CN107175338B - 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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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
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- 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
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- 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
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/66—Crystals of complex geometrical shape, e.g. tubes, cylinders
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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.This method utilizes the reduction and peptizaiton of polyvinylpyrrolidone, is not required to additional reducing agent；The nitrate ion that freely adjustable dosage is added improves the controllability of oxide etch as oxide etch agent, has sheltered the problem of independent oxide etch of dissolved oxygen of less content is vulnerable to interference；The exposure that iodide ion stablizes { 100 } crystal face as adsorbent is added, is also coordinated as complexant and presoma palladium to adjust rate of reduction；It is adjusted with comprehensively control nitrate ion and iodide ion dosage by pH value 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 fields such as optics, electricity.
Description
Technical field
The control preparation field of metal nano material of the present invention, in particular to a kind of trigonal biyramid palladium list twin and its preparation
Methods and applications.
Background technique
Noble metal nanometer material chemistry, optics, electricity and in terms of show many superior performances, wherein palladium
Nanocrystalline price is relatively low, is especially widely used in catalysis and electrochemical field, such as plus hydrogen, carbon carbon are coupled, electricity is urged
Change oxidation and selective reduction etc..The performance of palladium nano-crystal is usually related to its size and shape, therefore controls one scale of synthesis
Very little and with regular geometrical morphology nanocrystal is always research hotspot.Document report is passed through using wet chemistry synthesis at present
Balance controlled and dynamics Controlling can synthesize the palladium nano-crystal of a variety of different-shapes, such as raw by more twin crystal seeds
Long icosahedron, decahedron, five heavy twin lines, triangular plate, hexagonal piece etc., the triangle from the growth of single twin crystal seed
Bicone, cube, octahedron, cuboctahedron, cuboid etc. from single crystal seed growth.Studies have shown that control palladium
The rate of reduction of presoma is the key that 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 etched by the selection to twin crystal seed to obtain the excellent of needs
Gesture crystal seed.In numerous palladium nano-crystal kinds, { 100 } crystal face of trigonal biyramid palladium list twin due to 6 isosceles right triangles of exposure
And possess { 111 } twin plane and corresponding defect, excellent performance is shown in the reaction such as Oxidation of Formic Acid.But
Palladium triagonal bipyrimidal is a kind of single twin structure between more twins and monocrystalline, and synthesis is extremely difficult, is especially synthesized
The higher palladium trigonal biyramid of the more regular purity of pattern has very big challenge.It more successfully reports for only 2 at present, one
It is that Xiaohu Xia etc. (J.Am.Chem.Soc.2013,135,15706) uses EG as reducing agent and solvent, PVP makees dispersing agent,
KI makees adsorbent and oxide etch complexant, controls the oxide etch of dissolved oxygen in reaction solution by adjusting KI concentration to obtain
Obtain the mono- twin trigonal biyramid of 5-15nm；The second is Na Lu etc. (Chem.Mater.2014,26,2453) uses formaldehyde as reduction
Agent, PVP make dispersing agent, and KI makees adsorbent and oxide etch complexant, pass through addition ethyl alcohol or isopropanol and iodide ion phase interaction
For adjusting oxide etch complexant activity to control the oxide etch degree of dissolved oxygen in reaction solution, 35- is finally obtained
Single twin trigonal biyramid of 45nm.It is not difficult to find out that controlling oxide etch in above-mentioned more successful synthesis is to prepare single twin triangle
The key of bipyramid.But due to the uncontrollability of dissolved oxygen in reaction solution, only pass through regulation oxide etch complexant iodide ion
Come control oxide etch degree make entire synthetic system be highly susceptible to interference cause product purity not high.
Summary of the invention
In order to overcome the disadvantages and deficiencies of the prior art, the primary purpose of the present invention is that provide a kind of control synthesis certain
The preparation method of size and the high-purity trigonal biyramid palladium list twin with regular geometrical morphology.
Another object of the present invention is to provide a kind of trigonal biyramid palladium list twins that above-mentioned preparation method is prepared.
A further object of the present invention is to provide the applications of above-mentioned trigonal biyramid palladium list twin.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method of trigonal biyramid palladium list twin, including following operating procedure: by polyvinylpyrrolidone, iodate
Object and nitrate are soluble in water, stir and evenly mix, and palladium salt presoma is added and adjusts pH agent, has been transferred to polytetrafluoro after stirring 10min
Reaction kettle with ice bath is cooled to room temperature after reacting in an oven by the autoclave of ethylene liner, is centrifugated, with dehydrated alcohol and
Acetone washing sample repeatedly, is prepared trigonal biyramid palladium list twin.
The iodide are potassium iodide (KI) or sodium iodide (NaI)；The nitrate is sodium nitrate (NaNO3) or potassium nitrate
(KNO3)；The palladium salt presoma is one of sodium tetrachloropallate, palladium chloride, palladium acetylacetonate, palladium acetate and palladium nitrate
More than；The adjusting pH agent is sodium hydroxide (NaOH) or potassium hydroxide (KOH).
The monomer ethylene pyrrolidones in Pd element, polyvinylpyrrolidone in the palladium salt presoma, in iodide
I-, NO in nitrate3 -, adjust 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 being prepared according to above-mentioned preparation method.
Above-mentioned trigonal biyramid palladium list twin is in optical field, electricity field as the application in catalyst.
The principle of the present invention is:
The present invention is to restore palladium presoma using the reproducibility of polyvinylpyrrolidone (PVP) terminal hydroxyl, not in addition
Reducing agent is added, PVP is not only used as reducing agent, but also as dispersing agent；The nitrate ion that freely adjustable dosage is added simultaneously is made
The controllability that oxide etch is improved for oxide etch agent has sheltered the independent oxide etch of dissolved oxygen of less content vulnerable to interference
The problem of；The exposure that iodide ion stablizes { 100 } crystal face as adsorbent is added, be also coordinated as complexant and presoma palladium thus
Reduce rate of reduction.
PH value is that the key factor of rate of reduction is controlled in this reaction, and because PVP reducing power is weaker, higher pH value can be with
Its rate of reduction is improved, while higher pH value also reduces the rate of oxide etch, can be fitted in this synthetic system
The rate of reduction for closing single twin dominant growth avoids etched Johnson & Johnson at 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 lead to cubic monocrystalline body occur, very few nitre
Acid ion makes etched weak will lead to 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 comprehensively control nitrate ion and iodide ion dosage can obtain
The single twin for the advantage of obtaining.
The present invention has the following advantages and effects with respect to the prior art:
(1) utilize polyvinylpyrrolidone reduction and peptizaiton, by pH value adjust and comprehensively control nitrate anion from
Trigonal biyramid palladium list twin can be made in son and iodide ion dosage.
(2) operation of the present invention is relatively simple, it is easy to accomplish, controllability is good, and product purity is high.Below furtherly with example
It is bright.
Detailed description of the invention
Fig. 1 is the XRD diagram that preferably synthetic condition 1 prepares sample.
Fig. 2 is the TEM figure that preferably synthetic condition 1 prepares sample.
Fig. 3 is the TEM figure that sample is prepared 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 figure that preferably synthetic condition 2 prepares sample.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1 (preferably synthetic condition 1)
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, sodium tetrachloropallate and NaOH is added, wherein
Specific ratio is Na2PdCl4: PVP:KI:NaNO3: NaOH:H2O=1:35:20:8:0.62:6600 (molar 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
Reaction kettle is cooled to rapidly room temperature with ice bath after reaction 3h in case, is centrifugated, washs sample repeatedly with dehydrated alcohol and acetone
Product for several times, finally disperse product in ethyl alcohol.Gained presoma is characterized using XRD, TEM, XRD diagram and TEM figure point
Fig. 1 and Fig. 2 are not seen.XRD diagram is consistent with the standard spectrogram diffraction maximum of Metal Palladium, shows that Metal Palladium has been made.TEM figure shows sample
Projection mainly include triangle, irregular quadrangle and three kinds of diamond shape, consistent with the projection of trigonal biyramid, size is main
For 20-30nm.Further HRTEM test result shows { 100 } crystal face that 6 isosceles right triangles of exposure have been made really
And possess the trigonal biyramid palladium list twin of { 111 } twin plane.
Comparative example 1 (synthesizes) under lower ph
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, sodium tetrachloropallate and NaOH is added, wherein
Specific ratio is Na2PdCl4: PVP:KI:NaNO3: NaOH:H2O=1:35:20:8:0.12:6600 (molar ratio, wherein PVP with
Monomer meter), solution ph is about 7, the autoclave of polytetrafluoroethyllining lining is transferred to after stirring 10min, after reacting 3h in baking oven
Reaction kettle is cooled to rapidly room temperature with ice bath, is centrifugated, washing sample for several times, finally will repeatedly with dehydrated alcohol and acetone
Product is scattered in ethyl alcohol.TEM schemes (Fig. 3) and shows that sample is mainly cubic monocrystalline body, a small amount of trigonal biyramid of a large amount of about 40nm
Body and five heavy twin line compositions, show that lower ph etching is too strong and mainly generate cubic monocrystalline body.
Comparative example 2 (synthesizes) under the conditions of more nitrate ion
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, sodium tetrachloropallate and NaOH is added, wherein
Specific ratio is Na2PdCl4: PVP:KI:NaNO3: NaOH:H2O=1:35:20:10:0.62:6600 (molar ratio, wherein PVP
In terms of monomer), solution ph is about 11, and the autoclave of polytetrafluoroethyllining lining is transferred to after stirring 10min, reacts 3h in baking oven
Reaction kettle is cooled to rapidly room temperature with ice bath afterwards, is centrifugated, with dehydrated alcohol and acetone repeatedly washing sample for several times, finally
It disperses product in ethyl alcohol.TEM schemes (Fig. 4) and shows that sample is mainly cubic monocrystalline body, even if it is excessive to show that etchant is added
It still etches at higher ph values and too strong mainly generates cubic monocrystalline body.
Comparative example 3 (synthesizes) under the conditions of less nitrate ion
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, sodium tetrachloropallate and NaOH is added, wherein
Specific ratio is Na2PdCl4: PVP:KI:NaNO3: NaOH:H2O=1:35:20:3.5:0.62:6600 (molar ratio, wherein PVP
In terms of monomer), solution ph is about 11, and the autoclave of polytetrafluoroethyllining lining is transferred to after stirring 10min, reacts 3h in baking oven
Reaction kettle is cooled to rapidly room temperature with ice bath afterwards, is centrifugated, with dehydrated alcohol and acetone repeatedly washing sample for several times, finally
It disperses product in ethyl alcohol.TEM figure (Fig. 5) shows that sample contains a large amount of five heavy twin lines in addition to trigonal biyramid, shows to etch
Agent be added deficiency make it is etched weak, a large amount of five heavy twin crystal seed be able to retain generate nano wire.
Comparative example 4 (synthesizes) under the conditions of more iodide ion
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, sodium tetrachloropallate and NaOH is added, wherein
Specific ratio is Na2PdCl4: PVP:KI:NaNO3: NaOH:H2O=1:35:30:8:0.62:6600 (molar ratio, wherein PVP with
Monomer meter), solution ph is about 11, the autoclave of polytetrafluoroethyllining lining is transferred to after stirring 10min, after reacting 3h in baking oven
Reaction kettle is cooled to rapidly room temperature with ice bath, is centrifugated, washing sample for several times, finally will repeatedly with dehydrated alcohol and acetone
Product is scattered in ethyl alcohol.TEM schemes (Fig. 6) and shows that sample is mainly five heavy twin lines, shows 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 to be not obvious to the effect of initial reaction stage crystal seed selective oxidation etching.
Embodiment 2 (preferably synthetic condition 2)
By a certain proportion of polyvinylpyrrolidone, KI, NaNO3It is soluble in water, sodium tetrachloropallate and NaOH is added, wherein
Specific ratio is Na2PdCl4: PVP:KI:NaNO3: NaOH:H2O=1:35:15:8:0.62:6600 (molar ratio, wherein PVP with
Monomer meter), solution ph is about 11, the autoclave of polytetrafluoroethyllining lining is transferred to after stirring 10min, after reacting 3h in baking oven
Reaction kettle is cooled to rapidly room temperature with ice bath, is centrifugated, washing sample for several times, finally will repeatedly with dehydrated alcohol and acetone
Product is scattered in ethyl alcohol.TEM schemes (Fig. 7) and shows that sample is mainly trigonal biyramid palladium list twin.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (6)
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 palladium salt presoma is added and adjusts pH agent, in palladium salt presoma
The I in monomer ethylene pyrrolidones, iodide in Pd element, polyvinylpyrrolidone-, NO in nitrate3 -, adjust pH agent
In OH-Mol ratio with water is 1:20-70:10-25:5-9:0.4-0.7:5000-10000, pH value of solution 11, stirring
It is transferred to the autoclave of polytetrafluoroethyllining lining after 10min, reaction kettle is cooled to room temperature with ice bath after reacting in an oven, from
Trigonal biyramid palladium list twin is prepared with dehydrated alcohol and acetone washing sample repeatedly in heart separation.
2. a kind of preparation method of trigonal biyramid palladium list twin according to claim 1, it is characterised in that: the iodide
For potassium iodide or sodium iodide；The nitrate is sodium nitrate or potassium nitrate；The palladium salt presoma is sodium tetrachloropallate, dichloride
One or more of palladium, palladium acetylacetonate, palladium acetate and palladium nitrate；The adjusting 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: described in baking oven
The temperature of middle reaction is 180-220 DEG C, reaction time 2-4 hour.
4. 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.
5. a kind of trigonal biyramid palladium list twin that preparation method according to claim 1-4 is prepared.
6. trigonal biyramid palladium list twin according to claim 5 is in optical field, electricity field as answering in catalyst
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 |
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