CN107175338A - A kind of trigonal biyramid palladium list twin and its preparation method and application - Google Patents
A kind of trigonal biyramid palladium list twin and its preparation method and application Download PDFInfo
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Abstract
The control preparation field of metal nano material of the present invention, discloses a kind of trigonal biyramid palladium list twin and its preparation method and application.Reduction and peptizaiton of this method using polyvinylpyrrolidone, are not required to extra reducing agent；The nitrate ion for adding freely adjustable dosage improves the controllability of oxide etch as oxide etch agent, the problem of independent oxide etch of dissolved oxygen for having sheltered less content is easily disturbed；Iodide ion is added as the exposure of stable { 100 } crystal face of adsorbent, complexant is also served as and is coordinated to adjust rate of reduction with presoma palladium；Adjusted by pH value with Comprehensive Control nitrate ion and iodide ion dosage so as to obtain the trigonal biyramid palladium list twin of advantage.The present invention has prepared the large scale trigonal biyramid palladium list twin with regular geometrical morphology, operates relatively simple, it is easy to accomplish, controllability is good, and product purity is high.The trigonal biyramid palladium list twin material can be used as catalyst, it can also be used to the field such as optics, electricity.
Description
Technical field
The control preparation field of metal nano material of the present invention, more particularly to a kind of trigonal biyramid palladium list twin and its preparation
Methods and applications.
Background technology
Noble metal nanometer material shows many superior performances, wherein palladium in terms of chemistry, optics, electricity and magnetics
Nanocrystalline price is relatively low, is especially widely used in catalysis and electrochemical field, and for example hydrogenation, the coupling of carbon carbon, electricity are urged
Change oxidation and selective reduction etc..The performance of palladium nano-crystal is generally related to its size and pattern, therefore control one scale of synthesis
Very little and with regular geometrical morphology nanocrystal is always study hotspot.Current document report is passed through using wet chemistry synthesis
Balance controlled and dynamics Controlling can synthesize the palladium nano-crystal of a variety of different-shapes, for example, given birth to by many twin crystal seeds
Long and icosahedron, decahedron, five heavy twin lines, triangular plate, hexagonal piece for coming etc., by single twin seeded growth Lai triangle
Bicone, by single crystal seed grow and Lai cube, octahedron, cuboctahedron, cuboid etc..Research shows, controls palladium
The rate of reduction of presoma is the key of control synthesis palladium nano-crystal, and oxide etch is also the effective of metallic nano crystal control synthesis
One of means, can not only lower rate of reduction, while can be by obtaining the excellent of needs to the selection etching of twin crystal seed
Gesture crystal seed.In numerous palladium nano-crystal kinds, trigonal biyramid palladium list twin is due to { 100 } crystal face of 6 isosceles right triangles of exposure
And possess { 111 } twin plane and corresponding defect, show excellent performance in the reaction such as Oxidation of Formic Acid.But,
Palladium triagonal bipyrimidal is a kind of single twin structure between many twins and monocrystalline, and its synthesis is extremely difficult, especially synthesizes
The higher palladium trigonal biyramid of the more regular purity of pattern has very big challenge.More successfully report for only 2 at present, one
Be Xiaohu Xia etc. (J.Am.Chem.Soc.2013,135,15706) with EG as reducing agent and solvent, PVP makees dispersant,
KI makees adsorbent and oxide etch complexant, controls the oxide etch of dissolved oxygen in reaction solution to obtain by adjusting KI concentration
Obtain the mono- twin trigonal biyramids of 5-15nm；The second is Na Lu etc. (Chem.Mater.2014,26,2453) are used as reduction with formaldehyde
Agent, PVP makees dispersant, and KI makees adsorbent and oxide etch complexant, by adding ethanol or isopropanol and iodide ion phase interaction
For adjusting oxide etch complexant activity so as to control the oxide etch degree of dissolved oxygen in reaction solution, 35- is finally given
45nm single twin trigonal biyramid.It is not difficult to find out, controls oxide etch to be to prepare single twin triangle in above-mentioned more successful synthesis
The key of bipyramid.But, due to the uncontrollability of dissolved oxygen in reaction solution, only by regulating and controlling oxide etch complexant iodide ion
To control oxide etch degree so that whole synthetic system is highly susceptible to interference and causes product purity not high.
The content of the invention
In order to overcome the shortcoming and deficiency of prior art, primary and foremost purpose of the invention is to provide a kind of control synthesis necessarily
Size and with regular geometrical morphology high-purity trigonal biyramid palladium list twin preparation method.
Another object of the present invention is to provide the trigonal biyramid palladium list twin that a kind of above-mentioned preparation method is prepared.
It is still another object of the present invention to provide the application of above-mentioned trigonal biyramid palladium list twin.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of trigonal biyramid palladium list twin, including following operating procedure：By polyvinylpyrrolidone, iodate
Thing and nitrate are soluble in water, stir and evenly mix, and polytetrafluoro has been transferred to after adding palladium salt presoma and regulation pH agent, stirring 10min
The autoclave of ethene liner, by reactor room temperature is cooled to after reacting in an oven with ice bath, is centrifuged, with absolute ethyl alcohol and
Acetone cyclic washing sample, prepares trigonal biyramid palladium list twin.
The iodide are KI (KI) or sodium iodide (NaI)；The nitrate is sodium nitrate (NaNO3) or potassium nitrate
(KNO3)；The palladium salt presoma is one kind in tetrachloro-palladium acid sodium, palladium chloride, palladium acetylacetonate, palladium and palladium nitrate
More than；The regulation pH agent is sodium hydroxide (NaOH) or potassium hydroxide (KOH).
The monomer ethylene pyrrolidones in Pd elements, polyvinylpyrrolidone in the palladium salt presoma, in iodide
I-, NO in nitrate3 -, regulation pH agent in OH-Mol ratio with water is 1：20-70：10-25：5-9：0.4-0.7：
5000-10000。
The temperature reacted in an oven is 180-220 DEG C, reaction time 2-4 hour.
The size of gained trigonal biyramid palladium list twin is 20-30nm.
A kind of trigonal biyramid palladium list twin prepared according to above-mentioned preparation method.
Above-mentioned trigonal biyramid palladium list twin is used as the application in catalyst in optical field, electricity field.
The present invention principle be：
The present invention is to reduce palladium presoma using the reproducibility of polyvinylpyrrolidone (PVP) terminal hydroxyl, not in addition
Reducing agent is added, PVP is used as dispersant both as reducing agent；The nitrate ion for adding freely adjustable dosage simultaneously is made
The controllability of oxide etch is improved for oxide etch agent, the independent oxide etch of dissolved oxygen for having sheltered less content is easily disturbed
The problem of；Iodide ion is added as the exposure of stable { 100 } crystal face of adsorbent, also serve as complexant and the coordination of presoma palladium so as to
Reduce rate of reduction.
PH value is the key factor that rate of reduction is controlled in this reaction, because PVP reducing powers are weaker, and higher pH value can be with
Its rate of reduction is improved, while higher pH value also reduces the speed of oxide etch, can be fitted in this synthetic system
The rate of reduction for closing single twin dominant growth avoids etched Johnson ＆ Johnson into cubic monocrystalline body simultaneously.Experimental result is shown, preferred
PH value condition under excessive nitrate ion can still make initial reaction stage etching is too strong to cause cubic monocrystalline body occur, very few nitre
Acid ion make it is etched it is weak will cause a large amount of five heavy twin lines occur, the appropriate low iodine under suitable nitrate ion concentration
Ion concentration can increase the generation that rate of reduction is conducive to single twin, and Comprehensive Control nitrate ion and iodide ion dosage can be obtained
The single twin for the advantage of obtaining.
The present invention has the following advantages and effect relative to prior art：
(1) using polyvinylpyrrolidone reduction and peptizaiton, by pH value regulation and Comprehensive Control nitrate anion from
Trigonal biyramid palladium list twin can be made in son and iodide ion dosage.
(2) present invention operation is relatively simple, it is easy to accomplish, controllability is good, and product purity is high.Below with example furtherly
It is bright.
Brief description of the drawings
Fig. 1 is the XRD that preferably synthetic condition 1 prepares sample.
Fig. 2 is the TEM figures that preferably synthetic condition 1 prepares sample.
Fig. 3 schemes to prepare the TEM of sample under lower ph.
Fig. 4 schemes to prepare the TEM of sample under the conditions of more nitrate ion.
Fig. 5 schemes to prepare the TEM of sample under the conditions of less nitrate ion.
Fig. 6 schemes to prepare the TEM of sample under the conditions of more iodide ion.
Fig. 7 is the TEM figures that preferably synthetic condition 2 prepares sample.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Embodiment 1 (preferably synthetic condition 1)
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, tetrachloro-palladium acid sodium and NaOH are added, wherein
Specific ratio is Na2PdCl4：PVP：KI：NaNO3：NaOH：H2O=1：35：20：8：0.62：6600 (mol ratio, wherein PVP with
Monomer ethylene pyrrolidones meter), solution ph is about 11, and the autoclave of polytetrafluoroethyllining lining is transferred to after stirring 10min, is dried
Reactor is cooled to rapidly room temperature with ice bath after reaction 3h in case, centrifuged, with absolute ethyl alcohol and acetone cyclic washing sample
Product for several times, is finally scattered in ethanol by product.Gained presoma is characterized using XRD, TEM, XRD and TEM figures point
Fig. 1 and Fig. 2 are not seen.XRD is consistent with the standard spectrogram diffraction maximum of Metal Palladium, shows that Metal Palladium has been made.TEM figures show sample
Projection mainly include three kinds of triangle, irregular quadrangle and rhombus, the projection with trigonal biyramid is consistent, and its size is main
For 20-30nm.Further HRTEM test results show that { 100 } crystal face of 6 isosceles right triangles of exposure has been made really
And possess the trigonal biyramid palladium list twin of { 111 } twin plane.
Comparative example 1 (is synthesized) under lower ph
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, tetrachloro-palladium acid sodium and NaOH are added, wherein
Specific ratio is Na2PdCl4：PVP：KI：NaNO3：NaOH：H2O=1：35：20：8：0.12：6600 (mol ratio, wherein PVP with
Monomer meter), solution ph is about 7, is transferred to after stirring 10min in the autoclave of polytetrafluoroethyllining lining, baking oven after reaction 3h
Reactor is cooled to rapidly room temperature with ice bath, centrifuged, finally will with absolute ethyl alcohol and acetone cyclic washing sample for several times
Product is scattered in ethanol.TEM figures (Fig. 3) show that sample is mainly a large amount of about 40nm cubic monocrystalline body, a small amount of trigonal biyramid
Body and five heavy twin line compositions, show that lower ph etching is too strong and mainly generate cubic monocrystalline body.
Comparative example 2 (is synthesized) under the conditions of more nitrate ion
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, tetrachloro-palladium acid sodium and NaOH are added, wherein
Specific ratio is Na2PdCl4：PVP：KI：NaNO3：NaOH：H2O=1：35：20：10：0.62：6600 (mol ratios, wherein PVP
In terms of monomer), solution ph is about 11, is transferred to after stirring 10min in the autoclave of polytetrafluoroethyllining lining, baking oven and reacts 3h
Reactor is cooled to rapidly room temperature with ice bath afterwards, centrifuged, with absolute ethyl alcohol and acetone cyclic washing sample for several times, finally
Product is scattered in ethanol.TEM figures (Fig. 4) show that sample is mainly cubic monocrystalline body, even if it is excessive to show that etchant is added
Still etch at higher ph values and too strong mainly generate cubic monocrystalline body.
Comparative example 3 (is synthesized) under the conditions of less nitrate ion
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, tetrachloro-palladium acid sodium and NaOH are added, wherein
Specific ratio is Na2PdCl4：PVP：KI：NaNO3：NaOH：H2O=1：35：20：3.5：0.62：6600 (mol ratios, wherein PVP
In terms of monomer), solution ph is about 11, is transferred to after stirring 10min in the autoclave of polytetrafluoroethyllining lining, baking oven and reacts 3h
Reactor is cooled to rapidly room temperature with ice bath afterwards, centrifuged, with absolute ethyl alcohol and acetone cyclic washing sample for several times, finally
Product is scattered in ethanol.TEM figures (Fig. 5) show that sample contains a large amount of five heavy twin lines in addition to trigonal biyramid, show etching
Agent adds deficiency so that etched weak, and substantial amounts of five heavy twin crystal seed is able to retain generation nano wire.
Comparative example 4 (is synthesized) under the conditions of more iodide ion
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, tetrachloro-palladium acid sodium and NaOH are added, wherein
Specific ratio is Na2PdCl4：PVP：KI：NaNO3：NaOH：H2O=1：35：30：8：0.62：6600 (mol ratio, wherein PVP with
Monomer meter), solution ph is about 11, is transferred to after stirring 10min in the autoclave of polytetrafluoroethyllining lining, baking oven after reaction 3h
Reactor is cooled to rapidly room temperature with ice bath, centrifuged, finally will with absolute ethyl alcohol and acetone cyclic washing sample for several times
Product is scattered in ethanol.TEM figures (Fig. 6) show that sample is mainly five heavy twin lines, show that iodide ion is dropped by coordination
The low rate of reduction of palladium, and slower rate of reduction is conducive to the anisotropic growth of nano wire.In this instance, iodide ion
Due to being coordinated so as to which the effect etched to initial reaction stage crystal seed selective oxidation is not obvious.
Embodiment 2 (preferably synthetic condition 2)
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, tetrachloro-palladium acid sodium and NaOH are added, wherein
Specific ratio is Na2PdCl4：PVP：KI：NaNO3：NaOH：H2O=1：35：15：8：0.62：6600 (mol ratio, wherein PVP with
Monomer meter), solution ph is about 11, is transferred to after stirring 10min in the autoclave of polytetrafluoroethyllining lining, baking oven after reaction 3h
Reactor is cooled to rapidly room temperature with ice bath, centrifuged, finally will with absolute ethyl alcohol and acetone cyclic washing sample for several times
Product is scattered in ethanol.TEM figures (Fig. 7) show that sample is mainly trigonal biyramid palladium list twin.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of trigonal biyramid palladium list twin, it is characterised in that including following operating procedure：By polyvinyl pyrrole
Alkanone, iodide and nitrate are soluble in water, stir and evenly mix, and are transferred to after adding palladium salt presoma and regulation pH agent, stirring 10min
There is the autoclave of polytetrafluoroethyllining lining, reactor is cooled to room temperature with ice bath after reacting in an oven, centrifuge, with nothing
Water-ethanol and acetone cyclic washing sample, prepare trigonal biyramid palladium list twin.
2. a kind of preparation method of trigonal biyramid palladium list twin according to claim 1, it is characterised in that：The iodide
For KI or sodium iodide；The nitrate is sodium nitrate or potassium nitrate；The palladium salt presoma is tetrachloro-palladium acid sodium, dichloride
One or more of palladium, palladium acetylacetonate, palladium and palladium nitrate；The regulation pH agent is sodium hydroxide or potassium hydroxide.
3. a kind of preparation method of trigonal biyramid palladium list twin according to claim 1, it is characterised in that：Before the palladium salt
Drive the Pd elements in body, the monomer ethylene pyrrolidones in polyvinylpyrrolidone, the I in iodide-, NO in nitrate3 -、
Adjust the OH in pH agent-Mol ratio with water is 1：20-70：10-25：5-9：0.4-0.7：5000-10000.
4. a kind of preparation method of trigonal biyramid palladium list twin according to claim 1, it is characterised in that：It is described in baking oven
The temperature of middle reaction is 180-220 DEG C, reaction time 2-4 hour.
5. a kind of preparation method of trigonal biyramid palladium list twin according to claim 1, it is characterised in that：Gained triangle is double
The size for boring palladium list twin is 20-30nm.
6. the trigonal biyramid palladium list twin that a kind of preparation method according to claim any one of 1-5 is prepared.
7. trigonal biyramid palladium list twin according to claim 6 is used as answering in catalyst in optical field, electricity field
With.
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| CN101538735A (en) * | 2008-03-17 | 2009-09-23 | 国家纳米科学中心 | Nano or micron-scale gold disk and preparation method thereof |
| WO2010108158A2 (en) * | 2009-03-20 | 2010-09-23 | Northwestern University | Plasmon mediated, photoinduced synthesis of triangular bipyramids |
| CN103143718A (en) * | 2011-12-07 | 2013-06-12 | 中国科学院大连化学物理研究所 | Platinum nanometer material and preparation method thereof |
| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
| CN105127446A (en) * | 2015-09-18 | 2015-12-09 | 温州大学 | Precious-metal nanometer bipyramid and preparing method thereof |
| CN105834451A (en) * | 2016-05-25 | 2016-08-10 | 东华大学 | Preparation method for gold nanoparticle bipyramids |
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- 2017-04-10 CN CN201710229157.5A patent/CN107175338B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538735A (en) * | 2008-03-17 | 2009-09-23 | 国家纳米科学中心 | Nano or micron-scale gold disk and preparation method thereof |
| WO2010108158A2 (en) * | 2009-03-20 | 2010-09-23 | Northwestern University | Plasmon mediated, photoinduced synthesis of triangular bipyramids |
| CN103143718A (en) * | 2011-12-07 | 2013-06-12 | 中国科学院大连化学物理研究所 | Platinum nanometer material and preparation method thereof |
| CN104625086A (en) * | 2015-02-10 | 2015-05-20 | 纳米籽有限公司 | Gold nanoparticle triangular plate preparing method and method for preparing gold nanoparticle discs and gold nanoparticle hexagonal pieces on basis of gold nanoparticle triangular plate preparing method |
| CN105127446A (en) * | 2015-09-18 | 2015-12-09 | 温州大学 | Precious-metal nanometer bipyramid and preparing method thereof |
| CN105834451A (en) * | 2016-05-25 | 2016-08-10 | 东华大学 | Preparation method for gold nanoparticle bipyramids |
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