CN112661144A - Method for preparing nitrogen-doped graphene ink with assistance of sodium deoxycholate - Google Patents
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Abstract
The invention relates to a method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate, which is characterized in that natural crystalline flake graphite is oxidized into graphene oxide with high oxygen content and most carbon six-membered rings; carrying out hydrothermal nitrogen doping on graphene oxide; dispersing nitrogen-doped graphene in water, adding a surfactant in batches, performing ultrasonic treatment, alternately performing low-power and high-power ultrasonic treatment, dispersing and spreading solute sheets, and finally obtaining the nitrogen-doped graphene ink with large stably dispersed sheets, wherein the sheet size is 800-2000nm, and the thickness is 1-2 nm. The nitrogen-doped graphene ink can be used for a uniform droplet jetting printing platform, and particularly can be used for printing a graphene metamaterial wave-absorbing microstructure through uniform droplet jetting. The preparation method of the nitrogen-doped graphene ink has the advantages of stable dispersion, micron-scale lamellar spreading and the like.
Description
Technical Field
The invention belongs to the field of 3D printing materials, relates to a method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate, and particularly relates to a preparation method of large-sheet thin-layer nitrogen-doped graphene water-based ink for uniform droplet jetting.
Background
Graphene is a novel nano material consisting of six-membered rings formed by single-layer carbon atoms, and has great application potential in the aspects of electronics, energy and medical treatment due to excellent electric, optical, mechanical and thermal properties. However, the zero band gap property of graphene limits its application in the electronic field. The chemical doping modification can effectively regulate and control the graphene energy band structure and performance, and the nitrogen-doped graphene (NG) changes the graphene energy band structure, so that the graphene energy band structure is converted from a conductor material to a semiconductor material, and the graphene energy band structure has wide application prospects in photoelectric devices such as super capacitors, field effect transistors, terahertz wave absorbers and the like. The uniform droplet ejection technology is a new 3D printing technology, can realize rapid prototype manufacturing of a graphene microstructure with a micron scale, has the advantages of low cost, customization, simple process and the like, and has great advantages in the field of high-performance graphene photoelectric functional device preparation.
The nitrogen-doped graphene ink with the advantages of sheet wetting, proper size, stable aggregation dissociation and dispersion is the key for preparing a high-performance nitrogen-doped graphene photoelectric device by uniform droplet spraying. The strong hydrophobicity of the graphene surface is the root cause of aggregation and sedimentation of the sheet layer. Most preparation methods obtain graphene ink by repeatedly centrifuging and taking supernatant, so that graphene sheets remained in the ink are too small. The ultrasonic treatment is an effective means for dispersing graphene, can obtain graphene sheets with 1-10 layers, and can exert excellent electric, optical, force and thermal properties of graphene, but the size of the obtained single sheet is usually too small, about 200-300 nm, so that the number of overlapping points of the sheet layers is too large, and a conductive path is not smooth. Therefore, the method needs to continuously explore and optimize the ultrasonic dispersion process, and develop the nitrogen-doped graphene ink special for the uniform droplet jetting technology, which has the advantages of large sheet layer size and stable dispersion of the nitrogen-doped graphene.
Document 1 "Wang D W, Gentle I R, Lu G Q M. enhanced electrochemical sensitivity of PtRh electrodes coated with nitro-gene-doped graphene [ J ]. Electrochemistry communications,2010,1210: 1423-1427" discloses a method for dispersing and nitrogen doping graphene by using a hydrazine hydrate ultrasonic-assisted method. The prepared nitrogen-doped graphene crystal lattice is completely recovered, the size of the lamella is uniform, but the size of the lamella is too small and is only 200nm, and the improvement of the overlapping rate of the lamella in the process of uniform droplet jet printing is not facilitated.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate, and overcomes the defect that the size of the nitrogen-doped graphene ink prepared by the existing method is smaller.
Technical scheme
A method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate is characterized by comprising the following steps:
step 1, preparing graphene oxide powder by using natural crystalline flake graphite powder:
(1) adding graphite powder into concentrated sulfuric acid, wherein the concentration of the graphite powder is 0.02-0.06g/mL, fully mixing, mixing according to the mass ratio of graphite to potassium permanganate of 1:3-1:10, carrying out gradient heating reaction, and cooling to room temperature to obtain a mixture; the gradient heating comprises the following steps: setting 1-5 temperature gradients, controlling the temperature range to be 0-70 ℃, and controlling the total reaction time to be 4-100 h;
(2) washing the mixture with deionized water to neutrality, pouring out supernatant, and finishing the process with a centrifuge;
(3) collecting bottom layer slurry, carrying out ultrasonic treatment and freeze drying to obtain graphene oxide powder;
(1) dissolving graphene oxide in water, and performing ultrasonic treatment to obtain a dispersion liquid;
(2) adding ammonium carbonate into the dispersion liquid, and fully stirring; the mass ratio of the graphene oxide to the ammonium carbonate is 1: 1-500;
(3) putting the dispersion liquid added with the ammonium carbonate into a hydrothermal reaction kettle, sealing the reaction kettle, putting the reaction kettle into an oven, and carrying out hydrothermal reaction at 70-250 ℃ to obtain nitrogen-doped graphene;
step 3, preparing the nitrogen-doped graphene ink:
(1) adding nitrogen-doped graphene into water to prepare a dispersion liquid with the concentration of 1-5mg/mL, and performing ultrasonic treatment; in the ultrasonic process, adding a surfactant sodium deoxycholate into the system for multiple times;
the ultrasonic treatment comprises the following steps: the ultrasonic power is 30-240W and 400-800W, the ultrasonic time of each section is 0.4-2h, the ratio of the high-power ultrasonic time to the low-power ultrasonic time is 2: 1-5: 1, and the total ultrasonic treatment time is 12-300 h;
(2) and (4) standing for 3h after the ultrasonic treatment is finished, and collecting supernatant, namely the nitrogen-doped graphene ink.
The centrifugal rotation speed of the step 1 is 1000-10000 rpm, and the time is 3-20 min.
The ultrasonic time of the ultrasonic treatment in the step 1 and the step 2 is 0.5-3h, and the power is 200-300W.
The final concentration of sodium deoxycholate in the nitrogen-doped graphene ink is 0.003-0.007 g/mL.
Advantageous effects
The invention provides a method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate. And secondly, under the action of a nitrogen-doping agent and at a proper temperature, cutting and doping the graphene oxide through a hydrothermal reaction to obtain the nitrogen-doped graphene. And finally, mixing the nitrogen-doped graphene and a proper amount of sodium deoxycholate in water, and carrying out high-low power alternating ultrasound for a certain time length proportion, wherein the high power ultrasound aims at scattering agglomerated and stacked nitrogen-doped graphene blocks, the soft acting force of the low power ultrasound promotes the spreading of the sheets, the tearing of the sheets at the cooperative positions of the epoxy groups is effectively prevented, and the sheets with larger sizes are maintained. The ultrasonic process is repeated continuously, and finally the nitrogen-doped graphene water-based ink with the stably dispersed large thin layers is prepared, wherein the size of the thin layers is 800-2000nm, and the thickness is 1-2 nm.
The invention has the beneficial effects that: the technological parameters are strictly controlled in the whole preparation process, the stretching form of the micron-sized sheet layer in the ink is ensured, and the problems that the ink prepared by the existing method is complex in components, and the nitrogen-doped graphene sheet layer is trivial and serious in agglomeration are solved. Printing experiments prove that the nitrogen-doped graphene sheet is in a good lap joint state, and the preparation method has obvious cost benefit and environmental protection property and is excellent ink for realizing the rapid printing of a new generation of photoelectric devices. The nitrogen-doped graphene ink can be used for a uniform droplet jetting printing platform, and particularly can be used for printing a graphene metamaterial wave-absorbing microstructure through uniform droplet jetting. The preparation method of the nitrogen-doped graphene ink has the advantages of stable dispersion, micron-scale lamellar spreading and the like.
Drawings
Fig. 1 is a flow chart of nitrogen-doped graphene ink preparation.
Fig. 2 is an optical photograph of the nitrogen-doped graphene ink.
Fig. 3 is an atomic force microscope photograph of nitrogen-doped graphene.
Fig. 4 is a size measurement result of the photograph of fig. 3.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
step 1: graphene oxide preparation
(1) Adding graphite powder into concentrated sulfuric acid, wherein the concentration of the graphite powder is 0.04g/mL, fully mixing, mixing according to the mass ratio of graphite to potassium permanganate of 1:6, carrying out gradient heating reaction, and cooling to room temperature to obtain a mixture.
(2) The mixture was washed with deionized water to neutrality and the supernatant was decanted. This was done with a centrifuge.
(3) Collecting the bottom layer slurry, and carrying out freeze drying after ultrasonic treatment to obtain graphene oxide powder.
In the preparation method of the graphene oxide, in the step (1), the number of the temperature gradients is set to be 3, the temperature gradients are 5, 35 and 70 ℃ in sequence, and the reaction time is 0.5, 1 and 0.5h in sequence.
And/or, in the step (2), the centrifugal rotating speed is 8000rpm, and the time is 20 min.
In the step (3), the ultrasonic time is 0.5h, and the power is 200W.
Step 2: preparation of nitrogen-doped graphene
(1) And (3) dissolving the graphene oxide obtained in the step (1) in water, and carrying out ultrasonic treatment.
(2) Adding ammonium carbonate into the dispersion liquid obtained in the step (1), and fully stirring.
(3) And (3) putting the dispersion liquid obtained in the step (2) into a hydrothermal reaction kettle, sealing the reaction kettle, and putting the reaction kettle into a drying oven for hydrothermal reaction.
In the nitrogen doping process of the graphene oxide, in the step (1), the ultrasonic time is 0.5h, and the power is 200W.
In the step (2), the mass ratio of the graphene oxide to the ammonium carbonate is 1: 20.
In the step (3), the hydrothermal reaction temperature was set to 80 ℃.
And step 3: preparation of nitrogen-doped graphene ink
(1) And (3) adding the nitrogen-doped graphene obtained in the step (2) into water to prepare a dispersion liquid with the concentration of 2.7mg/mL, and performing ultrasonic treatment.
(2) And (3) adding a surfactant sodium deoxycholate into the dispersion system obtained in the step (1) for multiple times in an ultrasonic process.
(3) And (4) standing for 3h after the ultrasonic treatment is finished, and collecting supernatant, namely the nitrogen-doped graphene ink.
And (3) the final concentration of sodium deoxycholate in the nitrogen-doped graphene ink is 0.003 g/mL.
In the step 3, the ultrasonic power is 30W and 800W, the ultrasonic time of each section is 1.5h and 4.5h, and the total ultrasonic treatment time is 60 h.
Example 2:
step 1: preparation of graphene oxide powder from natural flake graphite powder
(1) Adding graphite powder into concentrated sulfuric acid, wherein the concentration of the graphite powder is 0.04g/mL, fully mixing, mixing according to the mass ratio of graphite to potassium permanganate of 1:6, carrying out gradient heating reaction, and cooling to room temperature to obtain a mixture.
(2) The mixture was washed with deionized water to neutrality and the supernatant was decanted. This was done with a centrifuge.
(3) Collecting the bottom layer slurry, and carrying out freeze drying after ultrasonic treatment to obtain graphene oxide powder.
In the preparation method of the graphene oxide, in the step (1), 5 temperature gradients are set, the temperature gradients are 5, 15, 35, 45 and 70 ℃ in sequence, and the reaction time is 0.5, 1, 0.5 and 1 hour in sequence.
And/or in the step (2), the centrifugal rotating speed is 6000rpm, and the time is 15 min.
In the step (3), the ultrasonic time is 2h, and the power is 300W.
Step 2: preparation of nitrogen-doped graphene powder from graphene oxide
(1) And (3) dissolving the graphene oxide obtained in the step (1) in water, and carrying out ultrasonic treatment.
(2) Adding ammonium carbonate into the dispersion liquid obtained in the step (1), and fully stirring.
(3) And (3) putting the dispersion liquid obtained in the step (2) into a hydrothermal reaction kettle, sealing the reaction kettle, and putting the reaction kettle into a drying oven for hydrothermal reaction.
In the nitrogen doping process of the graphene oxide, in the step (1), the ultrasonic time is 0.5h, and the power is 300W.
In the step (2), the mass ratio of the graphene oxide to the ammonium carbonate is 1: 100.
In the above (3), the hydrothermal reaction temperature was set to 130 ℃.
And step 3: preparation of nitrogen-doped graphene ink
(1) And (3) adding the nitrogen-doped graphene obtained in the step (2) into water to prepare a dispersion liquid with the concentration of 2.7mg/mL, and performing ultrasonic treatment.
(2) And (3) adding a surfactant sodium deoxycholate into the dispersion system obtained in the step (1) for multiple times in an ultrasonic process.
(3) And (4) standing for 3h after the ultrasonic treatment is finished, and collecting supernatant, namely the nitrogen-doped graphene ink.
And (3) the final concentration of sodium deoxycholate in the nitrogen-doped graphene ink is 0.006 g/mL.
In the step 3, the ultrasonic power is 120W and 400W, the ultrasonic treatment is performed alternately, the ultrasonic time length of each section is 1 and 2h, and the total ultrasonic treatment time length is 12 h.
Example 3:
step 1: preparation of graphene oxide powder from natural flake graphite powder
(1) Adding graphite powder into concentrated sulfuric acid, wherein the concentration of the graphite powder is 0.04g/mL, fully mixing, mixing according to the mass ratio of graphite to potassium permanganate of 1:6, carrying out gradient heating reaction, and cooling to room temperature to obtain a mixture.
(2) The mixture was washed with deionized water to neutrality and the supernatant was decanted. This was done with a centrifuge.
(3) Collecting the bottom layer slurry, and carrying out freeze drying after ultrasonic treatment to obtain graphene oxide powder.
In the preparation method of the graphene oxide, in the step (1), 2 temperature gradients are set, the temperature gradients are sequentially 2 and 65 ℃, and the reaction time is sequentially 2 and 8 hours.
And/or, in the step (2), the centrifugal rotating speed is 10000 rpm, and the time is 15 min.
In the step (3), the ultrasonic time is 0.5h, and the power is 200W.
Step 2: preparation of nitrogen-doped graphene powder from graphene oxide
(1) And (3) dissolving the graphene oxide obtained in the step (1) in water, and carrying out ultrasonic treatment.
(2) Adding ammonium carbonate into the dispersion liquid obtained in the step (1), and fully stirring.
(3) And (3) putting the dispersion liquid obtained in the step (2) into a hydrothermal reaction kettle, sealing the reaction kettle, and putting the reaction kettle into a drying oven for hydrothermal reaction.
In the nitrogen doping process of the graphene oxide, in the step (1), the ultrasonic time is 4 hours, and the power is 300W.
In the step (2), the mass ratio of the graphene oxide to the ammonium carbonate is 1: 50.
In the above (3), the hydrothermal reaction temperature was set to 240 ℃.
And step 3: preparation of nitrogen-doped graphene ink
(1) And (3) adding the nitrogen-doped graphene obtained in the step (2) into water to prepare a dispersion liquid with the concentration of 2.7mg/mL, and performing ultrasonic treatment.
(2) And (3) adding a surfactant sodium deoxycholate into the dispersion system obtained in the step (1) for multiple times in an ultrasonic process.
(3) And (4) standing for 3h after the ultrasonic treatment is finished, and collecting supernatant, namely the nitrogen-doped graphene ink.
And the final concentration of sodium deoxycholate in the nitrogen-doped graphene ink in the step (3) is 0.007 g/mL.
In the step 3, the ultrasonic power is 240W and 400W, the ultrasonic time of each section is 0.5h and 2h, and the total ultrasonic treatment time is 30 h.
Claims (4)
1. A method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate is characterized by comprising the following steps:
step 1, preparing graphene oxide powder by using natural crystalline flake graphite powder:
(1) adding graphite powder into concentrated sulfuric acid, wherein the concentration of the graphite powder is 0.02-0.06g/mL, fully mixing, mixing according to the mass ratio of graphite to potassium permanganate of 1:3-1:10, carrying out gradient heating reaction, and cooling to room temperature to obtain a mixture; the gradient heating comprises the following steps: setting 1-5 temperature gradients, controlling the temperature range to be 0-70 ℃, and controlling the total reaction time to be 4-100 h;
(2) washing the mixture with deionized water to neutrality, pouring out supernatant, and finishing the process with a centrifuge;
(3) collecting bottom layer slurry, carrying out ultrasonic treatment and freeze drying to obtain graphene oxide powder;
step 2, preparing nitrogen-doped graphene powder from graphene oxide:
(1) dissolving graphene oxide in water, and performing ultrasonic treatment to obtain a dispersion liquid;
(2) adding ammonium carbonate into the dispersion liquid, and fully stirring; the mass ratio of the graphene oxide to the ammonium carbonate is 1: 1-500;
(3) putting the dispersion liquid added with the ammonium carbonate into a hydrothermal reaction kettle, sealing the reaction kettle, putting the reaction kettle into an oven, and carrying out hydrothermal reaction at 70-250 ℃ to obtain nitrogen-doped graphene;
step 3, preparing the nitrogen-doped graphene ink:
(1) adding nitrogen-doped graphene into water to prepare a dispersion liquid with the concentration of 1-5mg/mL, and performing ultrasonic treatment; in the ultrasonic process, adding a surfactant sodium deoxycholate into the system for multiple times;
the ultrasonic treatment comprises the following steps: the ultrasonic power is 30-240W and 400-800W, the ultrasonic time of each section is 0.4-2h, the ratio of the high-power ultrasonic time to the low-power ultrasonic time is 2: 1-5: 1, and the total ultrasonic treatment time is 12-300 h;
(2) and (4) standing for 3h after the ultrasonic treatment is finished, and collecting supernatant, namely the nitrogen-doped graphene ink.
2. The method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate according to claim 1, is characterized in that: the centrifugal rotation speed of the step 1 is 1000-10000 rpm, and the time is 3-20 min.
3. The method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate according to claim 1, is characterized in that: the ultrasonic time of the ultrasonic treatment in the step 1 and the step 2 is 0.5-3h, and the power is 200-300W.
4. The method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate according to claim 1, is characterized in that: the final concentration of sodium deoxycholate in the nitrogen-doped graphene ink is 0.003-0.007 g/mL.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896254A (en) * | 2012-12-26 | 2014-07-02 | 海洋王照明科技股份有限公司 | Preparation method of nitrogen-doped graphene |
| CN104071782A (en) * | 2014-06-27 | 2014-10-01 | 广州市尤特新材料有限公司 | Preparation method of graphene |
| US20170369320A1 (en) * | 2016-06-26 | 2017-12-28 | Nanotek Instruments, Inc. | Direct Ultrasonication Production of Graphene Sheets from Coke or Coal |
| CN110079158A (en) * | 2019-03-12 | 2019-08-02 | 上海集成电路研发中心有限公司 | A method of preparing aqueous graphene oxide ink |
| CN110790267A (en) * | 2019-11-04 | 2020-02-14 | 淮阴师范学院 | Preparation method of nitrogen-doped graphene |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896254A (en) * | 2012-12-26 | 2014-07-02 | 海洋王照明科技股份有限公司 | Preparation method of nitrogen-doped graphene |
| CN104071782A (en) * | 2014-06-27 | 2014-10-01 | 广州市尤特新材料有限公司 | Preparation method of graphene |
| US20170369320A1 (en) * | 2016-06-26 | 2017-12-28 | Nanotek Instruments, Inc. | Direct Ultrasonication Production of Graphene Sheets from Coke or Coal |
| CN110079158A (en) * | 2019-03-12 | 2019-08-02 | 上海集成电路研发中心有限公司 | A method of preparing aqueous graphene oxide ink |
| CN110790267A (en) * | 2019-11-04 | 2020-02-14 | 淮阴师范学院 | Preparation method of nitrogen-doped graphene |
Non-Patent Citations (1)
| Title |
|---|
| HU KE-WEN ET AL.: "Preparation and physicochemical properties of nitrogen-doped graphene inks" * |
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