder's production technologies.Mixed solvent is obtained method includes the following steps: first mixing amide compound and water, soluble divalent metal salt is then dissolved in mixed solvent；Sodium molybdate is added under stiring again or ammonium heptamolybdate obtains precursors, finally precursors are transferred in reaction kettle and carry out hydro-thermal reaction, are precipitated；By washing of precipitate, drying, the metal molybdate micro nano structure powder of specific morphology structure, better crystallinity degree, purity is high can be prepared by.Molybdate micro nano structure raw powder's production technology proposed by the present invention; raw material is cheap and easy to get; preparation temperature is low (180 DEG C or less); synthesis device used is simple; and being not necessarily to surfactant is template or microemulsion environment to control pattern, structure; have many advantages, such as that preparation process is simple, it is low in cost, it is easy to accomplish large-scale production.
Description
Technical field
The present invention relates to a kind of metal molybdate micro nano structure raw powder's production technologies, belong to nano material preparation technology
Field.
Background technique
Metal molybdate is a kind of extremely important inorganic functional material, in photoelectricity, photocatalysis, energy stores, fluorescence
The fields such as (luminescence generated by light), microwave, optical fiber, scintillator material, moisture sensor have important application.Wherein XMoO4 (X =
Ca, Sr, Ba, Co, Mn, Zn, Cd etc.)) it the research of type molybdic acid salt material and is most widely used.It is well known that material
Performance depend on pattern, structure and the size etc. of material, therefore the metal molybdenum of specific structure, morphology and size is prepared
Hydrochlorate micro-nanometer structural material has highly important meaning in terms of fundamental research and the actual development of material
Justice.It prepares pattern and the special metal molybdate micro-nanometer structural material of structure and its performance is carried out studying to have become currently grinding
The hot spot studied carefully.For example, Lei etc. assists non-hydro-thermal method to synthesize the hierarchical structure with a thickness of 8 ~ 9nm using surfactant
SrMoO4Nanometer sheet, and (S.J. Lei, et al. is detected to its crystal structure, pattern and optical propertyMater. Res. Bull., 2011, 46: 601-608.).Yan Sun et al. synthesizes nanometer sheet using EDTA assisted microwave synthesis irradiation method
Assemble SrMoO4Nano flower, CaMoO4Nanometer persimmon and nano flower (Y. Sun, et al,Cryst. Res. Technol.,
2011, 46(9): 973-978.).Jiang Xiaohui et al. prepares CdMoO with reverse microemulsion process4Presoma obtain in turn it is micro-/receive
The CdMoO of metrical scale4Material, result of study show CdMoO4Wavelength can be obtained when excitation wavelength is 330 nm in nanocrystal
For the emission peak of 390nm；And CdMoO4Crystallite is when excitation wavelength is 320 nm, the emission peak (Jiang Xiao of available 390 nm
Brightness tungstates-molybdate nano material is synthetically prepared and the Shandong the research of luminescent properties [D]: Chinese Marine University,
2008.).Hu Bin etc. is prepared for that pattern is uniform, good dispersion in n-butanol/hexamethylene/water/SDS quaternary microemulsion system
ZnMoO4Nanometer rods (B. Hu, et al,CrystEngComm, 2011, 13(6):1755-1758.).Li et al. sun from
Sub- Surfactant CTAB is formed by the BaMoO for having synthesized that 30 microns of long diameters are 30 nm in Reverse Microemulsion System4Nanometer
Stick, and have studied response parameter for product influence (Z. Li, et al,Mater. Lett., 2005, 59(1):64-
68.).Yan etc. is using manganese acetate and sodium molybdate as raw material, and selecting hexamethylene is oily phase, and OP-10 is surfactant, and n-octyl alcohol is
Cosurfactant is successfully prepared for MnMoO using reverse microemulsion process at room temperature4Nanometer rods (M. Yan, et al,J. Phys.:conf. ser. 2009, 188(1):012056.).Vertical strong wait of wheat uses isooctane/n-butanol/CTAB/ water four
First microemulsion system be prepared for manganese molybdate monodimension nanometer material (L. Mai, et al,Mater. Today, 2011, 14:
346-353.).Such methods often are faced in soft template or microemulsion that surfactant removal etc. is a series of to be post-processed
Journey, the process is more complicated, it is difficult to a large amount of preparations and large-scale production.
Summary of the invention
It is an object of the invention to be directed to the preparation method of existing complexity, a kind of simple process is provided, is easily achieved industry
The metal molybdate micro nano structure raw powder's production technology that metaplasia produces.This method is easy to operate, low in cost, and universality is wide,
It is easy to be mass produced.Molybdate micro nano structure powder obtained by this method has specific morphology, biggish specific surface area,
Have in fields such as photoelectricity, photocatalysis, energy stores, fluorescence (luminescence generated by light), microwave, optical fiber, scintillator material, moisture sensors
Extraordinary application prospect.
The present invention provides a kind of metal molybdate micro nano structure raw powder's production technology, with sodium molybdate or seven molybdic acids
Ammonium and soluble divalent metal salt are as reaction raw materials, in the in the mixed solvent that amide compound and water are formed, 90 ~ 180
Metal molybdate micro nano structure powder is prepared in hydro-thermal reaction at a temperature of DEG C；Wherein: soluble divalent metal salt Ca
It is any in salt, Sr salt, Ba salt, Co salt, Mn salt, Zn salt or Cd salt；Amide compound be N- alkyl substituted amide or
Person's N, N- dialkyl group substituted amide.
In the present invention, in the mixed solvent, the volume ratio of amide compound and water is 6:1 ~ 1:6.
In the present invention, amide compound is selected from n,N-dimethylacetamide DMAc, N- methylacetamide MAc, N, N- diformazan
It is any in base formamide DMF, N, N- diethyl acetamide, N, N- diethylformamide or N- ethyl acetamide.
In the present invention, the molar ratio of sodium molybdate or ammonium heptamolybdate and soluble divalent metal salt is 1:1.
In the present invention, the hydro-thermal reaction time is 0.5 ~ 20 hour.
In the present invention, soluble divalent metal salt is selected from calcium chloride, strontium chloride, barium chloride, cobalt chloride, manganese chloride, chlorination
Cadmium, zinc chloride；Calcium nitrate, strontium nitrate, barium nitrate, cobalt nitrate, manganese nitrate, zinc nitrate, cadmium nitrate；Calcium acetate, strontium acetate, acetic acid
It is any in barium, cobalt acetate, manganese acetate, zinc acetate or cadmium acetate.
Specific step is as follows for preparation method of the invention:
1) amide compound is mixed with deionized water, is configured to mixed solvent；
2) soluble divalent metal salt is added to above-mentioned in the mixed solvent, is sufficiently stirred to form the first solution；Wherein, divalent gold
The concentration for belonging to salt is 0.02 ~ 0. 8 mol/l；
3) sodium molybdate or ammonium heptamolybdate are weighed, and is dissolved in the first solution formed by step 2, is sufficiently stirred that form second molten
Liquid；
4) the second solution is placed in hydro-thermal reaction in closed reaction vessel to be precipitated；
5) by obtained precipitating spend dehydrated alcohol, deionized water wash respectively for several times, it is dry, obtain specific morphology structure,
The metal molybdate micro nano structure powder of better crystallinity degree, purity is high.
Compared to the prior art, the present invention has the following advantages:
1, the metal molybdate (XMoO for the specific morphology structure that method provided by the invention is prepared4, X=Ca, Sr,
Ba, Co, Mn, Zn, Cd etc.) micro nano structure powder dispersity is good, and it is of uniform size；
2, the metal molybdate (XMoO for the specific morphology structure that method provided by the invention is prepared4, X=Ca, Sr,
Ba, Co, Mn, Zn, Cd etc.) micro nano structure powder regular crystal forms, better crystallinity degree, purity is high, free from admixture；
3, the cost of raw material needed for preparation method provided by the invention is cheap；
4, whole preparation process provided by the invention carries out under air conditions, is not necessarily to nitrogen protection；
5, whole preparation process provided by the invention without surfactant as being carried out under the conditions of template and non-micro emulsion, post-processing
Simply；
6, in preparation method provided by the invention, the metal molybdate (XMoO of specific morphology structure4, X=Ca, Sr, Ba,
Co, Mn, Zn, Cd etc.) micro nano structure powder hydro-thermal process under lower temperature (90~180 DEG C) can be obtained；
7, preparation method simple process provided by the invention, can largely prepare, and be suitable for large-scale production；
8, the metal molybdate (XMoO of the specific morphology structure obtained by the present invention4, X=Ca, Sr, Ba, Co, Mn,
Zn, Cd etc.) micro nano structure powder big specific surface area with higher, excellent optical property, be expected to be applied to optics device
The fields such as part, photocatalysis and energy stores.
Detailed description of the invention
The X ray diffracting spectrum of calcium molybdate powder prepared by Fig. 1 embodiment 1.
The stereoscan photograph of calcium molybdate powder prepared by Fig. 2 embodiment 1.
The X ray diffracting spectrum of strontium molybdate powder prepared by Fig. 3 embodiment 2.
The stereoscan photograph of strontium molybdate powder prepared by Fig. 4 embodiment 2.
The X ray diffracting spectrum of barium molybdate powder prepared by Fig. 5 embodiment 3.
The stereoscan photograph of barium molybdate powder prepared by Fig. 6 embodiment 3.
Specific embodiment
Embodiment and effect are further illustrated with following nonlimiting examples:
Embodiment 1
0.55g anhydrous calcium chloride is dissolved in 70mLN, the mixed solution of N- dimethyl acetamide (DMAc) and deionized water, and
The volume ratio of the two is 1:6, the ultrasound 30min in supersonic wave cleaning machine, weighs 6.18g ammonium heptamolybdate and is dissolved in the solution that ultrasound is crossed
In, it stirs at room temperature, until ammonium heptamolybdate is completely dissolved, obtains colorless and transparent precursor solution.By above-mentioned precursor solution
It pours into 100mL reaction kettle, reacts 30min at 180 DEG C, be cooled to room temperature to reaction kettle, obtained sample is spent respectively
Ionized water and dehydrated alcohol wash 3 times respectively, and then 80 DEG C of 8 ~ 10h of baking, can be obtained calcium molybdate powder.Fig. 1 is the present embodiment
Standard diagram (the JCPDS no 29- of the X ray diffracting spectrum of the calcium molybdate powder of preparation, all diffraction maximums and calcium molybdate
0351) it fits like a glove, does not find impurity peaks in spectrogram.Fig. 2 is its stereoscan photograph, and the calcium molybdate of preparation is by many red thin
The nanostructure of born of the same parents' shape is formed by self assembly, shows the pattern of Coiling-type and mean particle size is about 50 μm.
Embodiment 2
0.63g strontium nitrate is dissolved in 70mLN, the mixed solution of N- dimethyl acetamide (DMAc) and deionized water, and the two
Volume ratio be 1:4, the ultrasound 30min in supersonic wave cleaning machine, weigh 3.70g ammonium heptamolybdate be dissolved in ultrasound mistake solution in,
It stirs at room temperature, until ammonium heptamolybdate is completely dissolved, obtains colorless and transparent precursor solution.Above-mentioned precursor solution is poured into
In 100mL reaction kettle, 16h is reacted at 160 DEG C, is cooled to room temperature to reaction kettle, obtained sample is used into deionized water respectively
It is respectively washed with dehydrated alcohol time, then 80 DEG C of 8 ~ 10h of baking, can be obtained strontium molybdate powder.Fig. 3 is molybdic acid manufactured in the present embodiment
The standard diagram (JCPDS no 85-0586) of the X ray diffracting spectrum of strontium powder, all diffraction maximums and strontium molybdate is kissed completely
It closes, does not find impurity peaks in spectrogram.Fig. 4 is its stereoscan photograph, and the strontium molybdate powder of preparation is by many ultrathin nanometer pieces
The central area of the hierarchical structure of composition, single strontium molybdate is recessed inwardly, similar with red blood cell shape.Grain thickness is about 25 μ
M, partial size are about 75 ~ 125 μm.
Embodiment 3
0.50g barium acetate is dissolved in the mixed solution of 70mLN- methylacetamide (MAc) and deionized water, and the volume of the two
Than for 1:2, the ultrasound 30min in supersonic wave cleaning machine weighs 2.47g ammonium heptamolybdate and is dissolved in the solution that ultrasound is crossed, at room temperature
Stirring obtains milky precursor solution until ammonium heptamolybdate is completely dissolved.It is anti-that above-mentioned precursor solution is poured into 100mL
It answers in kettle, reacts 20h at 120 DEG C, be cooled to room temperature to reaction kettle, obtained sample is used into deionized water and anhydrous second respectively
Alcohol washs 3 times, and then 80 DEG C of 8 ~ 10h of baking, can be obtained barium molybdate powder.Fig. 5 is the X of barium molybdate powder manufactured in the present embodiment
The standard diagram (JCPDS no 29-0193) of x ray diffraction map, all diffraction maximums and barium molybdate fits like a glove, in spectrogram
Impurity peaks are not found.Fig. 6 be its stereoscan photograph, the barium molybdate powder of preparation be self-assembled by many thin slices it is flower-shaped,
Grain size is about 145 ~ 160 μm.
Embodiment 4
0.79g manganese chloride is dissolved in the mixed solution of 70mL dimethylformamide (DMF) and deionized water, and the volume of the two
Than weighing bis- molybdic acid hydrate sodium of 0.97g in supersonic wave cleaning machine ultrasound 30min for 1:5 and being dissolved in the solution that ultrasound is crossed, at room temperature
Stirring obtains precursor solution until two molybdic acid hydrate sodium all dissolve.Above-mentioned precursor solution is poured into 100mL reaction kettle
In, 20h is reacted at 180 DEG C, is cooled to room temperature to reaction kettle, obtained sample is washed with deionized water and dehydrated alcohol respectively
It washs 3 times, then 50 DEG C of 8 ~ 10h of baking, can be obtained manganese molybdate powder.The X-ray diffraction spectrum and molybdenum of obtained manganese molybdate powder
The standard diagram (JCPDS no 78-0221) of sour manganese fits like a glove, and does not find impurity peaks in spectrogram.The manganese molybdate being prepared
It is the crystal of a large amount of rod-type pattern, length range is at 100 ~ 200 μm, and dispersibility and homogeneity are fine.
Embodiment 5
0.93g chromic nitrate is dissolved in 70mLN, the mixed solution of N- dimethyl acetamide (DMAc) and deionized water, and the two
Volume ratio be 1:3, in supersonic wave cleaning machine ultrasound 30min, weigh bis- molybdic acid hydrate sodium of 0.73g and be dissolved in the solution that ultrasound is crossed,
It stirs at room temperature, until two molybdic acid hydrate sodium all dissolve, obtains precursor solution.Above-mentioned precursor solution is poured into 100mL
In reaction kettle, 20h is reacted at 90 DEG C, is cooled to room temperature to reaction kettle, obtained sample is used into deionized water and anhydrous respectively
Ethanol washing 3 times, then 50 DEG C of 8 ~ 10h of baking, can be obtained molybdic acid chromium powder body.The X-ray diffraction of obtained molybdic acid chromium powder body
It composes and fits like a glove with the standard diagram (JCPDS no 88-0182) of molybdic acid chromium, be tetragonal phase wolframite crystal, and in spectrogram not
It was found that impurity peaks.The nano particle of 30 ~ 50nm of particle size is obtained, and dispersibility and homogeneity are fine.
Embodiment 6
0.55g anhydrous calcium chloride is dissolved in 70mL dimethylformamide (DMF) and the mixed solution of deionized water, and the two
Volume ratio be 5:1, the ultrasound 30min in supersonic wave cleaning machine, weigh 6.18g ammonium heptamolybdate be dissolved in ultrasound mistake solution in,
It stirs at room temperature, until ammonium heptamolybdate is completely dissolved, obtains colorless and transparent precursor solution.Above-mentioned precursor solution is poured into
In 100mL reaction kettle, 30min is reacted at 180 DEG C, is cooled to room temperature to reaction kettle, obtained sample is used into deionization respectively
Water and dehydrated alcohol wash 3 times respectively, and then 80 DEG C of 8 ~ 10h of baking, can be obtained calcium molybdate powder.Molybdic acid manufactured in the present embodiment
The standard diagram (JCPDS no 29-0351) of the X ray diffracting spectrum of calcium powder body, prepared diffraction maximum and calcium molybdate is complete
It coincide, does not find impurity peaks in spectrogram.The calcium molybdate of preparation is to be formed by the nanostructure of many red blood cell shapes by self assembly,
The pattern of Coiling-type is showed, mean particle size is about 50 ~ 60 μm, and dispersibility and homogeneity are fine.
Embodiment 7
0.55g anhydrous calcium chloride is dissolved in 70mLN, in N- dimethyl acetamide (DMAc) and the mixed solution of deionized water,
And the volume ratio of the two is 4:3, the ultrasound 30min in supersonic wave cleaning machine, weighs 6.18g ammonium heptamolybdate and is dissolved in the molten of ultrasound mistake
It in liquid, stirs at room temperature, until ammonium heptamolybdate is completely dissolved, obtains the precursor solution of yellow.Above-mentioned precursor solution is fallen
Enter in 100mL reaction kettle, react 30min at 180 DEG C, be cooled to room temperature to reaction kettle, by obtained sample spend respectively from
Sub- water and dehydrated alcohol wash 3 times respectively, and then 80 DEG C of 8 ~ 10h of baking, can be obtained calcium molybdate powder.Molybdenum manufactured in the present embodiment
The standard diagram (JCPDS no 29-0351) of the X ray diffracting spectrum of sour calcium powder body, prepared diffraction maximum and calcium molybdate is complete
It is complete to coincide, impurity peaks are not found in spectrogram.The calcium molybdate of preparation be by the nanostructure of many red blood cell shapes by self assembly and
At showing the pattern of Coiling-type.
Comparative example 1
0.55g anhydrous calcium chloride is dissolved in 70mL deionized water, ultrasound 30min, weighs 6.18g in supersonic wave cleaning machine
Ammonium heptamolybdate is dissolved in the solution that ultrasound is crossed, and is stirred at room temperature, until ammonium heptamolybdate is completely dissolved, obtains colorless and transparent forerunner
Liquid solution.Above-mentioned precursor solution is poured into 100mL reaction kettle, reacts 30min at 180 DEG C, is cooled to room temperature to reaction kettle,
Obtained sample is washed 3 times with deionized water and dehydrated alcohol respectively respectively, then 80 DEG C of 8 ~ 10h of baking, can be obtained molybdenum
Sour calcium powder body.The X ray diffracting spectrum of calcium molybdate powder manufactured in the present embodiment, the standard of prepared diffraction maximum and calcium molybdate
Map (JCPDS no 29-0351) fits like a glove, and does not find impurity peaks in spectrogram.The calcium molybdate powder of preparation tends to generate
Red blood cell shape, and dispersibility and homogeneity are poor.Therefore, the amide compound of proper proportion and the mixed solution of deionized water exist
It is used as solvent in reaction system, plays a part of structure directing agent, red blood cell shape structure is promoted to be self-assembled into Coiling-type, obtains special
Shape looks.
Comparative example 2
0.55g anhydrous calcium chloride is dissolved in 70mLN, it is ultrasonic in supersonic wave cleaning machine in N- dimethyl acetamide (DMAc)
30min weighs 6.18g ammonium heptamolybdate and is dissolved in the solution that ultrasound is crossed, stir at room temperature, until ammonium heptamolybdate is completely dissolved, obtains
To the precursor solution of yellow.Above-mentioned precursor solution is poured into 100mL reaction kettle, 30min is reacted at 180 DEG C, wait react
Kettle is cooled to room temperature, and obtained sample is washed 3 times with deionized water and dehydrated alcohol respectively respectively, then 80 DEG C dry 8 ~
Calcium molybdate powder can be obtained in 10h.The X ray diffracting spectrum of calcium molybdate powder manufactured in the present embodiment, prepared diffraction maximum
It fits like a glove with the standard diagram (JCPDS no 29-0351) of calcium molybdate, does not find impurity peaks in spectrogram.The calcium molybdate of preparation
Powder is amorphous to reunite together, without specific pattern.Therefore, the amide compound of proper proportion and deionized water is mixed
It closes solution and is used as solvent in reaction system, play a part of structure directing agent, red blood cell shape structure can be promoted to be self-assembled into
Coiling-type obtains specific morphology.
Claims (7)
1. a kind of metal molybdate micro nano structure raw powder's production technology, which is characterized in that with sodium molybdate or ammonium heptamolybdate, with
And soluble divalent metal salt is as reaction raw materials, in the in the mixed solvent that amide compound and water are formed, at 90 ~ 180 DEG C
At a temperature of hydro-thermal reaction, metal molybdate micro nano structure powder is prepared；Wherein: soluble divalent metal salt is Ca salt,
It is any in Sr salt, Ba salt, Co salt, Mn salt, Zn salt or Cd salt；Amide compound be N- alkyl substituted amide or N,
N- dialkyl group substituted amide.
2. preparation method according to claim 1, which is characterized in that the volume of in the mixed solvent, amide compound and water
Than for 6:1 ~ 1:6.
3. preparation method according to claim 1, which is characterized in that amide compound is selected from n,N-dimethylacetamide
DMAc, N- methylacetamide MAc, N,N-dimethylformamide DMF, N, N- diethyl acetamide, N, N- diethylformamide or
It is any in N- ethyl acetamide.
4. preparation method according to claim 1, which is characterized in that sodium molybdate or ammonium heptamolybdate and soluble divalent metal
The molar ratio of salt is 1:1.
5. preparation method according to claim 1, which is characterized in that the hydro-thermal reaction time is 0.5 ~ 20 hour.
6. preparation method according to claim 1, which is characterized in that soluble divalent metal salt is selected from calcium chloride, chlorination
Strontium, barium chloride, cobalt chloride, manganese chloride, caddy, zinc chloride；Calcium nitrate, strontium nitrate, barium nitrate, cobalt nitrate, manganese nitrate, nitric acid
Zinc, cadmium nitrate；It is any in calcium acetate, strontium acetate, barium acetate, cobalt acetate, manganese acetate, zinc acetate or cadmium acetate.
7. preparation method according to claim 1, which is characterized in that specific step is as follows:
1) amide compound is mixed with deionized water, is configured to mixed solvent；
2) soluble divalent metal salt is added to above-mentioned in the mixed solvent, is sufficiently stirred to form the first solution；Wherein, divalent gold
The concentration for belonging to salt is 0.02 ~ 0. 8 mol/l；
3) sodium molybdate or ammonium heptamolybdate are weighed, and is dissolved in the first solution formed by step 2, is sufficiently stirred that form second molten
Liquid；
4) the second solution is placed in hydro-thermal reaction in closed reaction vessel to be precipitated；
5) by obtained precipitating spend dehydrated alcohol, deionized water wash respectively for several times, it is dry, obtain specific morphology structure,
The metal molybdate micro nano structure powder of better crystallinity degree, purity is high.
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| CN111704164A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of barium molybdate flower-like crystal |
| CN112939079A (en) * | 2021-02-18 | 2021-06-11 | 辽宁大学 | Preparation method and application of zinc molybdate powder |
| CN114751454A (en) * | 2022-03-24 | 2022-07-15 | 中国科学院兰州化学物理研究所 | Preparation of porous chromium molybdate flower ball material and application of porous chromium molybdate flower ball material as electrode material of supercapacitor |
| CN115072783A (en) * | 2022-07-05 | 2022-09-20 | 江西省农业科学院土壤肥料与资源环境研究所 | Method for preparing manganese molybdate nano material through phase inversion reaction in hydrothermal process |
| CN115611312A (en) * | 2022-11-04 | 2023-01-17 | 嘉兴市福思矼新材料有限公司 | Preparation method of zirconium molybdate ultrafine nanoparticles |
| CN116177603A (en) * | 2023-03-20 | 2023-05-30 | 洛阳理工学院 | Preparation method of calcium molybdate nanowire crystal |
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| CN111704164A (en) * | 2020-07-01 | 2020-09-25 | 洛阳理工学院 | Preparation method of barium molybdate flower-like crystal |
| CN111704164B (en) * | 2020-07-01 | 2023-01-24 | 洛阳理工学院 | Preparation method of barium molybdate flower-like crystal |
| CN112939079A (en) * | 2021-02-18 | 2021-06-11 | 辽宁大学 | Preparation method and application of zinc molybdate powder |
| CN114751454A (en) * | 2022-03-24 | 2022-07-15 | 中国科学院兰州化学物理研究所 | Preparation of porous chromium molybdate flower ball material and application of porous chromium molybdate flower ball material as electrode material of supercapacitor |
| CN114751454B (en) * | 2022-03-24 | 2023-06-09 | 中国科学院兰州化学物理研究所 | Preparation of porous chromium molybdate ball material and application of porous chromium molybdate ball material as supercapacitor electrode material |
| CN115072783A (en) * | 2022-07-05 | 2022-09-20 | 江西省农业科学院土壤肥料与资源环境研究所 | Method for preparing manganese molybdate nano material through phase inversion reaction in hydrothermal process |
| CN115072783B (en) * | 2022-07-05 | 2023-04-11 | 江西省农业科学院土壤肥料与资源环境研究所 | Method for preparing manganese molybdate nano material through phase inversion reaction in hydrothermal process |
| CN115611312A (en) * | 2022-11-04 | 2023-01-17 | 嘉兴市福思矼新材料有限公司 | Preparation method of zirconium molybdate ultrafine nanoparticles |
| CN116177603A (en) * | 2023-03-20 | 2023-05-30 | 洛阳理工学院 | Preparation method of calcium molybdate nanowire crystal |
| CN116177603B (en) * | 2023-03-20 | 2024-05-03 | 洛阳理工学院 | Preparation method of calcium molybdate nanowire crystal |
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