CN105537614A - Method for preparing hollow precious metal nano material with cuprous oxide as template - Google Patents
Method for preparing hollow precious metal nano material with cuprous oxide as template Download PDFInfo
- Publication number
- CN105537614A CN105537614A CN201510994851.7A CN201510994851A CN105537614A CN 105537614 A CN105537614 A CN 105537614A CN 201510994851 A CN201510994851 A CN 201510994851A CN 105537614 A CN105537614 A CN 105537614A
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- CN
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- Prior art keywords
- cuprous oxide
- noble metal
- nanometer material
- hollow
- metal nanometer
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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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for preparing a hollow precious metal nano material with cuprous oxide as a template. The method for preparing the hollow precious metal nano material with the cuprous oxide as the template comprises the following steps that (1) the cuprous oxide is evenly dispersed into low-molecular alcohol, precious metal salt is added into the low-molecular alcohol solution under the stirring condition, and ultrasonic stirring and mixing are conducted; (2) the mixed liquor obtained in the step (1) is dropwise added into water for a reaction; and (3) cuprous oxide nucleuses are removed after the reaction is completed, and the hollow precious metal nano material is obtained. According to the method, the cuprous oxide and the precious metal salt are ultrasonically stirred and mixed in the low-molecular alcohol firstly, and then the mixed liquor is added into water for the reaction, so that the defect of a nonuniform reaction of a conventional method is overcome, and the uniform hollow precious metal nano material accurately duplicating the morphology of the cuprous oxide template is prepared.
Description
Technical field
The present invention relates to hollow nano-material technical field, being specifically related to a kind of take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation.
Background technology
Hollow nanostructured have large specific area and abundant pore structure, small component units such as nano particle, nanocube, nanometer sheet etc. constitute the porous wall of hollow-core construction, make it have unique performance in actual applications, a large amount of guest molecules or larger-size molecule can be held.And the noble metal nanometer material with hollow-core construction combines the advantage of hollow-core construction and noble metal nano particles, have that density is low, specific area be large, the character such as high stability and Surface Permeability, there is more active site, electro catalytic activity increases substantially, and has special application prospect in fields such as biochemistry, catalysis, material science.And due to noble metal costly, hollow-core construction both can increase substantially electro catalytic activity, in turn saved cost.
Cu
2o is a kind of P-type semiconductor, has more application in energy storage, catalysis and sensor field.Cu
2o/Cu oxidation-reduction pair value (0.36V) is than precious metals pt Cl
6 2/ Pt(0.735V), PdCl
4 2/ Pd(0.987V) etc. noble metal much lower, therefore Cu
2o can with PtCl
6 2, PdCl
4 2deng there is spontaneous oxidation reduction reaction thus the object reached at its Surface coating precious metal element, finally remove Cu
2o template obtains based on Cu
2the noble metal hollow structure of O pattern.With Cu
2o prepares noble metal hollow material have the following advantages for sacrificing template: (1) avoids the use of reducing agent thus the negative effect decreased environment; (2) Cu
2o production cost is low, and technical maturity is easy to control, suitable for mass production; (3) Cu
2the diversity of O pattern and size also for design with synthesize different polynary noble metal hollow structure and provide support.
Cuprous oxide is utilized for the method for the hollow noble metal nanometer material of Template preparation to be at present: first by Cu
2precious metal salt solution, in water, is then joined Cu by O ultrasonic disperse under agitation
2in O suspension, through being obtained by reacting the coated Cu of noble metal
2o core, finally removes Cu
2o template, obtains based on Cu
2the noble metal hollow structure of O pattern.These class methods join Cu at precious metal salt solution
2time in O suspension, the uneven meeting due to reactant in system causes the Cu first contacting precious metal salt
2o, by excessively coated, causes the uneven of reaction, thus causes the inhomogeneities of final hollow noble metal nanometer material, shows as and accurately can not copy template pattern, the fragmentation of a large amount of local and surface roughness increase.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, can obtain the hollow noble metal nanometer material accurately copying cuprous oxide template pattern uniformly.
For achieving the above object, the invention provides following technical scheme:
Take cuprous oxide as a method for the hollow noble metal nanometer material of Template preparation, comprise the following steps:
(1) be dispersed in low mass molecule alcohol by cuprous oxide, add the low mass molecule alcohol solution of precious metal salt under agitation, ultrasonic agitation mixes;
(2) mixed liquor that step (1) obtains is added dropwise in water reacts;
(3) react rear removal cuprous oxide core, obtain hollow noble metal nanometer material.
Further, described cuprous oxide is the cuprous oxide of cubic structure.
Further, the cuprous oxide of described cubic structure is prepared by following methods: under 50-60 DEG C of stirring condition, toward CuCl
2add excessive NaOH solution reaction 0.5-1h in solution, and then slowly drip ascorbic acid solution, centrifugal after reaction 3-4h, then use water and ethanol purge respectively, last vacuum drying, obtain the cuprous oxide of cubic structure.
Further, in described step (1), the anion of precious metal salt is PtCl
6 2or/and PdCl
4 2 .
Further, in described step (1), precious metal salt is H
2ptCl
6or/and Na
2pdCl
4.
Further, in described step (1), low mass molecule alcohol is one or more in methyl alcohol, ethanol and ethylene glycol.
Further, in described step (1), the precious metal salt added and the mol ratio of cuprous oxide are 1.4-2.3:1.
Further, in described step (1), ultrasonic agitation mixing 60-90min at 20-25 DEG C.
Further, in described step (2), mixed liquor is added dropwise in the water of 10-15 times of volume with the rate of addition of 12-20ml/min and reacts 30-60min.
Further, in described step (3), by product centrifugal 2-5min under 4000-10000 turns condition after having reacted, cuprous oxide core is removed in the ammoniacal liquor complexing adding 18%-25%, then the nitric acid adding 0.1-0.5mol/L reacts the copper removed disproportionated reaction and produce at 10-25 DEG C, obtains hollow noble metal nanometer material.
Beneficial effect of the present invention is:
The present invention adopts the first ultrasonic agitation mixing in low mass molecule alcohol by cuprous oxide and precious metal salt, be added dropwise to the method for reacting in water again, overcome the shortcoming that the reaction of conventional method is uneven, prepare the hollow noble metal nanometer material accurately copying cuprous oxide template pattern uniformly.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearly, the invention provides following accompanying drawing and being described:
Fig. 1 is the stereoscan photograph of cube hollow Pt nano material prepared by embodiment 1;
Fig. 2 is the stereoscan photograph of cube hollow Pt nano material prepared by comparative example 1.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
According to the diversity of cuprous oxide pattern and size, can design and synthesize the hollow noble metal nanometer material of different structure, following examples and comparative example are for the cuprous oxide of cubic structure.
The cuprous oxide of the cubic structure that following examples and comparative example are used is prepared by following methods:
Under 55 DEG C of stirring conditions, be the CuCl of 0.01mol/L to 100ml concentration
2add the NaOH solution that 10mL concentration is 2mol/L in solution, after reaction 0.5h, more slowly dropwise add the ascorbic acid solution that 10ml concentration is 0.6mol/L, after reaction 3h, centrifugal, use water and ethanol purge respectively, last 40 DEG C of vacuum drying 12h, obtain the cuprous oxide of cubic structure.
embodiment 1
Embodiment 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, comprise the following steps:
(1) cuprous oxide of 10mg cubic structure is dispersed in 10ml ethanol, adds the H of 20mM under agitation
2ptCl
6ethanolic solution, makes H
2ptCl
6be 1.4:1 with the mol ratio of cuprous oxide, ultrasonic agitation mixing 60min at 25 DEG C;
(2) mixed liquor step (1) obtained is added dropwise to the rate of addition of 20ml/min in the water of 15 times of volumes and reacts 30min;
(3) by product centrifugal 5min under 5000 turns of conditions after having reacted, cuprous oxide core has been removed in the ammoniacal liquor complexing adding 20%, and the nitric acid then adding 0.1mol/L reacts the copper removed disproportionated reaction and produce at 25 DEG C, obtains a cube hollow Pt nano material.
embodiment 2
Embodiment 2 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, comprise the following steps:
(1) cuprous oxide of 10mg cubic structure is dispersed in 10ml methyl alcohol, adds the Na of 30mM under agitation
2pdCl
4methanol solution, makes Na
2pdCl
4be 2.0:1 with the mol ratio of cuprous oxide, ultrasonic agitation mixing 70min at 25 DEG C;
(2) mixed liquor step (1) obtained is added dropwise to the rate of addition of 15ml/min in the water of 12 times of volumes and reacts 50min;
(3) by product centrifugal 5min under 8000 turns of conditions after having reacted, cuprous oxide core has been removed in the ammoniacal liquor complexing adding 20%, and the nitric acid then adding 0.2mol/L reacts the copper removed disproportionated reaction and produce at 20 DEG C, obtains a cube hollow Pd nano material.
embodiment 3
Embodiment 3 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, comprise the following steps:
(1) cuprous oxide of 10mg cubic structure is dispersed in 10ml ethylene glycol, adds the H of 20mM under agitation
2ptCl
6the Na of ethylene glycol solution and 30mM
2pdCl
4ethylene glycol solution, makes H
2ptCl
6and Na
2pdCl
4the mol ratio of sum and cuprous oxide is 2.3:1, ultrasonic agitation mixing 90min at 20 DEG C;
(2) mixed liquor step (1) obtained is added dropwise to the rate of addition of 12ml/min in the water of 10 times of volumes and reacts 60min;
(3) by product centrifugal 2min under 10000 turns of conditions after having reacted, cuprous oxide core has been removed in the ammoniacal liquor complexing adding 18%, and the nitric acid then adding 0.5mol/L reacts the copper removed disproportionated reaction and produce at 10 DEG C, obtains a cube hollow PtPd nano material.
comparative example 1
Comparative example 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, comprise the following steps:
(1) cuprous oxide of 10mg cubic structure is dispersed in 10ml water, adds the H of 20mM under agitation
2ptCl
6the aqueous solution, makes H
2ptCl
6be 1.4:1 with the mol ratio of cuprous oxide, stirring reaction 60min at 25 DEG C;
(2) by product centrifugal 5min under 5000 turns of conditions after having reacted, cuprous oxide core has been removed in the ammoniacal liquor complexing adding 20%, and the nitric acid then adding 0.1mol/L reacts the copper removed disproportionated reaction and produce at 25 DEG C, obtains a cube hollow Pt nano material.
The stereoscan photograph of cube hollow Pt nano material prepared by embodiment 1 and comparative example 1 as depicted in figs. 1 and 2, the roughness of cube hollow Pt nano material prepared by embodiment 1 is 10-20nm, and the roughness of cube hollow Pt nano material prepared by comparative example 1 is 20-50nm.
As can be seen from the above results, comparative example 1 reacts uneven, causes cube hollow Pt nano material that obtains uneven, can not accurately copy template pattern, occurs the broken and surface roughness increase in a large amount of local; And embodiment 1 overcomes the uneven shortcoming of reaction, cube hollow Pt nano material obtained evenly and accurately copy template pattern.
What finally illustrate is, above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by above preferred embodiment to invention has been detailed description, but those skilled in the art are to be understood that, various change can be made to it in the form and details, and not depart from claims of the present invention limited range.
Claims (10)
1. be a method for the hollow noble metal nanometer material of Template preparation with cuprous oxide, it is characterized in that: comprise the following steps:
(1) be dispersed in low mass molecule alcohol by cuprous oxide, add the low mass molecule alcohol solution of precious metal salt under agitation, ultrasonic agitation mixes;
(2) mixed liquor that step (1) obtains is added dropwise in water reacts;
(3) react rear removal cuprous oxide core, obtain hollow noble metal nanometer material.
2. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, it is characterized in that: described cuprous oxide is the cuprous oxide of cubic structure.
3. according to claim 2 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, it is characterized in that: the cuprous oxide of described cubic structure is prepared by following methods: under 50-60 DEG C of stirring condition, toward CuCl
2add excessive NaOH solution reaction 0.5-1h in solution, and then slowly drip ascorbic acid solution, centrifugal after reaction 3-4h, then use water and ethanol purge respectively, last vacuum drying, obtain the cuprous oxide of cubic structure.
4. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, and it is characterized in that: in described step (1), the anion of precious metal salt is PtCl
6 2or/and PdCl
4 2 .
5. according to claim 4 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, and it is characterized in that: in described step (1), precious metal salt is H
2ptCl
6or/and Na
2pdCl
4.
6. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, and it is characterized in that: in described step (1), low mass molecule alcohol is one or more in methyl alcohol, ethanol and ethylene glycol.
7. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, and it is characterized in that: in described step (1), the precious metal salt added and the mol ratio of cuprous oxide are 1.4-2.3:1.
8. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, it is characterized in that: in described step (1), ultrasonic agitation mixing 60-90min at 20-25 DEG C.
9. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, it is characterized in that: in described step (2), mixed liquor is added dropwise in the water of 10-15 times of volume with the rate of addition of 12-20ml/min and reacts 30-60min.
10. according to claim 1 take cuprous oxide as the method for the hollow noble metal nanometer material of Template preparation, it is characterized in that: in described step (3), by product centrifugal 2-5min under 4000-10000 turns condition after having reacted, cuprous oxide core is removed in the ammoniacal liquor complexing adding 18%-25%, then the nitric acid adding 0.1-0.5mol/L reacts the copper removed disproportionated reaction and produce at 10-25 DEG C, obtains hollow noble metal nanometer material.
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|---|---|---|---|
| CN201711108148.7A CN107900374B (en) | 2015-12-28 | 2015-12-28 | Preparation method of cubic platinum nano material with good uniformity |
| CN201510994851.7A CN105537614B (en) | 2015-12-28 | 2015-12-28 | A kind of method that hollow noble metal nanometer material is prepared using cuprous oxide as template |
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| CN201510994851.7A CN105537614B (en) | 2015-12-28 | 2015-12-28 | A kind of method that hollow noble metal nanometer material is prepared using cuprous oxide as template |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109055961A (en) * | 2018-08-29 | 2018-12-21 | 深圳先进技术研究院 | A kind of noble metal support type nanometer frame catalyst and its preparation method and application |
| CN112028109A (en) * | 2020-08-24 | 2020-12-04 | 广东省医疗器械研究所 | Composite nano material and preparation method and application thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109759135B (en) * | 2019-02-02 | 2020-02-21 | 哈尔滨工业大学 | Preparation method of composite material for removing heavy metal/hydrophobic ppcps in reclaimed water |
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| CN109055961A (en) * | 2018-08-29 | 2018-12-21 | 深圳先进技术研究院 | A kind of noble metal support type nanometer frame catalyst and its preparation method and application |
| CN112028109A (en) * | 2020-08-24 | 2020-12-04 | 广东省医疗器械研究所 | Composite nano material and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107900374A (en) | 2018-04-13 |
| CN107900374B (en) | 2020-06-23 |
| CN105537614B (en) | 2017-11-28 |
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