CN104150438B - Single angle-hollow Nano Au composite and preparation method thereof - Google Patents
Single angle-hollow Nano Au composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the preparation method of single angle-hollow Nano Au composite, be single angle powder, water and PDDA are mixed, the ultrasonic single angle powder that makes dissolves completely, obtains single angle solution; Another by CoCl
2, PVP K30 and water mixing, stir make CoCl
2dissolve completely with PVP K30, obtain CoCl
2solution, logical nitrogen deoxygenation, then drip NaBH under agitation
4solution, reduction CoCl
2obtain cobalt colloidal sol; In cobalt colloidal sol, add single angle solution, after mixing, drip HAuCl again
4solution, centrifugal collecting precipitation, washing, resuspended with water, obtain single angle-hollow Nano Au composite; The present invention utilizes one-step method fabricated in situ single angle-hollow Nano Au composite, step is simple, the time is short, productive rate is high, not only effectively prevent the stripping between component, obtained compound steadiness is good, antivibration, anti-shear ability strong, and obtained complex binding site is more, specific area is larger, physics and chemistry adsorption capacity is stronger.
Description
Technical field
The invention belongs to technical field of nano material, relate to a kind of nano-complex and preparation method thereof.
Background technology
Nano material refers to the material of the size of construction unit between 1-100nm, has the good reputation of " 21 century the most promising material ".Because the size of nano material is close to the wavelength of light and the coherence length of electronics, in addition it has surface and interface effect, quantum size effect, small-size effect and macro quanta tunnel effect, in calorifics, mechanics, magnetics, electricity, chemistry, optics, superconductivity and catalysis etc., all show peculiar character, have broad application prospects.
Carbon nanomaterial, as one of important nano material, is this field study hotspot in recent years, mainly contains CNT, carbon nano-fiber, Nano carbon balls and Graphene etc.Carbon nanohorn is as catalyst carrier at lithium ion battery, and the research of polymer fuel cell and DMFC is also carried out gradually.(SWCNHs) has the structure similar to SWCN at single angle, and the difference of the two is that one end of carbon nanohorn is the sealing of horn shape.Single carbon nanohorn diameter is about 2-5nm, length 40-50nm.Carbon nanohorn exists with the morphology of the aggregate of diameter 80-100nm under normal circumstances.Research shows, not only has the effect of Van der Waals force between the carbon nanohorn in aggregation, also has carbon-carbon single bond effect.Similar with other carbon nanomaterial, the advantages such as carbon nanohorn has high mechanical strength and elasticity equally, specific area is large, absorption property is strong, optical property is excellent.In addition, carbon nanohorn also has the character relative to other carbon nanomaterial uniqueness.First, carbon nanohorn is under ar gas environment, utilize the direct calcination graphite rod of carbon dioxide-vapor to be formed, in preparation process, do not use metallic catalyst; Secondly, carbon nanohorn has stronger adsorption capacity than CNT, and under 3.5MPa pressure, the adsorbance of carbon nanohorn reaches 160cm
3/ cm
3.
Nm of gold refers to the molecule of gold, and its diameter is 1 ~ 100nm, has high electron density, dielectric property and catalytic action, can be combined with multiple large biological molecule and not affect its biologically active.Can be prepared the nm of gold of various different-grain diameter easily by reducing process by gold chloride, its color takes on a red color to purple according to diameter.Hollow Nano gold is the nm of gold of hollow structure, has the specific area larger than nm of gold and stronger biologically active.
In recent years, the decorative material of nano material as sensing interface and the immobilized matrix of biomolecule, be widely used in the construction work of electrochemica biological sensor, based on advantages such as they large specific area, good biocompatibility and high surface reaction activities, drastically increase sensitivity and the stability of sensor.Wherein, nm of gold is carried on the optimization of a series of performances that carbon nano tube surface is brought, causes the great interest of scholars to Gold Nanoparticles/CNT Composites.And prepare the conventional method of nano-complex at present for substep synthesis-mix and blend method, be each constituent first preparing compound respectively, then will stir and evenly mix after each constituent mixing, utilize the physical adsorption characteristic of composition to form compound.The method is owing to being electrostatic adsorption between component, and in conjunction with firm not, component is easily peeled off from compound, thus have impact on productive rate and the range of application of nano-complex.
Summary of the invention
In view of this, the object of the invention is to single angle for matrix, in conjunction with a kind of single angle-hollow Nano Au composite of hollow Nano gold preparation, have that preparation method is simple, the time is short, cost is low, gained compound steadiness is good, and antivibration, anti-shear ability are strong, and binding site is many, specific area is large, the advantages such as physics and chemistry high adsorption capacity.
After deliberation, the invention provides following technical scheme:
1. the preparation method of single angle-hollow Nano Au composite, comprises the following steps:
A. single angle powder, water and phthalic acid diethanol diacrylate (PDDA) are mixed with the ratio of 2mg:1.95mL:0.5mg, the ultrasonic single angle powder that makes dissolves completely, obtains single angle solution;
B. by CoCl
2, polyvinylpyrrolidone (PVP) K30 and water with the mixing of the ratio of 0.02mmol ~ 0.03mmol:100 ~ 150mg:50mL, stir and make CoCl
2dissolve completely with PVP K30, obtain CoCl
2solution; By CoCl
2solution leads to nitrogen deoxygenation, then drips NaBH under agitation
4solution, drips Bi Jixu and stirs 10 ~ 25min, make NaBH
4reduction CoCl
2obtain cobalt colloidal sol; Described NaBH
4consumption be every 50mL CoCl
2naBH is added in solution
48 ~ 12 μ g;
C. the single angle solution that steps A is obtained is added in the cobalt colloidal sol obtained to step B, the consumption of described single angle solution is every 70mL concentration is add single angle solution 0.5 ~ 1.5mL in the cobalt colloidal sol of 0.29 ~ 0.43 μm of ol/mL, stirs and evenly mixs; Drip HAuCl again
4solution, described HAuCl
4consumption be every 70mL concentration be add HAuCl in the cobalt colloidal sol of 0.29 ~ 0.43 μm of ol/mL
40.01 ~ 0.02g; Centrifugal collecting precipitation, washes 2 ~ 4 times with water, then uses water resuspended, obtains single angle-hollow Nano Au composite.
Preferably, described steps A is mixed with the ratio of 2mg:1.95mL:0.05mL single angle powder, water and 1wt% phthalic acid diethanol diacrylate ester solution, the ultrasonic single angle powder that makes dissolves completely, obtains single angle solution.
Preferably, described step B is by CoCl
2, PVP K30 and water mixes with the ratio of 0.025mmol:120mg:50mL, stir and make CoCl
2dissolve completely with PVP K30, obtain CoCl
2solution; By CoCl
2solution leads to nitrogen deoxygenation, then drips the NaBH of 0.5 μ g/mL under agitation
4solution, drips Bi Jixu and stirs 10 ~ 25min, make NaBH
4reduction CoCl
2obtain cobalt colloidal sol; Described NaBH
4consumption be every 50mL CoCl
2naBH is added in solution
410 μ g.
Preferably, described step C adds the obtained single angle solution of steps A in the cobalt colloidal sol obtained to step B, the consumption of described single angle solution is every 70mL concentration is add single angle solution 1.0mL in the cobalt colloidal sol of 0.36 μm of ol/mL, stirs and evenly mixs; Drip HAuCl again
4solution, described HAuCl
4consumption be every 70mL concentration be add HAuCl in the cobalt colloidal sol of 0.36 μm of ol/mL
40.012g; Centrifugal collecting precipitation, washes 2 ~ 4 times with water, then uses water resuspended, obtains single angle-hollow Nano Au composite.
2. adopt single angle-hollow Nano Au composite prepared by said method.
Beneficial effect of the present invention is: the present invention utilizes one-step method original position to prepare single angle-hollow Nano Au composite innovatively, wherein, at dropping NaBH
4reduction CoCl
2adding single angle after becoming cobalt colloidal sol again and dripping 1mg/mL single angle solution 0.5 ~ 1.5mL is the key that can compound be successfully prepared.Compare conventional substep synthesis-mix and blend method, the inventive method preparation process is simple, the time is short, productive rate is high, not only effectively prevent the stripping between component, obtained compound steadiness is good, and antivibration, anti-shear ability are strong, and the ability of bearing subsequent treatment (as ultrasonic, thermal agitation etc.) is strong, and obtained complex binding site is more, specific area is larger, and physics and chemistry adsorption capacity is stronger, and range of application is wider.
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 ESEM (SEM) figure of fabricated in situ single angle-hollow Nano Au composite.
Fig. 2 is the SEM figure of conventional substep synthesis-mix and blend method synthesizing single-wall carbon nanohorn-hollow Nano Au composite.
Fig. 3 is the fabricated in situ single angle-cyclic voltammetry curve of hollow Nano Au composite modified electrode in 1 × PBS.
Fig. 4 is the ultraviolet wave spectrum scanning analysis result of fabricated in situ single angle-hollow Nano Au composite.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.The experimental technique of unreceipted actual conditions in preferred embodiment, usually conveniently condition, or carry out according to the condition that reagent manufacturer advises.
Main material and equipment: CoCl
26H
2o, HAuCl
4with 1%PDDA available from Sigma; PVP K30 and NaBH
4purchased from Shanghai traditional Chinese medicines Group Co., Ltd; Single angle is purchased from Ji'an, Beijing letter Science and Technology Ltd.; SB-80 sonic oscillation instrument is purchased from NingBo XinZhi Biology Science Co., Ltd; Magnetic stirring apparatus and magnetic stir bar are purchased from upper Haikang instrument Instrument Ltd.; Electronic balance is purchased from German Sai Duolisi company; Hitachi S-4800 ESEM is purchased from Hitachi, Ltd.
Synthetic example, fabricated in situ single angle-hollow Nano Au composite
A. in 5mL EP pipe, add 2mg single angle powder, 1.95mL deionized water and 50 μ L 1wt%PDDA solution, single angle was dissolved completely in ultrasonic 3 hours, obtain single angle solution;
B. in 100mL beaker, 6mg CoCl is added
26H
2o, 120mg PVP K30 and 50mL tri-distilled water, stir and make CoCl
26H
2o and PVP K30 dissolves completely, obtains CoCl
2solution; By CoCl
2solution leads to nitrogen 20min, drips 0.5 μ g/mL NaBH under agitation
4solution 20mL, drips Bi Jixu and stirs 20min, make NaBH
4reduction CoCl
2obtain cobalt colloidal sol;
C. add the single angle solution 1.0mL that steps A is obtained in the cobalt colloidal sol obtained to step B, stir and evenly mix, then drip 1wt%HAuCl
4solution 1.2mL, centrifugal collecting precipitation, with deionized water centrifuge washing 3 times, then use tri-distilled water resuspended, obtain single angle-hollow Nano Au composite, 4 DEG C save backup.
In research process, the present invention had once investigated the impact of single angle addition sequence in step C, taked two kinds of methods respectively: 1) at CoCl
2first add single angle solution in solution, then add NaBH
4solution reduction CoCl
2become cobalt colloidal sol, all the other steps are identical; 2) at CoCl
2first NaBH is added in solution
4solution, at NaBH
4reduction CoCl
2add single angle solution again after becoming cobalt colloidal sol, all the other steps are identical.Result shows, and first method is at NaBH
4reduction CoCl
2time occur that flocculence bulk precipitates, cobalt colloidal sol can not be formed; And second method does not affect the overall dissolubility of solution, the hollow golden dissolubility of sequential reduction is also fine.
Contrast synthetic example, conventional substep synthesis-mix and blend method synthesizing single-wall carbon nanohorn-hollow Nano Au composite
A. in 50mL beaker, add 2mg single angle powder, 1.95mL deionized water and 50 μ L 1wt%PDDA solution, single angle was all dissolved in ultrasonic 3 hours, obtain single angle solution;
B. in 100mL beaker, 6mg CoCl is added
26H
2o, 120mg PVP K30 and 50mL tri-distilled water, stir and make CoCl
26H
2o and PVP K30 dissolves completely, obtains CoCl
2solution; By CoCl
2solution leads to nitrogen 20min, drips 0.5 μ g/mL NaBH under agitation
4solution 20mL, then drip 1wt%HAuCl
4solution 1.2mL, centrifugal collecting precipitation, with deionized water centrifuge washing 3 times, then uses the resuspended precipitation of 2mL tri-distilled water, obtains hollow Nano gold solution;
C. the hollow Nano gold solution that single angle solution steps A obtained and step B obtain by volume 1:2 mixes, stir 4 ~ 6 hours, centrifugal collecting precipitation, with deionized water centrifuge washing 3 times, finally use tri-distilled water resuspended, obtain single angle-hollow Nano Au composite, 4 DEG C save backup.
The ESEM of the single angle-hollow Nano Au composite of experimental example 1, distinct methods synthesis characterizes
Get synthetic example and contrast obtained each 3 ~ 5 μ L of single angle-hollow Nano Au composite of synthetic example, characterize with SEM respectively.
Fig. 1 is the SEM figure of the single angle-hollow Nano Au composite of fabricated in situ.As can be seen from Fig., the composite surface of fabricated in situ of the present invention adheres to the hollow Nano gold grain of the more hollow spheres structure of number, and diameter range is about 30nm ~ 200nm, and the particle diameter of about 75% is positioned at about 100nm; The particle intermediate luminance of about 75% ~ 95% weakens, and surrounding brightness is comparatively strong, is shown as hollow spheres structure.On the other hand, the distribution of hollow Nano gold grain on single angle also comparatively evenly (in figure shown in arrow).
Fig. 2 is the SEM figure of conventional substep synthesis-mix and blend method synthesizing single-wall carbon nanohorn-hollow Nano Au composite.As can be seen from Fig., even if under the more prerequisite of hollow Nano gold addition, the hollow Nano golden number amount of composite surface attachment is still less, and skewness, single angle exposed more (in figure shown in arrow).
The structure of the single angle-hollow Nano Au composite of more above-mentioned distinct methods synthesis, can draw the following conclusions: 1) there is more hollow Nano gold binding site on the single angle-hollow Nano Au composite surface of fabricated in situ of the present invention, there is larger specific area, stronger physics and chemistry characterization of adsorption, mechanical strength is large; 2) the hollow golden binding site quantity of composite surface of conventional substep synthesis-mix and blend method synthesis significantly reduces, and specific area is less, and physics and chemistry absorption property is not good.
The cyclic voltammetry of the single angle-hollow Nano Au composite of experimental example 2, fabricated in situ characterizes
Get the single angle-hollow Nano Au composite 10 μ L of fabricated in situ, drip on clean naked glass-carbon electrode of polishing, dry in rearmounted 1 × PBS (pH7.4) for 37 DEG C and characterize by cyclic voltammetry.Result as shown in Figure 3, compared to naked glass-carbon electrode, the electrode current value of having modified the single angle-hollow Nano Au composite of fabricated in situ obviously increases, 5.277 μ A are increased to from 2.167 μ A, add 2.435 times, illustrate that the single angle-hollow Nano Au composite of fabricated in situ has excellent electric conductivity.
The uv scan analysis of the single angle-hollow Nano Au composite of experimental example 3, fabricated in situ
Get each 10 μ L of single angle-hollow Nano Au composite of single angle solution, hollow Nano gold solution, fabricated in situ, be diluted to 1mL by deionized water, carry out uv scan analysis, sweep limits is 190nm ~ 800nm.As shown in Figure 4, the maximum absorption band at single angle is positioned at 267nm to result, and absorbance is 0.401; The maximum absorption band of hollow Nano gold is positioned at 201nm, and absorbance is 0.503; Single angle-hollow Nano the Au composite of fabricated in situ has 2 maximum absorption bands, and one is positioned at 201nm, and absorbance is 0.465; Another is positioned near 235nm, and absorbance is 0.425; Illustrate that the absworption peak corresponding to single angle in the single angle-hollow Nano Au composite of fabricated in situ is not subjected to displacement, just absorbance slightly reduces, and the absworption peak corresponding to hollow Nano gold there occurs displacement, from 267nm violet shift to 235nm, its reason may be the surface that hollow Nano gold covers single angle, create space steric effect, thus have impact on UV absorption.
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 (5)
1. the preparation method of single angle-hollow Nano Au composite, is characterized in that, comprise the following steps:
A. single angle powder, water and diallyl dimethyl ammoniumchloride are mixed with the ratio of 2mg:1.95mL:0.5mg, the ultrasonic single angle powder that makes dissolves completely, obtains single angle solution;
B. by CoCl
2, PVP K30 and water with the mixing of the ratio of 0.02mmol ~ 0.03mmol:100 ~ 150mg:50mL, stir and make CoCl
2dissolve completely with PVP K30, obtain CoCl
2solution; By CoCl
2solution leads to nitrogen deoxygenation, then drips NaBH under agitation
4solution, drips Bi Jixu and stirs 10 ~ 25min, make NaBH
4reduction CoCl
2obtain cobalt colloidal sol; Described NaBH
4consumption be every 50mL CoCl
2naBH is added in solution
48 ~ 12 μ g;
C. the single angle solution that steps A is obtained is added in the cobalt colloidal sol obtained to step B, the consumption of described single angle solution is every 70mL concentration is add single angle solution 0.5 ~ 1.5mL in the cobalt colloidal sol of 0.29 ~ 0.43 μm of ol/mL, stirs and evenly mixs; Drip HAuCl again
4solution, described HAuCl
4consumption be every 70mL concentration be add HAuCl in the cobalt colloidal sol of 0.29 ~ 0.43 μm of ol/mL
40.01 ~ 0.02g; Centrifugal collecting precipitation, washes 2 ~ 4 times with water, then uses water resuspended, obtains single angle-hollow Nano Au composite.
2. the preparation method of single angle-hollow Nano Au composite as claimed in claim 1, it is characterized in that, described steps A is mixed with the ratio of 2mg:1.95mL:0.05mL single angle powder, water and 1wt% diallyl dimethyl ammoniumchloride solution, the ultrasonic single angle powder that makes dissolves completely, obtains single angle solution.
3. the preparation method of single angle-hollow Nano Au composite as claimed in claim 1, it is characterized in that, described step B is by CoCl
2, PVP K30 and water mixes with the ratio of 0.025mmol:120mg:50mL, stir and make CoCl
2dissolve completely with PVP K30, obtain CoCl
2solution; By CoCl
2solution leads to nitrogen deoxygenation, then drips the NaBH of 0.5 μ g/mL under agitation
4solution, drips Bi Jixu and stirs 10 ~ 25min, make NaBH
4reduction CoCl
2obtain cobalt colloidal sol; Described NaBH
4consumption be every 50mL CoCl
2naBH is added in solution
410 μ g.
4. the preparation method of single angle-hollow Nano Au composite as claimed in claim 1, it is characterized in that, described step C adds the obtained single angle solution of steps A in the cobalt colloidal sol obtained to step B, the consumption of described single angle solution is every 70mL concentration is add single angle solution 1.0mL in the cobalt colloidal sol of 0.36 μm of ol/mL, stirs and evenly mixs; Drip 1wt% HAuCl again
4solution, described HAuCl
4consumption be every 70mL concentration be add HAuCl in the cobalt colloidal sol of 0.36 μm of ol/mL
40.012g; Centrifugal collecting precipitation, washes 2 ~ 4 times with water, then uses water resuspended, obtains single angle-hollow Nano Au composite.
5. adopt single angle-hollow Nano Au composite that described in any one of Claims 1-4 prepared by method.
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CN105879042A (en) * | 2015-04-02 | 2016-08-24 | 中国药科大学 | Drug loading system for loading docetaxel based on oxidized single-walled carbon nanohorns |
CN109966533A (en) * | 2019-05-23 | 2019-07-05 | 李学书 | It is a kind of to utilize deodorant and purposes made of carbon nanohorn |
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