CN113620264A - Preparation method of nano black phosphorus/graphene - Google Patents
Preparation method of nano black phosphorus/graphene Download PDFInfo
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- CN113620264A CN113620264A CN202110992596.8A CN202110992596A CN113620264A CN 113620264 A CN113620264 A CN 113620264A CN 202110992596 A CN202110992596 A CN 202110992596A CN 113620264 A CN113620264 A CN 113620264A
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- phosphorus
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 100
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 34
- 239000011574 phosphorus Substances 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 29
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000010453 quartz Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 16
- 239000010439 graphite Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 7
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims abstract description 7
- OZRUMCFJDUAWLN-UHFFFAOYSA-N [I].[Sn].[P] Chemical compound [I].[Sn].[P] OZRUMCFJDUAWLN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000004146 energy storage Methods 0.000 abstract description 3
- 239000012974 tin catalyst Substances 0.000 abstract 1
- 230000007704 transition Effects 0.000 abstract 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of nano black phosphorus/graphene, which comprises the steps of filling red phosphorus or yellow phosphorus serving as a phosphorus source and a graphite-based phosphorus-iodine-tin catalyst into a quartz tube in a segmented manner, utilizing a perforated quartz column to separate the red phosphorus or the yellow phosphorus, enabling the phosphorus raw material and the catalyst to have a certain temperature difference, enabling the phosphorus raw material to be in a high-temperature section, enabling the phosphorus raw material to be in a low-temperature section, enabling a simple substance phosphorus to be vaporized to pass through a catalyst bed layer at a high temperature and be converted into a gaseous intermediate transition state substance, enabling the simple substance phosphorus to move reversely under the action of concentration difference, enabling the simple substance phosphorus to pass through the catalyst bed layer again and stripping graphite into graphene, generating a nano black phosphorus/graphene composite material in the process, and finally moving to the position of the phosphorus source together to generate the nano black phosphorus/graphene composite material. The nano black phosphorus/graphene composite material is prepared by a catalytic method in one step, the preparation method is simple and efficient, a strong acting force can be formed between the nano black phosphorus and the graphene, and the nano black phosphorus/graphene composite material has great application prospects in the fields of energy storage, catalysis, flame retardance and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and relates to a preparation method of nano black phosphorus/graphene.
Background
The nano black phosphorus has high carrier mobility, adjustable direct band gap, large specific surface area and high theoretical specific capacity, so that the nano black phosphorus has good application prospects in the fields of energy storage, catalysis, flame retardance and the like, however, single nano black phosphorus is unstable and has limited performance, the stability of the nano black phosphorus can be improved by compounding the nano black phosphorus with graphene, and meanwhile, the nano black phosphorus and the graphene can realize synergistic effect and play excellent performance. At present, the preparation of the nano black phosphorus/graphene composite material is divided into two types, one type is that massive black phosphorus is stripped into nano black phosphorus and then is compounded with graphene, and the method has the disadvantages of complex steps, high cost, long time consumption, easy oxidation and weak acting force of the composite material; in the other method, elemental phosphorus is used as a raw material, and nano black phosphorus is directly deposited on graphene by a catalytic method to obtain the nano black phosphorus/graphene composite material. Although the invention patent CN201911220206.4 has already prepared the nano black phosphorus/graphene composite material by the catalytic method, the steps are complicated because graphene needs to be prepared by other methods first and then used as a substrate to prepare the composite material, and the composite material prepared by this method may contain impurities such as red phosphorus, white phosphorus, etc., which affect the material properties. Therefore, the method for directly preparing the nano black phosphorus/graphene composite material by one-step catalysis by taking the elemental phosphorus and the graphite as raw materials has important significance for improving the practical application of the nano black phosphorus.
Disclosure of Invention
Aiming at the problems of complicated preparation steps, impure prepared composite material and the like of the existing preparation method of the nano black phosphorus/graphene composite material at present, the invention provides a method for directly preparing the nano black phosphorus/graphene composite material by one-step catalysis.
The invention is realized by the following technical scheme:
a preparation method of nano black phosphorus/graphene comprises the following specific steps:
(1) taking red phosphorus or yellow phosphorus as a phosphorus source, uniformly mixing phosphorus iodine tin powder and graphite, tabletting and forming, encapsulating the mixture and the red phosphorus or the yellow phosphorus in a quartz tube, placing single phosphorus in a high-temperature region, placing a catalyst in a low-temperature region, and separating the middle by using a porous quartz column;
(2) and (3) putting the packaged quartz tube into a two-section tube furnace for high-temperature treatment, preserving heat for a period of time, stripping graphite into graphene by phosphorus steam through a catalyst bed layer, simultaneously forming a nano black phosphorus/graphene composite material, and finally moving the nano black phosphorus/graphene composite material to the position of a phosphorus source together to generate the nano black phosphorus/graphene composite material.
The mass ratio of the phosphorus-iodine-tin powder to the graphite is 5:1-2: 1.
The length of the elemental phosphorus bed layer is 1-7cm away from the length of the catalyst bed layer.
The two-stage heating temperature is 475-.
The heat preservation time is 6-24 h.
The ratio of the elemental phosphorus to the tablet forming catalyst is more than or equal to 0.2
The invention has the beneficial effects that:
1. the method takes the elemental phosphorus as the raw material and takes the phosphorus-iodine-tin containing graphite as the catalyst to prepare the nano black phosphorus/graphene composite material, and has the advantages of simple and efficient preparation process, low cost and short time consumption.
2. The nano black phosphorus/graphene composite material prepared by the invention can be widely applied to the fields of energy storage, catalysis, flame retardance, biomedicine, field effect transistors, sensors and the like, and is expected to show excellent performance.
Drawings
Fig. 1 is an XRD pattern of the nano black phosphorus/graphene composite of example 1;
fig. 2 is a raman diagram of the nano black phosphorus/graphene composite material of example 1.
Detailed Description
The invention is explained in more detail below with reference to the figures and examples.
Example 1
A preparation method of nano black phosphorus/graphene comprises the following specific steps:
(1) weighing 1.35g of elemental red phosphorus, wherein the mass ratio of phosphorus, iodine and tin powder to graphite is 5: 2, tabletting and forming the red phosphorus, serving as a catalyst, and encapsulating the catalyst and elemental phosphorus in a quartz tube, placing red phosphorus in a high-temperature region, placing the catalyst in a low-temperature region, wherein the temperature of the high-temperature region is 540 ℃, the temperature of the low-temperature region is 505 ℃, a bed layer of the elemental phosphorus is separated from a bed layer of the catalyst by 1cm, and the middle of the bed layer is separated by a porous quartz column.
(2) And (3) putting the packaged quartz tube into a two-end temperature control tube furnace, preserving the heat for 6 hours, and cooling to room temperature to obtain the nano black phosphorus/graphene composite material.
Fig. 1 is an XRD pattern of the nano black phosphorus/graphene composite material prepared in example 1. They were compared to a black phosphorus standard card (#73-1358) and a graphite standard card (# 75-1621).
Fig. 2 is a raman diagram of the nano black phosphorus/graphene composite material prepared in example 1. As can be seen from the figure, the characteristic peak A of black phosphorus appearsg 1(358cm-1)、B2g(438cm-1) And Ag 2(465cm-1). There is a distinct graphene D peak (1326 cm)-1) G peak (1583 cm)-1) The D peak is a defect peak of carbon atoms, the G peak is a characteristic peak of carbon, ID/IGThe number is related to the average particle size of the graphite, with a larger value indicating a smaller particle size. I of the sampleD/IGA value of approximately 1 indicates that the graphite particle size of the material is small.
Example 2
(1) Weighing 1.35g of simple yellow phosphorus, wherein the mass ratio of phosphorus, iodine and tin powder to graphite is 1: 1, tabletting and forming the red phosphorus, serving as a catalyst, and encapsulating the catalyst and elemental phosphorus in a quartz tube, placing red phosphorus in a high-temperature region, placing the catalyst in a low-temperature region, wherein the temperature of the high-temperature region is 480 ℃, the temperature of the low-temperature region is 465 ℃, a simple substance phosphorus bed layer and a catalyst bed layer are separated by 5cm, and the middle of the simple substance phosphorus bed layer and the catalyst bed layer are separated by a porous quartz column.
(2) And (3) putting the packaged quartz tube into a two-end temperature control tube furnace, preserving the heat for 15h, and cooling to room temperature to obtain the nano black phosphorus/graphene composite material.
Example 3
(1) Weighing 1.35g of elemental red phosphorus, wherein the mass ratio of phosphorus, iodine and tin powder to graphite is 3: 2, tabletting and forming the red phosphorus, serving as a catalyst, and encapsulating the catalyst and elemental phosphorus in a quartz tube, placing red phosphorus in a high-temperature region, placing the catalyst in a low-temperature region, wherein the temperature of the high-temperature region is 530 ℃, the temperature of the low-temperature region is 500 ℃, and the distance between an elemental phosphorus bed layer and a catalyst bed layer is 7cm and the elemental phosphorus bed layer and the catalyst bed layer are separated by a porous quartz column.
(2) And (3) putting the packaged quartz tube into a two-end temperature control tube furnace, preserving the heat for 24 hours, and cooling to room temperature to obtain the nano black phosphorus/graphene composite material.
Claims (6)
1. A preparation method of nano black phosphorus/graphene is characterized by comprising the following specific steps:
(1) taking red phosphorus or yellow phosphorus as a phosphorus source, uniformly mixing phosphorus iodine tin powder and graphite, tabletting and forming, encapsulating the mixture and the red phosphorus or the yellow phosphorus in a quartz tube, placing single phosphorus in a high-temperature region, placing a catalyst in a low-temperature region, and separating the middle by using a porous quartz column;
(2) and (3) putting the packaged quartz tube into a two-section tube furnace for high-temperature treatment, preserving heat for a period of time, stripping graphite into graphene by phosphorus steam through a catalyst bed layer, simultaneously forming a nano black phosphorus/graphene composite material, and finally moving the nano black phosphorus/graphene composite material to the position of a phosphorus source together to generate the nano black phosphorus/graphene composite material.
2. The method for preparing nano black phosphorus/graphene according to claim 1, wherein the method comprises the following steps: the mass ratio of the phosphorus-iodine-tin powder to the graphite is 5:1-2: 1.
3. The method for preparing nano black phosphorus/graphene according to claim 1, wherein the method comprises the following steps: the length of the elemental phosphorus bed layer is 1-7cm away from the length of the catalyst bed layer.
4. The method for preparing nano black phosphorus/graphene according to claim 1, wherein the method comprises the following steps: the two-stage heating temperature is 475-.
5. The method for preparing nano black phosphorus/graphene according to claim 1, wherein the method comprises the following steps: the heat preservation time is 6-24 h.
6. The method for preparing nano black phosphorus/graphene according to claim 1, wherein the method comprises the following steps: the ratio of the simple substance phosphorus to the tabletting catalyst is more than or equal to 0.2.
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Cited By (2)
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| CN116443862A (en) * | 2023-03-14 | 2023-07-18 | 昆明理工大学 | High-performance sodium ion battery negative electrode material and preparation method thereof |
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| CN114276762A (en) * | 2021-12-30 | 2022-04-05 | 福建科顺新材料有限公司 | Butyl hot melt adhesive composition, butyl hot melt adhesive, and preparation method and application thereof |
| CN116443862A (en) * | 2023-03-14 | 2023-07-18 | 昆明理工大学 | High-performance sodium ion battery negative electrode material and preparation method thereof |
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