CN109908939A - A kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent - Google Patents
A kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent Download PDFInfo
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- CN109908939A CN109908939A CN201910242546.0A CN201910242546A CN109908939A CN 109908939 A CN109908939 A CN 109908939A CN 201910242546 A CN201910242546 A CN 201910242546A CN 109908939 A CN109908939 A CN 109908939A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
A kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent, is with graphite foil, HNO3、H2SO4, ammonium fluoride, thiocarbamide, nickel nitrate, ultrapure water is raw material, is realized respectively by preparation, hydrothermal synthesis reaction, clean dry of graphite oxide foil etc. that nitrogen, sulphur atom adulterate.Nickel phosphide-N doping graphite oxide foil obtained by preparation method of the present invention has excellent flexibility, nitrogen is not only doped in graphite foil, and is able to enter the lattice of nickel phosphide, has good catalytic effect to electrocatalytic hydrogen evolution, catalytic process product stability is good, and product uniformity is good.In addition, the material be expected to flexible battery, in terms of have good application.
Description
The present invention is number of patent application 201810395795.9, a kind of entitled " nickel phosphide-N doping graphite oxide
The divisional application of the preparation method of foil composite nano materials ".
Technical field
The present invention relates to a kind of preparation methods of graphite foil composite nano materials, and in particular to a kind of nickel phosphide-N doping
The preparation method of graphite oxide foil nano material.
Background technique
Catalyst nitrating, sulphur, boron and the oxygen doping of HER has been reported that, because the catalyst after doping is than traditional catalyst
Activity is stronger.Wherein nitrogen and sulfur doping, which can enhance, significantly increases HER activity, this is because atom doped adjustable electron energy level
To improve chemical activity.Epitaxial growth may insure the bonding of the atomic level between material, effectively facilitates the transfer of charge, mentions
Rise the electrocatalysis characteristic of material.Up to the present, people, which have passed through, prepares diversified molybdenum disulfide nano-composite material
Improved properties are carried out to molybdenum disulfide, such as carbon fiber-molybdenum disulfide composite material, graphene-molybdenum disulfide composite material etc..Though
There are many right method, but still all come with some shortcomings, and mainly include experimentation complexity, are not easy to form mass production, product yield
Low, product flexibility obtained is poor, poor to the catalytic effect of electrocatalytic hydrogen evolution, and catalytic process stability is poor, obtains at present
Molybdenum disulfide composite material is to electrocatalytic hydrogen evolution performance still wait improve.Seek inexpensive, environmental-friendly and with high catalytic activity
Electrocatalysis material is the key that the development of electro-catalysis technology.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of graphite foil composite nano materials that catalytic performance is excellent.This hair
Improving eyesight is achieved through the following technical solutions:
A kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent, which is characterized in that it be with graphite foil,
HNO3、H2SO4, ammonium fluoride, thiocarbamide, nickel nitrate, ultrapure water is raw material, the graphite oxide foil adulterated respectively by nitrogen, sulphur atom
Preparation, hydrothermal synthesis reaction, clean dry and etc. realization.Graphite foil composite nano materials obtained are as follows: NiP/N-
Graphene Foil, wherein the mass percentage of the NiP is 5% ~ 15%, the mass percentage of the N is 0.1% ~ 1%,
The mass percentage of the Graphene Foil is 84.9% ~ 94.9%.
Further, graphite foil need to be put into equipped with HNO by the preparation for the graphite oxide foil that above-mentioned nitrogen, sulphur atom adulterate3With
H2SO4Mixed solution in impregnate, then cleaned with deionized water and ethyl alcohol.
Further, it also needs to carry out low temperature cold after the completion of cleaning in the preparation for the graphite oxide foil that above-mentioned nitrogen, sulphur atom adulterate
It is lyophilized dry.
Further, above-mentioned graphite foil, ammonium fluoride, thiocarbamide, nickel nitrate, pure water/ultra-pure water mass ratio be 0.2:0.222:
0.54:0.29:40。
Further, above-mentioned hydrothermal synthesis reaction need to be carried out in the case where being passed through nitrogen, after reaction, also need to carry out cold
It is lyophilized dry.
Specifically, a kind of nickel phosphide-N doping graphite oxide foil composite nano materials preparation method, it is special
In it is to include the following steps to be made:
1. the preparation of the graphite oxide foil of nitrogen atom doping
Graphite foil is put into equipped with HNO3And H2SO4Mixed solution in impregnate, with microwave heating and keep the temperature dipping, after reaction will
Soaked graphite foil sample takes out, respectively with the deionized water of 100ml and washes of absolute alcohol 3 ~ 4 times, after to be put into freezing dry
Dry case is dry, and freeze-drying terminates to obtain the graphite oxide foil sample of nitrogen, sulfur doping；The HNO3And H2SO4Mixing
Solution is to take mass fraction for 65% ~ 68% HNO3The H that solution and mass fraction are 96% ~ 98%2SO4Solution, 1:1 is mixed by volume
It closes, it is 12 ~ 48 hours that graphite foil, which keeps the temperature dip time,；The microwave heating temperature is 80 ~ 85 DEG C, and the microwave power is
300W, the freeze-drying temperature are -55 ~ -45 DEG C, and vacuum degree is 10 ~ 50Pa, 24 ~ 48h of drying time；
2. hydrothermal synthesis reaction
By nitrogen atom doping graphite oxide foil sample and ammonium fluoride described in step 1, thiocarbamide, nickel nitrate, purified water is put into togerther instead
It answers in kettle, is reacted using hydrothermal synthesis, hydro-thermal reaction terminates to be freeze-dried, and freeze-drying terminates to get hydroxide
Nickel/graphite oxide foil；The hydrothermal synthesis reaction is that sample glass slide is fixed to graphite oxide foil in an inclined manner anti-
Kettle middle position is answered, the oxygen being passed through in nitrogen removal reaction solution, and it is passed through nitrogen protection during the reaction, nitrogen pressure
For 2 ~ 3MPa, 115 ~ 125 DEG C of 5 ~ 7h of reaction of reaction temperature are set, are taken out after reaction kettle is cooling, by sample tweezers after taking-up
It gently presss from both sides out, is then washed 3-4 times respectively with the deionized water of 100ml and dehydrated alcohol, it is then dry in freeze-dryer,
The freeze-drying temperature be -55 ~ -45 DEG C, vacuum degree be 10 ~ 50Pa, 24 ~ 48h of drying time to get arrive nickel hydroxide/oxygen
Graphite foil；
3. clean dry
It takes nickel hydroxide obtained in step 2/graphite oxide foil to place and is warming up to 20 ~ 25 DEG C under room temperature environment, take out, clean dry
It is dry to obtain sample, then with sodium hypophosphite in N2It is heated in atmosphere, sodium hypophosphite is placed on upstream, while using heat plasma
Device is to N2Atmosphere carries out plasma, and power 500W, then sample naturally cools to 20 ~ 25 DEG C to get finished product；The secondary phosphorus
The dosage of sour sodium is sodium hypophosphite: nickel hydroxide/graphite oxide foil=x:1, x 0.01-1, and in N2With heating rate in atmosphere
2 ~ 3 DEG C/min are warming up to 330 ~ 360 DEG C of heating and are kept for 110 ~ 130 minutes, N2Flow is 70 ~ 80ml/min, while using heat etc.
Ion generator is to N2Atmosphere carries out plasma, and power 500W, then sample naturally cools to 20 ~ 25 DEG C.
The present invention have it is following the utility model has the advantages that
The method of the present invention uses hydro-thermal method for preparation process, and raw material is simple and easy to get, is obtained by hydro-thermal and parkerizing process compound
Material, whole experiment process process is simple, easy to operate, it is easy to the large-scale production of product is realized, in product use process
There can be excellent flexibility with 100% recycling, gained nickel phosphide-N doping graphite oxide foil, nitrogen is not only enterprising in graphite foil
Row doping, and it is able to enter the lattice of nickel phosphide, there is good catalytic effect to electrocatalytic hydrogen evolution, catalytic process product is stablized
Property is good, and sample carries out 11 hours stability tests under the constant voltage of 80mV, and Hydrogen Evolution Performance maintains 96% or more, and product is equal
Even property is good.In addition, the material be expected to flexible battery, in terms of have good application.
Detailed description of the invention
Fig. 1 is the SEM figure (low power) that embodiment 1 prepares sample.
Fig. 2 is the SEM figure (high power) that embodiment 1 prepares sample.
Fig. 3 is the SEM figure (side) that embodiment 1 prepares sample.
Fig. 4 is the TEM figure (low power) that embodiment 1 prepares sample.
Fig. 5 is the TEM figure (high power) that embodiment 1 prepares sample.
Fig. 6 is the bending lab diagram that embodiment 1 prepares sample.
Fig. 7 is the distribution diagram of element that embodiment 1 prepares sample.
Fig. 8 is the XPS figure that embodiment 1 prepares sample.
Fig. 9 is 1 electro-catalysis H2-producing capacity figure (volt-ampere linear scan) of embodiment.
Figure 10 is that 1 electro-catalysis of embodiment produces stabilized hydrogen performance map.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations to the present invention according to aforementioned present invention content.
Embodiment 1
A kind of preparation for the graphite foil composite nano materials that catalytic performance is excellent:
Weigh about 0.6g with 4 3cm*5cm(of ruler clip) GF be put into equipped with 25ml65%HNO3And 25mL98%H2SO4 Mixing
36h is impregnated in solution, and is taken soaked graphite oxide foil after reaction to 80 DEG C, microwave power 300W with microwave heating
Out, respectively with deionized water and washes of absolute alcohol it is multiple after be put into freeze drying box and be dried, the freeze-drying temperature
It is -50 DEG C, vacuum degree 30Pa, drying time 30h.
It weighs ammonium fluoride (0.222g), thiocarbamide (0.54g), nickel nitrate (0.29g), water (40mL) is dissolved in 40ml deionized water
In, the solution of homogeneous transparent is obtained after stirring 30min, which is poured into 50ml reaction kettle, 0.2g is added and aoxidizes stone
Black foil, position between sample is fixed graphite oxide foil in a kettle with glass slide in an inclined manner, it is anti-to be passed through nitrogen removal
The oxygen in solution is answered, and is passed through nitrogen protection during the reaction, nitrogen pressure 2MPa, 120 DEG C of reaction 6h, by sample after taking-up
Product are gently pressed from both sides out with tweezers, are then washed respectively 3 times with the deionized water of 100ml and dehydrated alcohol, then in freeze-dryer
Middle drying, the freeze-drying temperature be -50 DEG C, vacuum degree 30Pa, drying time 30h to get arrive nickel hydroxide/oxidation stone
Black foil.
Nickel hydroxide/graphite oxide foil is subjected to phosphatization, weighs 30mg sodium hypophosphite, and in N2With heating rate in atmosphere
2 DEG C/min is warming up to 350 DEG C and heats 120 minutes, gas flow 80ml/min, while using heat plasma generator to N2Gas
Atmosphere carry out plasma, power 500W, then sample naturally cool to 20 DEG C to get.
The power spectrum attachment of sample spherical aberration transmission electron microscope shows that the Elemental redistribution of sample is highly uniform.Sample can be with
270 degree are bent over, there is good flexibility.
Experiment one: the electrocatalysis characteristic test of material
Electro-chemical test uses three-electrode system, is tested by AUTOLAB PGSTAT302N work station, tests the sample of preparation
It being cut into after 0.5cm*2cm directly as working electrode, immersion electrolyte area is 0.5cm*1cm, and carbon electrode is used as to electrode,
Silver/silver chloride electrode (Ag/AgCl) is used as reference electrode.Electro-chemical test electrolyte is 0.5M H2SO4Molten before solution testing
Lead to nitrogen 30min in liquid to remove the air in electrolyte, when test each electrode to remain stationary state accurate to be conducive to obtain
Experimental data.The result shows that the alkaline electrocatalytic hydrogen evolution starting voltage of sample is 30mVvsRHE, electricity when overpotential is 80 mV
Current density can reach 10mA/cm2。
Experiment two: electrocatalysis characteristic stability test
It continues with three-electrode system to be tested, be measured using constant pressure power mode, sample obtained by embodiment 1 is adopted
With 80mV voltage, the testing time is 11 hours, and Hydrogen Evolution Performance is kept at 96% or more.
Embodiment 2
A kind of preparation for the graphite foil composite nano materials that catalytic performance is excellent:
Weigh about 0.6g with 4 3cm*5cm(of ruler clip) GF be put into equipped with 25ml65%HNO3With 25mL98% H2SO4 It is mixed
It closes in solution and impregnates 12h, and with microwave heating to 80 DEG C, microwave power 300W, by soaked graphite oxide foil after reaction
Take out, respectively with deionized water and washes of absolute alcohol it is multiple after be put into freeze drying box and be dried, the freeze-drying is warm
Degree is -52 DEG C, vacuum degree 50Pa, drying time 36h.
It weighs ammonium fluoride (0.222g), thiocarbamide (0.54g), nickel nitrate (0.29g), water (40mL) is dissolved in 40ml deionized water
In, the solution of homogeneous transparent is obtained after stirring 30min, which is poured into 50ml reaction kettle, 0.2g is added and aoxidizes stone
Black foil, position between sample is fixed graphite oxide foil in a kettle with glass slide in an inclined manner, it is anti-to be passed through nitrogen removal
The oxygen in solution is answered, and is passed through nitrogen protection during the reaction, nitrogen pressure 3MPa, 115 DEG C of reaction 7h, by sample after taking-up
Product are gently pressed from both sides out with tweezers, are then washed respectively 3 times with the deionized water of 100ml and dehydrated alcohol, then in freeze-dryer
Middle drying, the freeze-drying temperature be -52 DEG C, vacuum degree 50Pa, drying time 36h to get arrive nickel hydroxide/oxidation stone
Black foil.
Nickel hydroxide/graphite oxide foil is subjected to phosphatization, weighs 30mg sodium hypophosphite, and in N2With heating rate in atmosphere
2 DEG C/min is warming up to 360 DEG C and heats 110 minutes, gas flow 82ml/min, while using heat plasma generator to N2Gas
Atmosphere carry out plasma, power 500W, then sample naturally cool to 20 DEG C to get.
The power spectrum attachment of sample spherical aberration transmission electron microscope shows that the Elemental redistribution of sample is highly uniform.Sample can be with
270 degree are bent over, there is good flexibility.The alkaline electrocatalytic hydrogen evolution starting voltage of sample is 40mV vs RHE, excessively electric
Current density can reach 10 mA/cm when position is 93 mV2.As described in Example 1, by sample obtained using 80mV electricity
Pressure, testing time are 11 hours, and Hydrogen Evolution Performance is kept at 96% or more.
Embodiment 3
A kind of preparation for the graphite foil composite nano materials that catalytic performance is excellent:
Weigh about 0.6g with 4 3cm*5cm(of ruler clip) GF be put into equipped with 25ml65%HNO3And 25mL98%H2SO4 Mixing
48h is impregnated in solution, and is taken soaked graphite oxide foil after reaction to 80 DEG C, microwave power 300W with microwave heating
Out, respectively with deionized water and washes of absolute alcohol it is multiple after be put into freeze drying box and be dried, the freeze-drying temperature
It is -48 DEG C, vacuum degree 10Pa, drying time 36h.
It weighs ammonium fluoride (0.222g), thiocarbamide (0.54g), nickel nitrate (0.29g), water (40mL) is dissolved in 40ml deionized water
In, the solution of homogeneous transparent is obtained after stirring 30min, which is poured into 50ml reaction kettle, 0.2g is added and aoxidizes stone
Black foil, position between sample is fixed graphite oxide foil in a kettle with glass slide in an inclined manner, it is anti-to be passed through nitrogen removal
The oxygen in solution is answered, and is passed through nitrogen protection during the reaction, nitrogen pressure 3MPa, 125 DEG C of reaction 5h will after taking-up
Sample is gently pressed from both sides out with tweezers, is then washed 4 times with the deionized water of 100ml and dehydrated alcohol, is then being freeze-dried respectively
Dry in device, the freeze-drying temperature is -48 DEG C, vacuum degree 10Pa, drying time 36h to get to nickel hydroxide/oxidation
Graphite foil.
Nickel hydroxide/graphite oxide foil is subjected to phosphatization, weighs 30mg sodium hypophosphite, and in N2With heating rate in atmosphere
3 DEG C/min is warming up to 330 DEG C and heats 130 minutes, gas flow 78ml/min, while using heat plasma generator to N2Gas
Atmosphere carry out plasma, power 500W, then sample naturally cool to 25 DEG C to get.
The power spectrum attachment of sample spherical aberration transmission electron microscope shows that the Elemental redistribution of sample is highly uniform.Sample can be with
270 degree are bent over, there is good flexibility.The alkaline electrocatalytic hydrogen evolution starting voltage of sample is 42mV vs RHE, excessively electric
Current density can reach 10 mA/cm when position is 92 mV2.As described in Example 1, by sample obtained using 80mV electricity
Pressure, testing time are 11 hours, and Hydrogen Evolution Performance is kept at 96% or more.
Claims (4)
1. a kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent, it is characterised in that: it is with graphite
Foil, HNO3、H2SO4, ammonium fluoride, thiocarbamide, nickel nitrate, ultrapure water be raw material, respectively by nitrogen, sulphur atom adulterate graphite oxide
Preparation, hydrothermal synthesis reaction, the preparation of clean dry step of foil；Nano material material composition obtained is that nickel phosphide-nitrogen sulphur is mixed
Miscellaneous graphite oxide foil, wherein the mass percentage of the nickel phosphide is 5% ~ 15%, the mass percentage of the nitrogen is 0.1% ~
1%, the mass percentage of the graphite oxide foil is 84.9% ~ 94.9%；The graphite foil, ammonium fluoride, thiocarbamide, nickel nitrate,
The mass ratio of ultrapure water is 0.2:0.222:0.54:0.29:40.
2. the preparation method of graphite foil composite nano materials as described in claim 1, it is characterised in that: the nitrogen, sulphur atom
Graphite foil need to be put into equipped with HNO by the preparation of the graphite oxide foil of doping3And H2SO4Mixed solution in impregnate, then use
Deionized water and ethyl alcohol cleaning.
3. the preparation method of graphite foil composite nano materials as claimed in claim 2, it is characterised in that: the hydrothermal synthesis is anti-
It should need to be carried out in the case where being passed through nitrogen, after reaction, also need to be freeze-dried.
4. a kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent, which is characterized in that as follows:
4 3cm*5cm(of clip weigh about 0.6g) GF be put into equipped with 25ml65%HNO3And 25mL98%H2SO4 Mixed solution in
36h is impregnated, and with microwave heating to 80 DEG C, microwave power 300W, take out soaked graphite oxide foil after reaction, respectively
It is dried with freeze drying box is put into after deionized water and washes of absolute alcohol, the freeze-drying temperature is -50 DEG C, vacuum
Degree is 30Pa, drying time 30h；
It weighing ammonium fluoride (0.222g), thiocarbamide (0.54g), nickel nitrate (0.29g), water (40mL) is dissolved in 40ml deionized water,
The solution of homogeneous transparent is obtained after stirring 30min, which is poured into 50ml reaction kettle, 0.2g graphite oxide is added
Foil, position between glass slide to be fixed to graphite oxide foil in an inclined manner in a kettle, is passed through in nitrogen removal reaction solution
Oxygen, and be passed through nitrogen protection during the reaction, nitrogen pressure 2MPa, 120 DEG C of reaction 6h, by sample tweezers after taking-up
It gently presss from both sides out, is then washed respectively 3 times with the deionized water of 100ml and dehydrated alcohol, then dry in freeze-dryer, institute
Stating freeze-drying temperature is -50 DEG C, vacuum degree 30Pa, drying time 30h to get to nickel hydroxide/graphite oxide foil；
Nickel hydroxide/graphite oxide foil is subjected to phosphatization, weighs 30mg sodium hypophosphite, and in N2In atmosphere with 2 DEG C of heating rate/
Min is warming up to 350 DEG C and heats 120 minutes, gas flow 80ml/min, while using heat plasma generator to N2Atmosphere into
Then row plasma, power 500W naturally cool to 20 DEG C to obtain the final product.
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| CN201810395795.9A CN108543543B (en) | 2018-04-27 | 2018-04-27 | A kind of preparation method of nickel phosphide-N doping graphite oxide foil composite nano materials |
| CN201910242546.0A CN109908939A (en) | 2018-04-27 | 2018-04-27 | A kind of preparation method for the graphite foil composite nano materials that catalytic performance is excellent |
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| CN110518254A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of lithium metal battery negative current collector and its preparation method and application |
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| CN109701575A (en) * | 2018-12-11 | 2019-05-03 | 武汉工程大学 | A kind of nitrogen, NiP/ graphene composite aerogel of phosphorus doping and preparation method thereof |
| CN110820010A (en) * | 2019-11-12 | 2020-02-21 | 长沙理工大学 | Self-supporting Ni2P/Ni @ C composite cathode hydrogen evolution material and preparation method thereof |
| CN111270264B (en) * | 2020-02-11 | 2021-04-20 | 中国工程物理研究院材料研究所 | Preparation method and application of monatomic platinum-nitrogen-doped graphite foil self-supporting hydrogen evolution electrode |
| CN112403503B (en) * | 2020-11-27 | 2021-08-03 | 电子科技大学 | Preparation method of nitrogen-doped MOF structure modified two-phase sulfide material |
| CN114878648B (en) * | 2022-04-11 | 2024-02-27 | 上海健康医学院 | Cysteine electrochemical sensor and preparation method and application thereof |
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| CN107138173A (en) * | 2017-05-10 | 2017-09-08 | 江南大学 | A kind of simple and convenient process for preparing of unformed nickel phosphide/class graphene carbon nitrogen compound composite catalyst |
| CN107235472B (en) * | 2017-05-24 | 2019-03-08 | 华中科技大学 | Porous vertical graphene nano wall array of N doping and the preparation method and application thereof |
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Application publication date: 20190621 |