CN102500755B - Preparation method for graphene-supported metal nanoparticle compound - Google Patents
Preparation method for graphene-supported metal nanoparticle compound Download PDFInfo
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- CN102500755B CN102500755B CN2011103427382A CN201110342738A CN102500755B CN 102500755 B CN102500755 B CN 102500755B CN 2011103427382 A CN2011103427382 A CN 2011103427382A CN 201110342738 A CN201110342738 A CN 201110342738A CN 102500755 B CN102500755 B CN 102500755B
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000007864 aqueous solution Substances 0.000 claims description 22
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- 239000010439 graphite Substances 0.000 claims description 17
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- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 6
- 230000001988 toxicity Effects 0.000 abstract description 4
- 231100000419 toxicity Toxicity 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 239000012279 sodium borohydride Substances 0.000 abstract description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract description 2
- 229910000510 noble metal Inorganic materials 0.000 abstract description 2
- 229910021524 transition metal nanoparticle Inorganic materials 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000010931 gold Substances 0.000 description 18
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 17
- 229910052737 gold Inorganic materials 0.000 description 17
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 5
- -1 graphite alkene Chemical class 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- 230000002194 synthesizing effect Effects 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000012456 homogeneous solution Substances 0.000 description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229960005070 ascorbic acid Drugs 0.000 description 2
- 235000010323 ascorbic acid Nutrition 0.000 description 2
- 239000011668 ascorbic acid Substances 0.000 description 2
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 description 2
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 description 1
- NJSSICCENMLTKO-HRCBOCMUSA-N [(1r,2s,4r,5r)-3-hydroxy-4-(4-methylphenyl)sulfonyloxy-6,8-dioxabicyclo[3.2.1]octan-2-yl] 4-methylbenzenesulfonate Chemical compound C1=CC(C)=CC=C1S(=O)(=O)O[C@H]1C(O)[C@@H](OS(=O)(=O)C=2C=CC(C)=CC=2)[C@@H]2OC[C@H]1O2 NJSSICCENMLTKO-HRCBOCMUSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
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- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
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Abstract
The invention discloses a preparation method for a graphene-supported metal nanoparticle compound. The method comprises the following steps of: preparing metal nanoparticles with uniform size through controllable synthesis; uniformly supporting the metal nanoparticles on graphene oxide through adsorption; and catalyzing NaBH4 at normal temperature to reduce the graphene oxide by taking the metal nanoparticles as a catalyst so as to obtain the graphene-supported metal nanoparticle compound. By using the method provided by the invention, the compounds with strong toxicity and volatility such as hydrazine hydrate and derivatives thereof are prevented from being used as reducing agents to prepare the graphene-supported metal nanoparticle compound; the method has the characteristics of environmental friendliness, safety and the like; meanwhile, the method can be performed under the conditions of room temperature and different acid-base (pH) conditions with mild reaction conditions. Through the method, various noble metals and transition metal nanoparticles can be supported on the graphene, and some metal oxides for catalyzing decomposition of NaBH4 can also be supported.
Description
Technical field
The present invention relates to the Nano-composite materials technical field, be specifically related to a kind of preparation method of graphene-supported metal nanoparticle compound.
Background technology
Graphene-supported metal nanoparticle compound, have excellent catalytic capability, and outstanding electric conductivity and optical property can be widely used in the numerous areas such as sensor, photovoltaic cell, organic catalyst compound.
Hummer, Brodie, the methods such as Staudenmaier can prepare graphene oxide on a large scale, and then, by adding hydrazine hydrate, the reducing agents such as benzylamine just can reduce and obtain Graphene under heating condition.At present, mainly contain two kinds of methods and prepare graphene-supported metal nanoparticle compound, a kind of is first the presoma of graphene oxide and metal ion to be mixed, then add reducing agent one-step synthesis graphene-supported metal nanoparticle compound, this method simple and fast, but the metal nanoparticle structure of preparation and pattern are difficult to control, and have affected the character of compound; Another kind is to distinguish in two steps redox graphene and metal ion presoma, prepare graphene-supported metal nanoparticle compound by absorption, this method is more complicated, but can effectively control structure and the pattern of metal nanoparticle, give full play of the excellent properties of graphene-supported metal nanoparticle compound.
Before the present invention, work in the past is mainly to remove to prepare graphene-supported metal nanoparticle compound with hydrazine hydrate and derivative thereof as reducing agent, but hydrazine hydrate and derivative thereof have very strong toxicity and volatility, can not be for large-scale use, and compound a lot of nitrogen-atoms that can adulterate of preparation, affect the physics and chemistry character of compound.Ascorbic acid for bibliographical information (VC), sodium borohydride (NaBH are also arranged in nearest 2 years
4), diallyl dimethyl ammoniumchloride (PDDA) etc. prepares graphene-supported metal nanoparticle compound as reducing agent, but these reactions must just can be advanced ability under high-temperature condition, react comparatively violent, easily increase the defect of Graphene.
Summary of the invention
The deficiency existed in order to overcome prior art, the invention provides the preparation method who prepares graphene-supported metal nanoparticle compound under a kind of normal temperature condition.
To achieve the above object of the invention, the technical solution adopted in the present invention is: shown in Fig. 1, prepare the metal nanoparticle with single-size by controlledly synthesis, by absorption, metal nanoparticle is loaded on graphene oxide equably, use metal nanoparticle as catalyst NaBH
4redox graphene at normal temperatures, thus graphene-supported metal nanoparticle compound obtained, specifically comprise the following steps:
Step 1: graphene oxide is purified repeatedly with hydrochloric acid and deionized water washing respectively, obtain pure graphite oxide aqueous solution, and ultrasonic dispersion a period of time;
Step 2: by controlledly synthesis, add reducing agent that metal ion precursor solution is reduced to metal nanoparticle, be dispersed in uniformly in the aqueous solution, obtain the metal nanoparticle aqueous solution;
Step 3: the graphite oxide aqueous solution is joined in the metal nanoparticle aqueous solution, be uniformly dispersed under room temperature, obtain once uniform graphene oxide-loaded metal nanoparticle mixed solution;
Step 4: incite somebody to action once uniform graphene oxide-loaded centrifugal a period of time of metal nanoparticle mixed solution, wash with water repeatedly, add ultrasonic dispersion a period of time of deionized water, obtain the uniform graphene oxide-loaded metal nanoparticle mixing mixed solution of secondary;
Step 5: add NaBH
4, reaction a period of time, use respectively deionized water and ethanol centrifuge washing repeatedly, and vacuum drying.
Preferably:
In step 1, described graphene oxide is made by the Hummer method, and the mass concentration of graphene oxide is 0.1～1mg/ml; The volumetric concentration of the described hydrochloric acid for purification is 2%-4%, and the time of ultrasonic dispersion is 15-30 minute.
In step 2, the molar concentration of described metal ion precursor solution is 10
-5mol/L-1 mol/L.Described metal nanoparticle comprises, the simple metal of Au Ag Pt Pd, rhodium, ruthenium, iron, cobalt, nickel or by alloy that wherein several metallic elements form.
In step 4; to incite somebody to action once uniform graphene oxide-loaded metal nanoparticle mixed solution centrifugal 15 minutes with the speed of 20000 rev/mins; wash repetition with water 6 times, add deionized water within ultrasonic 5 minutes, to obtain the uniform graphene oxide-loaded metal nanoparticle mixed solution of secondary.
In step 5, add NaBH
4rear reaction 2 hours, use respectively deionized water and ethanol with the speed centrifuge washing of 20000 rev/mins three times, 60 ℃ of lower vacuum drying 2 hours.
The present invention is directed to that current graphene-supported metal nanoparticle compound is synthetic need to the shortcoming such as must carry out with the toxicity reducing agent such as hydrazine hydrate and reaction under heating condition, adopt NaBH
4as reducing agent synthesizing graphite alkene carried metal nano-particle complex at ambient temperature, its advantage is:
(1) avoid having used hydrazine hydrate and derivative thereof etc. to there is strong toxicity and volatile compound as reducing agent, there are the characteristics such as environmental protection and safety;
(2) this preparation method can at room temperature carry out, and applicable ambient temperature range is 0 ℃-100 ℃, and the reaction condition gentleness, reduced the generation of defect;
(3) this preparation method can carry out under the 2-12 condition in the pH value;
(4) can be by controlling the synthetic of metal nanoparticle, the metal nanoparticle of load different size and structure is to Graphene;
(5) this preparation method not only can the multiple noble metal of load and transition metal nanoparticles to Graphene, can also load some there is catalyzing N aBH
4the metal oxide decomposed.
The accompanying drawing explanation
Fig. 1 is the reaction schematic diagram that the inventive method prepares graphene-supported metal nanoparticle compound.
The specific embodiment
Embodiment 1:
(1) washing, purification
The 1mg graphene oxide is dissolved in 10ml water, after ultrasonic dispersing and dissolving, 20000 rev/mins of HCl that are 3% by volumetric concentration respectively and water centrifuge washing 3 times, adds deionized water, make uniform 1mg/ml graphite oxide aqueous solution;
(2) synthetic 3nm gold grain
0.5mM HAuCl by 5ml
4join in the 25ml conical flask with the 0.2M softex kw (CTAB) of 5ml, mix, add the 0.01M NaBH of 0.6ml
4, under room temperature, place 3 hours;
(3) synthetic graphene oxide-loaded 3nm gold grain compound
Add the 1mg/ml graphite oxide aqueous solution of 1ml in 3nm gold grain solution, mix, 20000 rev/mins of lower water centrifuge washings 6 times, obtain graphene oxide-loaded 3nm gold nano grain compound, add the 5ml deionized water, within ultrasonic 5 minutes, obtain homogeneous solution;
(4) synthesizing graphite alkene load 3nm gold grain compound
Add 10mg NaBH
4in the graphene oxide-loaded 3nm gold grain aqueous solution, evenly, room temperature is placed 2 hours in vibration, 20000 rev/mins of washings 6 times, and 60 degrees centigrade of dryings 2 hours, obtain graphene-supported 3nm gold nano grain compound.
Embodiment 2:
(1) washing, purification
The 1mg graphene oxide is dissolved in 10ml water, after ultrasonic dispersing and dissolving, at 20000 rev/mins, uses respectively 3%HCl and water centrifuge washing 3 times, add deionized water, make uniform 1mg/ml graphite oxide aqueous solution;
(2) synthetic 10nm gold grain
0.5mM HAuCl by 5ml
4join in the 25ml conical flask with the 0.2M softex kw (CTAB) of 5ml, mix, add the 0.01M NaBH of 0.6ml
4, under room temperature, place 3 hours, obtain the gold grain of 3nm;
0.5mM HAuCl by 6ml
4with the 0.02M hexadecyltrimethylammonium chloride (CTAC) of 6ml, join in the 25ml conical flask, mix, add again the 0.1M ascorbic acid (Vc) of 4.5ml in flask, finally adding the 3nm gold grain seed of 0.3ml, place 3 hours under room temperature, obtain the gold grain of 10nm;
(3) synthetic graphene oxide-loaded 10nm gold grain compound
Add the 1mg/ml graphite oxide aqueous solution of 1ml in gold nano grain solution, mix, 20000 rev/mins of lower water centrifuge washings 6 times, obtain graphene oxide-loaded 10nm gold nano grain compound, add the 5ml deionized water, within ultrasonic 5 minutes, obtain homogeneous solution;
(4) synthesizing graphite alkene load 10nm gold grain compound
Add 10mg NaBH
4in the graphene oxide-loaded 10nm gold nano grain aqueous solution, evenly, room temperature is placed 2 hours in vibration, 20000 rev/mins of washings 6 times, and 60 degrees centigrade of dryings 2 hours, obtain graphene-supported 10nm gold grain compound.
Embodiment 3:
(1) washing, purification
The 1mg graphene oxide is dissolved in 10ml water, after ultrasonic dispersing and dissolving, at 20000 rev/mins, uses respectively 3%HCl and water centrifuge washing 3 times, add deionized water, make uniform 0.1mg/ml graphite oxide aqueous solution;
(2) synthetic graphene oxide@Pt nanoparticle compound
0.01M H by 100ul
2ptCl
6join in the 0.1mg/ml graphite oxide aqueous solution of 10ml, mix, add the NaBH of 1mg
4, under room temperature, to place 3 hours, 20000 rev/mins of lower water centrifuge washings 6 times, obtain graphene oxide-loaded Pt nanoparticle compound, adds the 5ml deionized water, within ultrasonic 5 minutes, obtains homogeneous solution;
(3) synthesizing graphite alkene supported platinum nano particle composites
Add 10mg NaBH
4in the graphene oxide-loaded Pt nanoparticle aqueous solution, evenly, room temperature is placed 2 hours in vibration, 20000 rev/mins of centrifugal washings 6 times, and 60 degrees centigrade of dryings 2 hours, obtain graphene-supported Pt nanoparticle compound.
Embodiment 4:
(1) washing, purification
The 1mg graphene oxide is dissolved in 10ml water, after ultrasonic dispersing and dissolving, at 20000 rev/mins, uses respectively 3%HCl and water centrifuge washing 3 times, add deionized water, make uniform 0.1mg/ml graphite oxide aqueous solution;
(2) synthetic graphene oxide-loaded palladium nano-particles compound
0.01M K by 100ul
2pdCl
6join in the 0.1mg/ml graphite oxide aqueous solution of 10ml, mix, add the NaBH of 1mg
4, under room temperature, to place 3 hours, 20000 rev/mins of lower water centrifuge washings 6 times, obtain graphene oxide-loaded palladium nano-particles compound, adds the 5ml deionized water, within ultrasonic 5 minutes, obtains homogeneous solution;
(3) synthesizing graphite alkene supported palladium nano-particle complex
Add 10mg NaBH
4in the graphene oxide-loaded palladium nano-particles aqueous solution, evenly, room temperature is placed 2 hours in vibration, 20000 rev/mins of centrifugal washings 6 times, and 60 degrees centigrade of dryings 2 hours, obtain graphene-supported palladium nano-particles compound.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. the preparation method of a graphene-supported metal nanoparticle compound, is characterized in that, comprises the steps:
Step 1: graphene oxide is purified 3 times with hydrochloric acid and deionized water washing respectively, obtain pure graphite oxide aqueous solution, and ultrasonic dispersion 15-30 minute; The volumetric concentration that is used for the hydrochloric acid of purification is 2%-4%; Described graphene oxide is made by the Hummer method, and the mass concentration of graphene oxide is 0.1～1mg/ml;
Step 2: by controlledly synthesis, add reducing agent that metal ion precursor solution is reduced to metal nanoparticle, be evenly dispersed in the aqueous solution, obtain the metal nanoparticle aqueous solution; The molar concentration of described metal ion precursor solution is 10
-5mol/L-1 mol/L;
Step 3: the graphite oxide aqueous solution is joined in the metal nanoparticle aqueous solution, be uniformly dispersed under room temperature, obtain once uniform graphene oxide-loaded metal nanoparticle mixed solution;
Step 4: will incite somebody to action once uniform graphene oxide-loaded metal nanoparticle mixed solution centrifugal 15 minutes with the speed of 20000 rev/mins, wash repetition with water 6 times, add deionized water within ultrasonic 5 minutes, to obtain the uniform graphene oxide-loaded metal nanoparticle mixed solution of secondary;
Step 5: add NaBH
4rear reaction 2 hours, use respectively deionized water and ethanol with the speed centrifuge washing of 20000 rev/mins three times, and 60 ℃ of lower vacuum drying 2 hours, obtain graphene-supported metal nanoparticle compound.
2. the preparation method of graphene-supported metal nanoparticle compound according to claim 1, it is characterized in that, described metal nanoparticle comprises, the simple metal of Au Ag Pt Pd, rhodium, ruthenium, iron, cobalt, nickel or by alloy that wherein several metallic elements form.
3. the preparation method of graphene-supported metal nanoparticle compound according to claim 1, is characterized in that, the described method of take prepares the temperature that the applicable ambient temperature range of graphene-supported metal nanoparticle compound is 0 ℃～100 ℃.
4. the preparation method of graphene-supported metal nanoparticle compound according to claim 1, is characterized in that, the applicable reaction PH condition that the described method of take prepares graphene-supported metal nanoparticle compound as pH value be 2-12.
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| JP4484043B2 (en) * | 2004-07-23 | 2010-06-16 | 戸田工業株式会社 | Method for producing Ag nanoparticles |
| KR101337994B1 (en) * | 2010-04-14 | 2013-12-06 | 한국과학기술원 | Graphene/metal nanocomposite powder and method of manufacturing thereof |
| CN101962183B (en) * | 2010-11-09 | 2012-07-04 | 厦门大学 | Amphipathic graphene composite membrane and preparation method thereof |
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| CN108378440A (en) * | 2018-03-15 | 2018-08-10 | 广西中医药大学 | Chinese medicine antibacterial mask containing graphene oxide-copper silver nanoparticle compound |
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