CN115849344A - Preparation of two self-separated fullerene C with different sizes simultaneously 60 Method for producing nano-rod - Google Patents
Preparation of two self-separated fullerene C with different sizes simultaneously 60 Method for producing nano-rod Download PDFInfo
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- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 93
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 69
- 239000002073 nanorod Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title description 2
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000002904 solvent Substances 0.000 claims abstract description 45
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 33
- 239000002244 precipitate Substances 0.000 claims abstract description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000001338 self-assembly Methods 0.000 description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- MARCAKLHFUYDJE-UHFFFAOYSA-N 1,2-xylene;hydrate Chemical compound O.CC1=CC=CC=C1C MARCAKLHFUYDJE-UHFFFAOYSA-N 0.000 description 1
- -1 biomedicine Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a method for simultaneously preparing two self-separated fullerenes C with different sizes 60 The method of the nano rod comprises the following steps: reacting fullerene C 60 Dissolving in meta-xylene to obtain fullerene C 60 A meta-xylene solution of (a); h is to be 2 Mixing O, N-dimethylformamide and isopropanol to obtain fullerene C 60 A poor solvent of (4); adding fullerene C to a poor solvent 60 Adding isopropanol into the interface of the two solutions, making the solution become turbid immediately and have precipitate, standing, layering the precipitate, concentrating the precipitate at the bottom and the upper part of the solution, and separating the precipitate at the two different positions to obtain two fullerenes C with different sizes 60 And (4) nanorods. The invention is through the reaction of fullereneThe concentration of the solution, the step of adding the liquid and other conditions are controlled, and two kinds of high-quality C are successfully prepared 60 The nano-rod has the characteristics of simple preparation method, easy operation and high efficiency.
Description
Technical Field
The invention belongs to the field of preparation and development of fullerene self-assembly structures, and particularly relates to a method for simultaneously preparing two self-separated fullerene C with different sizes 60 A method of nano-rod.
Background
The related performance of the device of the fullerene material is not only related to the intrinsic characteristics of fullerene but also closely inseparable with the appearance of the fullerene, and the fullerene structure with fixed appearance, such as fullerene nanorods, fullerene nanotubes, fullerene micro-squares and other structures, is proved to have the potential of development and application in the aspects of optics, electrics, electrochemistry, nano materials, biomedicine, chemical catalysis and the like. Therefore, the development of a simple and effective method for preparing the high-quality fullerene micro-nano structure plays an important role in expanding and developing the application of fullerene. After decades of researches, the current methods for preparing fullerene include: liquid-liquid interface self-assembly, gas-liquid-solid interface self-assembly, gas-solid interface self-assembly, vacuum solid interface self-assembly, and the like. The two methods of gas-solid interface self-assembly and vacuum solid interface self-assembly need to be assisted by complex instruments and equipment processes and the like, and are not beneficial to further utilization of the fullerene material. Liquid-liquid interface self-assembly and gas-liquid-solid interface self-assembly do not depend on equipment, the preparation process is simple and convenient, and the prepared fullerene self-assembly structure has various and adjustable appearances and is widely concerned by researchers. Wherein the liquid-liquid interface method is to convert fullerene C 60 Fullerene C formed by dissolving in good solvent (such as toluene, benzene, carbon tetrachloride and carbon disulfide) 60 The solution is then formed into an interface with a poor solvent for the fullerene (e.g., methanol, ethanol, isopropanol, t-butanol, etc.), at which the fullerene molecules assume a supersaturated state for nucleation and crystallization. The liquid-liquid interface method can regulate the types of good solvents and poor solvents of fullerene and fullerene dissolutionThe appearance of the fullerene self-assembly structure is effectively regulated and controlled by the concentration of the liquid, the proportion of the fullerene solution and the poor solvent and external conditions such as illumination and temperature. For example, when a reagent such as toluene or m-xylene is used as a good solvent, fullerene C 60 Tends to form one-dimensional nanorod or nanotube structures, and C is a good solvent when carbon tetrachloride is used 60 Tend to form two-dimensional nano-platelet structures.
When a liquid-liquid interface method is adopted, the prepared one-dimensional nanorod structure generally has the condition of nonuniform appearance and size, for example, the distribution of length and diameter is wide, and the preparation of a high-precision device is not easy; most of the liquid-liquid interface methods can only prepare one sample, limiting the diversity of the method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for simultaneously preparing two self-separated fullerenes C with different sizes 60 Method for preparing nano-rod, two kinds of fullerene C obtained by preparation 60 The size distribution of the nano-rods is uniform, which is beneficial to the preparation of high-precision nano-devices.
In order to achieve the purpose, the invention adopts the technical scheme that:
method for simultaneously preparing two self-separated fullerenes C with different sizes 60 A method of nanorods, comprising the steps of:
(1) Preparation of Fullerene C 60 The concentration of the m-xylene solution is 0.75-1.75mg/ml: adding proper amount of fullerene C 60 The powder was added to 50ml of m-xylene solvent and sonicated for 30 minutes.
(2) Preparation of mixed poor solvents: will firstly be H 2 O, N-dimethylformamide and isopropanol were mixed at a volume ratio of 1 60 A poor solvent of (4). The poor solvent has water and m-xylene immiscible, thereby allowing the poor solvent and fullerene C to react 60 The meta-xylene solution of (a) forms a layered state at the time of initial contact; the density of the poor solvent can be regulated and controlled to a certain degree by N, N-dimethylformamide; the main function of the isopropanol is to promote the growth of the fullerene nanorod.
(3) Has been prepared byThe process: 2ml of fullerene C 60 The poor solvent (2) is added into a 10ml clean glass bottle, and 1ml of fullerene C is added 60 M-xylene solution of (2), in which case fullerene C can be seen 60 The meta-xylene solution and the poor solvent are insoluble to each other, forming an interface at the position where they contact; then adding 1ml of isopropanol at the interface of the fullerene solution and the solution to form supersaturation with the fullerene solution to promote the nucleation and growth of the fullerene nanorods, wherein the solution immediately turns turbid and precipitates appear, the precipitates are layered and respectively concentrated at the bottom and the upper part of the solution after standing, and the precipitates at the two different positions are separated to obtain two fullerenes C with different sizes 60 And (4) nanorods.
Compared with the prior art, the invention has the beneficial effects that:
firstly, preparing fullerene C respectively 60 Mixed poor solvent, and then the fullerene C 60 Adding the m-xylene solution into a poor solvent, adding isopropanol at the interface of the poor solvent, standing and separating after precipitates appear to obtain two fullerenes C with different sizes 60 A nano-rod. The method successfully prepares two high-quality C by controlling the conditions of the fullerene solution such as the concentration (excessive or insufficient concentration of the fullerene solution can cause the layering failure or only one structure, the isopropanol solvent around the fullerene with excessive concentration is too little, the fullerene molecules are too aggregated, the growth is blocked to easily generate only one structure, and the concentration of the fullerene is low, so that the subsequent continuous growth of the fullerene molecules becomes less to be unfavorable for the subsequent growth of the fullerene), the liquid adding step and the like 60 The nano-rod has the characteristics of simple preparation method, easy operation and high efficiency; and two kinds of fullerene C obtained by preparation 60 The nano rods have uniform size distribution, and are beneficial to the preparation of high-precision nano devices.
Drawings
FIG. 1 shows the preparation of two fullerenes C of different sizes simultaneously in example 1 of the present invention 60 Process diagram of the nano-rod;
FIG. 2 shows two fullerenes C of different sizes 60 Of nanorodsSEM images at different magnifications;
FIG. 3 is a diagram showing preparation of fullerene C in comparative example 1 60 Process diagram of the nano-rod;
FIG. 4 shows preparation of Fullerene C in comparative example 2 60 Process diagram of nanorods.
Detailed Description
The present invention will be further described with reference to the following examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
In addition, the preparation processes in the following examples are conventional means in the prior art unless otherwise specified, and therefore, detailed descriptions thereof are omitted; the starting materials used in the following experiments are all commercially available products.
Examples
Method for simultaneously preparing two self-separated fullerenes C with different sizes 60 A method of nanorods, comprising the steps of:
(1) Preparation of Fullerene C 60 M-xylene solution of (a): 62.5mg of fullerene C 60 Adding the powder into 50ml of m-xylene solvent, and performing ultrasonic treatment for 30 minutes to obtain fullerene C 60 M-xylene solution of (a).
(2) Preparation of mixed poor solvents: h is to be 2 Mixing O, N-dimethylformamide and isopropanol in a volume ratio of 1 60 A poor solvent of (4).
(3) The preparation process comprises the following steps: 4ml of fullerene C 60 The poor solvent (2) is added into a 10ml clean glass bottle, and 1ml of fullerene C is added 60 When fullerene C is observed 60 The meta-xylene solution and the poor solvent are insoluble to each other, and an interface is formed at the position where they contact, as shown in fig. 1 (a). Subsequently 1ml of isopropanol solvent was added at their interface, at which time the solution immediately became cloudy and a precipitate appeared, as in FIG. 1 (b); standing for 24 hr, separating precipitate at different positions to obtain two kinds of precipitate with different sizesFullerene C 60 And (4) nanorods.
The two precipitates were subjected to morphological characterization to analyze the difference and formation mechanism of the two precipitates, and fig. 2 (a, b) is an SEM image of the upper precipitate, which can be seen as a one-dimensional nanorod structure having an average diameter of about 230nm and a length of several tens to several hundreds of micrometers by statistics. FIG. 2 (c, d) is an SEM image of the lower precipitate, and it can be seen that the lower precipitate is also a one-dimensional nanorod structure, but the sizes thereof are different, and the average diameter thereof is about 986nm and the average length thereof is about 14.93 μm by statistics. From this data, it can be analyzed that the nanorods of the upper layer are elongated, while the precipitates of the lower layer are coarse and short. In conclusion, the method provided by the invention successfully obtains two fullerenes C with different sizes at the same time 60 A nanorod, and two fullerenes C of different sizes 60 The nanorods are respectively gathered at different positions in the reaction solution due to the difference of the self-structures, and show a self-separation state, so that the nanorods are convenient to be respectively separated and processed subsequently, the preparation process is simple, and the operation is easy.
Comparative example 1:
(1) Preparation of Fullerene C 60 M-xylene solution of (a): 62.5mg of fullerene C 60 Adding the powder into 50ml of m-xylene solvent, and performing ultrasonic treatment for 30 minutes to obtain fullerene C 60 M-xylene solution of (a).
(2) Preparation of mixed poor solvents: h is to be 2 Mixing O and isopropanol in a volume ratio of 1 60 A poor solvent of (4).
(3) The preparation process comprises the following steps: 4ml of fullerene C 60 The poor solvent (2) is added into a 10ml clean glass bottle, and 1ml of fullerene C is added 60 The meta-xylene solution of (a) in FIG. 3. Then 1ml of isopropanol solvent was added at their interface and after standing for 24h the precipitate only did not separate at the bottom of the solution with a small amount of unassembled fullerene solution in the upper layer.
The comparative examples differ from the examples in that: no N, N-dimethylformamide was added to the poor solvent.
Comparative example 2
(1) Preparation of Fullerene C 60 M-xylene solution of (a): adding 200mg of fullerene C 60 Adding the powder into 50ml of m-xylene solvent, and performing ultrasonic treatment for 30 minutes to obtain fullerene C 60 M-xylene solution of (a).
(2) Preparation of mixed poor solvents: h is to be 2 Mixing O, N-dimethylformamide and isopropanol in a volume ratio of 1 60 The poor solvent of (4).
(3) The preparation process comprises the following steps: 4ml of fullerene C 60 The poor solvent (2) is added into a 10ml clean glass bottle, and 1ml of fullerene C is added 60 M-xylene solution of (2), in which case fullerene C can be seen 60 The meta-xylene solution and the poor solvent of (a) do not dissolve each other, forming an interface at the position where they contact, as shown in fig. 4 (a). 1ml of isopropanol solvent was then added at their interface and after 24h of standing the precipitate was mostly concentrated at the bottom of the bottle with no significant delamination.
The comparative examples differ from the examples in that: fullerene C 60 The concentration of meta-xylene of (a) is different.
It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Claims (6)
1. Method for simultaneously preparing two self-separated fullerenes C with different sizes 60 The method for preparing the nano-rod is characterized by comprising the following steps: the method comprises the following steps:
(1) Fullerene C 60 Dissolving in meta-xylene to obtain fullerene C 60 A meta-xylene solution of (a); the fullerene C 60 In meta-xylene solution of (2) 60 The concentration of (A) is 0.75-1.75mg/ml;
(2) H is to be 2 Mixing O, N-dimethylformamide and isopropanol to obtain fullerene C 60 The poor solvent of (4);
(3) Adding fullerene C to the poor solvent 60 Due to fullerene C 60 Are incompatible with the poor solvent, forming an interface at the point where they contact; adding isopropanol to the interface, allowing the solution to become turbid and precipitate to appear, standing, layering the precipitate, concentrating at the bottom and upper part of the solution, and separating the precipitate at the two different positions to obtain two kinds of fullerene C with different sizes 60 And (4) nanorods.
2. Simultaneous preparation of two different sized and self-separated fullerenes C according to claim 1 60 The method for preparing the nano-rod is characterized by comprising the following steps: in the step (1), fullerene C is added 60 Dissolving in m-xylene, ultrasonic treating to obtain fullerene C 60 The dispersion is uniform in the m-xylene.
3. Simultaneous preparation of two different sized and self-separated fullerenes C according to claim 2 60 The method for preparing the nano-rod is characterized by comprising the following steps: the time of the ultrasonic treatment is 20-40 minutes.
4. The simultaneous preparation of two different sized and self-segregating fullerenes C as claimed in claim 1 60 The method for preparing the nano-rod is characterized by comprising the following steps: in the step (2), the fullerene C 60 In a poor solvent of (3) H 2 The volume ratio of O, N-dimethylformamide to isopropanol is 1.
5. Simultaneous preparation of two different sized and self-separated fullerenes C according to claim 1 60 The method for preparing the nano-rod is characterized by comprising the following steps: in the step (3), fullerene C is added to the poor solvent 60 In the case of a meta-xylene solution, a poor solvent and fullerene C 60 The volume ratio of the m-xylene solution of (a) is 2.
6. Simultaneous preparation of two different sized and self-separated fullerenes C according to claim 1 60 The method for preparing the nano-rod is characterized by comprising the following steps: in the step (3)The standing time is 12-48h.
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