CN102059346B - Method for preparing aurum-manganese dioxide nuclear shell structure nano particle - Google Patents
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- CN102059346B CN102059346B CN201010579638A CN201010579638A CN102059346B CN 102059346 B CN102059346 B CN 102059346B CN 201010579638 A CN201010579638 A CN 201010579638A CN 201010579638 A CN201010579638 A CN 201010579638A CN 102059346 B CN102059346 B CN 102059346B
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Abstract
The invention discloses a method for preparing an aurum-manganese dioxide nuclear shell structure nano particle, which relates to a nano particle. The invention provides a method for preparing an aurum-manganese dioxide nuclear shell structure nano particle. The synthesizing method has the characteristics of simple synthesizing process, short cycle, high yield, and the like. The method comprises the following steps of: preparing an aurum nano particle with the particle diameter of 20-55nm; preparing an aurum nano particle with the particle diameter of 56-200nm; and finally growing an ultrathin and dense manganese dioxide shell layer on the surface of the aurum nano particle to obtain the aurum-manganese dioxide nuclear shell structure nano particle. The invention has wide application prospect in electro-catalysis, Raman spectrometric detection and organic matter and pollutant treatment.
Description
Technical field
The present invention relates to a kind of nano particle, especially relate to the preparation method of a kind of gold-manganese dioxide core-shell structure nanometer particle.
Background technology
The composite nanoparticle that metal and semiconductor are formed has extremely important application in fields such as photochemistry, electrochemistry, catalysis and biologies.Its main existence form is the semiconductor coated metal, i.e. the metal-semiconductor core-shell structure nanometer particle.The specific function that this type composite nanoparticle is had is to be caused by metal and semi-conductive physics and chemical interaction.Because some physics and chemical action, have distant effect like the surperficial enhanced activity of catalytic performance and Raman spectrum, obvious more apart from shorter effect, therefore, semi-conductive shell thickness plays critical effect for the performance of composite nanoparticle.Simultaneously, the compactness of shell is also to the performance important influence of composite nanoparticle, can prevent to come from the interference of examining metal such as the shell of densification.Yet because metal and semiconductor lattice do not match, the metal-semiconductor core-shell structure nanometer particle for preparing ultra-thin densification is a kind of great challenge.This type of nano particle of being reported on the document at present exists problems such as shell thickness is excessive, shell is loose porous, has seriously limited the range of application of metal-semiconductor core-shell structure nanometer particle.Be reported in like (Xiao F.Wu.et al.Langmuir 2009,25,6438) such as Xiao F.Wu under the condition of hydro-thermal with ascorbic acid and reduce TiF
4Prepared AuTiO
2Core-shell structure nanometer particle is the loose out-of-shape of shell not only, and thickness is also excessive, reaches tens nm.And for example Jin M.Zhu etc. (Jin M.Zhu.et al.J Mater Chem 2009,19,8871) the report AuAg nano particle that will obtain in advance with thiocarbamide is converted into AuAg
2The S nano particle, the AuAg of gained
2The shell of S nano particle is the structure of ghost.
Summary of the invention
The object of the invention aims to provide the preparation method of a kind of gold-manganese dioxide core-shell structure nanometer particle, and this synthetic method has that building-up process is simple, the cycle is short and characteristics such as productive rate height.
The present invention realizes through following two step technical schemes:
1) the preparation particle diameter is 20～55nm golden nanometer particle;
In step 1), the concrete steps that said preparation particle diameter is 20～55nm golden nanometer particle are following:
Measuring the 100mL mass fraction and be 0.01% chlorauric acid solution is sodium citrate solution 2.5～0.7mL of 1% to refluxing, adding mass fraction again in vessel in heating, condensing reflux, and can obtain particle diameter after the cooling is 20～55nm golden nanometer particle.
Said golden nanometer particle also can adopt other metal nanoparticle, for example nano particles such as Ag, Pd, Pt.
2) the preparation particle diameter is 56～200nm golden nanometer particle;
In step 2) in, said preparation particle diameter is that 56～200nm golden nanometer particle can add thermal reduction and the preparation of hydroxylamine hydrochloride reduction two-step method through natrium citricum, its concrete steps are following:
Measure the 100mL mass fraction and be 0.01% chlorauric acid solution in vessel in heating to refluxing; The adding mass fraction is 1% sodium citrate solution 1mL; Can get the golden nanometer particle that average grain diameter is 40nm after the cooling; With average grain diameter be the golden nanometer particle of 40nm as crystal seed, add the dilution of 80～96mL water, add the natrium citricum 1～2mL of mass fraction 1%; The chlorauric acid solution that then adds 0.08～6mL concentration 24.28mM, stirring back adding 0.12～9mL concentration is the hydroxylamine hydrochloride solution of 10mM, continues to stir, can obtain particle diameter is 56～200nm golden nanometer particle;
3) at the manganese dioxide shell of the ultra-thin densification of golden nanometer particle superficial growth, De Jin-manganese dioxide core-shell structure nanometer particle.
In step 3), the concrete steps of said manganese dioxide shell in the ultra-thin densification of golden nanometer particle superficial growth can be:
Measure the 10mL golden nanometer particle in colorimetric cylinder, use concentration is that the KOH solution adjusting pH of 0.1～1M is 9.5～11, and adding 0.02～0.8mL concentration is the KMnO of 10mM
4Solution and 0.1～4mL concentration are the K of 10mM
2C
2O
4Solution keeps KMnO
4Solution and K
2C
2O
4The final concentration of solution is respectively 0.02～0.5mM and 0.1～2.5mM, places 50～70 ℃ of water-baths to keep 1～3h reactant liquor after mixing, and can obtain the gold-manganese dioxide core-shell structure nanometer particle of different shell thicknesses; The thickness of said manganese dioxide shell can be 0.5～10nm.
Said manganese dioxide shell also can adopt suitable semiconductor shells such as sulfide, selenides, arsenide, and said sulfide can be copper sulfide etc., and said selenides can be zinc selenide etc., and said arsenide can be GaAs etc.
Compared with prior art, the present invention has following outstanding advantage and technique effect:
1) the manganese dioxide shell of composite nanoparticle of the present invention can control to about 1nm and fine and close free of pinholes.
2) protective agent and additive that composite nanoparticle synthesis condition of the present invention is gentle, the reaction time is short, need not various complicacies.
3) compare with shells such as aluminium dioxide, silica, manganese dioxide can anti-highly basic, thereby composite nanoparticle of the present invention can use under strong alkali solution.
Description of drawings
Fig. 1 is that the golden nanometer particle size is 55nm, and the manganese dioxide shell is the low power transmission electron microscope picture (TEM) of gold-manganese dioxide core-shell structure nanometer particle of 0.5nm.In Fig. 1, scale is 10nm.
Fig. 2 is that the golden nanometer particle size is 55nm, and the manganese dioxide shell is gold-manganese dioxide core-shell structure nanometer particle low power transmission electron microscope picture (TEM) of 0.7nm.In Fig. 2, scale is 10nm.
Fig. 3 is that the golden nanometer particle size is 55nm, and the manganese dioxide shell is gold-manganese dioxide core-shell structure nanometer particle low power transmission electron microscope picture (TEM) of 1.2nm.In Fig. 3, scale is 10nm.
Fig. 4 is that the golden nanometer particle size is 55nm, and the manganese dioxide shell is gold-manganese dioxide core-shell structure nanometer particle low power transmission electron microscope picture (TEM) of 1.8nm.In Fig. 4, scale is 10nm.
Fig. 5 is that the golden nanometer particle size is 55nm, and the manganese dioxide shell is gold-manganese dioxide core-shell structure nanometer particle low power transmission electron microscope picture (TEM) of 2.5nm.In Fig. 5, scale is 10nm.
Fig. 6 is that the golden nanometer particle size is 55nm, and the manganese dioxide shell is gold-manganese dioxide core-shell structure nanometer particle high power transmission electron microscope picture (HRTEM) of 1.2nm.In Fig. 6, scale is 2nm.
The pyridine Raman spectrogram that Fig. 7 measures on silicon chip for the gold-manganese dioxide core-shell structure nanometer particle of different shell thicknesses.In Fig. 7, abscissa is Raman shift (Raman Shift/cm
-1); 1008cm
-1And 1035cm
-1Corresponding to the spectrum peak of pyridine adsorption on the acupuncture needle hole; Curve 1 is shell thickness 0.5nm (the unsound core-shell structure nanometer particle of shell); Curve 2 is shell thickness 0.7nm (the unsound core-shell structure nanometer particle of shell); Curve 3 is shell thickness 1.2nm (core-shell structure nanometer particle that shell is fine and close); Curve 4 is shell thickness 1.8nm (core-shell structure nanometer particle that shell is fine and close), and curve 5 is shell thickness 2.5nm (core-shell structure nanometer particle that shell is fine and close).
Fig. 8 is for strengthening the Raman spectrogram of pyridine at the suprabasil signal of silver with the fine and close core-shell structure nanometer particle of shell.In Fig. 8, abscissa is Raman shift (Raman Shift/cm
-1); 1007cm
-1And 1035cm
-1Corresponding to the spectrum peak of pyridine adsorption on silver electrode; Curve 1 is for to use the golden nanometer particle size to be 55nm, the manganese dioxide shell thickness be gold-manganese dioxide core-shell structure nanometer particle spreading of 1.2nm on smooth silver electrode, carry out the Raman spectrogram that pyridine is measured; Curve 2 is the Raman spectrogram of pyridine on smooth silver electrode that the core-shell structure nanometer particle of not spreading shell densification is directly measured; Not corresponding spectrum peak among the figure; Promptly at gold-when the manganese dioxide core-shell structure nanometer particle exists, the Raman signal of pyridine has obtained to strengthen significantly.
The specific embodiment
Through specific embodiment the present invention is described further below.
Embodiment 1: with the golden nanometer particle size is 55nm, and the manganese dioxide shell is that the core-shell structure nanometer particle of 1.2nm is an example.Measure the 100mL mass fraction and be 0.01% chlorauric acid solution and in round-bottomed flask, be heated to backflow, add mass fraction and be 1% sodium citrate solution 0.7mL, condensing reflux 30min gets final product to such an extent that average grain diameter is the golden nanometer particle of 55nm after the cooling.Measure the above-mentioned golden nanometer particle of 10ml in colorimetric cylinder, dripping concentration is the KOH solution adjusting pH to 9.5 of 1M, and adding 0.07mL concentration is the KMnO of 10mM
4Solution and 0.35mL concentration are the K of 10mM
2C
2O
4Solution places 60 ℃ of water-baths to keep 2h colorimetric cylinder, gets final product to such an extent that the manganese dioxide shell thickness is gold-manganese dioxide core-shell structure nanometer particle of 1.2nm, like Fig. 3 and shown in Figure 6.Keep other condition constant, change the KMnO that is added
4Solution and K
2C
2O
4The volume of solution can synthesize the gold-manganese dioxide core-shell structure nanometer particle of different shell thicknesses, as add 0.02,0.05,0.1 respectively, the KMnO of 0.14mL
4Solution and 0.1,0.25,0.5,0.7mLK
2C
2O
4The available manganese dioxide thickness of solution is respectively 0.5nm, 0.7nm, and 1.8nm, 2.5nm is respectively like Fig. 1, Fig. 2, Fig. 4, shown in Figure 5.
With these have different shell thicknesses the composite nanoparticle eccentric cleaning, be assembled on the clean silicon chip, splash into pyridine solution, carry out raman detection.600cm among Fig. 3
-1About be the characteristic peak of manganese dioxide, 1008cm
-1And 1035cm
-1Be the characteristic peak of pyridine adsorption on the acupuncture needle hole, it is fine and close the characteristic peak of manganese dioxide only occurring and the shell that the pyridine characteristic peak shows nano particle not occurring, in follow-up raman detection, can not receive the interference from the signal on the nano particle.As shown in Figure 7, shell thickness all is fine and close free of pinholes greater than the composite nanoparticle of 1.2nm.
(shell thickness 1.2nm) places on the smooth silver electrode with gold-manganese dioxide core-shell structure nanometer particle, splashes into pyridine solution, carries out raman detection.In Fig. 8,1007cm in the curve 1
-1And 1035cm
-1The peak be the characteristic peak of pyridine adsorption on silver; Curve 2 is that no nano particle exists down, can't detect the characteristic peak of pyridine adsorption on silver, shows that the pyridine signal of curve 1 comes from the enhancing of gold-manganese dioxide core-shell structure nanometer particle really.
Embodiment 2: with preparation golden nanometer particle size is 20nm, and the manganese dioxide shell is that the core-shell structure nanometer particle of 2.5nm is an example.Measure the 100mL mass fraction and be 0.01% chlorauric acid solution and in round-bottomed flask, be heated to backflow, add mass fraction and be 1% sodium citrate solution 2.5mL, condensing reflux 30min gets final product to such an extent that average grain diameter is the golden nanometer particle of 20nm after the cooling.Measure the above-mentioned golden nanometer particle of 10ml in colorimetric cylinder, dripping concentration is the KOH solution adjusting pH to 9.5 of 1M, and adding 0.38mL concentration is the KMnO of 10mM
4Solution and 1.9mL concentration are the K of 10mM
2C
2O
4Solution places 70 ℃ of water-baths to keep 2.5h colorimetric cylinder, gets final product to such an extent that the manganese dioxide shell thickness is gold-manganese dioxide core-shell structure nanometer particle of 2.5nm.
Embodiment 3: preparation golden nanometer particle size is 40nm, and the manganese dioxide shell is that the core-shell structure nanometer particle of 10nm is an example.Measure the 100mL mass fraction and be 0.01% chlorauric acid solution and in round-bottomed flask, be heated to backflow, add mass fraction and be 1% sodium citrate solution 1mL, condensing reflux 30min promptly gets the golden nanometer particle that average grain diameter is 40nm after the cooling.Measure the above-mentioned golden nanometer particle of 10ml in colorimetric cylinder, dripping concentration is the KOH solution adjusting pH to 9.5 of 0.5M, and adding 0.19mL concentration is the KMnO of 10mM
4Solution and 0.95mL concentration are the K of 10mM
2C
2O
4Solution places 60 ℃ of water-baths to keep 2h colorimetric cylinder, gets final product to such an extent that the manganese dioxide shell thickness is gold-manganese dioxide core-shell structure nanometer particle of 2.5nm.
Embodiment 4: with preparation golden nanometer particle size is 130nm, and the manganese dioxide shell is that the core-shell structure nanometer particle of 10nm is an example.Measure the 100mL mass fraction and be 0.01% chlorauric acid solution and in round-bottomed flask, be heated to backflow, add mass fraction and be 1% sodium citrate solution 1mL, condensing reflux 30min gets final product to such an extent that average grain diameter is the golden nanometer particle of 40nm after the cooling.Get the above-mentioned 40nm gold nano of 4mL as crystal seed; Add the dilution of 83mL water; Add the natrium citricum 1mL of mass fraction 1%, then add the chlorauric acid solution of 0.9mL concentration 24.28mM, slowly dripping 1.4mL concentration behind the stirring 5min is the hydroxylamine hydrochloride solution of 10mM; Continue to stir 30min, get the golden nanometer particle of 130nm.Get the above-mentioned 130nm golden nanometer particle of 10mL as crystal seed in colorimetric cylinder, drip the pH to 11 of the KOH solution regulator solution of 1M, adding 0.4mL concentration is the KMnO of 10mM
4Solution and 2mL concentration are the K of 10mM
2C
2O
4Solution places 50 ℃ of water-baths to shake 2h cuvette, promptly obtains golden nanometer particle size 130nm, the gold of shell thickness 10nm-manganese dioxide core-shell structure nanometer particle.
Claims (4)
1. the preparation method of gold-manganese dioxide core-shell structure nanometer particle is characterized in that may further comprise the steps:
1) the preparation particle diameter is 20～55nm golden nanometer particle;
2) the preparation particle diameter is 56～200nm golden nanometer particle;
3) at the manganese dioxide shell of the ultra-thin densification of golden nanometer particle superficial growth, De Jin-manganese dioxide core-shell structure nanometer particle; The concrete steps of said manganese dioxide shell in the ultra-thin densification of golden nanometer particle superficial growth are:
Measure the 10mL golden nanometer particle in colorimetric cylinder, use concentration is that the KOH solution adjusting pH of 0.1～1M is 9.5～11, and adding 0.02～0.8mL concentration is the KMnO of 10mM
4Solution and 0.1～4mL concentration are the K of 10mM
2C
2O
4Solution keeps KMnO
4Solution and K
2C
2O
4The final concentration of solution is respectively 0.02～0.5mM and 0.1～2.5mM, places 50～70 ℃ of water-baths to keep 1～3h reactant liquor after mixing, and promptly obtains the gold-manganese dioxide core-shell structure nanometer particle of different shell thicknesses; The thickness of said manganese dioxide shell is 0.5～10nm.
2. the preparation method of a kind of gold as claimed in claim 1-manganese dioxide core-shell structure nanometer particle is characterized in that in step 1), and the concrete steps that said preparation particle diameter is 20～55nm golden nanometer particle are following:
Measuring the 100mL mass fraction and be 0.01% chlorauric acid solution is sodium citrate solution 2.5～0.7mL of 1% to refluxing, adding mass fraction again in vessel in heating, condensing reflux, and promptly obtaining particle diameter after the cooling is 20～55nm golden nanometer particle.
3. the preparation method of a kind of gold as claimed in claim 1-manganese dioxide core-shell structure nanometer particle; It is characterized in that in step 2) in, said preparation particle diameter is that 56～200nm golden nanometer particle is to add thermal reduction and the preparation of hydroxylamine hydrochloride reduction two-step method through natrium citricum.
4. the preparation method of a kind of gold as claimed in claim 3-manganese dioxide core-shell structure nanometer particle is characterized in that said to add the concrete steps of thermal reduction and hydroxylamine hydrochloride reduction two-step method preparation through natrium citricum following:
Measure the 100mL mass fraction and be 0.01% chlorauric acid solution in vessel in heating to refluxing; The adding mass fraction is 1% sodium citrate solution 1mL; Getting average grain diameter after the cooling is the golden nanometer particle of 40nm; With average grain diameter be the golden nanometer particle of 40nm as crystal seed, add the dilution of 80～96mL water, add the natrium citricum 1～2mL of mass fraction 1%; The chlorauric acid solution that then adds 0.08～6mL concentration 24.28mM, stirring back adding 0.12～9mL concentration is the hydroxylamine hydrochloride solution of 10mM, continues to stir, obtaining particle diameter is 56～200nm golden nanometer particle.
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