CN109604625B - Method for preparing platinum-based binary alloy nanoparticles by using transition metal oxide and platinum metal nanoparticles as precursors - Google Patents
Method for preparing platinum-based binary alloy nanoparticles by using transition metal oxide and platinum metal nanoparticles as precursors Download PDFInfo
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 216
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 166
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 100
- 229910000314 transition metal oxide Inorganic materials 0.000 title claims abstract description 51
- 229910002056 binary alloy Inorganic materials 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002243 precursor Substances 0.000 title claims abstract description 18
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 15
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 26
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 120
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 60
- 229910052786 argon Inorganic materials 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000009210 therapy by ultrasound Methods 0.000 claims description 18
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 239000012798 spherical particle Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 150000003624 transition metals Chemical class 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- 229910052723 transition metal Inorganic materials 0.000 abstract description 5
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 27
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 11
- GUBSQCSIIDQXLB-UHFFFAOYSA-N cobalt platinum Chemical compound [Co].[Pt].[Pt].[Pt] GUBSQCSIIDQXLB-UHFFFAOYSA-N 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- OBACEDMBGYVZMP-UHFFFAOYSA-N iron platinum Chemical compound [Fe].[Fe].[Pt] OBACEDMBGYVZMP-UHFFFAOYSA-N 0.000 description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 229910001260 Pt alloy Inorganic materials 0.000 description 5
- 229910000428 cobalt oxide Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- IGOJMROYPFZEOR-UHFFFAOYSA-N manganese platinum Chemical compound [Mn].[Pt] IGOJMROYPFZEOR-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 150000001728 carbonyl compounds Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
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- 239000000696 magnetic material Substances 0.000 description 2
- 230000005298 paramagnetic effect Effects 0.000 description 2
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 description 1
- 229910018979 CoPt Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910005335 FePt Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical group [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- -1 amine iodide Chemical class 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 231100000481 chemical toxicant Toxicity 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- WBLJAACUUGHPMU-UHFFFAOYSA-N copper platinum Chemical compound [Cu].[Pt] WBLJAACUUGHPMU-UHFFFAOYSA-N 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
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PCLURTMBFDTLSK-UHFFFAOYSA-N nickel platinum Chemical compound [Ni].[Pt] PCLURTMBFDTLSK-UHFFFAOYSA-N 0.000 description 1
- SKJKDBIPDZJBPK-UHFFFAOYSA-N platinum zinc Chemical compound [Zn].[Pt] SKJKDBIPDZJBPK-UHFFFAOYSA-N 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/04—Alloys based on a platinum group metal
Abstract
A method for preparing platinum-based binary alloy nanoparticles by using transition metal oxides and platinum metal nanoparticles as precursors relates to a method for preparing platinum-based binary alloy nanoparticles. The invention aims to solve the technical problems of harsh conditions and non-uniform material morphology and size in the existing preparation process of the platinum-based binary alloy nanoparticles. The invention uses simple transition metal oxide nano-particles and platinum metal nano-particles as precursors, does not use any surfactant, and obtains binary alloy nano-particles of transition metal and platinum by heating to 350 ℃ in oleylamine and preserving heat. The invention uses nontoxic, simple and easily obtained precursor, has low cost of raw materials in the preparation process, simple and controllable process, reduces economic cost and is beneficial to industrial production.
Description
Technical Field
The invention relates to a method for preparing platinum-based binary alloy nanoparticles.
Background
Binary platinum-based alloys, such as iron-platinum and cobalt-platinum nanoparticles, have two phase structures, a face-centered tetragonal structure and a face-centered cubic structure, respectively. The Fe/Co and Pt atoms in the face-centered tetragonal nanoparticles are distributed in a layered manner in crystal lattice and are a chemical ordered phase, so that the particles have high magnetocrystalline anisotropy (K)FePt＝7×106J/m3，KCoPt＝4.9×106J/m3) And high coercive force, and is an excellent hard magnetic material. The iron-platinum and cobalt-platinum alloy nano particles with the face-centered cubic structure are soft magnetic materials because iron/cobalt and platinum atoms are randomly distributed in crystal lattices and belong to chemically disordered phases.
In recent years, with the development of energy conversion technology, platinum nanoparticles have been used as electrode materials for polymer membrane fuel cells because of their excellent catalytic properties. However, the price and efficiency of platinum have limited its development in the fuel cell field. Research results show that if transition metal atoms such as iron, cobalt, nickel, copper and the like are doped to generate platinum-based binary alloy nanoparticles such as iron platinum, cobalt platinum and the like, the economic cost can be reduced, and simultaneously, due to the synergistic effect between platinum and the transition metal atoms and the contraction/silver edge effect of electrons and crystal lattices, the utilization efficiency, the catalytic activity and the structural stability of platinum can be improved. Therefore, the platinum-based binary alloy nanoparticles with controllable morphology, size and components have potential application values in the fields of magnetic recording, information storage, batteries, energy sources, catalysis and the like.
Binary platinum-based alloy nanoparticles are generally prepared by thermally decomposing a carbonyl compound and platinum acetylacetonate while adding a surfactant such as polyol, ammonium bromide, amine iodide, and ascorbic acid at a high temperature. The precursor carbonyl compounds used in the preparation process, such as iron pentacarbonyl, cobalt octacarbonyl, etc., are expensive and belong to highly toxic chemicals, and are decomposed by light, so that the conditions for the transportation, storage and use processes are very strict. The use of multiple surfactants also increases economic costs in order to obtain good morphology and uniformly distributed size, which is not conducive to large-scale production.
Disclosure of Invention
The invention provides a method for preparing platinum-based binary alloy nanoparticles by taking transition metal oxide and platinum metal nanoparticles as precursors, aiming at solving the technical problems of harsh conditions and nonuniform material morphology and size in the existing preparation process of the platinum-based binary alloy nanoparticles.
The method for preparing the platinum-based binary alloy nanoparticles by using the transition metal oxide and the platinum metal nanoparticles as precursors is carried out according to the following processes:
adding oleylamine into a three-neck flask, starting stirring, introducing argon into the three-neck flask at room temperature to discharge air, heating the mixed system to 120-125 ℃ at a heating rate of 5-10 ℃/min under the protection of argon, injecting a normal hexane solution of platinum nanoparticles and a normal hexane solution of transition metal oxide nanoparticles into a three-neck flask, keeping the temperature for 1 h-1.5 h under the protection of argon and at the temperature of 120-125 ℃ to evaporate the normal hexane in the system, heating the mixed system to 350-370 ℃ at a heating rate of 5-10 ℃/min under the protection of argon, preserving heat for 9-10 h, cooling to room temperature under the protection of argon after the reaction is finished, adding n-hexane I for ultrasonic treatment for 5min, adding ethanol for ultrasonic treatment for 5min, centrifuging after ultrasonic treatment, and drying in vacuum to obtain platinum-based binary alloy nanoparticles;
the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL-0.3 mmol/mL;
the amount of substances of transition metals in the n-hexane solution of the transition metal oxide nanoparticles is equal to that of the substances of platinum nanoparticles in the n-hexane solution of the platinum nanoparticles;
the volume of the n-hexane solution of the platinum nanoparticles is equal to that of the n-hexane solution of the transition metal oxide nanoparticles;
the volume ratio of the n-hexane solution of the platinum nanoparticles to the oleylamine is 1 (10-11);
the volume ratio of the n-hexane I to the oleylamine is 1 (1-1.2);
the volume ratio of oleylamine to ethanol is 1 (3-4).
The invention uses simple transition metal oxide nano-particles and platinum metal nano-particles as precursors, does not use any surfactant, and obtains binary alloy nano-particles of transition metal and platinum by heating to 350 ℃ in oleylamine and preserving heat. The invention uses nontoxic, simple and easily obtained precursor, has low cost of raw materials in the preparation process, simple and controllable process, reduces economic cost and is beneficial to industrial production.
The invention has the advantage that binary platinum-based alloy nanoparticles with the size of about 6.5nm are prepared by adopting a simple liquid phase synthesis method and taking transition metal oxide and platinum metal nanoparticles as precursors respectively. By adjusting the types of the oxides, the nano-particles can be used for preparing binary platinum-based alloy nano-particles such as iron platinum, cobalt platinum, copper platinum, manganese platinum, nickel platinum, zinc platinum and the like. The composition can be adjusted by the ratio of the amounts of the precursor oxide and platinum metal nanoparticles species. The preparation process is simple, the shape and the size of the nano particles are uniform, and the expanded production is easy. Can be used for preparing different components and has potential application value in the fields of bioengineering, magnetic recording, storage, electrocatalysis and the like.
Drawings
FIG. 1 is a TEM image of ferroferric oxide nanoparticles in experiment one;
fig. 2 is a TEM picture of platinum nanoparticles in experiment one;
FIG. 3 is a TEM image of a platinum-based binary alloy nanoparticle prepared in experiment one;
FIG. 4 is an XRD spectrum;
FIG. 5 is a hysteresis loop analysis diagram;
FIG. 6 is a TEM picture of cobalt oxide nanoparticles in trial two;
FIG. 7 is a TEM picture of platinum nanoparticles in experiment two;
FIG. 8 is a TEM picture of platinum-based binary alloy nanoparticles prepared in experiment two;
FIG. 9 is an XRD spectrum;
FIG. 10 is a graph of a hysteresis loop analysis of platinum-based binary alloy nanoparticles prepared in experiment two;
FIG. 11 is a TEM picture of manganomanganic oxide nanoparticles in trial three;
FIG. 12 is a TEM picture of platinum nanoparticles in run three;
FIG. 13 is a TEM picture of platinum-based binary alloy nanoparticles prepared in run three;
figure 14 is an XRD spectrum.
Detailed Description
The first embodiment is as follows: the embodiment is a method for preparing platinum-based binary alloy nanoparticles by taking transition metal oxide and platinum metal nanoparticles as precursors, which is specifically carried out according to the following processes:
adding oleylamine into a three-neck flask, starting stirring, introducing argon into the three-neck flask at room temperature to discharge air, heating the mixed system to 120-125 ℃ at a heating rate of 5-10 ℃/min under the protection of argon, injecting a normal hexane solution of platinum nanoparticles and a normal hexane solution of transition metal oxide nanoparticles into a three-neck flask, keeping the temperature for 1 h-1.5 h under the protection of argon and at the temperature of 120-125 ℃ to evaporate the normal hexane in the system, heating the mixed system to 350-370 ℃ at a heating rate of 5-10 ℃/min under the protection of argon, preserving heat for 9-10 h, cooling to room temperature under the protection of argon after the reaction is finished, adding n-hexane I for ultrasonic treatment for 5min, adding ethanol for ultrasonic treatment for 5min, centrifuging after ultrasonic treatment, and drying in vacuum to obtain platinum-based binary alloy nanoparticles;
the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL-0.3 mmol/mL;
the amount of substances of transition metals in the n-hexane solution of the transition metal oxide nanoparticles is equal to that of the substances of platinum nanoparticles in the n-hexane solution of the platinum nanoparticles;
the volume of the n-hexane solution of the platinum nanoparticles is equal to that of the n-hexane solution of the transition metal oxide nanoparticles;
the volume ratio of the n-hexane solution of the platinum nanoparticles to the oleylamine is 1 (10-11);
the volume ratio of the n-hexane I to the oleylamine is 1 (1-1.2);
the volume ratio of oleylamine to ethanol is 1 (3-4).
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are ferroferric oxide nanoparticles. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are cobalt oxide nanoparticles. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are trimanganese tetroxide nanoparticles. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL; the concentration of the transition metal in the n-hexane solution of the transition metal oxide nanoparticles is 0.2 mmol/mL. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a method for preparing platinum-based binary alloy nanoparticles by taking transition metal oxide and platinum metal nanoparticles as precursors, and is specifically carried out according to the following processes:
adding oleylamine into a three-neck flask, starting stirring, introducing argon into the three-neck flask at room temperature to discharge air, heating a mixed system to 120 ℃ at a heating rate of 5 ℃/min under the protection of argon, injecting a normal hexane solution of platinum nanoparticles and a normal hexane solution of transition metal oxide nanoparticles into the three-neck flask, preserving heat for 1h under the protection of argon and at a temperature of 120 ℃ to evaporate the normal hexane in the system, heating the mixed system to 350 ℃ at a heating rate of 5 ℃/min under the protection of argon and preserving heat for 9h, cooling to room temperature under the protection of argon after reaction is finished, adding normal hexane I for carrying out ultrasonic treatment for 5min, adding ethanol for carrying out ultrasonic treatment for 5min, centrifuging after ultrasonic treatment, carrying out vacuum drying at 55 ℃ for 24h, and obtaining platinum-based binary alloy nanoparticles;
the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL;
the concentration of the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles is 0.0667 mmol/mL;
the volume of the n-hexane solution of the platinum nanoparticles is equal to that of the n-hexane solution of the transition metal oxide nanoparticles;
the volume ratio of the n-hexane solution of the platinum nanoparticles to oleylamine is 1: 10;
the volume ratio of the n-hexane I to the oleylamine is 1: 1;
the volume ratio of oleylamine to ethanol is 1: 3;
the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are ferroferric oxide nanoparticles.
And (2) test II: the test is a method for preparing platinum-based binary alloy nanoparticles by taking transition metal oxide and platinum metal nanoparticles as precursors, and is specifically carried out according to the following processes:
adding oleylamine into a three-neck flask, starting stirring, introducing argon into the three-neck flask at room temperature to discharge air, heating a mixed system to 120 ℃ at a heating rate of 5 ℃/min under the protection of argon, injecting a normal hexane solution of platinum nanoparticles and a normal hexane solution of transition metal oxide nanoparticles into the three-neck flask, preserving heat for 1h under the protection of argon and at a temperature of 120 ℃ to evaporate the normal hexane in the system, heating the mixed system to 350 ℃ at a heating rate of 5 ℃/min under the protection of argon and preserving heat for 9h, cooling to room temperature under the protection of argon after reaction is finished, adding normal hexane I for carrying out ultrasonic treatment for 5min, adding ethanol for carrying out ultrasonic treatment for 5min, centrifuging after ultrasonic treatment, carrying out vacuum drying at 55 ℃ for 24h, and obtaining platinum-based binary alloy nanoparticles;
the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL;
the concentration of the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles is 0.2 mmol/mL;
the volume of the n-hexane solution of the platinum nanoparticles is equal to that of the n-hexane solution of the transition metal oxide nanoparticles;
the volume ratio of the n-hexane solution of the platinum nanoparticles to oleylamine is 1: 10;
the volume ratio of the n-hexane I to the oleylamine is 1: 1;
the volume ratio of oleylamine to ethanol is 1: 3;
the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are cobalt monoxide nanoparticles.
And (3) test III: the test is a method for preparing platinum-based binary alloy nanoparticles by taking transition metal oxide and platinum metal nanoparticles as precursors, and is specifically carried out according to the following processes:
adding oleylamine into a three-neck flask, starting stirring, introducing argon into the three-neck flask at room temperature to discharge air, heating a mixed system to 120 ℃ at a heating rate of 5 ℃/min under the protection of argon, injecting a normal hexane solution of platinum nanoparticles and a normal hexane solution of transition metal oxide nanoparticles into the three-neck flask, preserving heat for 1h under the protection of argon and at a temperature of 120 ℃ to evaporate the normal hexane in the system, heating the mixed system to 350 ℃ at a heating rate of 5 ℃/min under the protection of argon and preserving heat for 9h, cooling to room temperature under the protection of argon after reaction is finished, adding normal hexane I for carrying out ultrasonic treatment for 5min, adding ethanol for carrying out ultrasonic treatment for 5min, centrifuging after ultrasonic treatment, carrying out vacuum drying at 55 ℃ for 24h, and obtaining platinum-based binary alloy nanoparticles;
the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL;
the concentration of the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles is 0.0667 mmol/mL;
the volume of the n-hexane solution of the platinum nanoparticles is equal to that of the n-hexane solution of the transition metal oxide nanoparticles;
the volume ratio of the n-hexane solution of the platinum nanoparticles to oleylamine is 1: 10;
the volume ratio of the n-hexane I to the oleylamine is 1: 1;
the volume ratio of oleylamine to ethanol is 1: 3;
the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are trimanganese tetroxide nanoparticles.
Fig. 1 is a TEM picture of the ferriferrous oxide nanoparticles in test one, fig. 2 is a TEM picture of the platinum nanoparticles in test one, and fig. 3 is a TEM picture of the platinum-based binary alloy nanoparticles prepared in test one, it can be seen that ferriferrous oxide, platinum nanoparticles, and iron-platinum nanoparticles are spherical particles having sizes of 7.6nm, 7.5nm, and 6.4nm, respectively.
Fig. 4 is an XRD spectrogram, curve 1 is the platinum-based binary alloy nanoparticles prepared in test one, curve 2 is the platinum nanoparticles in test one, and curve 3 is the ferroferric oxide nanoparticles in test one, which shows that only characteristic peaks (111), (200) and (220) of the iron-platinum alloy are present in the spectrogram of the iron-platinum nanoparticles, and the characteristic peaks move to the right compared with the spectrogram of the platinum nanoparticles, indicating that iron atoms are doped and the iron-platinum alloy is formed.
Fig. 5 is a hysteresis loop analysis chart, in which curve 1 is the ferroferric oxide nanoparticles in test one and curve 2 is the platinum-based binary alloy nanoparticles prepared in test one, and the results show that the ferroferric oxide is paramagnetic nanoparticles and the saturation magnetization is 45.5 emu/g; the Fe-Pt binary alloy nanoparticles are weak ferromagnetic nanoparticles, the saturation magnetization is 12emu/g, and the coercive force is 463.5 Oe.
Fig. 6 is a TEM picture of cobalt oxide nanoparticles in test two, fig. 7 is a TEM picture of platinum nanoparticles in test two, and fig. 8 is a TEM picture of platinum-based binary alloy nanoparticles prepared in test two, and it can be seen that cobalt oxide is cubic particles having a size of 8nm, platinum nanoparticles are spherical particles having a size of 7.5nm, and cobalt-platinum nanoparticles are spherical particles having a size of 6.5 nm.
Fig. 9 is an XRD spectrum, curve 1 is the platinum-based binary alloy nanoparticles prepared in test two, curve 2 is the platinum nanoparticles in test two, and curve 3 is the cobalt oxide nanoparticles in test two, and it can be seen that the characteristic peaks (111), (200), and (220) of the cobalt-platinum nanoparticles are significantly shifted to the right compared to the spectrum of the platinum nanoparticles, indicating that the cobalt atoms are doped and the cobalt-platinum alloy is formed.
Fig. 10 is a hysteresis loop analysis diagram of the platinum-based binary alloy nanoparticles prepared in experiment two, and the result shows that the cobalt-platinum nanoparticles are paramagnetic nanoparticles and have a saturation magnetization of 11.4 emu/g.
Fig. 11 is a TEM picture of the trimanganese tetroxide nanoparticles in test three, fig. 12 is a TEM picture of the platinum nanoparticles in test three, and fig. 13 is a TEM picture of the platinum-based binary alloy nanoparticles prepared in test three, and it can be seen that trimanganese tetroxide is a cubic particle with a size of 11nm, the platinum nanoparticles are spherical particles with a size of 7.5nm, and the manganese-platinum nanoparticles are spherical particles with a size of 6.5 nm.
Fig. 14 is an XRD spectrum, curve 1 is the platinum-based binary alloy nanoparticles prepared in test three, curve 2 is the platinum nanoparticles in test three, and curve 3 is the trimanganese tetroxide nanoparticles in test three, it can be seen that the characteristic peaks (111), (200) and (220) of the manganese-platinum nanoparticles are significantly shifted to the right compared to the spectrum of the platinum nanoparticles, indicating that the manganese atom is combined with platinum to form a cobalt-platinum alloy.
Claims (1)
1. A method for preparing platinum-based binary alloy nanoparticles by taking transition metal oxide and platinum metal nanoparticles as precursors is characterized in that the method for preparing the platinum-based binary alloy nanoparticles by taking the transition metal oxide and the platinum metal nanoparticles as the precursors is carried out according to the following processes:
adding oleylamine into a three-neck flask, starting stirring, introducing argon into the three-neck flask at room temperature to discharge air, heating a mixed system to 120 ℃ at a heating rate of 5 ℃/min under the protection of argon, injecting a normal hexane solution of platinum nanoparticles and a normal hexane solution of transition metal oxide nanoparticles into the three-neck flask, preserving heat for 1h under the protection of argon and at a temperature of 120 ℃ to evaporate the normal hexane in the system, heating the mixed system to 350 ℃ at a heating rate of 5 ℃/min under the protection of argon and preserving heat for 9h, cooling to room temperature under the protection of argon after reaction is finished, adding normal hexane I for carrying out ultrasonic treatment for 5min, adding ethanol for carrying out ultrasonic treatment for 5min, centrifuging after ultrasonic treatment, carrying out vacuum drying at 55 ℃ for 24h, and obtaining platinum-based binary alloy nanoparticles;
the concentration of the platinum nanoparticles in the n-hexane solution of the platinum nanoparticles is 0.2 mmol/mL;
the concentration of the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles is 0.0667 mmol/mL;
the volume of the n-hexane solution of the platinum nanoparticles is equal to that of the n-hexane solution of the transition metal oxide nanoparticles;
the volume ratio of the n-hexane solution of the platinum nanoparticles to oleylamine is 1: 10;
the volume ratio of the n-hexane I to the oleylamine is 1: 1;
the volume ratio of oleylamine to ethanol is 1: 3;
the transition metal oxide nanoparticles in the n-hexane solution of the transition metal oxide nanoparticles are ferroferric oxide nanoparticles;
the ferroferric oxide, platinum nanoparticles and platinum-based binary alloy nanoparticles are spherical particles with the sizes of 7.6nm, 7.5nm and 6.4nm respectively.
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