CN107224983A - A kind of Ag/Cu2O/CeO2One pot of solid phase reaction preparation method of ternary nano compound - Google Patents
A kind of Ag/Cu2O/CeO2One pot of solid phase reaction preparation method of ternary nano compound Download PDFInfo
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- CN107224983A CN107224983A CN201710661477.8A CN201710661477A CN107224983A CN 107224983 A CN107224983 A CN 107224983A CN 201710661477 A CN201710661477 A CN 201710661477A CN 107224983 A CN107224983 A CN 107224983A
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000003746 solid phase reaction Methods 0.000 title claims abstract description 24
- 150000001875 compounds Chemical class 0.000 title description 14
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 77
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 239000002114 nanocomposite Substances 0.000 claims abstract description 16
- 238000005580 one pot reaction Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 150000000703 Cerium Chemical class 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 7
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 239000010949 copper Substances 0.000 claims description 39
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver nitrate Substances [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 30
- 235000013339 cereals Nutrition 0.000 claims description 16
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 14
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical group O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000012153 distilled water Substances 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims description 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 150000001879 copper Chemical class 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000007790 solid phase Substances 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 17
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 16
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 description 15
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 229910052684 Cerium Inorganic materials 0.000 description 7
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 7
- 150000004677 hydrates Chemical class 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CQPFMGBJSMSXLP-ZAGWXBKKSA-M Acid orange 7 Chemical compound OC1=C(C2=CC=CC=C2C=C1)/N=N/C1=CC=C(C=C1)S(=O)(=O)[O-].[Na+] CQPFMGBJSMSXLP-ZAGWXBKKSA-M 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- 239000003638 chemical reducing agent 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
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002023 wood Substances 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/894—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of Ag/Cu2O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, Solid raw materials silver salt, mantoquita, cerium salt is mixed in molar ratio with alkali, ball milling solid phase reaction, products therefrom washing, is prepared after centrifuging and drying.The present invention is using solid mixing, and raw material room temperature solid-phase ball milling reaction, preparation process is simple, it is easy to controls and can largely reduce the reunion of product particles；Avoid using reductant-oxidant, template and solvent, improve product purity, meet the requirement that material green is combined to, be also suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of Ag/Cu2O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, belongs to
Nano composite material preparing technical field.
Background technology
Cu2O/CeO2Composite is a kind of quite varied functional material of purposes, is had in fields such as catalysis, electrode materials
Important application.Wherein, Cu2O/CeO2Compound shows stronger visible absorption ability and light is urged as photochemical catalyst
Change activity, be a kind of outstanding visible-light photocatalysis material.
At present, Cu2O/CeO2The preparation method of composite is mainly liquid phase reactor method.
Such as：Using glucose as reducing agent, Cu is prepared by soaking and reducing method2O/CeO2Heterojunction photocatalyst
（Shichao Hu, et. al. Preparation of Cu2O/CeO2 heterojunction photocatalyst for
The degradation of Acid Orange 7 under visible light irradiation, Catalysis
Communications, 2011,12:794–797）；
With cube and octahedron Cu2O prepares Cu as template is sacrificed by template auxiliary law2O/CeO2Nano-complex
（Huizhi Bao, et. al. Compositions, structures, and catalytic activities of
CeO2@Cu2O nanocomposites prepared by the template-assisted method, Langmuir, 30
(22):6427–6436）；
Caught up with by Argon Bubble gas pre-treatment except the oxygen in reaction medium, with Ce (OH) in alkaline solution3For template, oxygen is utilized
Change the Cu that core shell structure is prepared in reduction assembling2O/CeO2Nanocube（Xiao Wang, et. al. Clean
synthesis of Cu2O@CeO2Core@shell nanocubes with highly active interface, NPG
Asia Materials, 2015,7 (1):7-19）；
With cube and octahedron Cu2O prepares Cu as template is sacrificed by template auxiliary law2O/CeO2Nano-complex,
Subsequent amination Cu2O/CeO2Obtain Cu2O/CeO2-NH2Compound, then pass through reduction of sodium citrate AuCl4 -Ion obtains Au and received
Rice corpuscles, passes through Au nano-particles and-NH2Between build stable chemical bond and obtain Cu2O@CeO2- Au nano-complexes
（Faying Li, et. al. Ultrasensitive amperometric immunosensor for PSA
detection based on Cu2O@CeO2-Au nanocomposites as integrated triple signal
Amplification strategy, Biosensors and Bioelectronics, 2017,87:630–637）.
Although a variety of preparation methods can prepare Cu disclosed in prior art2O/CeO2Composite, can also use above-mentioned side
Method is produced such as Au/Cu2O/CeO2A large amount of solvents are needed to use in ternary complex, but Shortcomings, liquid phase method preparation process,
In preparation process, the need for having using reductant-oxidant, have the need for using template, have the need for use inert gas before
Processing, particularly the chemical reaction in solution is also increasingly complex, while ultra-fine product particles be easier occur reunite, it is necessary to after
Continuous further investigation.
The content of the invention
For above-mentioned technical problem underlying, it is an object of the invention to provide one kind without using solvent, also without
Need to add reductant-oxidant or template, process be simple and convenient to operate, the Ag/Cu of environmental protection2O/CeO2Ternary nano is combined
One pot of solid phase reaction preparation method of material.
To achieve the above object, the technological means taken of the present invention is：A kind of Ag/Cu2O/CeO2Ternary nano composite wood
Expect one pot of solid phase reaction preparation method, Solid raw materials silver salt, mantoquita, cerium salt mixed in molar ratio with alkali, ball milling solid phase reaction,
Products therefrom is washed, and is prepared after centrifuging and drying.
Further, in preparation process, product Ag/ is controlled by the mol ratio for adjusting Ball-milling Time and silver nitrate
Cu2O/CeO2Cu in ternary nano compound2O and CeO2Average grain size and Ag load capacity and its average crystal grain chi
It is very little.
Further, the silver salt, mantoquita, cerium salt and alkali are well mixed for x: 1-x: 1: 8 in molar ratio, wherein x=0~
0.2, but x is not equal to 0.
Further, the silver salt is silver nitrate.
Further, the mantoquita is cupric salt.
Further, the cupric salt is Gerhardite, Salzburg vitriol, the one of Copper dichloride dihydrate
Kind.
Further, the cerium salt is Ce (NO3)3·6H2O。
Further, the alkali is sodium hydroxide.
Further, the ball milling solid phase reaction refers to：It is put into ball milling zirconium tank, is placed in ball mill after raw material mixing,
The rpm/min of setting speed 480, ball-milling reaction 1~5 hour.
Further, the product is washed with distilled water, is centrifuged and true under 60 DEG C and 0.1Mpa vacuums
Sky is dried 2 hours.
The beneficial effects of the present invention are：Mixed using solid, raw material room temperature solid-phase ball milling reaction, preparation process is simple,
Reunion that is easily controllable and can largely reducing product particles；Avoid using reductant-oxidant, template and solvent, improve product
Purity, meets the requirement that material green is combined to, and is also suitable for large-scale production.
Brief description of the drawings
The present invention is further elaborated with embodiment below in conjunction with the accompanying drawings.
Fig. 1 is Ag/Cu prepared by the embodiment of the present invention 1,2,3,4 and 52O/CeO2Ternary nano compound XRD spectrum；
Fig. 2 is Ag/Cu prepared by the embodiment of the present invention 2,6,7 and 82O/CeO2Ternary nano compound XRD spectrum.
Embodiment
Embodiment 1
According to 0.05: 0.95: 1: 8 mol ratio weigh 0.0005 mole of analytically pure silver nitrate, 0.0095 mole it is analytically pure
Gerhardite, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide add and are equipped with 50
In the 50ml zirconia ball grinding jars of individual diameter 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls, in QM-3SP04 planets
In continuously grinding 1 hour under 480 rpm in formula high energy ball mill, product is washed with distilled water, centrifuged and 60
DEG C and 0.1Mpa vacuums under be dried in vacuo 2 hours, obtain Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Cu in ternary nano compound2O and CeO2Average grain size is respectively 9.6 nm and 13.2 nm.
Embodiment 2
According to 0.05: 0.95: 1: 8 mol ratio weigh 0.0005 mole of analytically pure silver nitrate, 0.0095 mole it is analytically pure
Gerhardite, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide add and are equipped with 50
In the 50ml zirconia ball grinding jars of individual diameter 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls, in QM-3SP04 planets
In continuously grinding 2 hours under 480 rpm in formula high energy ball mill, product is washed with distilled water, centrifuged and 60
DEG C and 0.1Mpa vacuums under be dried in vacuo 2 hours, obtain Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Cu in ternary nano compound2O and CeO2Average grain size is respectively 11.4 nm and 14.9 nm.
Embodiment 3
According to 0.05: 0.95: 1: 8 mol ratio weigh 0.0005 mole of analytically pure silver nitrate, 0.0095 mole it is analytically pure
Gerhardite, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide add and are equipped with 50
In the 50ml zirconia ball grinding jars of individual diameter 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls, in QM-3SP04 planets
In continuously grinding 3 hours under 480 rpm in formula high energy ball mill, product is washed with distilled water, centrifuged and 60
DEG C and 0.1Mpa vacuums under be dried in vacuo 2 hours, obtain Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Cu in ternary nano compound2O and CeO2Average grain size is respectively 13.0 nm and 16.1 nm.
Embodiment 4
According to 0.05: 0.95: 1: 8 mol ratio weigh 0.0005 mole of analytically pure silver nitrate, 0.0095 mole it is analytically pure
Gerhardite, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide add and are equipped with 50
In the 50ml zirconia ball grinding jars of individual diameter 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls, in QM-3SP04 planets
In continuously grinding 4 hours under 480 rpm in formula high energy ball mill, product is washed with distilled water, centrifuged and 60
DEG C and 0.1Mpa vacuums under be dried in vacuo 2 hours, obtain Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Cu in ternary nano compound2O and CeO2Average grain size is respectively 14.5 nm and 17.4 nm.
Embodiment 5
According to 0.05: 0.95: 1: 8 mol ratio weigh 0.0005 mole of analytically pure silver nitrate, 0.0095 mole it is analytically pure
Gerhardite, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide add and are equipped with 50
In the 50ml zirconia ball grinding jars of individual diameter 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls, in QM-3SP04 planets
In continuously grinding 5 hours under 480 rpm in formula high energy ball mill, product is washed with distilled water, centrifuged and 60
DEG C and 0.1Mpa vacuums under be dried in vacuo 2 hours, obtain Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Cu in ternary nano compound2O and CeO2Average grain size is respectively 15.8 nm and 18.2 nm.
Embodiment 6
0.01 mole of analytically pure Gerhardite, 0.01 mole of analytically pure six hydration are weighed according to 1: 1: 8 mol ratio
Cerous nitrate, 0.08 mole of analytically pure sodium hydroxide, which are added, is equipped with 50 diameter 6mm zirconium oxide balls and 8 diameter 10mm oxidations
In the 50ml zirconia ball grinding jars of zirconium abrading-ball, in continuously grinding 2 under 480 rpm in QM-3SP04 planetary high-energy ball mills
Hour, product is washed with distilled water, centrifuges and is dried in vacuo 2 hours under 60 DEG C and 0.1Mpa vacuums, obtained
To Cu2O-2CeO2Nano-complex.
To Cu2O-2CeO2Product carries out XRD analysis, is calculated according to Scherrer formula, Cu2O-2CeO2Nanometer is multiple
Cu in compound2O and CeO2Average grain size is respectively 11.5 nm and 14.9 nm.
Embodiment 7
0.001 mole of analytically pure silver nitrate, 0.009 mole of analytically pure three water are weighed according to 0.1: 0.9: 1: 8 mol ratio
Copper nitrate, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide is closed to add and be equipped with 50 directly
In the 50ml zirconia ball grinding jars of footpath 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls, in the planetary height of QM-3SP04
In ball mill in continuously grinding 5 hours under 480 rpm, product can be washed with distilled water, centrifuge and 60 DEG C with
It is dried in vacuo 2 hours under 0.1Mpa vacuums, obtains Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Cu in ternary nano compound2O and CeO2Average grain size is respectively 11.3 nm and 14.9 nm.
Embodiment 8
According to 0.2: 0.8: 1: 8 mol ratio weigh 0.0015 mole of analytically pure silver nitrate, 0.0085 mole analytically pure three
Nitric hydrate copper, 0.01 mole of analytically pure six nitric hydrates cerium, 0.08 mole of analytically pure sodium hydroxide add and are equipped with 50
It is planetary in QM-3SP04 in the 50ml zirconia ball grinding jars of diameter 6mm zirconium oxide balls and 8 diameter 10mm zirconium oxide balls
In continuously grinding 5 hours under 480 rpm in high energy ball mill, product is washed with distilled water, centrifuged and at 60 DEG C
It is dried in vacuo 2 hours with 0.1Mpa vacuums, obtains Ag/Cu2O/CeO2Ternary nano compound.
To Ag/Cu2O/CeO2Ternary product carries out XRD analysis, is calculated according to Scherrer formula, Ag/Cu2O/
CeO2Ag, Cu in ternary nano compound2O and CeO2Average grain size is respectively 7.7 nm, 10.9 nm and 14.5 nm.
The X-ray diffraction analysis of above-described embodiment（XRD analysis）：Respectively by Ag/ made from embodiment 1,2,3,4 and 5
Cu2O/CeO2Ternary nano compound carries out XRD analysis, as a result sees Fig. 1.Calculated and obtained by Scherrer formula：Reaction raw materials nitre
Sour silver, Gerhardite, six nitric hydrate ceriums and sodium hydroxide are according to ball respectively after 0.05: 0.95: 1: 8 mixed in molar ratio
When grinding solid phase reaction 1h, 2h, 3h, 4h, 5h, products therefrom Ag/Cu2O/CeO2Cu in ternary nano compound2O and CeO2It is average
Crystallite dimension is respectively 9.6 nm, the nm of the nm of 11.4 nm, 13.0,14.5,15.8 and 13.2,14.9,16.1,17.4,18.2,
Show the change of ball milling solid phase reaction time to Ag/Cu2O/CeO2Cu in ternary nano compound2O and CeO2Average grain size
Size have certain influence, with the extension of ball milling solid phase reaction time, Ag/Cu2O/CeO2Cu in ternary nano compound2O and
CeO2Crystal grain is gradually being grown up.
Meanwhile, to Ag/Cu made from embodiment 2,6,7 and 82O/CeO2Ternary nano compound carries out XRD analysis, as a result
See Fig. 2.Same calculated by Scherrer formula obtains：When silver nitrate, Gerhardite, six nitric hydrate ceriums and sodium hydroxide
Mol ratio when bringing up to 0.2: 0.8: 1: 8 by 0: 1: 1: 8, products therefrom Ag/Cu2O/CeO2Cu in ternary nano compound2O
And CeO2Average grain size is respectively 11.5,11.4,11.3,10.9 nm and 14.9,14.9,14.9,14.8nm, show with
The raising of silver nitrate mol ratio, to Ag/Cu2O/CeO2Cu in ternary nano compound2O average crystal grain sizes reduce slightly, and
CeO2Average crystal grain size is almost unchanged, and rubbing when silver nitrate, Gerhardite, six nitric hydrate ceriums and sodium hydroxide
When you are than being 0.2: 0.8: 1: 8, calculated according to Scherrer formula, Ag/Cu2O/CeO2The average crystalline substances of Ag in ternary nano compound
Particle size is 7.7 nm.So, in preparation process, it can be controlled by suitably changing the mol ratio of Ball-milling Time and silver nitrate
Product Ag/Cu processed2O/CeO2Cu in ternary nano compound2O and CeO2Average grain size and Ag load capacity and its
Average grain size.
One of ordinary skill in the art will appreciate that：Various embodiments above is merely illustrative of the technical solution of the present invention, and
It is non-that it is limited；Although the present invention is described in detail with reference to foregoing embodiments, one of ordinary skill in the art
It should be understood that：It can still modify to the technical scheme described in foregoing embodiments, or to which part or
All technical characteristic carries out equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is departed from this hair
The scope of bright each embodiment technical scheme.
Claims (10)
1. a kind of Ag/Cu2O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, by Solid raw materials silver salt, copper
Salt, cerium salt are mixed in molar ratio with alkali, ball milling solid phase reaction, products therefrom washing, are prepared after centrifuging and drying.
2. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：In preparation process, product Ag/Cu is controlled by the mol ratio for adjusting Ball-milling Time and silver nitrate2O/CeO2Ternary is received
Cu in rice compound2O and CeO2Average grain size and Ag load capacity and its average grain size.
3. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The silver salt, mantoquita, cerium salt are well mixed for x: 1-x: 1: 8 in molar ratio with alkali, wherein x=0~0.2, but x
In 0.
4. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The silver salt is silver nitrate.
5. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The mantoquita is cupric salt.
6. Ag/Cu according to claim 52O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The cupric salt is Gerhardite, Salzburg vitriol, one kind of Copper dichloride dihydrate.
7. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The cerium salt is Ce (NO3)3·6H2O。
8. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The alkali is sodium hydroxide.
9. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, it is special
Levy and be：The ball milling solid phase reaction refers to：It is put into ball milling zirconium tank, is placed in ball mill, setting speed 480 after raw material mixing
Rpm/min, ball-milling reaction 1~5 hour.
10. Ag/Cu according to claim 12O/CeO2One pot of solid phase reaction preparation method of ternary nano composite material, its
It is characterised by：The product is washed with distilled water, is centrifuged and small with vacuum drying 2 under 0.1Mpa vacuums at 60 DEG C
When.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318689A (en) * | 2008-05-16 | 2008-12-10 | 深圳市危险废物处理站 | Method for preparing monoclinic system crystalline state cupric oxide and uses thereof |
| CN104001519A (en) * | 2014-06-12 | 2014-08-27 | 淮北师范大学 | Method for preparing Cu2O/Bi2O3 nanometer compound photocatalysts in indoor temperature solid-phase one-step mode |
-
2017
- 2017-08-04 CN CN201710661477.8A patent/CN107224983B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318689A (en) * | 2008-05-16 | 2008-12-10 | 深圳市危险废物处理站 | Method for preparing monoclinic system crystalline state cupric oxide and uses thereof |
| CN104001519A (en) * | 2014-06-12 | 2014-08-27 | 淮北师范大学 | Method for preparing Cu2O/Bi2O3 nanometer compound photocatalysts in indoor temperature solid-phase one-step mode |
Non-Patent Citations (2)
| Title |
|---|
| FAYING LI ET AL: ""Ultrasensitive amperometric immunosensor for PSA detection based on Cu2O@CeO2-Au nanocomposites as integrated triple signal amplification strategy"", 《BIOSENSORS AND BIOELECTRONICS》 * |
| 田俊杰: ""介孔氧化铈及其金属负载复合物的合成及性能研究"", 《中国优秀硕士学位论文全文数据库》 * |
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|---|---|---|---|---|
| CN108376742A (en) * | 2018-03-09 | 2018-08-07 | 湖南文理学院 | A kind of preparation method of cerium oxide base solar cell nanometer powder body material and application |
| CN108376742B (en) * | 2018-03-09 | 2021-12-07 | 湖南文理学院 | Preparation method and application of cerium oxide-based solar cell nano powder material |
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