CN106179290A - A kind of method preparing load type gold metal nano-particle - Google Patents
A kind of method preparing load type gold metal nano-particle Download PDFInfo
- Publication number
- CN106179290A CN106179290A CN201610496157.7A CN201610496157A CN106179290A CN 106179290 A CN106179290 A CN 106179290A CN 201610496157 A CN201610496157 A CN 201610496157A CN 106179290 A CN106179290 A CN 106179290A
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- solution
- particle
- tio
- matrix
- load type
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- 238000000034 method Methods 0.000 title claims abstract description 102
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 39
- 239000010931 gold Substances 0.000 title claims abstract description 39
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 118
- 239000011159 matrix material Substances 0.000 claims abstract description 70
- 230000008569 process Effects 0.000 claims abstract description 28
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 25
- 239000012670 alkaline solution Substances 0.000 claims abstract description 19
- 210000002381 plasma Anatomy 0.000 claims description 83
- 239000007921 spray Substances 0.000 claims description 46
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- 229910052703 rhodium Inorganic materials 0.000 claims description 6
- 229910052707 ruthenium Inorganic materials 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 229910052793 cadmium Inorganic materials 0.000 claims description 5
- 230000005495 cold plasma Effects 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910052763 palladium Inorganic materials 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052745 lead Inorganic materials 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- -1 step 1 Substances 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract 1
- 238000004659 sterilization and disinfection Methods 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 79
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 72
- 239000007789 gas Substances 0.000 description 65
- 239000007864 aqueous solution Substances 0.000 description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 47
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 31
- 239000001257 hydrogen Substances 0.000 description 31
- 229910052739 hydrogen Inorganic materials 0.000 description 31
- 238000005507 spraying Methods 0.000 description 30
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 28
- 239000008187 granular material Substances 0.000 description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 26
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 26
- 235000011121 sodium hydroxide Nutrition 0.000 description 23
- 239000002245 particle Substances 0.000 description 21
- 238000012360 testing method Methods 0.000 description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 19
- 230000001699 photocatalysis Effects 0.000 description 18
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- 239000004744 fabric Substances 0.000 description 14
- 239000008246 gaseous mixture Substances 0.000 description 14
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 229910021529 ammonia Inorganic materials 0.000 description 13
- 230000004888 barrier function Effects 0.000 description 13
- 239000001569 carbon dioxide Substances 0.000 description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 12
- 230000010718 Oxidation Activity Effects 0.000 description 12
- JISVROCKRBFEIQ-UHFFFAOYSA-N [O].O=[C] Chemical compound [O].O=[C] JISVROCKRBFEIQ-UHFFFAOYSA-N 0.000 description 12
- 230000000844 anti-bacterial effect Effects 0.000 description 12
- 229910002091 carbon monoxide Inorganic materials 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 10
- 239000010949 copper Substances 0.000 description 10
- 238000010531 catalytic reduction reaction Methods 0.000 description 9
- 235000013339 cereals Nutrition 0.000 description 9
- 239000011651 chromium Substances 0.000 description 9
- 238000007146 photocatalysis Methods 0.000 description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 9
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 8
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 8
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 8
- 229910052734 helium Inorganic materials 0.000 description 8
- 239000001307 helium Substances 0.000 description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 8
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 229910000000 metal hydroxide Inorganic materials 0.000 description 7
- 150000004692 metal hydroxides Chemical class 0.000 description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 7
- 239000004332 silver Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000010948 rhodium Substances 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 229910052684 Cerium Inorganic materials 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 4
- UKHWJBVVWVYFEY-UHFFFAOYSA-M silver;hydroxide Chemical compound [OH-].[Ag+] UKHWJBVVWVYFEY-UHFFFAOYSA-M 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 239000003638 chemical reducing agent Substances 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 229910052756 noble gas Inorganic materials 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 101710134784 Agnoprotein Proteins 0.000 description 2
- 206010051548 Burn infection Diseases 0.000 description 2
- 229910021556 Chromium(III) chloride Inorganic materials 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000011636 chromium(III) chloride Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 239000011565 manganese chloride Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910004042 HAuCl4 Inorganic materials 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 229910002249 LaCl3 Inorganic materials 0.000 description 1
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 1
- 229910015221 MoCl5 Inorganic materials 0.000 description 1
- 229910003206 NH4VO3 Inorganic materials 0.000 description 1
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910002666 PdCl2 Inorganic materials 0.000 description 1
- 101150003085 Pdcl gene Proteins 0.000 description 1
- 206010037211 Psychomotor hyperactivity Diseases 0.000 description 1
- 229910019032 PtCl2 Inorganic materials 0.000 description 1
- 229910021604 Rhodium(III) chloride Inorganic materials 0.000 description 1
- 229910019891 RuCl3 Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 229920002334 Spandex Polymers 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- 229910003091 WCl6 Inorganic materials 0.000 description 1
- 229910007926 ZrCl Inorganic materials 0.000 description 1
- 229910007932 ZrCl4 Inorganic materials 0.000 description 1
- SGDPVQRGBHPKIH-UHFFFAOYSA-L [Ni].Cl[Ni]Cl Chemical compound [Ni].Cl[Ni]Cl SGDPVQRGBHPKIH-UHFFFAOYSA-L 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 229940097267 cobaltous chloride Drugs 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 125000001145 hydrido group Chemical group *[H] 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- 229940099607 manganese chloride Drugs 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- PDKHNCYLMVRIFV-UHFFFAOYSA-H molybdenum;hexachloride Chemical compound [Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Cl-].[Mo] PDKHNCYLMVRIFV-UHFFFAOYSA-H 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 description 1
- 229960001180 norfloxacin Drugs 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000003380 propellant Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 description 1
- 229910001630 radium chloride Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010944 silver (metal) Substances 0.000 description 1
- 229960003600 silver sulfadiazine Drugs 0.000 description 1
- UEJSSZHHYBHCEL-UHFFFAOYSA-N silver(1+) sulfadiazinate Chemical compound [Ag+].C1=CC(N)=CC=C1S(=O)(=O)[N-]C1=NC=CC=N1 UEJSSZHHYBHCEL-UHFFFAOYSA-N 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004449 solid propellant Substances 0.000 description 1
- 239000004759 spandex Substances 0.000 description 1
- YOUIDGQAIILFBW-UHFFFAOYSA-J tetrachlorotungsten Chemical compound Cl[W](Cl)(Cl)Cl YOUIDGQAIILFBW-UHFFFAOYSA-J 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention discloses a kind of method preparing load type gold metal nano-particle, including step 1, matrix solution and alkaline solution by metal ion successively processes;Step 2, the matrix after utilizing reducibility gas to process step 1 carries out discharge of plasma in low temperature process, obtains described load type gold metal nano-particle.The method preparing load type gold metal nano-particle disclosed by the invention, simple to operate, the process time is short, environmental friendliness, and the load type gold metal nano-particle obtained has nano effect, embodies the performances such as various excellent catalysis, sterilization, efficient burning.
Description
Technical field
The invention belongs to nano material preparation and application technical field, be specifically related to one and prepare load type metal nanometer
The method of grain.
Background technology
Metal nanoparticle is particle diameter metallic between 1-100nm, and owing to its granule is the most small, surface area is relatively
Greatly, there is significant skin effect, quantum size effect and quantum tunneling effect.It is fine that metal nanoparticle can be loaded into activated carbon
In the products such as dimension, textile, coating, prepare and there is catalysis, the product of the function such as antibacterial.
Nano aluminum, copper, nikel powder body have overactivity surface, can implement in the temperature less than powder body fusing point under anaerobic
Coating, this technology can be applicable to the production of microelectronic component.
Copper and alloy nano powder body thereof are used as catalyst, and efficiency is high, selectivity is strong, can be used for carbon dioxide and becomes first with hydrido
In the courses of reaction such as alcohol.Substitute, with copper nanoparticle, the electric slurry that noble metal powder processability is superior, cost can be substantially reduced,
This technology can promote the further optimization of microelectronic technique.
Owing to specific surface is huge and high activity, nano-nickel powder has extremely strong catalytic effect, can be used for Organic substance hydrogenation anti-
Should, vehicle maintenance service etc..Nano-nickel powder is added to the combustion that can increase substantially fuel in the solid fuel propellant of rocket
Burn-out, efficiency of combustion, improve the stability of burning.By the additional suitable technique of nano-nickel powder, can produce and there is huge surface area
Electrode, discharging efficiency can be increased substantially.
Load silver activated carbon and activated carbon fiber antibacterial are usually used in water purification and process;Nanometer silver is penetrated into fabric
In, multiple antibacterial fabric can be prepared;Nanometer silver is scattered in coating and can prepare the coating products with antibacterial functions, will receive
Rice silver particles appendix can make it have anti-microbial property on rustless steel device medical apparatus and instruments, tableware etc., the load nanometer developed such as Japan
The rustless steel medical apparatus and instruments etc. of level silver granuel;Antibacterial gauze containing nanometer silver can be used for treatment burn, scalds, when being used for treating burn
Can divide each bacterioid causing burn infection in 30min, sustainable 3 days of its antibacterial effect, it controls the effect of burn infection
Fruit is more far better than the silver sulfadiazine of present Clinical practice, zinc norfloxacin.At present existing special about antibiotic fabric of China
Profit product, a kind of nanometer silver antimicrobial bafta as disclosed in patent CN105088780A, it is possible to the antibacterial of high-efficient simple environmental protection presses down
Bacterium.
The preparation method of load type gold metal nano-particle mainly has chemical reduction method, deposition-precipitation and infusion process at present
Deng.Chemical reduction method needs to use a large amount of poisonous and hazardous reducing agent, wayward load capacity, and environment is unfriendly;Deposition-heavy
Shallow lake method generally can be with the higher load type gold metal particles of processability, but it is not suitable for the carrier of low isoelectric point, IP and is difficult to realize
Deposit completely, simultaneously need to more harsh reaction condition;Infusion process be prepare load type gold metal nano-particle a kind of simple,
Easy method, it is possible to control the load capacity of metallic particles well, but its load type metal grain diameter prepared is relatively big, point
Dissipate property poor, so that its activity is poor.
Summary of the invention
For shortcoming present in above-mentioned load type metal nanometer grain preparation method, the invention provides a kind of operation letter
Single, the process time method preparing load type gold metal nano-particle short, eco-friendly.
A kind of method preparing load type gold metal nano-particle, including:
Step 1, matrix solution and alkaline solution by metal ion successively processes;
Step 2, the matrix after utilizing reducibility gas to process step 1 carries out discharge of plasma in low temperature process, obtains
Described load type gold metal nano-particle.
Matrix solution and alkaline solution by metal ion successively processes, precipitate metal hydroxide on matrix
Granule, is reduced to the metal hydroxide particle on matrix by the reducibility gas in step 2, obtains metal nano
Grain.
As preferably, described metal is Ag, Cu, Pt, Au, Pd, Ni, Ru, Rh, Fe, Co, Al, Zn, Cr, Ti, Ce, W,
Simple substance in Zr, Pb, Cd, Mn, Mo, Nb, V, La or alloy.
Matrix in step 1 preferably selects porous, and the solid-state material that breathability is good, by solution and the alkali of metal ion
After property solution, matrix can capture the metal hydroxide particle small with in adsorbent solution.As preferably, described matrix is
TiO2、CeO2、Fe2O3、SiO2, Inorganic Non-metallic Materials or the high-molecular organic material such as fiber cloth.Described fiber cloth includes
The non-woven fabrics of the material such as acrylon, spandex, also includes pure cotton cloth, Carbon fibe blanket, screen window and drainage screen etc..
In order to ensure the load effect of particulate matter on matrix, it is preferable that matrix uses stratified material, the thickness of stratified material
It is 1~5mm.
The thickness of matrix determines the adsorption effect of particulate matter, if matrix thickness is blocked up, it is right that intrinsic silicon cannot realize
The active adsorption of metal hydroxide particle, if matrix thickness is the thinnest, then the metal hydroxide particle mistake of absorption in matrix
Few, affect load factor, therefore, the thickness of matrix needs to be maintained in certain scope, can meet the need of high density absorption
Ask.
In load type gold metal nano-particle prepared by the present invention, metal nanoparticle is dispersed in matrix microstructure
Surface, to obtain preferable load type gold metal nano-particle.
Further preferably, described matrix is acrylon cloth, and thickness is 1~5mm.Described metal ion is silver ion.
As preferably, the concentration of metal ion in solution is 0.01g/L~20g/L.Further preferably, GOLD FROM PLATING SOLUTION belong to from
The concentration of son is 0.1g/L~10g/L.Further preferably, the concentration of metal ion in solution is 1g/L~5g/L.
Metal ion in solution needs the hole through matrix to enter into inside matrix material, if the concentration of metal ion
Excessive, although to ensure that the load factor in matrix, but the utilization rate of metal ion is low, if the concentration of metal ion is too small,
The performance of the load type gold metal nano-particle then prepared can not meet requirement.
As preferably, in step 1, the solution of metal ion and alkaline solution use spray mode or dipping method successively
Act on matrix.
In step 1, matrix uses the solution of metal ion and alkaline solution to carry out spraying or impregnation process successively, makes base
Body and solution can be uniformly in contact with, and alkaline solution and the metal ion generation chemical reaction of absorption on matrix generate insoluble
Precipitate metal hydroxides is attached on matrix.
The solution of metal ion and alkaline solution use spray or impregnation method to act on successively on matrix, it is simple to realize
Continuous prodution.For ensureing absorption and the reaction effect of matrix and solution, spray and be advisable being impregnated with matrix, be i.e. metal ion
Solution and alkaline solution be required for spray or dipping be fully wet out to matrix.
The solution of described metal ion and alkaline solution all make solvent with water, and described alkaline solution is sodium hydroxide water
At least one in solution, potassium hydroxide aqueous solution, ammonia.
As preferably, the concentration of described alkaline solution is 0.01mol/L~10mol/L.Further preferably, described alkalescence is molten
The concentration of liquid is 0.1mol/L~8mol/L.Further preferably, the concentration of described alkaline solution is 1mol/L~6mol/L.
As preferably, the solution of metal ion is 5s-10min to the process time of matrix, and alkaline solution is to matrix
The process time is 5s-10min.Further preferably, the solution of metal ion is 5s-5min to the spray time of matrix, alkalescence
Solution is 5s-5min to the spray time of matrix.Further preferably, the solution of metal ion is 5s-to the spray time of matrix
1min, alkaline solution is 5s-1min to the spray time of matrix.
Step 2 is selected reducibility gas the metal hydroxide particle obtained in step 1 is reduced to metal nano
Grain, as preferably, containing noble gas in described reducibility gas, the volume fraction of noble gas is 0%~90%.Further
Preferably, described reducibility gas is the gaseous mixture of hydrogen, carbon monoxide or hydrogen and noble gas.Further preferably, described reproducibility
Gas be hydrogen, hydrogen and the gaseous mixture of argon, carbon monoxide and the gaseous mixture of argon, the gaseous mixture of carbon monoxide and helium,
Or the gaseous mixture of hydrogen and helium.
The each step of the present invention the most at room temperature operates, it is preferable that in step 2, uses dielectric barrier discharge low-temperature etc.
Gas ions, radio-frequency glow discharge plasmas or glow discharge cold plasma, applying voltage is 1-40kV, and power is 10-
500W。
Further preferably, in step 2, using the method for dielectric barrier discharge to produce low temperature plasma, applying voltage is
10-40kV, power is 10-200W.Further preferably, in step 2, the method for dielectric barrier discharge is used to produce low temperature plasma,
Applying voltage is 20-30kV, and power is 10-100W.
When step 2 using medium blocking-discharge method produce low temperature plasma, with reducibility gas as plasma
Atmosphere.
As preferably, in step 2, the time that cold plasma discharge processes is 10s-10min.Further preferably, step 2
In, the time that cold plasma discharge processes is 10s-5min.Further preferably, in step 3, the time that cold plasma discharge processes
For 10s-1min.
Beneficial effects of the present invention is as follows:
(1) preparation method is simple, low raw-material cost, and whole preparation process is carried out in air atmosphere, equipment needed thereby letter
Single, it is not necessary to special device;
(2) combine the method for lower temperature plasma technology by hydro-thermal to prepare there is the nanometer gold of catalysis, antibacterial activity
Belong to composite, efficient pollution-free, environmental friendliness;
(3) the load type gold metal nano-particle utilizing low-temperature plasma body method to prepare can be used as catalyst, it is possible to notable
Improve the transformation efficiency of reaction.
Accompanying drawing explanation
Fig. 1 is the device schematic diagram that each embodiment uses;
Fig. 2 is the transmission electron microscope picture of the matrix in the embodiment of the present invention 1 after loading nano silvery granule;
Fig. 3 is the XRD of loaded nano platinum grain in loaded nano Argent grain and embodiment 2 in the embodiment of the present invention 1
Collection of illustrative plates;
Fig. 4 is urging after loaded nano platinum grain platinum in loading nano silvery granule and embodiment 2 in the embodiment of the present invention 1
Change design sketch;
Fig. 5 is the scanning electron microscope (SEM) photograph in the embodiment of the present invention 3 after loading nano silvery granule;
Fig. 6 is the bactericidal effect schematic diagram of the embodiment of the present invention 3.
Detailed description of the invention
Device schematic diagram that each embodiment is used as it is shown in figure 1, include the transporter 5 for moving matrix 1 and
It is in the sprinkling equipment 2 of the metal ion solution that successively matrix is carried out above transporter 5 respective handling, alkaline solution
Sprinkling equipment 3 and discharge of plasma in low temperature processing equipment 4.
During work, selected matrix 1 is placed on transporter 5 (such as conveyer belt), is continuously traveling, at predetermined station
On, sequentially pass through the sprinkling equipment 2 of metal ion solution, the sprinkling equipment 3 of alkaline solution and discharge of plasma in low temperature
Processing equipment 4, finally obtains load type gold metal nano-particle on matrix.
Embodiment 1
(1) TiO is selected2Nanometer rods, as matrix, uses Ag-containing solution to TiO2Nanometer rods sprays, and spray time is
5s, the silver nitrate (AgNO that Ag-containing solution uses concentration to be 20g/L3) solution.
Use potassium hydroxide aqueous solution to through Cu (NO3)2TiO after solution process2Nanometer rods sprays, during spray
Between be 5s, potassium hydroxide aqueous solution concentration 10mol/L of employing.
(2) by the TiO through above-mentioned process2Nanometer rods carries out Low Temperature Plasma Treating, and reducibility gas uses hydrogen
With the mixed gas of argon, wherein the volume fraction of hydrogen is 10%.Low temperature plasma uses dielectric barrier discharge to produce, and executes
Making alive is 25kV, and power is 100W, and the whole Low Temperature Plasma Treating time is 10min.
Through the process of step (1), at substrate deposit silver hydroxide granule, in step (2), silver hydroxide granule with
Hydrogen reacts, and final acquisition is loaded with the TiO of nano-Ag particles2Catalyst, transmission electron microscope picture is as shown in Figure 2.
Take the TiO being loaded with nano-Ag particles prepared by 1g the present embodiment2Catalyst, puts in the reaction vessel of 4L,
It is passed through CO2And H2In the case of O, carrying out light-catalyzed reaction, result is as shown in Figure 4.
Embodiment 2
(1) TiO is selected2As matrix, use platiniferous solution to TiO2Nanometer rods impregnates, and the time is 10s, and platiniferous is molten
Platinum chloride (the PtCl that liquid uses concentration to be 15g/L2) solution.
Use sodium hydrate aqueous solution to through PtCl2TiO after solution process2Spraying, spray time is 10s, adopts
Sodium hydrate aqueous solution concentration 8mol/L.
(2) by the TiO through above-mentioned process2Carry out Low Temperature Plasma Treating, reducibility gas use carbon monoxide with
The mixed gas of argon, wherein the volume fraction of carbon monoxide is 20%.Low temperature plasma uses radio-frequency discharge to produce, and applies
Voltage is 30kV, and power is 300W, and the whole Low Temperature Plasma Treating time is 5min.
Through the process of step (1), at substrate deposit platinic hydroxide granule, in step (2), platinic hydroxide granule with
Hydrogen reacts, and final acquisition is loaded with the TiO of nano-platinum particle2Catalyst, its XRD figure is as shown in Figure 3.
Take the TiO being loaded with nano-platinum particle prepared by 1g the present embodiment2Catalyst, puts in the reaction vessel of 4L,
It is passed through CO2And H2In the case of O, carrying out light-catalyzed reaction, result is as shown in Figure 4.
Embodiment 3
(1) the acrylon material cloth (acrylon cloth) selecting thickness to be 2mm is as matrix, uses Ag-containing solution to enter acrylon cloth
Row dipping, dip time is 30s, the silver nitrate (AgNO that Ag-containing solution uses concentration to be 10g/L3) solution.
Use potassium hydroxide aqueous solution to through AgNO3Acrylon cloth after solution processes impregnates, and the time is 30s, directly
To acrylon cloth by potassium hydroxide aqueous solution thorough impregnation, potassium hydroxide aqueous solution concentration 6mol/L of employing.
(2) the acrylon cloth through above-mentioned process carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and argon
The mixed gas of gas, wherein the volume fraction of hydrogen is 40%.Low temperature plasma uses glow discharge to produce, and applies voltage and is
15kV, power is 50W, and the whole Low Temperature Plasma Treating time is 3min.
Through the process of step (1), at substrate deposit silver hydroxide granule, in step (2), silver hydroxide granule with
Hydrogen reacts, and final obtains the acrylon cloth being loaded with nano-Ag particles, and scanning electron microscope (SEM) photograph is as it is shown in figure 5, the grain of nano-Ag particles
Footpath scope is 2nm-10nm, and the nano-Ag particles in this particle size range has the strongest bactericidal effect, and effect is as shown in Figure 6.
1,2, No. 3 samples are the samples having loaded nano-Ag particles, and 4, No. 5 is the matched group of unsupported nano-Ag particles, and result shows
1-3 sample occurs in that obvious antibacterial ring, and 4, No. 5 antibacterial ring do not occur.
Embodiment 4
(1) TiO is selected2Nanometer rods, as matrix, uses copper-containing solution to TiO2Nanometer rods sprays, and spray time is
5s, the copper nitrate (Cu (NO that copper-containing solution uses concentration to be 20g/L3)2) solution.
Use potassium hydroxide aqueous solution to through Cu (NO3)2TiO after solution process2Nanometer rods sprays, during spray
Between be 5s, potassium hydroxide aqueous solution concentration 10mol/L of employing.
(2) by the TiO through above-mentioned process2Nanometer rods carries out Low Temperature Plasma Treating, and reducibility gas uses hydrogen
With the mixed gas of argon, wherein the volume fraction of hydrogen is 10%.Low temperature plasma uses dielectric barrier discharge to produce, and executes
Making alive is 25kV, and power is 100W, and the whole Low Temperature Plasma Treating time is 10min.
Through the process of step (1), at substrate deposit Copper hydrate granule, in step (2), Copper hydrate granule with
Hydrogen reacts, and final acquisition is loaded with the TiO of nano copper particle2Catalyst, transmission electron microscope picture is as shown in Figure 2.
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to metallographic specific catalytic activity and improve 31%.
Embodiment 5
(1) SiO is selected2As matrix, use palladium-containing solution to SiO2Spraying, spray time is 1min, palladium-containing solution
Palladous chloride. (the PdCl using concentration to be 5g/L2) solution.
Use sodium hydrate aqueous solution to through PdCl2SiO after solution process2Spraying, spray time is 1min,
Sodium hydrate aqueous solution concentration 4mol/L used.
(2) by the SiO through above-mentioned process2Carry out Low Temperature Plasma Treating, reducibility gas use carbon monoxide with
The gaseous mixture of helium, the volume fraction of carbon monoxide is 50%.Low temperature plasma uses dielectric barrier discharge to produce, and applies electricity
Pressure is 40kV, and power is 10W, and the whole Low Temperature Plasma Treating time is 1min.Final acquisition is loaded with nanoparticle palladium
SiO2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 170 DEG C
Turn to carbon dioxide.
Embodiment 6
(1) Fe is selected2O3As matrix, use gold-containing solution to Fe2O3Impregnating, the time is 5min, and gold-containing solution is adopted
With the gold chloride (HAuCl that concentration is 2g/L4) solution.
Use ammonia to through HAuCl4Fe after solution process2O3Impregnating, dip time is 5min, until Fe2O3
By ammonia thorough impregnation, the ammonia concn 2mol/L of employing.
(2) by the Fe through above-mentioned process2O3Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and helium
Mixed gas, wherein the volume fraction of hydrogen is 60%.Low temperature plasma uses radio-frequency discharge to produce, and applies voltage and is
10kV, power is 20W, and the whole Low Temperature Plasma Treating time is 30s.Final acquisition is loaded with the Fe of nanogold particle2O3。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to metallographic specific catalytic activity and improve 36%.
Embodiment 7
(1) TiO is selected2As matrix, use rhodium-containing solution to TiO2Spraying, spray time is 8min, rhodium-containing solution
Radium chloride (the RhCl using concentration to be 1g/L3) solution.
Use sodium hydrate aqueous solution to through RhCl3TiO after solution process2Spraying, spray time is 8min,
Sodium hydrate aqueous solution concentration 1mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and argon
Mixed gas, wherein the volume fraction of hydrogen is 70%.Low temperature plasma uses glow discharge to produce, and applies voltage and is
40kV, power is 10W, and the whole Low Temperature Plasma Treating time is 20s.Final acquisition is loaded with the TiO of nanometer rhodium granule2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to rhodium phase specific catalytic activity and improve 41%.
Embodiment 8
(1) TiO is selected2As matrix, use containing ruthenium solution TiO2Spraying, spray time is 5min, containing ruthenium solution
Ruthenic chloride (the RuCl using concentration to be 0.5g/L3) solution.
Use ammonia to through RuCl3TiO after solution process2Spraying, spray time is 5min, the ammonia of employing
Concentration 0.1mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen.Low temperature etc.
Gas ions uses dielectric barrier discharge to produce, and applying voltage is 20kV, and power is 30W, the whole Low Temperature Plasma Treating time
For 10s.Final acquisition is loaded with the TiO of nanometer ruthenium granule2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to ruthenium phase specific catalytic activity and improve 27%.
Embodiment 9
(1) TiO is selected2As matrix, use iron-containing liquor to TiO2Spraying, spray time is 5min, iron-containing liquor
Iron chloride (the FeCl using concentration to be 0.1g/L3) aqueous solution.
Use sodium hydrate aqueous solution to through FeCl3TiO after solution process2Spraying, spray time is 5min,
Sodium hydrate aqueous solution concentration 0.05mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and argon
Mixed gas, wherein the volume fraction of hydrogen is 80%.Low temperature plasma uses radio-frequency discharge to produce, and applies voltage and is
20kV, power is 150W, and the whole Low Temperature Plasma Treating time is 15s.Final acquisition is loaded with the TiO of nano iron particles2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to ferrum phase specific catalytic activity and improve 25%.
Embodiment 10
(1) TiO is selected2As matrix, use cobalt-carrying solution to TiO2Spraying, spray time is 5min, cobalt-carrying solution
Cobaltous chloride (the CoCl using concentration to be 0.05g/L2) aqueous solution.
Use potassium hydroxide aqueous solution to through CoCl2TiO after solution process2Impregnating, the time is 5min, uses
Potassium hydroxide aqueous solution concentration 0.01mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and argon
Mixed gas, wherein the volume fraction of hydrogen is 90%.Low temperature plasma uses dielectric barrier discharge to produce, and applies voltage
For 30kV, power is 180W, and the whole Low Temperature Plasma Treating time is 18s.Final acquisition is loaded with nano cobalt granule
TiO2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 155 DEG C
Turn to carbon dioxide.
Embodiment 11
(1) TiO is selected2As matrix, use containing aluminum solutions TiO2Spraying, spray time is 5min, containing aluminum solutions
Aluminum chloride (the AlCl using concentration to be 0.01g/L3) solution.
Use sodium hydrate aqueous solution to through AlCl3TiO after solution process2Spraying, spray time is 5min,
Sodium hydrate aqueous solution concentration 10mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and helium
Mixed gas, wherein the volume fraction of hydrogen is 20%.Low temperature plasma uses dielectric barrier discharge to produce, and applies voltage
For 40kV, power is 220W, and the whole Low Temperature Plasma Treating time is 20s.Final acquisition is loaded with nano aluminum granule
TiO2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to aluminum phase specific catalytic activity and improve 27%.
Embodiment 12
(1) TiO is selected2As matrix, use the solution containing zinc and chromium to TiO2Spraying, spray time is 5min, contains
Zinc chloride (the ZnCl that the solution of zinc and chromium uses concentration to be 0.01g/L2) solution and the Chlorizate chromium (CrCl of 0.01g/L3) solution.
Use potassium hydroxide aqueous solution to through ZnCl2Solution and CrCl3TiO after solution process2Impregnate, the time
For 5min, potassium hydroxide aqueous solution concentration 0.01mol/L of employing.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and helium
Mixed gas, wherein the volume fraction of hydrogen is 45%.Low temperature plasma uses radio-frequency discharge to produce, and applies voltage and is
30kV, power is 210W, and the whole Low Temperature Plasma Treating time is 1min.Final acquisition is loaded with Nano-Zinc and nanometer chromium
The TiO of grain2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported phase
Specific catalytic activity improves 48%.
Embodiment 13
(1) TiO is selected2As matrix, use chromium-containing solution to TiO2Impregnating, the time is 6s, and chromium-containing solution uses dense
Degree is the Chlorizate chromium (CrCl of 20g/L3) solution.
Use sodium hydrate aqueous solution to through CrCl3TiO after solution process2Impregnating, the time is 6s, employing
Sodium hydrate aqueous solution concentration 10mol/L.
(2) by the TiO through above-mentioned process2Carry out Low Temperature Plasma Treating, reducibility gas use carbon monoxide with
The mixed gas of helium, wherein the volume fraction of carbon monoxide is 20%.Low temperature plasma uses glow discharge to produce, and applies
Voltage is 20kV, and power is 230W, and the whole Low Temperature Plasma Treating time is 40s.Final acquisition is loaded with nanometer chromium granule
TiO2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 165 DEG C
Turn to carbon dioxide.
Embodiment 14
(1) select ZnO as matrix, use titaniferous solution to TiO2Spraying, spray time is 11s, titaniferous solution
Titanium chloride (the TiCl using concentration to be 15g/L4) solution.
Use potassium hydroxide aqueous solution to through TiCl4TiO after solution process2Spraying, spray time is 11s, adopts
Concentration 9mol/L of potassium hydroxide aqueous solution.
(2) ZnO through above-mentioned process is carried out Low Temperature Plasma Treating, use the gaseous mixture of carbon monoxide and helium
Body, wherein the volume fraction of carbon monoxide is 80%.Low temperature plasma uses dielectric barrier discharge to produce, and applies voltage and is
10kV, power is 250W, and the whole Low Temperature Plasma Treating time is 2min.Final acquisition is loaded with the ZnO of nano-titanium granule.
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 165 DEG C
Turn to carbon dioxide.
Embodiment 15
(1) TiO is selected2As matrix, use the solution Han cerium to TiO2Impregnating, the time is 31s, uses containing cerium solution
Concentration is the cerium chloride (CeCl of 10g/L2) solution.
Use potassium hydroxide aqueous solution to through CeCl2TiO after solution process2Spraying, spray time is 31s, adopts
Potassium hydroxide aqueous solution concentration 7mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 20%.Low temperature plasma uses glow discharge to produce, and applying voltage is 8kV, power
For 430W, the whole Low Temperature Plasma Treating time is 50s.Final acquisition is loaded with the TiO of nano cerium granule2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to cerium phase specific catalytic activity and improve 39%.
Embodiment 16
(1) TiO is selected2As matrix, use tungstenic solution to TiO2Spraying, spray time is 1min, tungstenic solution
Tungsten chloride (the WCl using concentration to be 5g/L6) solution.
Use potassium hydroxide aqueous solution to through WCl6TiO after solution process2Spraying, spray time is 1min, adopts
Potassium hydroxide aqueous solution concentration 5mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 30%.Low temperature plasma uses dielectric barrier discharge to produce, and applying voltage is 5kV,
Power is 110W, and the whole Low Temperature Plasma Treating time is 7min.Final acquisition is loaded with the TiO of nanometer tungsten particle2。
Using photo catalytic reduction device to test its photocatalysis performance identical with embodiment 1, result shows than unsupported gold
Belong to tungsten phase specific catalytic activity and improve 32%.
Embodiment 17
(1) TiO is selected2As matrix, use containing zirconium solution TiO2Spraying, spray time is 2min, containing zirconium solution
Zirconium chloride (the ZrCl using concentration to be 2g/L4) solution.
Use sodium hydrate aqueous solution to through ZrCl4TiO after solution process2Spraying, spray time is 2min,
Sodium hydrate aqueous solution concentration 3mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 80%.Low temperature plasma uses glow discharge to produce, and applying voltage is 7kV, power
For 160W, the whole Low Temperature Plasma Treating time is 5min.Final acquisition is loaded with the TiO of nanometer zirconium granule2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 120 DEG C
Turn to carbon dioxide.
Embodiment 18
(1) TiO is selected2As matrix, use containing lead solution TiO2Spraying, spray time is 3min, containing lead solution
Lead chloride (the PbCl using concentration to be 1g/L2) solution.
Use sodium hydrate aqueous solution to through PbCl2TiO after solution process2Spraying, spray time is 3min,
Sodium hydrate aqueous solution concentration 2mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 70%.Low temperature plasma uses dielectric barrier discharge to produce, and applies voltage and is
10kV, power is 480W, and the whole Low Temperature Plasma Treating time is 9min.Final acquisition is loaded with nanometer lead granule
TiO2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 130 DEG C
Turn to carbon dioxide.
Embodiment 19
(1) TiO is selected2As matrix, use cadmium-containing solution to TiO2Spraying, spray time is 5min, cadmium-containing solution
Caddy (Cleary) (the CdCl using concentration to be 0.5g/L2) solution.
Use potassium hydroxide aqueous solution to through CdCl2TiO after solution process2Impregnating, the time is 5min, uses
Potassium hydroxide aqueous solution concentration 1mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 91%.Low temperature plasma uses radio-frequency discharge to produce, and applying voltage is 15kV, merit
Rate is 340W, and the whole Low Temperature Plasma Treating time is 6min.Final acquisition is loaded with the TiO of nanometer cadmium granule2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 140 DEG C
Turn to carbon dioxide.
Embodiment 20
(1) TiO is selected2As matrix, use manganese containing solution to TiO2Impregnating, the time is 6min, and manganese containing solution uses
Concentration is the manganese chloride (MnCl of 0.1g/L2) solution.
Use potassium hydroxide aqueous solution to through MnCl2TiO after solution process2Impregnating, the time is 6min, uses
Potassium hydroxide aqueous solution concentration 0.3mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses carbon monoxide.Low
Isothermal plasma uses glow discharge to produce, and applying voltage is 18kV, and power is 370W, the whole Low Temperature Plasma Treating time
For 8min.Final acquisition is loaded with the TiO of nanostructured manganese granule2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 170 DEG C
Turn to carbon dioxide.
Embodiment 21
(1) TiO is selected2As matrix, use containing molybdenum solution TiO2Spraying, spray time is 8min, containing molybdenum solution
Molybdenum chloride (the MoCl using concentration to be 0.05g/L5) solution.
Use sodium hydrate aqueous solution to through MoCl5TiO after solution process2Spraying, spray time is 8min,
Sodium hydrate aqueous solution concentration 0.1mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 10%.Low temperature plasma uses radio-frequency discharge to produce, and applying voltage is 25kV, merit
Rate is 50W, and the whole Low Temperature Plasma Treating time is 6min.Final acquisition is loaded with the TiO of nanometer molybdenum granule2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 140 DEG C
Turn to carbon dioxide.
Embodiment 22
(1) TiO is selected2As matrix, use containing vanadium solution TiO2Spraying, spray time is 10min, molten containing vanadium
Ammonium metavanadate (the NH that liquid uses concentration to be 0.01g/L4VO3) solution.
Use sodium hydrate aqueous solution to through NH4VO3TiO after solution process2Impregnating, the time is 9min, uses
Sodium hydrate aqueous solution concentration 0.01mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses nitrogen and hot ammonia
The gaseous mixture of gas, wherein nitrogen ratios is 67%.Low temperature plasma uses dielectric barrier discharge to produce, and applies voltage and is
35kV, power is 170W, and the whole Low Temperature Plasma Treating time is 10s.Final acquisition is loaded with the TiO of nano V granule2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 110 DEG C
Turn to carbon dioxide.
Embodiment 23
(1) TiO is selected2As matrix, use the solution Han lanthanum to TiO2Impregnating, the time is 15s, uses containing lanthanum solution
Concentration is the lanthanum chloride (LaCl of 16g/L3) solution.
Use potassium hydroxide aqueous solution to through LaCl3TiO after solution process2Spraying, spray time is 15s, adopts
Potassium hydroxide aqueous solution concentration 8mol/L.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen.Low temperature etc.
Gas ions uses radio-frequency discharge to produce, and applying voltage is 16kV, and power is 210W, and the whole Low Temperature Plasma Treating time is
1min.Final acquisition is loaded with the TiO of nanometer lanthanum granule2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 170 DEG C
Turn to carbon dioxide.
Embodiment 24
(1) TiO is selected2As matrix, use solution containing nickel to TiO2Spraying, spray time is 5min, solution containing nickel
Nickel dichloride. (the NiCl using concentration to be 0.1g/L2) aqueous solution.
Use sodium hydrate aqueous solution to through NiCl2TiO after solution process2Spraying, spray time is 5min,
Sodium hydrate aqueous solution concentration 0.05mol/L used.
(2) by the TiO through above-mentioned process2Carrying out Low Temperature Plasma Treating, reducibility gas uses hydrogen and argon
Mixed gas, wherein the volume fraction of hydrogen is 80%.Low temperature plasma uses radio-frequency discharge to produce, and applies voltage and is
18kV, power is 450W, and the whole Low Temperature Plasma Treating time is 27s.Final acquisition is loaded with the TiO of nano nickle granules2。
Take this sample of 0.1g, put in the reaction tube that internal diameter is 6mm, be passed through the CO calibrating gas (CO:O of 20mL/min2: N2
=1:20:79), carry out CO oxidation activity test.Result shows, this sample can be by complete for carbon monoxide oxygen under the conditions of 135 DEG C
Turn to carbon dioxide.
Solution in each embodiment, without particular determination, all uses water to make solvent.
Claims (7)
1. the method preparing load type gold metal nano-particle, it is characterised in that including:
Step 1, matrix solution and alkaline solution by metal ion successively processes;
Step 2, the matrix after utilizing reducibility gas to process step 1 carries out discharge of plasma in low temperature process, obtains described
Load type gold metal nano-particle.
The method preparing load type gold metal nano-particle the most as claimed in claim 1, it is characterised in that described metal be Ag,
Simple substance in Cu, Pt, Au, Pd, Ni, Ru, Rh, Fe, Co, Al, Zn, Cr, Ti, Ce, W, Zr, Pb, Cd, Mn, Mo, Nb, V, La or
Alloy.
The method preparing load type gold metal nano-particle the most as claimed in claim 1, it is characterised in that metal ion in solution
Concentration is 0.01g/L~20g/L.
The method preparing load type gold metal nano-particle the most as claimed in claim 1, it is characterised in that in step 1, containing metal from
The solution of son and alkaline solution use spray mode or dipping method to act on successively on matrix.
The method preparing load type gold metal nano-particle the most as claimed in claim 1, it is characterised in that the solution of metal ion
The process time to matrix is 5s-10min, and alkaline solution is 5s-10min to the process time of matrix.
The method preparing load type gold metal nano-particle the most as claimed in claim 1, it is characterised in that step 2, uses medium resistance
Gear discharge low-temperature plasma, radio-frequency glow discharge plasmas or glow discharge cold plasma, applying voltage is 1-50kV,
Power is 10-500W.
The method preparing load type gold metal nano-particle the most as claimed in claim 1, it is characterised in that in step 2, low temperature etc. from
The time that electron discharge processes is 10s-10min.
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CN113318795A (en) * | 2021-06-24 | 2021-08-31 | 大连海事大学 | Device and method for preparing liquid metal catalyst by using plasma |
CN113318795B (en) * | 2021-06-24 | 2023-07-14 | 大连海事大学 | Device and method for preparing liquid metal catalyst by using plasma |
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