CN103508444A - Phosphorus doped graphene and preparation method thereof - Google Patents
Phosphorus doped graphene and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method for phosphorus doped graphene. The preparation method comprises the following steps: uniformly mixing graphite oxide and phosphorus pentoxide in a mass ratio of 1: 0.5-3 and placing an obtained mixture in a reactor; introducing protective gas into the reactor, wherein introduction flow velocity of the protective gas is 200 to 400 ml/min; heating the interior of the reactor to a temperature of 800 to 900 DEG C at a heating speed of 15 to 20 DEG C/min and maintaining the temperature for 30 min to 2 h; and cooling the reactor to room temperature in the protective gas with flow velocity of 200 to 400 ml/min so as to prepare the phosphorus doped graphene. According to the method, phosphorus pentoxide is used as a phosphorus source, the maximum doping amount of elemental phosphorus can approach 10%, so the adjustable range of phosphorus is wide; and the method has the advantages of simple process, convenient operation, no special requirements on equipment and easy realization of large scale industrial production. The invention further provides the phosphorus doped graphene prepared by using the preparation method.
Description
Technical field
The present invention relates to the synthetic field of material, particularly relate to a kind of phosphorus doping Graphene and preparation method thereof.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal of the discoveries such as the strong K sea nurse of the peace moral of Univ Manchester UK in 2004 (Andre K.Geim), is the carbon material as thin as a wafer of single or multiple lift.Single-layer graphene has good conduction, heat conductivility and low thermal expansivity, and its theoretical specific surface area is up to 2630m
2/ g (A Peigney, Ch Laurent, et al.Carbon, 2001,39,507), can be used for effect transistor, electrode materials, matrix material, liquid crystal display material, sensor.
The method of preparing at present Graphene mainly contain graphite breakaway (Novoselov K S, Geim A K, et al. Science 2004,306,666), chemistry redox method [D A Dikin, et al.Nature 2007,448,457; Sasha Stankovich, Dmitriy A Dikin, Richard D Piner, et al.Carbon 2007,45,1558], ultrasonic stripping method (Guohua Chen, Wengui Weng, Dajun Wu, et al.Carbon.2004,42,753), chemical Vapor deposition process (Alexander N, Obraztsov.Nature nanotechnology.2009,4,212) etc.Conventionally, the Graphene that prepared by these methods is all the Graphene of intrinsic.
Research carries out to Graphene the large focus that element doping modification is current field of nanometer material technology.Theoretical investigation shows, Graphene energy band structure after element doping has adjustment, thereby can greatly expand Graphene in the application in the fields such as optics, electricity and magnetics.At present, doped graphene preparation method's research is not very abundant, and focuses mostly in the research of nitrating Graphene and the research of boron-doping Graphene, and phosphorus doping Graphene is comparatively rare, and in the phosphorus doping Graphene of reporting, phosphorus element content is lower, and the variable range of phosphorus content is narrower.Because phosphorus is lower than nitrogen electronegativity, so after phosphorus doping, the characteristic electron impact on Graphene is different, and therefore, the exploitation of phosphorus doping Graphene is significant.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of preparation method of phosphorus doping Graphene, and this preparation method is usingd Vanadium Pentoxide in FLAKES and prepared phosphorus doping Graphene as phosphorus source, and the most highly doped amount of phosphoric can approach 10%, so the variable range of phosphorus content is wide.Meanwhile, the invention provides the phosphorus doping Graphene making by this preparation method.
The preparation method who the invention provides a kind of phosphorus doping Graphene, comprises the following steps:
First, be that 1: 0.5～3 ratio is got graphite oxide and Vanadium Pentoxide in FLAKES and mixed and be placed in reactor in mass ratio; Then, in reactor, pass into protective gas, the flow velocity that passes into of described protective gas is 200～400ml/min; Then, with the heat-up rate of 15～20 ℃/min, the temperature in reactor is warming up to 800～900 ℃, and keeps 30min～2h; Finally, in the protective gas that is 200～400ml/min at flow velocity, be cooled to room temperature, make phosphorus doping Graphene.
Preferably, described protective gas is at least one in argon gas, nitrogen and helium.
Preferably, described reactor is tube furnace.
Preferably, the mass ratio of described graphite oxide and Vanadium Pentoxide in FLAKES is 1: 1～2.
Preferably, described graphite oxide adopts following steps to make:
In the mix acid liquor that adds the vitriol oil and concentrated nitric acid to form in graphite, form mixed solution, the temperature of mixed solution is remained on to-2～2 ℃ and stir 10～30min; In mixed solution, add at leisure potassium permanganate, continue that the temperature of mixed solution is remained on to-2～2 ℃ and stir 1h; Mixed solution is warming up to 80～90 ℃ and keep 0.5～2h; In mixed solution, add deionized water, continue at 80～90 ℃ of insulation 0.5～2h; And adding hydrogen peroxide to remove potassium permanganate in mixed solution, suction filtration, washs solids with dilute hydrochloric acid and deionized water successively, after drying solid thing, obtains graphite oxide; The solid-to-liquid ratio of described graphite and the described vitriol oil and concentrated nitric acid is 1g: 80～110ml: 15～35ml; The mass ratio of described graphite and described potassium permanganate is 1: 1～10; The solid-to-liquid ratio of potassium permanganate and hydrogen peroxide is 1g: 1～3ml.
Preferably, the purity of described graphite is 90%～99.9%.
The preparation method of phosphorus doping Graphene of the present invention is usingd Vanadium Pentoxide in FLAKES and is prepared phosphorus doping Graphene as phosphorus source, the most highly doped amount of phosphoric can approach 10%, therefore the variable range of phosphorus content is wide, width adjusting wide ranges between energy level, so can prepare according to the requirement of device performance the phosphorus doping Graphene of suitable phosphorus element content.In addition this preparation method's technique is simple, and convenient operation without particular requirement, is easy to realize large-scale industrial production to equipment.
The present invention also provides a kind of phosphorus doping Graphene, and described phosphorus doping Graphene makes by above-mentioned preparation method.
Preferably, in described phosphorus doping Graphene, the doping of phosphoric is 5%～10%.
In this phosphorus doping Graphene, mixed phosphoric, because phosphorus is lower than nitrogen electronegativity, so after phosphorus doping, the characteristic electron impact on Graphene is different.Phosphorus doping belongs to the doping of P type, the impurity level that phosphorus impurities produces can be distributed in fermi level both sides, one approaches conduction band, one approaches valence band, and between two energy levels, the relative nitrogen doping in interval is wide, therefore the phosphorus doping Graphene making is thus applicable to some specific component structure, for example sensor.In addition, the doping of phosphoric does not affect the conjugated structure of Graphene self, does not destroy the electronics transmission between large π key, has retained the excellent specific conductivity of Graphene self.
A kind of phosphorus doping Graphene provided by the invention and preparation method thereof, has following beneficial effect:
This preparation method is usingd Vanadium Pentoxide in FLAKES as phosphorus source, and the variable range of phosphorus content is wide, and technique is simple, and convenient operation without particular requirement, is easy to realize large-scale industrial production to equipment;
In the phosphorus doping Graphene making by this preparation method, mixed phosphoric, it is applicable to some specific component structure, sensor for example, in addition, the doping of phosphoric does not affect the conjugated structure of Graphene self, has retained the excellent specific conductivity of Graphene self.
Embodiment
The preparation method who the invention provides a kind of phosphorus doping Graphene, comprises the following steps:
First, be that 1: 0.5～3 ratio is got graphite oxide and Vanadium Pentoxide in FLAKES and mixed and be placed in reactor in mass ratio; Then, in reactor, pass into protective gas, the flow velocity that passes into of described protective gas is 200～400ml/min; Then, with the heat-up rate of 15～20 ℃/min, the temperature in reactor is warming up to 800～900 ℃, and keeps 30min～2h; Finally, in the protective gas that is 200～400ml/min at flow velocity, be cooled to room temperature, make phosphorus doping Graphene.
Described protective gas is at least one in argon gas, nitrogen and helium.
Described reactor is tube furnace.
The mass ratio of described graphite oxide and Vanadium Pentoxide in FLAKES is 1: 1～2.
Described graphite oxide adopts following steps to make:
In the mix acid liquor that adds the vitriol oil and concentrated nitric acid to form in graphite, form mixed solution, the temperature of mixed solution is remained on to-2～2 ℃ and stir 10～30min; In mixed solution, add at leisure potassium permanganate, continue that the temperature of mixed solution is remained on to-2～2 ℃ and stir 1h; Mixed solution is warming up to 80～90 ℃ and keep 0.5～2h; In mixed solution, add deionized water, continue at 80～90 ℃ of insulation 0.5～2h; And adding hydrogen peroxide to remove potassium permanganate in mixed solution, suction filtration, washs solids with dilute hydrochloric acid and deionized water successively, after drying solid thing, obtains graphite oxide; The solid-to-liquid ratio of described graphite and the described vitriol oil and concentrated nitric acid is 1g: 80～110ml: 15～35ml; The mass ratio of described graphite and described potassium permanganate is 1: 1～10; The solid-to-liquid ratio of potassium permanganate and hydrogen peroxide is 1g: 1～3ml.
The purity of described graphite is 90%～99.9%.
The preparation method of phosphorus doping Graphene of the present invention is usingd Vanadium Pentoxide in FLAKES and is prepared phosphorus doping Graphene as phosphorus source, the most highly doped amount of phosphoric can approach 10%, therefore the variable range of phosphorus content is wide, width adjusting wide ranges between energy level, so can prepare according to the requirement of device performance the phosphorus doping Graphene of suitable phosphorus element content.In addition this preparation method's technique is simple, and convenient operation without particular requirement, is easy to realize large-scale industrial production to equipment.
The present invention also provides a kind of phosphorus doping Graphene, and described phosphorus doping Graphene makes by above-mentioned preparation method.
In described phosphorus doping Graphene, the doping of phosphoric is 5%～10%.
In this phosphorus doping Graphene, mixed phosphoric, because phosphorus is lower than nitrogen electronegativity, so after phosphorus doping, the characteristic electron impact on Graphene is different.Phosphorus doping belongs to the doping of P type, the impurity level that phosphorus impurities produces can be distributed in fermi level both sides, one approaches conduction band, one approaches valence band, and between two energy levels, the relative nitrogen doping in interval is wide, therefore the phosphorus doping Graphene making is thus applicable to some specific component structure, for example sensor.In addition, the doping of phosphoric does not affect the conjugated structure of Graphene self, does not destroy the electronics transmission between large π key, has retained the excellent specific conductivity of Graphene self.
A kind of phosphorus doping Graphene provided by the invention and preparation method thereof, has following beneficial effect:
This preparation method is usingd Vanadium Pentoxide in FLAKES as phosphorus source, and the variable range of phosphorus content is wide, and technique is simple, and convenient operation without particular requirement, is easy to realize large-scale industrial production to equipment;
In the phosphorus doping Graphene making by this preparation method, mixed phosphoric, it is applicable to some specific component structure, sensor for example, in addition, the doping of phosphoric does not affect the conjugated structure of Graphene self, has retained the excellent specific conductivity of Graphene self.
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment mono-
A preparation method for phosphorus doping Graphene, comprises the following steps:
It is to mix in 65% the concentrated nitric acid vitriol oil that is 98% with 90ml massfraction that the graphite that is 95% by 1g purity adds 24ml massfraction, mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add potassium permanganate at leisure again, the mass ratio of potassium permanganate and graphite is 5: 1, stir 1 hour, then mixture is heated to keep 30min at 85 ℃, add afterwards deionized water to continue to keep 30min at 85 ℃, the liquid-solid ratio of deionized water and graphite is 90ml: 1g, finally adding massfraction is 30% superoxol, the liquid-solid ratio of superoxol and graphite is 10ml: 1g, stir 10min, mixture is carried out to suction filtration, with dilute hydrochloric acid and deionized water, solids is washed respectively successively again, dilute hydrochloric acid, the solid-to-liquid ratio of deionized water and graphite is 100ml: 150ml: 1g, wash altogether 3 times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ℃ of vacuum drying ovens.
Be that the ratio of 1: 3 is got graphite oxide and Vanadium Pentoxide in FLAKES mixes in mass ratio, be placed in the argon atmosphere that flow velocity is 300ml/min, heat-up rate with 15 ℃/min is warming up to 900 ℃, keep 2h, in the argon atmosphere that is 300ml/min at flow velocity subsequently, be down to room temperature, make phosphorus doping Graphene.
Embodiment bis-
A preparation method for phosphorus doping Graphene, comprises the following steps:
It is to mix in 68% the concentrated nitric acid vitriol oil that is 80% with 350ml massfraction that the graphite that is 90% by 5g purity adds 100ml massfraction, mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add potassium permanganate at leisure again, the mass ratio of potassium permanganate and graphite is 4: 1, stir 1 hour, then mixture is heated to keep 30min at 85 ℃, add afterwards deionized water to continue to keep 30min at 85 ℃, the liquid-solid ratio of deionized water and graphite is 60ml: 1g, finally adding massfraction is 30% superoxol, the liquid-solid ratio of superoxol and graphite is 5ml: 1g, stir 10min, mixture is carried out to suction filtration, with dilute hydrochloric acid and deionized water, solids is washed respectively successively again, dilute hydrochloric acid, the solid-to-liquid ratio of deionized water and graphite is 90ml: 60ml: 1g, wash altogether 3 times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ℃ of vacuum drying ovens.
Be that the ratio of 1: 2 is got graphite oxide and Vanadium Pentoxide in FLAKES mixes in mass ratio, be placed in the nitrogen atmosphere that flow velocity is 200ml/min, heat-up rate with 20 ℃/min is warming up to 850 ℃, keep 1h, in the nitrogen atmosphere that is 200ml/min at flow velocity subsequently, be down to room temperature, make phosphorus doping Graphene.
Embodiment tri-
A preparation method for phosphorus doping Graphene, comprises the following steps:
It is to mix in 50% the concentrated nitric acid vitriol oil that is 98% with 180ml massfraction that the graphite that is 99.9% by 2g purity adds 48ml massfraction, mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add potassium permanganate at leisure again, the mass ratio of potassium permanganate and graphite is 4: 1, stir 1 hour, then mixture is heated to keep 30min at 85 ℃, add afterwards deionized water to continue to keep 30min at 85 ℃, the liquid-solid ratio of deionized water and graphite is 90ml: 1g, finally adding massfraction is 30% superoxol, the liquid-solid ratio of superoxol and graphite is 7.5ml: 1g, stir 10min, mixture is carried out to suction filtration, with dilute hydrochloric acid and deionized water, solids is washed respectively successively again, dilute hydrochloric acid, the solid-to-liquid ratio of deionized water and graphite is 100ml: 150ml: 1g, wash altogether 3 times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ℃ of vacuum drying ovens.
Be that the ratio of 1: 1 is got graphite oxide and Vanadium Pentoxide in FLAKES mixes in mass ratio, being placed in flow velocity is the helium atmosphere of 400ml/min, heat-up rate with 20 ℃/min is warming up to 900 ℃, keep 1h, in the helium atmosphere that is 400ml/min at flow velocity subsequently, be down to room temperature, make phosphorus doping Graphene.
Embodiment tetra-
A preparation method for phosphorus doping Graphene, comprises the following steps:
It is to mix in 65% the concentrated nitric acid vitriol oil that is 90% with 95ml massfraction that the graphite that is 95% by 1g purity adds 25ml massfraction, mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add potassium permanganate at leisure again, the mass ratio of potassium permanganate and graphite is 3: 1, stir 1 hour, then mixture is heated to keep 30min at 85 ℃, add afterwards deionized water to continue to keep 30min at 85 ℃, the liquid-solid ratio of deionized water and graphite is 100ml: 1g, finally adding massfraction is 30% superoxol, the liquid-solid ratio of superoxol and graphite is 8ml: 1g, stir 10min, mixture is carried out to suction filtration, with dilute hydrochloric acid and deionized water, solids is washed respectively successively again, dilute hydrochloric acid, the solid-to-liquid ratio of deionized water and graphite is 100ml: 150ml: 1g, wash altogether 3 times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ℃ of vacuum drying ovens.
Be that the ratio of 2: 1 is got graphite oxide and Vanadium Pentoxide in FLAKES mixes in mass ratio, be placed in the argon atmosphere that flow velocity is 200ml/min, heat-up rate with 15 ℃/min is warming up to 800 ℃, keep 30min, in the argon atmosphere that is 200ml/min at flow velocity subsequently, be down to room temperature, make phosphorus doping Graphene.
Effect embodiment
The prepared phosphorus doping Graphene of embodiment mono-～tetra-is passed through to the wherein content of each principal element of XPS measurements determination, and test result is as following table 1.
Each principal element content of phosphorus doping Graphene in table 1 embodiment mono-～embodiment tetra-
| Carbon (%) | Phosphoric (%) | Oxygen element (%) | |
| Embodiment mono- | 80.2 | 9.2 | 10.6 |
| Embodiment bis- | 81.3 | 8.6 | 10.1 |
| Embodiment tri- | 81.4 | 7.2 | 11.4 |
| Embodiment tetra- | 83.2 | 5.9 | 10.9 |
As can be seen from Table 1, the phosphorus content of the phosphorus doping Graphene that the embodiment of the present invention makes can reach 9.2%, has higher phosphorus content, and the content of phosphorus can regulate in wider scope.
Phosphorus doping Graphene specific conductivity performance test in table 2 embodiment mono-～embodiment tetra-
| Specific conductivity (S/m) | |
| Embodiment mono- | 1783 |
| Embodiment bis- | 1742 |
| Embodiment tri- | 1623 |
| Embodiment tetra- | 1522 |
As can be seen from Table 2, through the test of four point probe resistance meter, the specific conductivity of the phosphorus doping Graphene that the embodiment of the present invention makes is higher, is up to 1783S/m.
Claims (8)
1. a preparation method for phosphorus doping Graphene, is characterized in that, comprises the following steps: first, be that 1: 0.5～3 ratio is got graphite oxide and Vanadium Pentoxide in FLAKES and mixed and be placed in reactor in mass ratio; Then, in reactor, pass into protective gas, the flow velocity that passes into of described protective gas is 200～400ml/min; Then, with the heat-up rate of 15～20 ℃/min, the temperature in reactor is warming up to 800～900 ℃, and keeps 30min～2h; Finally, in the protective gas that is 200～400ml/min at flow velocity, be cooled to room temperature, make phosphorus doping Graphene.
2. the preparation method of a kind of phosphorus doping Graphene as claimed in claim 1, is characterized in that, described protective gas is at least one in argon gas, nitrogen and helium.
3. the preparation method of a kind of phosphorus doping Graphene as claimed in claim 1, is characterized in that, described reactor is tube furnace.
4. the preparation method of a kind of phosphorus doping Graphene as claimed in claim 1, is characterized in that, the mass ratio of described graphite oxide and Vanadium Pentoxide in FLAKES is 1: 1～2.
5. the preparation method of a kind of phosphorus doping Graphene as claimed in claim 1, is characterized in that, described graphite oxide adopts following steps to make:
In the mix acid liquor that adds the vitriol oil and concentrated nitric acid to form in graphite, form mixed solution, the temperature of mixed solution is remained on to-2～2 ℃ and stir 10～30min; In mixed solution, add at leisure potassium permanganate, continue that the temperature of mixed solution is remained on to-2～2 ℃ and stir 1h; Mixed solution is warming up to 80～90 ℃ and keep 0.5～2h; In mixed solution, add deionized water, continue at 80～90 ℃ of insulation 0.5～2h; And adding hydrogen peroxide to remove potassium permanganate in mixed solution, suction filtration, washs solids with dilute hydrochloric acid and deionized water successively, after drying solid thing, obtains graphite oxide; The solid-to-liquid ratio of described graphite and the described vitriol oil and concentrated nitric acid is 1g: 80～110ml: 15～35ml; The mass ratio of described graphite and described potassium permanganate is 1: 1～10; The solid-to-liquid ratio of potassium permanganate and hydrogen peroxide is 1g: 1～3ml.
6. the preparation method of a kind of phosphorus doping Graphene as claimed in claim 5, is characterized in that, the purity of described graphite is 90%～99.9%.
7. a phosphorus doping Graphene, is characterized in that, described phosphorus doping Graphene is made by the preparation method described in arbitrary claim in claim 1～6.
8. a kind of phosphorus doping Graphene as claimed in claim 7, is characterized in that, in described phosphorus doping Graphene, the doping of phosphoric is 5%～10%.
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| JP2018536102A (en) * | 2015-11-20 | 2018-12-06 | 済南聖泉集団股▲ふん▼有限公司Ｊｉｎａｎ Ｓｈｅｎｇｑｕａｎ Ｇｒｏｕｐ Ｓｈａｒｅ Ｈｏｌｄｉｎｇ Ｃｏ．， Ｌｔｄ | Functional regenerated cellulose fiber and its preparation and use |
| US10941273B2 (en) | 2015-11-20 | 2021-03-09 | Jinan Shengquan Group Share Holding Co., Ltd. | Graphene-containing modified latex as well as preparation method therefor and application thereof |
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