CN110921649A - Two-dimensional carbon nanosheet and method for preparing two-dimensional carbon nanosheets in large scale - Google Patents

Two-dimensional carbon nanosheet and method for preparing two-dimensional carbon nanosheets in large scale Download PDF

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CN110921649A
CN110921649A CN201911054440.4A CN201911054440A CN110921649A CN 110921649 A CN110921649 A CN 110921649A CN 201911054440 A CN201911054440 A CN 201911054440A CN 110921649 A CN110921649 A CN 110921649A
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dimensional carbon
nitrate
transition metal
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CN110921649B (en
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王东
温广武
亓帅
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Shandong University of Technology
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Abstract

The invention relates to a two-dimensional carbon nanosheet and a method for preparing the two-dimensional carbon nanosheet in a large scale. The carbohydrate is creatively used as a carbon source for preparing the two-dimensional carbon nano-sheet, esterification reaction is not needed between the carbon sources, and the hydroxyl of the carbon source is directly complexed with the transition metal provided by the nitrate to form a metal polymer skeleton, so that the forming time of the aqueous solution is greatly simplified, and only the time is less than 1h, which is unachievable for the existing preparation process and has important significance, and the formation time of precursor colloid is further reduced by the use of the carbohydrate for less than 2 h. In addition, nitrate provided by the nitrate can generate a large amount of gas in the instant or fast pyrolysis process, and a strong impact force is provided to offset the stacking force between carbon sources, so that the ultrathin carbon nanosheets are obtained, and thus the short-time and high-quality large-scale preparation of the two-dimensional carbon nanosheets is realized, which is a qualitative improvement for the preparation technology of the two-dimensional carbon nanosheets, and is shorter than 3-4 h.

Description

Two-dimensional carbon nanosheet and method for preparing two-dimensional carbon nanosheets in large scale
Technical Field
The invention relates to a two-dimensional carbon nanosheet, in particular to a two-dimensional carbon nanosheet and a method for preparing the two-dimensional carbon nanosheet in a large scale.
Background
Since the advent of graphene, graphene-like two-dimensional materials (e.g., Transition Metal Sulfides (TMDs), transition metal oxides, carbon nanoplatelets) have been extensively studied in recent years due to their excellent diffusion properties. In the two-dimensional material, the two-dimensional carbon nanosheet is widely applied to the field of electrochemical energy storage due to the high specific surface area and the adjustable pore size distribution, which is of great significance to the increasing global energy demand, so that in the face of the huge market demand, how to shorten the production period and improve the product quality is the most key problem that each two-dimensional carbon nanosheet production enterprise occupies the market and improves the competition. However, the carbon sources used in the existing two-dimensional carbon nanosheet process need to be esterified to form a long chain, and then the long chain is complexed with metal ions in nitrate to form a metal polymer skeleton, and the progress of the reaction mechanism inevitably leads to the lengthening of the preparation period, so that the method is quite passive for the production enterprises with high competitiveness at present and urgently needs to be solved as soon as possible.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a two-dimensional carbon nanosheet and a method for preparing the two-dimensional carbon nanosheet in a large scale.
According to one aspect of the present invention, there is provided a method for large-scale preparation of two-dimensional carbon nanosheets, comprising the steps of:
heating a mixture of saccharides, transition metal nitrate and water to obtain precursor colloid;
and preparing the two-dimensional carbon nanosheet by using the precursor colloid in a spreading method under a protective atmosphere in an instant or fast firing manner.
The mixture of the saccharides, the transition metal nitrate and the water is an aqueous solution of the saccharides and the transition metal nitrate, wherein the mixing and dissolving time of the saccharides, the transition metal nitrate and the water is less than 1 h.
The saccharides are macromolecular chains, the saccharides are used as carbon sources, the esterification reaction in the prior art is not needed, the hydroxyl groups of the saccharides can be directly complexed with the transition metal provided by the nitrate to form a metal polymer skeleton, the whole dissolving time is short and less than 1h, and the existing preparation process is not realizable. In addition, nitrate provided by the nitrate can generate a large amount of gas in the process of immediate or fast pyrolysis by using a spreading method, and a strong impact force is provided to offset the accumulation force between carbon sources, so that ultrathin carbon nanosheets are obtained, the performance of the carbon nanosheets can be effectively improved, and the large-scale preparation of short-time and high-quality two-dimensional carbon nanosheets is realized, wherein the whole preparation process is less than 3-4h, which is a qualitative improvement for the existing two-dimensional carbon nanosheet preparation technology, and has important significance for the development of two-dimensional carbon nanomaterials.
Further, the transition metal nitrate includes at least one of cobalt nitrate, iron nitrate, and nickel nitrate.
Further, the saccharide includes at least one of glucose, sucrose, maltose, maltodextrin, corn dextrin, starch, and trehalose.
Further, the mass ratio of the saccharides to the transition metal nitrate is 1-6: 1.
Further, the dosage ratio of the transition metal nitrate to the water is 3:15-30, and the dosage ratio of the transition metal nitrate to the water is calculated according to the weight ratio of g: and (5) measuring the ml.
Furthermore, an oil bath is adopted as a heating mode, the heating temperature of the oil bath is 70-160 ℃, and the heating time of the oil bath is less than 2 h.
Further, the firing temperature is 500-.
According to another aspect of the invention, the two-dimensional carbon nanosheet is prepared according to the method for preparing the two-dimensional carbon nanosheet on a large scale.
Furthermore, the two-dimensional carbon nanosheet is applied to at least one of a battery, a supercapacitor, a wave-absorbing material and an electro-catalytic material.
Compared with the prior art, the invention has the following beneficial effects:
1. the method for preparing the two-dimensional carbon nano-sheets in a large scale, which is disclosed by the invention, creatively takes saccharides with macromolecular chains as carbon sources for preparing the two-dimensional carbon nano-sheets, the carbon sources do not need to carry out esterification reaction, and hydroxyl groups of the carbon sources are directly complexed with transition metals provided by nitrates to form a metal polymer framework, so that the forming time of the saccharides and a transition metal nitrate aqueous solution is greatly simplified, and only the time is less than 1h, which is unachievable for the existing preparation process and has important significance, and the formation time of precursor colloids is further shortened by using the saccharides and is less than 2h, which is an important progress for the existing preparation process. In addition, nitrate provided by the nitrate can generate a large amount of gas in the process of immediate or fast pyrolysis by using a spreading method, and a strong impact force is provided to offset the accumulation force between carbon sources, so that ultrathin carbon nanosheets are obtained, the performance of the carbon nanosheets can be effectively improved, and the large-scale preparation of short-time and high-quality two-dimensional carbon nanosheets is realized.
2. The two-dimensional carbon nanosheets exemplified by the invention are thin, uniform in thickness, good in large size and morphology, can be widely applied to lithium ion batteries, sodium ion batteries, lithium sulfur batteries, lithium air batteries, supercapacitors, wave-absorbing materials, catalytic materials and the like, and the appearance of the two-dimensional carbon nanosheets with adjustable size, morphology and redox reaction caters to a new era of high-performance electrode materials for next-generation rechargeable batteries, so that the performance of the rechargeable batteries is remarkably improved, the development of nanotechnology and the practical application of the rechargeable batteries are greatly promoted by providing a higher chemical activity interface, greatly shortening the ion diffusion length and improving the power required by in-plane carrier/charge transportation, and the development and application of a high-performance energy storage device are effective and convenient alternative methods for reducing the consumption of traditional fossil fuels and maintaining sustainable environment and energy supply without doubt, has important influence on the sustainable development of China.
Drawings
FIG. 1 is a high power scan of a two-dimensional carbon nanoplate of the present invention;
FIG. 2 is a high power scan of a two-dimensional carbon nanoplate of the present invention;
FIG. 3 is a lower-power scan of a two-dimensional carbon nanosheet of the present invention;
FIG. 4 is a macroscopic scan of a two-dimensional carbon nanosheet of the present invention;
FIG. 5 is an XRD pattern of a two-dimensional carbon nanosheet obtained in accordance with the present invention;
FIG. 6 is an XRD (X-ray diffraction) pattern of a product obtained by selenizing a two-dimensional carbon nanosheet obtained in the invention;
FIG. 7 is a cyclic voltammetry test chart of the present invention;
FIG. 8 is a typical charge-discharge plot for a wide range of current densities in accordance with the present invention;
FIG. 9 shows (NiCo) Se according to the present invention2Testing figure for outstanding multiplying power characteristic of @ NCNs electrode;
FIG. 10 is a test chart of the cycle performance of the super capacitor of the present invention.
Detailed Description
In order to better understand the technical scheme of the invention, the invention is further explained by combining the drawings and the specific embodiments in the specification.
Example one
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 1g of nickel nitrate, 2g of cobalt nitrate, 6g of glucose and 25mL of deionized water to obtain a mixed solution, wherein the mixing time is 7 min;
s2, placing the mixed solution in an oil bath pan, and heating the mixed solution in the oil bath for 1.7 hours at the temperature of 100 ℃ to obtain precursor colloid;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tubular furnace filled with the protective gas nitrogen to 750 ℃, then placing the quartz tube filled with the precursor colloid in the tubular furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min.
As can be seen from fig. 1 to 4, the obtained two-dimensional carbon nanosheet is thin and uniform in thickness, and the nickel-cobalt metal particle is wrapped by the carbon nanosheet.
As can be seen from fig. 5, the composition of the resulting two-dimensional carbon nanoplatelets comprises N in addition to the presence of carbon and metal particles.
When the obtained two-dimensional carbon nanosheets are applied to a supercapacitor, selenization (reaction of selenium powder and the two-dimensional ultrathin carbon nanosheets) needs to be carried out in advance, and fig. 6 shows that (NiCo) Se is obtained after the obtained two-dimensional carbon nanosheets are subjected to vulcanization treatment2XRD Pattern of @ NCNs, it can be seen from FIG. 6 that nickel-cobalt metal particles wrapped with carbon nanosheets are selenized into CoSe after selenization treatment2/NiSe2The final product is CoSe2/NiSe2Composite material ((NiCo) Se) with ultrathin carbon nanosheets2@ NCNs) applied to supercapacitors.
FIG. 7 is a graph of Cyclic Voltammetry (CV) curves obtained from the application of the material characterized in FIG. 6 to a supercapacitor at a scan rate of 2-50mV s over a voltage range of 0-0.5V-1When (NiCo) Se2@ NCNs electrode. Pseudocapacitance characteristics are clearly shown from the shape of the cyclic voltammogram, and two pairs of redox peaks may be observed. Represents NiSe2/CoSe2The material serves as the source mechanism for the capacitive behavior of the electrode.
FIG. 8 shows a cross section at 1 to 30A g-1Typical charge-discharge diagram over a wide range of current densities. The non-linear shape of these galvanostatic curves at different rates shows a distinct plateau region, indicating that the high coulombic efficiency of the electrode is due to rapid faradaic reactions and multivalent switching.
As can be seen from FIG. 9, (NiCo) Se2Specific capacitances for the @ NCNs electrode were calculated as 1195,1115,980.6,860.5,775 and 725F g-1Corresponding to current densities of 1,2,3,5,10,20 and 30A g, respectively-1. In such a wide current range, the specific capacity retention is 60.6%, showing (NiCo) Se2The excellent rate characteristics of the @ NCNs electrode are attributable to the low resistance and small charge transfer resistance during its internal faradaic redox process.
FIG. 10 is a graph of the cycling performance of a supercapacitor, which is (NiCo) Se2Long term cycling stability of the @ NCNs electrode at a current density of 3A g-1Further study was conducted. As can be seen from the graph, only 9.2% of the specific capacitance after 3000 consecutive cycles was observed compared with the initial specific capacitanceIndicating that the electrode material has excellent long-term electrochemical stability.
Example two
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 3g of ferric nitrate, 3g of sucrose and 15mL of deionized water to obtain a mixed solution, wherein the mixing time is 20 min;
s2, placing the mixed solution in an oil bath pan, and heating the oil bath for 1.9 hours at the temperature of 70 ℃ to obtain precursor colloid;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tubular furnace filled with the protective gas nitrogen to 500-550 ℃, then placing the quartz tube filled with the precursor colloid in the tubular furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min. .
EXAMPLE III
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 1g of nickel nitrate, 2g of cobalt nitrate, 3g of maltose and 20mL of deionized water to obtain a mixed solution, wherein the mixing time is 20 min;
s2, placing the mixed solution in an oil bath pan, and heating the oil bath for 1 hour at 160 ℃ to obtain precursor colloid;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tubular furnace filled with the protective gas nitrogen to 850-900 ℃, then placing the quartz tube filled with the precursor colloid in the tubular furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min.
Example four
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 1g of nickel nitrate, 2g of ferric nitrate, 18g of maltodextrin and 30mL of deionized water to obtain a mixed solution, wherein the mixing time is 58 min;
s2, placing the mixed solution in an oil bath pan, and heating the oil bath for 1.9 hours at the temperature of 120 ℃ to obtain precursor colloid;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tubular furnace filled with the protective gas nitrogen to 700 ℃, then placing the quartz tube filled with the precursor colloid in the tubular furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min.
EXAMPLE five
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 2g of nickel nitrate, 1g of cobalt nitrate, 9g of corn dextrin and 25mL of deionized water to obtain a mixed solution, wherein the mixing time is 55 min;
s2, placing the mixed solution in an oil bath pan, and heating the oil bath for 1.6 hours at the temperature of 140 ℃ to obtain precursor colloid;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tube furnace filled with the protective gas argon to 650 ℃, then placing the quartz tube filled with the precursor colloid in the tube furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min.
EXAMPLE six
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 3g of ferric nitrate, 6g of starch and 30mL of deionized water to obtain a mixed solution;
s2, placing the mixed solution in an oil bath pan, and heating the mixed solution in the oil bath for 1.7 hours at the temperature of 100 ℃ to obtain precursor colloid, wherein the mixing time is 50 min;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tubular furnace filled with the protective gas nitrogen to 750 ℃, then placing the quartz tube filled with the precursor colloid in the tubular furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min.
EXAMPLE seven
The process for preparing the two-dimensional carbon nanosheets on a large scale in the embodiment is as follows:
s1, uniformly mixing 2g of nickel nitrate, 3g of ferric nitrate, 6g of trehalose and 25mL of deionized water to obtain a mixed solution, wherein the mixing time is 45 min;
s2, placing the mixed solution in an oil bath pan, and heating the oil bath for 1.9 hours at the temperature of 120 ℃ to obtain precursor colloid;
s6, sintering the nano powder by a self-propagating method: and (3) heating the tubular furnace filled with the protective gas nitrogen to 780 ℃, then placing the quartz tube filled with the precursor colloid in the tubular furnace, and instantly burning or quickly burning to obtain the two-dimensional carbon nanosheet, wherein the burning process is about 2 min.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.

Claims (10)

1. A method for preparing two-dimensional carbon nanosheets in a large scale is characterized by comprising the following steps:
heating a mixture of saccharides, transition metal nitrate and water to obtain precursor colloid;
and preparing the two-dimensional carbon nanosheet by using the precursor colloid in a spreading method under a protective atmosphere in an instant or fast firing manner.
2. The method for large-scale preparation of two-dimensional carbon nanosheets as recited in claim 1, wherein the mixture of the saccharide, the transition metal nitrate, and the water is an aqueous solution of the saccharide and the transition metal nitrate, wherein the mixing dissolution time of the saccharide, the transition metal nitrate, and the water is less than 1 hour.
3. The method of large scale production of two-dimensional carbon nanoplates as in claim 1, wherein the transition metal nitrate comprises at least one of cobalt nitrate, iron nitrate, and nickel nitrate.
4. The method of mass producing two-dimensional carbon nanoplatelets of claim 1 wherein the carbohydrate comprises at least one of glucose, sucrose, maltose, maltodextrin, corn dextrin, starch, trehalose.
5. The method for mass production of two-dimensional carbon nanoplatelets as in claim 1 wherein the mass ratio of saccharide to transition metal nitrate is 1-6: 1.
6. The method for large-scale preparation of two-dimensional carbon nanoplatelets as claimed in claim 1 wherein the transition metal nitrate is present in a water dosage ratio of 3:15-30 in g: and (5) measuring the ml.
7. The method for preparing two-dimensional carbon nanosheets in large scale according to claim 1, wherein the heating means is an oil bath, the oil bath heating temperature is 70-160 ℃, and the oil bath heating time is less than 2 h.
8. The method for large-scale preparation of two-dimensional carbon nanoplatelets of any of claims 1-7 wherein the firing temperature is 500-.
9. A two-dimensional carbon nanosheet, characterized by being produced by the method for large scale production of two-dimensional carbon nanosheets according to any one of claims 1 to 8.
10. Two-dimensional carbon nanoplatelets according to claim 9 applied to at least one of a battery, a supercapacitor, a wave absorbing material, an electro-catalytic material.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925658A (en) * 2020-08-14 2020-11-13 山东理工大学 In-situ foaming process for preparing thin-layer carbon-loaded nano-silica material
CN112250057A (en) * 2020-10-30 2021-01-22 山东理工大学 Preparation method of ammonium nitrate-assisted macroporous thin-layer carbon

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Publication number Priority date Publication date Assignee Title
CN101012058A (en) * 2007-02-07 2007-08-08 中国科学院山西煤炭化学研究所 Method for preparing medium pore carbon of narrow aperture and high degree of graphitization
CN106219545A (en) * 2016-07-25 2016-12-14 句容市百诚活性炭有限公司 A kind of preparation method of sucrose base grading-hole activated carbon
CN108585027A (en) * 2018-03-15 2018-09-28 山东理工大学 A method of the extensive composite material for preparing two-dimensional metallic oxide and carbon

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101012058A (en) * 2007-02-07 2007-08-08 中国科学院山西煤炭化学研究所 Method for preparing medium pore carbon of narrow aperture and high degree of graphitization
CN106219545A (en) * 2016-07-25 2016-12-14 句容市百诚活性炭有限公司 A kind of preparation method of sucrose base grading-hole activated carbon
CN108585027A (en) * 2018-03-15 2018-09-28 山东理工大学 A method of the extensive composite material for preparing two-dimensional metallic oxide and carbon

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925658A (en) * 2020-08-14 2020-11-13 山东理工大学 In-situ foaming process for preparing thin-layer carbon-loaded nano-silica material
CN112250057A (en) * 2020-10-30 2021-01-22 山东理工大学 Preparation method of ammonium nitrate-assisted macroporous thin-layer carbon

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