CN114682786A - 一种微纳米金属粉体的制备方法 - Google Patents
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- 239000000843 powder Substances 0.000 title claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 32
- 239000002184 metal Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 23
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 9
- 229910000103 lithium hydride Inorganic materials 0.000 claims abstract description 9
- 229910001510 metal chloride Inorganic materials 0.000 claims abstract description 9
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 9
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 3
- 239000012265 solid product Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910021450 lithium metal oxide Inorganic materials 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- 229940045803 cuprous chloride Drugs 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 4
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 4
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-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
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 3
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- 229910021552 Vanadium(IV) chloride Inorganic materials 0.000 claims description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 claims description 2
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 claims description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 229940032296 ferric chloride Drugs 0.000 claims description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 2
- 229960002089 ferrous chloride Drugs 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 2
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 claims description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 2
- 229910003445 palladium oxide Inorganic materials 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 2
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- 229910001923 silver oxide Inorganic materials 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 2
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 claims description 2
- FKZFOHABAHJDIK-UHFFFAOYSA-K trichloroscandium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Sc+3] FKZFOHABAHJDIK-UHFFFAOYSA-K 0.000 claims description 2
- JTJFQBNJBPPZRI-UHFFFAOYSA-J vanadium tetrachloride Chemical compound Cl[V](Cl)(Cl)Cl JTJFQBNJBPPZRI-UHFFFAOYSA-J 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 2
- 229940117975 chromium trioxide Drugs 0.000 claims 1
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims 1
- 239000007769 metal material Substances 0.000 abstract description 8
- 238000012824 chemical production Methods 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 12
- 238000002441 X-ray diffraction Methods 0.000 description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 8
- 229910052721 tungsten Inorganic materials 0.000 description 7
- 239000010937 tungsten Substances 0.000 description 7
- 239000010949 copper Substances 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- 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
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- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
一种微纳米金属粉体的制备方法,涉及金属材料合成技术领域,本发明利用氢化锂和金属氧化物在加热条件下反应或者利用锂粉和金属氯化物在加热条件下反应,分别能够生成纳米以及亚微米金属粉体。本发明的制备方法低成本、高效环保、易于工业化生产。本发明制备的亚微米金属可用于化工生产、工业催化、机械制造和生物制药等领域,制备的纳米金属材料可用于化工生产与材料改性等领域。本发明制备的纳米及亚微米金属粉体,其形貌较为规整,分散性高,产物纯度高。
Description
技术领域
本发明涉及金属材料合成技术领域,具体是涉及一种微纳米金属粉体的制备方法。
背景技术
纳米金属材料作为典型的纳米材料,具有特有的纳米尺寸效应,广泛应用于对材料的改性,尤其是在催化、电学、磁学和力学等方面。目前合成纳米金属材料的方法通常有液相水热法、固相高温法和气相蒸发法等。这些制备方法都存在工艺复杂、污染严重、能耗高等缺点,不利于大规模生产。
亚微米金属材料作为典型的超微粉体材料,具有优异的表面效应、小尺寸效应和独特的物理化学特性,被广泛应用于化工生产、工业催化、机械制造和生物制药等领域。目前合成亚微米金属材料的方法通常有液相还原法和高温固相还原法等。部分液相合成法需要用到剧毒药剂水合肼,高温固相还原法通常需要加热到1000℃以上。这些制备方法都存在工艺复杂、浪费能源等缺点,不利于大规模生产。
有鉴于此,本发明提出一种新型、便宜、节约能源、环境友好、易于工业化生产的微纳米金属粉体制备方法,具有重要意义。
发明内容
本发明目的是为了提供一种微纳米金属粉体的制备方法,利用氢化锂和金属氧化物在加热条件下反应或者利用锂粉和金属氯化物在加热条件下反应,分别能够生成纳米以及亚微米金属粉体。
为了实现上述目的,本发明所采用的技术方案为:一种微纳米金属粉体的制备方法,其特征在于,利用氢化锂和金属氧化物在加热条件下反应生成纳米金属粉体,具体包括以下步骤:
(1)在真空或惰性气氛保护下,将氢化锂和金属氧化物按摩尔比1∶0.01~1混合,置于加热炉中;
(2)将加热炉以1~15℃/min的升温速率升至350~600℃,保温1~12h;
(3)加热结束后将固体产物取出,用去离子水浸泡、洗涤、离心并干燥,即可得到纳米金属粉体;
或者,利用锂粉和金属氯化物在加热条件下反应生成亚微米金属粉体,具体包括以下步骤:
(1)在真空或惰性气氛保护下,将锂粉和金属氯化物按摩尔比1∶0.1~10混合,置于加热炉中;
(2)将加热炉以1~20℃/min的升温速率升至300~650℃,保温2~10h;
(3)加热结束后将固体产物取出,用去离子水浸泡、洗涤、分离并干燥,即可得到亚微米金属粉体。
作为本发明的优选技术方案,所述的金属氧化物为三氧化钼、三氧化钨、氧化铜、二氧化钛、五氧化二钒、氧化钪、三氧化二铬、氧化锰、三氧化二铁、四氧化三铁、氧化亚铁、氧化钴、氧化镍、氧化锌、二氧化锆、五氧化二铌、氧化银、氧化钯、二氧化钌、三氧化二铟中的至少一种。
作为本发明的优选技术方案,所述的金属氯化物为六氯化钨、氯化亚铜、四氯化钛、四氯化钒、氯化钼、六水氯化钪、六水氯化铬、氯化锰、氯化铁、氯化亚铁、氯化亚铜、六水合氯化钴、氯化镍、氯化镉、氯化锌、氯化锆、氯化银、氯化钯、三氯化钌、氯化钇、氯化铱中的至少一种。
作为本发明的优选技术方案,所述的惰性气体为氮气、氩气、氦气中的一种或多种混合气。
作为本发明的优选技术方案,所述的干燥包括常压干燥、冷冻干燥和真空干燥。
作为本发明的优选技术方案,所述的分离包括抽滤分离和离心分离。
与现有技术相比,本发明的有益效果表现在:
(1)本发明的制备方法低成本、高效环保、易于工业化生产。
(2)本发明制备的亚微米金属可用于化工生产、工业催化、机械制造和生物制药等领域,制备的纳米金属材料可用于化工生产与材料改性等领域。
(3)本发明制备的纳米及亚微米金属粉体,其形貌较为规整,分散性高,产物纯度高。
附图说明
图1为实施例1制备的纳米金属Mo粉末的X射线衍射图谱。
图2为实施例1制备的纳米金属Mo粉末的扫描电子显微镜图(a、b分别代表低、高倍率)。
图3为实施例2制备的纳米金属W粉末的X射线衍射图谱。
图4为实施例2制备的纳米金属W粉末的扫描电子显微镜图(a、b分别代表低、高倍率)。
图5为实施例9制备的亚微米金属W粉末的X射线衍射图谱。
图6为实施例9制备的亚微米金属W粉末的扫描电子显微镜图(a、b分别代表低、高倍率)。
图7为实施例10制备的亚微米金属Cu粉末的X射线衍射图谱。
图8为实施例10制备的亚微米金属Cu粉末的扫描电子显微镜图(a、b分别代表低、高倍率)。
具体实施方式
实施例1
真空条件下,将氢化锂和三氧化钼按摩尔比6:1混合,置于加热炉中,以5℃/min的升温速率升至400℃,反应2h。加热结束后将固体产物取出,用去离子水浸泡、洗涤、离心分离出固体产物并进行常压干燥,即可得到分散均匀的金属钼纳米颗粒。
图1为实施例1制备产物的X射线衍射图谱,图2为实施例1制备产物的扫描电子显微镜图。从图1中可以看出样品衍射峰位置与钼的PDF#-42-1120卡片完全对应,表明本发明成功制备出纳米金属钼粉末。通过图2可以看出,制备的金属钼颗粒呈椭球形,尺寸大小分布为30~50nm,形貌较为均匀,分散性高。
实施例2
氩气氛围下,将氢化锂和三氧化钨按摩尔比6:1混合,置于加热炉中,以10℃/min的升温速率升至550℃,反应4h。加热结束后将固体产物取出,用去离子水浸泡、洗涤、离心分离出固体产物并进行真空干燥,即可得到分散均匀的金属钨纳米颗粒。
图3为实施例2制备产物的X射线衍射图谱,图4为实施例2制备产物的扫描电子显微镜图。从图3中可以看出样品衍射峰位置与钨的PDF#-47-1319和PDF#04-0806卡片完全对应,表明本发明成功制备出纳米金属钨粉末。通过图4可以看出,制备的金属钨颗粒,尺寸大小分布为50~100nm。
实施例3-8
将氢化锂和金属氧化物粉末混合,置于加热炉中升温反应。反应结束后待样品冷却,取出固体产物并使用去离子水浸泡、洗涤、离心分离并进行干燥,即可得到纳米金属粉体。各工艺参数按照表1执行。
表1
实施例9
真空条件下,将锂粉和六氯化钨粉末按摩尔比6:1混合,置于加热炉中,以5℃/min的升温速率升至400℃,反应2h。反应结束后待样品冷却,取出固体产物并使用去离子水浸泡、洗涤、过滤分离,并进一步对产物进行真空干燥处理,即可得到亚微米金属钨。
图5为实施例9制备产物的X射线衍射图谱,图6为实施例9制备产物的扫描电子显微镜图。从图5中可以看出样品衍射峰位置与钨的PDF#-04-0806卡片完全对应,表明本发明成功制备出亚微米金属钨。通过图6可以看出,制备的金属钨颗粒呈椭球形,尺寸大小分布为100~300nm之间。
实施例10
氩气氛围下,将锂粉和氯化亚铜粉末按摩尔比1:1混合,置于加热炉中,以2℃/min的升温速率升至500℃,反应4h。反应结束后待样品冷却,取出固体产物并使用去离子水浸泡、洗涤、过滤分离,并进一步对产物进行真空干燥处理,即可得到亚微米金属铜。
图7为实施例10制备产物的X射线衍射图谱,图8为实施例10制备产物扫描电子显微镜图。从图7中可以看出样品衍射峰位置与铜的PDF#-48-0836卡片完全对应,表明本发明成功制备出亚微米金属铜。通过图8可以看出,制备的金属铜颗粒呈片层状,尺寸大小分布为100~300nm之间。
实施例11-15
将锂粉和金属氯化物粉末混合,置于加热炉中升温反应。反应结束后待样品冷却,取出固体产物并使用去离子水浸泡、洗涤、过滤分离,并进一步对产物进行干燥处理,即可得到亚微米金属粉体。各工艺参数按照表2执行。
表2
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (6)
1.一种微纳米金属粉体的制备方法,其特征在于,利用氢化锂和金属氧化物在加热条件下反应生成纳米金属粉体,具体包括以下步骤:
(1)在真空或惰性气氛保护下,将氢化锂和金属氧化物按摩尔比1∶0.01~1混合,置于加热炉中;
(2)将加热炉以1~15℃/min的升温速率升至350~600℃,保温1~12h;
(3)加热结束后将固体产物取出,用去离子水浸泡、洗涤、离心并干燥,即可得到纳米金属粉体;
或者,利用锂粉和金属氯化物在加热条件下反应生成亚微米金属粉体,具体包括以下步骤:
(1)在真空或惰性气氛保护下,将锂粉和金属氯化物按摩尔比1∶0.1~10混合,置于加热炉中;
(2)将加热炉以1~20℃/min的升温速率升至300~650℃,保温2~10h;
(3)加热结束后将固体产物取出,用去离子水浸泡、洗涤、分离并干燥,即可得到亚微米金属粉体。
2.如权利要求1所述的制备方法,其特征在于:所述的金属氧化物为三氧化钼、三氧化钨、氧化铜、二氧化钛、五氧化二钒、氧化钪、三氧化二铬、氧化锰、三氧化二铁、四氧化三铁、氧化亚铁、氧化钴、氧化镍、氧化锌、二氧化锆、五氧化二铌、氧化银、氧化钯、二氧化钌、三氧化二铟中的至少一种。
3.如权利要求1所述的制备方法,其特征在于:所述的金属氯化物为六氯化钨、氯化亚铜、四氯化钛、四氯化钒、氯化钼、六水氯化钪、六水氯化铬、氯化锰、氯化铁、氯化亚铁、氯化亚铜、六水合氯化钴、氯化镍、氯化镉、氯化锌、氯化锆、氯化银、氯化钯、三氯化钌、氯化钇、氯化铱中的至少一种。
4.如权利要求1所述的制备方法,其特征在于:所述的惰性气体为氮气、氩气、氦气中的一种或多种混合气。
5.如权利要求1所述的制备方法,其特征在于:所述的干燥包括常压干燥、冷冻干燥和真空干燥。
6.如权利要求1所述的制备方法,其特征在于:所述的分离包括抽滤分离和离心分离。
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