CN112661144B - 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 by sodium deoxycholate, which oxidizes natural crystalline flake graphite into graphene oxide with higher oxygen content and maximum carbon six-element environmental protection; 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 large-sheet stable-dispersion nitrogen-doped graphene ink, wherein the size of the sheets is 800-2000nm and the thickness is 1-2nm. The nitrogen-doped graphene ink can be used for a uniform droplet ejection printing platform, and particularly can be used for printing a graphene metamaterial wave-absorbing microstructure through uniform droplet ejection. The preparation method of the nitrogen-doped graphene ink has the advantages of stable dispersion, micron-sized sheet 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 by sodium deoxycholate, and particularly relates to a method for preparing large-sized thin-layer nitrogen-doped graphene water-based ink for uniform droplet ejection.
Background
Graphene is a novel nanomaterial 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 electricity, light, force and thermal properties. However, the zero band gap characteristics of graphene limit its application in the electronics field. The chemical doping modification can effectively regulate and control the energy band structure and performance of the graphene, and the nitrogen doped graphene (NG) changes the energy band structure of the graphene, so that the graphene is converted from a conductor material to a semiconductor material, and has wide application prospects in photoelectric devices such as supercapacitors, field effect transistors, terahertz wave absorbers and the like. The uniform droplet jetting technology is an emerging 3D printing technology, can realize the rapid prototype manufacture of the micrometer-scale graphene microstructure, has the advantages of low cost, customization, simple process and the like, and has great advantages in the field of preparation of high-performance graphene photoelectric functional devices.
The nitrogen-doped graphene ink with the advantages of sheet wetting, proper size and stable agglomeration and dissociation and dispersion is a key for preparing a high-performance nitrogen-doped graphene photoelectric device by uniform droplet ejection. The strong hydrophobicity of the graphene surface is the root cause of platelet aggregation and sedimentation. Most preparation methods adopt a mode of repeatedly centrifuging to obtain supernatant liquid to obtain graphene ink, so that graphene sheets remained in the ink are too small. The ultrasonic treatment is an effective means for dispersing the graphene, can obtain graphene sheets with 1-10 layers, and can exert excellent electric, optical, force and thermal properties of the graphene, but the commonly obtained single sheet size is too small and is about 200-300 nm, so that the number of overlapping points of the sheets is too large, and the conductive path is not smooth. Therefore, continuous exploration is needed, and an ultrasonic dispersion process is optimized, so that the nitrogen-doped graphene ink special for the uniform droplet ejection technology with larger size and stable dispersion is developed.
Document 1"Wang D W,Gentle I R,Lu G Q M.Enhanced electrochemical sensitivity of PtRh electrodes coated with nitrogen-dopped graphene [ J ]. Electrochemistry communications,2010,1210:1423-1427." discloses a method of dispersing and nitrogen doping graphene using a hydrazine hydrate ultrasound-assisted method. The prepared nitrogen-doped graphene has complete lattice recovery, uniform sheet size, but undersize sheet size of only 200nm, and is unfavorable for improving the sheet lap rate in the uniform droplet jet printing process.
Document 2, the chinese patent application publication No. CN 105860677A, discloses graphene oxide ink, and a preparation method and application thereof, and the obtained ink has good stability, and can be widely used in a household inkjet printer, but the method of centrifugally retaining supernatant and filtering with a microfiltration membrane for multiple times to remove non-exfoliated graphite flakes, so that the size of flakes is too small, which is not beneficial to the improvement of the lap rate of flakes in the uniform droplet jet printing process, and greatly influences the recovery of the conductivity of graphene.
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 by sodium deoxycholate in an auxiliary way, and the defect that the size of the nitrogen-doped graphene ink prepared by the prior method is smaller is overcome.
Technical proposal
The method for preparing the nitrogen-doped graphene ink with the assistance of sodium deoxycholate is characterized by comprising the following steps of:
step 1, preparing graphene oxide powder by using natural crystalline flake graphite powder:
(1) Adding graphite powder into concentrated sulfuric acid, mixing the mixture fully, wherein the concentration of the graphite powder is 0.02-0.06g/mL, mixing the mixture 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: setting 1-5 temperature gradients, wherein the temperature range is 0-70 ℃, and the total reaction time is 4-100h;
(2) Washing the mixture with deionized water to neutrality, pouring out the supernatant, and completing the process with a centrifuge;
(3) Collecting the bottom layer slurry, performing ultrasonic treatment, and performing freeze drying to obtain graphene oxide powder;
step 2, preparing nitrogen-doped graphene powder by oxidizing graphene:
(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) Placing the dispersion liquid added with ammonium carbonate into a hydrothermal reaction kettle, sealing the reaction kettle, placing the reaction kettle into an oven, and performing hydrothermal reaction at 70-250 ℃ to obtain nitrogen-doped graphene;
step 3, preparing 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 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 length of each section is 0.4-2h, the ratio of the ultrasonic time length of high power to the ultrasonic time length of low power is 2:1-5:1, and the total ultrasonic treatment time length is 12h-300h;
(2) And (3) after the ultrasonic treatment is finished, standing for 3 hours, and collecting supernatant fluid, namely the nitrogen-doped graphene ink.
The centrifugal rotating speed of the step 1 is 1000-10 000rpm, and the time is 3-20min.
The ultrasonic duration 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 the deoxycholate sodium in the nitrogen-doped graphene ink is 0.003-0.007g/mL.
Advantageous effects
According to the method for preparing the nitrogen-doped graphene ink with the assistance of the sodium deoxycholate, firstly, concentrated sulfuric acid and potassium permanganate mixed oxidant are adopted to convert natural crystalline flake graphite into graphene oxide, the heat preservation temperature in the oxidation process is not higher than 70 ℃, more carbon six-membered ring structures are reserved, and high-concentration oxygen atom grafting is realized. And secondly, cutting and doping nitrogen into graphene oxide through hydrothermal reaction under the action of a proper temperature and a nitrogen doping agent to prepare the nitrogen doped graphene. Finally, mixing the nitrogen-doped graphene and a proper amount of sodium deoxycholate in water, and performing high-low power alternate ultrasound with a certain time period proportion, wherein the high-power ultrasound aims at breaking up agglomerated and stacked nitrogen-doped graphene blocks, the soft acting force of the low-power ultrasound promotes the spreading of the sheets, and effectively prevents the tearing of the sheets at the synergistic position of epoxy groups, and maintains the sheets with larger size. The ultrasonic process is repeated continuously, and finally the large-sheet thin-layer stable-dispersion nitrogen-doped graphene water-based ink is prepared, wherein the sheet size is 800-2000nm, and the thickness is 1-2nm.
The beneficial effects of the invention are as follows: the technological parameters are strictly controlled in the whole preparation process, so that the stretching form of the micron-sized sheets in the ink is ensured, and the problems of complex components, trivial and serious agglomeration of the nitrogen-doped graphene sheets in the ink prepared by the existing method are solved. The printing experiment proves that the lapping state of the nitrogen-doped graphene sheet is good, and the preparation method has obvious cost benefit and environmental protection 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 ejection printing platform, and particularly can be used for printing a graphene metamaterial wave-absorbing microstructure through uniform droplet ejection. The preparation method of the nitrogen-doped graphene ink has the advantages of stable dispersion, micron-sized sheet spreading and the like.
Drawings
FIG. 1 is a flow chart of a nitrogen-doped graphene ink preparation.
Fig. 2 is an optical photograph of a nitrogen-doped graphene ink.
Fig. 3 is an atomic force microscope photograph of nitrogen-doped graphene.
Fig. 4 is a measurement of the dimensions of the photograph of fig. 3.
Detailed Description
The invention will now be further described with reference to examples, figures:
example 1:
step 1: preparation of graphene oxide
(1) Adding graphite powder into concentrated sulfuric acid, mixing the mixture fully, wherein the concentration of the graphite powder is 0.04g/mL, mixing the mixture 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 is done with a centrifuge.
(3) Collecting the bottom layer slurry, performing ultrasonic treatment, and performing freeze drying to obtain graphene oxide powder.
In the preparation method of graphene oxide, in the step (1), the temperature gradients are set to be 3, the temperature gradients are sequentially 5, 35 and 70 ℃, and the reaction time is sequentially 0.5, 1 and 0.5h.
And/or, in the step (2), the centrifugal speed is 8000rpm, and the time is 20min.
In the step (3), the ultrasonic duration 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) Ammonium carbonate was added to the dispersion obtained in the above (1), and the mixture was sufficiently stirred.
(3) And (3) placing the dispersion liquid obtained in the step (2) into a hydrothermal reaction kettle, sealing the reaction kettle, and placing the reaction kettle into an oven for hydrothermal reaction.
In the above graphene oxide nitrogen doping process, in the step (1), the ultrasonic duration is 0.5h, and the power is 200W.
In the step (2), the mass ratio of graphene oxide to ammonium carbonate is 1:20.
In the above (3), the hydrothermal reaction temperature was set to 80 ℃.
Step 3: preparation of nitrogen-doped graphene ink
(1) 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) During the ultrasonic process, the surfactant sodium deoxycholate is added into the dispersion system obtained in the step (1) in multiple times.
(3) And (3) after the ultrasonic treatment is finished, standing for 3 hours, and collecting supernatant fluid, namely the nitrogen-doped graphene ink.
The final concentration of the sodium deoxycholate in the nitrogen-doped graphene ink in the step (3) is 0.003g/mL.
In the step 3, ultrasonic power is 30W and 800W, ultrasonic time is 1.5h and 4.5h in each section, and total ultrasonic treatment time is 60h.
Example 2:
step 1: preparation of graphene oxide powder by using natural crystalline flake graphite powder
(1) Adding graphite powder into concentrated sulfuric acid, mixing the mixture fully, wherein the concentration of the graphite powder is 0.04g/mL, mixing the mixture 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 is done with a centrifuge.
(3) Collecting the bottom layer slurry, performing ultrasonic treatment, and performing freeze drying to obtain graphene oxide powder.
In the preparation method of 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 1h in sequence.
And/or, in the step (2), the centrifugal speed is 6000rpm, and the time is 15min.
In the step (3), the ultrasonic duration is 2h, and the power is 300W.
Step 2: preparation of nitrogen-doped graphene powder by oxidizing graphene
(1) And (3) dissolving the graphene oxide obtained in the step (1) in water, and carrying out ultrasonic treatment.
(2) Ammonium carbonate was added to the dispersion obtained in the above (1), and the mixture was sufficiently stirred.
(3) And (3) placing the dispersion liquid obtained in the step (2) into a hydrothermal reaction kettle, sealing the reaction kettle, and placing the reaction kettle into an oven for hydrothermal reaction.
In the above graphene oxide nitrogen doping process, in the step (1), the ultrasonic duration is 0.5h, and the power is 300W.
In the step (2), the mass ratio of graphene oxide to ammonium carbonate is 1:100.
In the above (3), the hydrothermal reaction temperature was set to 130 ℃.
Step 3: preparation of nitrogen-doped graphene ink
(1) 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) During the ultrasonic process, the surfactant sodium deoxycholate is added into the dispersion system obtained in the step (1) in multiple times.
(3) And (3) after the ultrasonic treatment is finished, standing for 3 hours, and collecting supernatant fluid, namely the nitrogen-doped graphene ink.
The final concentration of the sodium deoxycholate in the nitrogen-doped graphene ink in the step (3) is 0.006g/mL.
In the step 3, ultrasonic power is 120W and 400W, ultrasonic power is alternately carried out, the ultrasonic duration of each section is 1h and 2h, and the total ultrasonic treatment duration is 12h.
Example 3:
step 1: preparation of graphene oxide powder by using natural crystalline flake graphite powder
(1) Adding graphite powder into concentrated sulfuric acid, mixing the mixture fully, wherein the concentration of the graphite powder is 0.04g/mL, mixing the mixture 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 is done with a centrifuge.
(3) Collecting the bottom layer slurry, performing ultrasonic treatment, and performing freeze drying to obtain graphene oxide powder.
In the preparation method of 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 (2), the centrifugal rotation speed is 10 000rpm for 15min.
In the step (3), the ultrasonic duration is 0.5h, and the power is 200W.
Step 2: preparation of nitrogen-doped graphene powder by oxidizing graphene
(1) And (3) dissolving the graphene oxide obtained in the step (1) in water, and carrying out ultrasonic treatment.
(2) Ammonium carbonate was added to the dispersion obtained in the above (1), and the mixture was sufficiently stirred.
(3) And (3) placing the dispersion liquid obtained in the step (2) into a hydrothermal reaction kettle, sealing the reaction kettle, and placing the reaction kettle into an oven for hydrothermal reaction.
In the above graphene oxide nitrogen doping process, in the step (1), the ultrasonic duration is 4 hours, and the power is 300W.
In the step (2), the mass ratio of graphene oxide to ammonium carbonate is 1:50.
In the above (3), the hydrothermal reaction temperature was set to 240 ℃.
Step 3: preparation of nitrogen-doped graphene ink
(1) 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) During the ultrasonic process, the surfactant sodium deoxycholate is added into the dispersion system obtained in the step (1) in multiple times.
(3) And (3) after the ultrasonic treatment is finished, standing for 3 hours, and collecting supernatant fluid, namely the nitrogen-doped graphene ink.
The final concentration of sodium deoxycholate in the nitrogen-doped graphene ink in the step (3) is 0.007g/mL.
In the step 3, ultrasonic power is 240W and 400W, ultrasonic power is alternately carried out, the ultrasonic duration of each section is 0.5h and 2h, and the total ultrasonic treatment duration is 30h.
Claims (4)
1. The method for preparing the nitrogen-doped graphene ink with the assistance of sodium deoxycholate is characterized by comprising the following steps of:
step 1, preparing graphene oxide powder by using natural crystalline flake graphite powder:
(1) Adding graphite powder into concentrated sulfuric acid, mixing the mixture fully, wherein the concentration of the graphite powder is 0.02-0.06g/mL, mixing the mixture 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: setting 1-5 temperature gradients, wherein the temperature range is 0-70 ℃, and the total reaction time is 4-100h;
(2) Washing the mixture with deionized water to neutrality, pouring out the supernatant, and completing the process with a centrifuge;
(3) Collecting the bottom layer slurry, performing ultrasonic treatment, and performing freeze drying to obtain graphene oxide powder;
step 2, preparing nitrogen-doped graphene powder by oxidizing graphene:
(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) Placing the dispersion liquid added with ammonium carbonate into a hydrothermal reaction kettle, sealing the reaction kettle, placing the reaction kettle into an oven, and performing hydrothermal reaction at 70-250 ℃ to obtain nitrogen-doped graphene;
step 3, preparing 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 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 length of each section is 0.4-2h, the ratio of the ultrasonic time length of high power to the ultrasonic time length of low power is 2:1-5:1, and the total ultrasonic treatment time length is 12h-300h;
(2) After the ultrasonic treatment is finished, standing for 3 hours, and collecting supernatant fluid, namely the nitrogen-doped graphene ink; the size of the lamellar of the nitrogen-doped graphene ink is 800-2000nm, and the thickness of the lamellar is 1-2nm.
2. The method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate according to claim 1, wherein the method comprises the following steps of: the centrifugal rotating speed of the step 1 is 1000-10 000rpm, and the time is 3-20min.
3. The method for preparing nitrogen-doped graphene ink with the assistance of sodium deoxycholate according to claim 1, wherein the method comprises the following steps of: the ultrasonic duration 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, wherein the method comprises the following steps of: the final concentration of the deoxycholate sodium in the nitrogen-doped graphene ink is 0.003-0.007g/mL.
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