CN109604625A - A method of using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano particle - Google Patents
A method of using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano particle Download PDFInfo
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- CN109604625A CN109604625A CN201910126803.4A CN201910126803A CN109604625A CN 109604625 A CN109604625 A CN 109604625A CN 201910126803 A CN201910126803 A CN 201910126803A CN 109604625 A CN109604625 A CN 109604625A
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- metal oxide
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- platinum
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 161
- 229910000314 transition metal oxide Inorganic materials 0.000 title claims abstract description 56
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 55
- 229910002056 binary alloy Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 18
- 239000002243 precursor 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
- 150000003624 transition metals Chemical class 0.000 claims abstract description 9
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 207
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 60
- 229910052786 argon Inorganic materials 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000008187 granular material Substances 0.000 claims description 12
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical group [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 12
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical group O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 11
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 229910017052 cobalt Inorganic materials 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000004321 preservation Methods 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 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 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- GUBSQCSIIDQXLB-UHFFFAOYSA-N cobalt platinum Chemical compound [Co].[Pt].[Pt].[Pt] GUBSQCSIIDQXLB-UHFFFAOYSA-N 0.000 description 9
- 229910045601 alloy Inorganic materials 0.000 description 8
- 239000000956 alloy Substances 0.000 description 8
- 235000013495 cobalt Nutrition 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 229910052742 iron Inorganic materials 0.000 description 5
- OBACEDMBGYVZMP-UHFFFAOYSA-N iron platinum Chemical compound [Fe].[Fe].[Pt] OBACEDMBGYVZMP-UHFFFAOYSA-N 0.000 description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 229910001260 Pt alloy Inorganic materials 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 239000011572 manganese 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
- 230000003197 catalytic effect Effects 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical group [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 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
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229940056319 ferrosoferric oxide Drugs 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 230000005291 magnetic effect Effects 0.000 description 2
- 239000000696 magnetic material Substances 0.000 description 2
- 230000005298 paramagnetic effect Effects 0.000 description 2
- 229910018979 CoPt Inorganic materials 0.000 description 1
- 229910005335 FePt Inorganic materials 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 241000353345 Odontesthes regia Species 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
- 229910000428 cobalt oxide Inorganic materials 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
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- -1 iodate amine Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- IGOJMROYPFZEOR-UHFFFAOYSA-N manganese platinum Chemical compound [Mn].[Pt] IGOJMROYPFZEOR-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000015689 metaplastic ossification Effects 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
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- 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 of using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano particle, it is related to a kind of method for preparing platinum base binary alloy nano particle.It is harsh that the present invention is to solve existing platinum base binary alloy nano particulate production conditions, material morphology and the inhomogenous technical problem of size.The present invention makees presoma using simple transition metal oxide nano particle and platinum metal nano-particle, does not use any surfactant, 350 DEG C of heat preservations are heated in oleyl amine and obtain the binary alloy nano particle of transition metal and platinum.The present invention uses presoma nontoxic, simple and easy to get, and preparation process chinese raw materials is at low cost, process is simply controllable, reduces economic cost, is conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of methods for preparing platinum base binary alloy nano particle.
Background technique
Binary platinum base alloy such as iron platinum and cobalt platinum nano particle, tool there are two types of phase structure, respectively face-centered tetragonal structure and
Face-centred cubic structure.Iron/cobalt and pt atom are in layered distribution in lattice in the nano particle of face-centered tetragonal structure, are a kind ofization
Learn ordered phase, thus magnetocrystalline anisotropy (K with higherFePt=7 × 106J/m3, KCoPt=4.9 × 106J/m3) and height rectify
Stupid power is a kind of excellent hard magnetic material.And the iron platinum and cobalt-platinum alloy nano particle of face-centred cubic structure, due to iron/cobalt and
Pt atom random distribution in lattice belongs to the unordered phase of chemistry, thus is a kind of soft magnetic materials.
In recent years, with the development of energy conversion technology, Pt nanoparticle due to having excellent catalytic properties, and by with
In the electrode material of polymer-membrane fuel battery.But it limits it since the price of platinum is higher and low efficiency and is led in fuel cell
The development in domain.Result of study is shown, if doping such as iron, cobalt, nickel and copper transition metal atoms, generate platinum base bianry alloy such as
The nano particles such as iron platinum, cobalt platinum can not only reduce economic cost, simultaneously because cooperateing with effect between platinum and transition metal atoms
It answers, contraction/silver side effect of electronics and lattice, additionally it is possible to improve the utilization efficiency, catalytic activity and structural stability of platinum.Cause
This, pattern, size and the controllable platinum base binary alloy nano particle of component in magnetic recording, information storage, battery, the energy and are urged
There is potential application value in the fields such as change.
Binary platinum base alloy nano particle generally passes through thermal decomposition carbonyls and acetylacetone,2,4-pentanedione platinum, while being added polynary
The surfactants such as alcohol, ammonium bromide, iodate amine and ascorbic acid, prepare under the high temperature conditions.Before using during the preparation process
Drive body carbonyls, such as iron pentacarbonyl, eight carbonyl cobalts are expensive, and belong to severe poisonous chemicals, decompose in light, thus right
The condition of its transport, storage and use process is very harsh.In order to obtain good pattern and equally distributed size, using more
Kind of surfactant but also economic cost increase, be unfavorable for being mass produced.
Summary of the invention
It is harsh that the present invention is to solve existing platinum base binary alloy nano particulate production conditions, material morphology and ruler
Very little inhomogenous technical problem, and one kind is provided using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base
The method of binary alloy nano particle.
It is of the invention using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano
The method of particle is carried out by following procedure:
Oleyl amine is added in three-necked flask, stirring is opened, is passed through argon gas discharge air into three-necked flask at room temperature,
Mixed system is heated to 120 DEG C~125 DEG C with 5 DEG C/min~10 DEG C/min rate of heat addition under argon gas protection, is burnt to three mouthfuls
The hexane solution of Pt nanoparticle and the hexane solution of transition metal oxide nano particle are injected in bottle, are protected in argon gas
N-hexane under conditions of lower and temperature is 120 DEG C~125 DEG C in heat preservation 1h~1.5h evaporation system, under protection of argon gas again with
Mixed system is heated to 350 DEG C~370 DEG C and keeps the temperature 9h~10h by 5/min~10 DEG C/min rate of heat addition, after reaction
It is cooled to room temperature under protection of argon gas, n-hexane I ultrasound 5min is added, add EtOH Sonicate 5min, be centrifuged after ultrasound, be true
Sky is dry, obtains platinum base binary alloy nano particle；
The concentration of Pt nanoparticle is 0.2mmol/mL~0.3mmol/ in the hexane solution of the Pt nanoparticle
mL；
The amount Yu platinum nanometer of the substance of transition metal in the hexane solution of the transition metal oxide nano particle
The amount of the substance of Pt nanoparticle is equal in the hexane solution of particle；
The body of the hexane solution of the hexane solution and transition metal oxide nano particle of the Pt nanoparticle
Product is equal；
The hexane solution of the Pt nanoparticle and the volume ratio of oleyl amine are 1:(10~11)；
The volume ratio of the n-hexane I and oleyl amine are 1:(1~1.2)；
The volume ratio of the oleyl amine and ethyl alcohol is 1:(3~4).
The present invention makees presoma using simple transition metal oxide nano particle and platinum metal nano-particle, does not use
Any surfactant is heated to 350 DEG C of heat preservations in oleyl amine and obtains the binary alloy nano particle of transition metal and platinum.This hair
It is bright that using presoma nontoxic, simple and easy to get, preparation process chinese raw materials is at low cost, process is simply controllable, reduce it is economical at
This, is conducive to industrialized production.
The advantage of the invention is that using a kind of simple liquid phase synthesizing method, with transition metal oxide and platinum nanometer
Particle is respectively presoma to prepare the binary platinum base alloy nano particle that size is about 6.5nm.By the kind for adjusting oxide
Class can be used for preparing the binary platinum base alloy nano particle such as iron platinum, cobalt platinum, copper platinum, manganese platinum, nickel platinum and zinc platinum.Component can lead to
The ratio for crossing the amount of the substance of oxidation of precursor object and platinum metal nano-particle is adjusted.Preparation process is simple, nano particle pattern and
Size uniformity is easily enlarged metaplasia production.It can be used for preparing heterogeneity in bioengineering and magnetic recording, storage and electro-catalysis etc.
Field has potential application.
Detailed description of the invention
Fig. 1 is the TEM picture for testing the ferroferric oxide nano granules in one；
Fig. 2 is the TEM picture for testing the Pt nanoparticle in one；
Fig. 3 is the TEM picture for testing the platinum base binary alloy nano particle of a preparation；
Fig. 4 is XRD spectra；
Fig. 5 is hysteresis loop analysis chart；
Fig. 6 is the TEM picture for testing the oxidation cobalt nano-particle in two；
Fig. 7 is the TEM picture for testing the Pt nanoparticle in two；
Fig. 8 is the TEM picture for testing the platinum base binary alloy nano particle of two preparations；
Fig. 9 is XRD spectra；
Figure 10 is the hysteresis loop analysis chart for testing the platinum base binary alloy nano particle of two preparations；
Figure 11 is the TEM picture for testing the trimanganese tetroxide nano particle in three；
Figure 12 is the TEM picture for testing the Pt nanoparticle in three；
Figure 13 is the TEM picture for testing the platinum base binary alloy nano particle of three preparations；
Figure 14 is XRD spectra.
Specific embodiment
Specific embodiment 1: present embodiment be one kind with transition metal oxide and platinum metal nano-particle for forerunner
The method that body prepares platinum base binary alloy nano particle is specifically carried out by following procedure:
Oleyl amine is added in three-necked flask, stirring is opened, is passed through argon gas discharge air into three-necked flask at room temperature,
Mixed system is heated to 120 DEG C~125 DEG C with 5 DEG C/min~10 DEG C/min rate of heat addition under argon gas protection, is burnt to three mouthfuls
The hexane solution of Pt nanoparticle and the hexane solution of transition metal oxide nano particle are injected in bottle, are protected in argon gas
N-hexane under conditions of lower and temperature is 120 DEG C~125 DEG C in heat preservation 1h~1.5h evaporation system, under protection of argon gas again with
Mixed system is heated to 350 DEG C~370 DEG C and keeps the temperature 9h~10h by 5/min~10 DEG C/min rate of heat addition, after reaction
It is cooled to room temperature under protection of argon gas, n-hexane I ultrasound 5min is added, add EtOH Sonicate 5min, be centrifuged after ultrasound, be true
Sky is dry, obtains platinum base binary alloy nano particle；
The concentration of Pt nanoparticle is 0.2mmol/mL~0.3mmol/ in the hexane solution of the Pt nanoparticle
mL；
The amount Yu platinum nanometer of the substance of transition metal in the hexane solution of the transition metal oxide nano particle
The amount of the substance of Pt nanoparticle is equal in the hexane solution of particle；
The body of the hexane solution of the hexane solution and transition metal oxide nano particle of the Pt nanoparticle
Product is equal；
The hexane solution of the Pt nanoparticle and the volume ratio of oleyl amine are 1:(10~11)；
The volume ratio of the n-hexane I and oleyl amine are 1:(1~1.2)；
The volume ratio of the oleyl amine and ethyl alcohol is 1:(3~4).
Specific embodiment 2: the present embodiment is different from the first embodiment in that: the transiting metal oxidation
Transition metal oxide nano particle in the hexane solution of object nano particle is ferroferric oxide nano granules.Other and tool
Body embodiment one is identical.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: the transition metal
Transition metal oxide nano particle in the hexane solution of oxide nano particles is oxidation cobalt nano-particle.Other and tool
Body embodiment one or two is identical.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: the transition
Transition metal oxide nano particle in the hexane solution of metal oxide nanoparticles is trimanganese tetroxide nano particle.
Other are identical as one of specific embodiment one to three.
Specific embodiment 5: present embodiment is unlike specific embodiment four: the Pt nanoparticle
The concentration of Pt nanoparticle is 0.2mmol/mL in hexane solution；The n-hexane of the transition metal oxide nano particle
The concentration of transition metal is 0.2mmol/mL in solution.Other are identical as specific embodiment four.
The present invention is verified with following tests:
Test one: this test is one kind using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base two
The method of first alloy nanoparticle is specifically carried out by following procedure:
Oleyl amine is added in three-necked flask, stirring is opened, is passed through argon gas discharge air into three-necked flask at room temperature,
Mixed system is heated to 120 DEG C with the rate of heat addition of 5 DEG C/min under argon gas protection, Pt nanoparticle is injected into three-necked flask
Hexane solution and transition metal oxide nano particle hexane solution, be under protection of argon gas 120 DEG C with temperature
Under the conditions of keep the temperature 1h evaporation system in n-hexane, mixed system is added with the rate of heat addition of 5 DEG C/min again under protection of argon gas
Heat is to 350 DEG C and keeps the temperature 9h, is cooled to room temperature under protection of argon gas after reaction, and n-hexane I ultrasound 5min is added, adds
EtOH Sonicate 5min puts into a centrifuge centrifugation after ultrasonic, is dried in vacuo, and 55 DEG C of dryings for 24 hours, obtain platinum base binary alloy nano
Particle；
The concentration of Pt nanoparticle is 0.2mmol/mL in the hexane solution of the Pt nanoparticle；
Transition metal oxide nano particle is dense in the hexane solution of the transition metal oxide nano particle
Degree is 0.0667mmol/mL；
The body of the hexane solution of the hexane solution and transition metal oxide nano particle of the Pt nanoparticle
Product is equal；
The hexane solution of the Pt nanoparticle and the volume ratio of oleyl amine are 1:10；
The volume ratio of the n-hexane I and oleyl amine are 1:1；
The volume ratio of the oleyl amine and ethyl alcohol is 1:3；
Transition metal oxide nano particle in the hexane solution of the transition metal oxide nano particle is
Ferroferric oxide nano granules.
Test two: this test is one kind using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base two
The method of first alloy nanoparticle is specifically carried out by following procedure:
Oleyl amine is added in three-necked flask, stirring is opened, is passed through argon gas discharge air into three-necked flask at room temperature,
Mixed system is heated to 120 DEG C with the rate of heat addition of 5 DEG C/min under argon gas protection, Pt nanoparticle is injected into three-necked flask
Hexane solution and transition metal oxide nano particle hexane solution, be under protection of argon gas 120 DEG C with temperature
Under the conditions of keep the temperature 1h evaporation system in n-hexane, mixed system is added with the rate of heat addition of 5 DEG C/min again under protection of argon gas
Heat is to 350 DEG C and keeps the temperature 9h, is cooled to room temperature under protection of argon gas after reaction, and n-hexane I ultrasound 5min is added, adds
EtOH Sonicate 5min puts into a centrifuge centrifugation after ultrasonic, is dried in vacuo, and 55 DEG C of dryings for 24 hours, obtain platinum base binary alloy nano
Particle；
The concentration of Pt nanoparticle is 0.2mmol/mL in the hexane solution of the Pt nanoparticle；
Transition metal oxide nano particle is dense in the hexane solution of the transition metal oxide nano particle
Degree is 0.2mmol/mL；
The body of the hexane solution of the hexane solution and transition metal oxide nano particle of the Pt nanoparticle
Product is equal；
The hexane solution of the Pt nanoparticle and the volume ratio of oleyl amine are 1:10；
The volume ratio of the n-hexane I and oleyl amine are 1:1；
The volume ratio of the oleyl amine and ethyl alcohol is 1:3；
Transition metal oxide nano particle in the hexane solution of the transition metal oxide nano particle is
Cobalt black nano particle.
Test three: this test is one kind using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base two
The method of first alloy nanoparticle is specifically carried out by following procedure:
Oleyl amine is added in three-necked flask, stirring is opened, is passed through argon gas discharge air into three-necked flask at room temperature,
Mixed system is heated to 120 DEG C with the rate of heat addition of 5 DEG C/min under argon gas protection, Pt nanoparticle is injected into three-necked flask
Hexane solution and transition metal oxide nano particle hexane solution, be under protection of argon gas 120 DEG C with temperature
Under the conditions of keep the temperature 1h evaporation system in n-hexane, mixed system is added with the rate of heat addition of 5 DEG C/min again under protection of argon gas
Heat is to 350 DEG C and keeps the temperature 9h, is cooled to room temperature under protection of argon gas after reaction, and n-hexane I ultrasound 5min is added, adds
EtOH Sonicate 5min puts into a centrifuge centrifugation after ultrasonic, is dried in vacuo, and 55 DEG C of dryings for 24 hours, obtain platinum base binary alloy nano
Particle；
The concentration of Pt nanoparticle is 0.2mmol/mL in the hexane solution of the Pt nanoparticle；
Transition metal oxide nano particle is dense in the hexane solution of the transition metal oxide nano particle
Degree is 0.0667mmol/mL；
The body of the hexane solution of the hexane solution and transition metal oxide nano particle of the Pt nanoparticle
Product is equal；
The hexane solution of the Pt nanoparticle and the volume ratio of oleyl amine are 1:10；
The volume ratio of the n-hexane I and oleyl amine are 1:1；
The volume ratio of the oleyl amine and ethyl alcohol is 1:3；
Transition metal oxide nano particle in the hexane solution of the transition metal oxide nano particle is
Trimanganese tetroxide nano particle.
Fig. 1 is the TEM picture for testing the ferroferric oxide nano granules in one, and Fig. 2 is the Pt nanoparticle tested in one
TEM picture, Fig. 3 be test one preparation platinum base binary alloy nano particle TEM picture, it can be seen that ferroso-ferric oxide,
Pt nanoparticle and nanometer Fe-Pt particle are the spheric granules that size is respectively 7.6nm, 7.5nm and 6.4nm.
Fig. 4 is XRD spectra, and curve 1 is the platinum base binary alloy nano particle for testing a preparation, and curve 2 is in test one
Pt nanoparticle, curve 3 be test one in ferroferric oxide nano granules, it can be seen that in the spectrogram of nanometer Fe-Pt particle
The only characteristic peak (111), (200) and (220) of ferroplatinum, compared with the spectrogram of Pt nanoparticle, characteristic peak moves right,
Show to be mixed with iron atom and forms ferroplatinum.
Fig. 5 is hysteresis loop analysis chart, and curve 1 is the ferroferric oxide nano granules tested in one, and curve 2 is test one
The platinum base binary alloy nano particle of preparation, the results show that ferroso-ferric oxide is paramagnetic nanoparticle, saturation magnetization is
45.5emu/g；Iron platinum binary alloy nano particle is weak ferromagnetism nano particle, saturation magnetization 12emu/g, coercivity
For 463.5Oe.
Fig. 6 is the TEM picture for testing the oxidation cobalt nano-particle in two, and Fig. 7 is the TEM for testing the Pt nanoparticle in two
Picture, Fig. 8 are the TEM pictures for testing the platinum base binary alloy nano particle of two preparations, it can be seen that cobalt oxide is having a size of 8nm
Cube particle, Pt nanoparticle be 7.5nm spheric granules, cobalt platinum nano particle be 6.5nm spheric granules.
Fig. 9 is XRD spectra, and curve 1 is the platinum base binary alloy nano particle for testing two preparations, and curve 2 is in test two
Pt nanoparticle, curve 3 be test two in oxidation cobalt nano-particle, it can be seen that the characteristic peak of cobalt platinum nano particle
(111), (200) and (220), compared with the spectrogram of Pt nanoparticle, characteristic peak obviously moves right, and shows to be mixed with cobalt atom
And form cobalt-platinum alloy.
Figure 10 is the hysteresis loop analysis chart for testing the platinum base binary alloy nano particle of two preparations, the results show that cobalt platinum
Nano particle is paramagnetic nanoparticle, saturation magnetization 11.4emu/g.
Figure 11 is the TEM picture for testing the trimanganese tetroxide nano particle in three, and Figure 12 is the platinum nanometer tested in three
The TEM picture of grain, Figure 13 are the TEM pictures for testing the platinum base binary alloy nano particle of three preparations, it can be seen that four oxidations three
Manganese is the cube particle having a size of 11nm, and Pt nanoparticle is the spheric granules of 7.5nm, and manganese Pt nanoparticle is 6.5nm's
Spheric granules.
Figure 14 is XRD spectra, and curve 1 is the platinum base binary alloy nano particle for testing three preparations, and curve 2 is in test three
Pt nanoparticle, curve 3 be test three in trimanganese tetroxide nano particle, it can be seen that the characteristic peak of manganese Pt nanoparticle
(111), (200) and (220), compared with the spectrogram of Pt nanoparticle, characteristic peak obviously moves right, and shows manganese atom and platinum knot
Conjunction forms cobalt-platinum alloy.
Claims (5)
1. a kind of using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano particle
Method, it is characterised in that using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano
The method of grain is carried out by following procedure:
Oleyl amine is added in three-necked flask, stirring is opened, argon gas discharge air is passed through into three-necked flask at room temperature, in argon gas
Mixed system is heated to 120 DEG C~125 DEG C with 5 DEG C/min~10 DEG C/min rate of heat addition under protection, into three-necked flask
Inject Pt nanoparticle hexane solution and transition metal oxide nano particle hexane solution, under protection of argon gas and
Temperature keeps the temperature the n-hexane in 1h~1.5h evaporation system under conditions of being 120 DEG C~125 DEG C, under protection of argon gas again with 5/
Mixed system is heated to 350 DEG C~370 DEG C and keeps the temperature 9h~10h by min~10 DEG C/min rate of heat addition, is existed after reaction
It is cooled to room temperature under argon gas protection, n-hexane I ultrasound 5min is added, added EtOH Sonicate 5min, be centrifuged after ultrasound, vacuum
It is dry, obtain platinum base binary alloy nano particle；
The concentration of Pt nanoparticle is 0.2mmol/mL~0.3mmol/mL in the hexane solution of the Pt nanoparticle；
The amount and Pt nanoparticle of the substance of transition metal in the hexane solution of the transition metal oxide nano particle
Hexane solution in Pt nanoparticle substance amount it is equal；
The volume phase of the hexane solution of the hexane solution and transition metal oxide nano particle of the Pt nanoparticle
Deng；
The hexane solution of the Pt nanoparticle and the volume ratio of oleyl amine are 1:(10~11)；
The volume ratio of the n-hexane I and oleyl amine are 1:(1~1.2)；
The volume ratio of the oleyl amine and ethyl alcohol is 1:(3~4).
2. one kind according to claim 1 is using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base
The method of binary alloy nano particle, it is characterised in that in the hexane solution of the transition metal oxide nano particle
Transition metal oxide nano particle is ferroferric oxide nano granules.
3. one kind according to claim 1 is using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base
The method of binary alloy nano particle, it is characterised in that in the hexane solution of the transition metal oxide nano particle
Transition metal oxide nano particle is oxidation cobalt nano-particle.
4. one kind according to claim 1 is using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base
The method of binary alloy nano particle, it is characterised in that in the hexane solution of the transition metal oxide nano particle
Transition metal oxide nano particle is trimanganese tetroxide nano particle.
5. one kind according to claim 1 is using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base
The method of binary alloy nano particle, it is characterised in that Pt nanoparticle is dense in the hexane solution of the Pt nanoparticle
Degree is 0.2mmol/mL；The concentration of transition metal is in the hexane solution of the transition metal oxide nano particle
0.2mmol/mL。
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