CN108046241A - A kind of 3D printing surpasses the method for poroelasticity graphene aerogel - Google Patents
A kind of 3D printing surpasses the method for poroelasticity graphene aerogel Download PDFInfo
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- CN108046241A CN108046241A CN201711368901.6A CN201711368901A CN108046241A CN 108046241 A CN108046241 A CN 108046241A CN 201711368901 A CN201711368901 A CN 201711368901A CN 108046241 A CN108046241 A CN 108046241A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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Abstract
The present invention relates to a kind of methods that 3D printing surpasses poroelasticity graphene aerogel, it comprises the following steps：(a) graphene oxide, ascorbic acid and deionized water are mixed to form graphene hydrogel ink；(b) micropore graphene hydrogel ink is heated to obtain；(c) the micropore graphene hydrogel ink is transferred in 3D printer；(d) the 3D graphene oxides hydrogel is freeze-dried, then heating reacts graphene oxide and ascorbic acid, removes soluble impurity with soaked overnight in deionized water, then is freeze-dried to obtain redox graphene aeroge；(e) the redox graphene aeroge is subjected to high-temperature calcination under inert gas conditions.3D printing graphene aerogel with outstanding elasticity, anti-fatigue performance and crushing resistance while can so obtaining with compared with low-density.
Description
Technical field
The invention belongs to graphene aerogel fields, are related to a kind of preparation method of super poroelasticity graphene aerogel,
Surpass the method for poroelasticity graphene aerogel more particularly to a kind of 3D printing.
Background technology
Graphene is a kind of ultra-thin two-dimension (2D) carbon material, possesses very high specific surface area, excellent elastic, goodization
Learn stability and excellent conduction, heat conductivility.Above-mentioned excellent physical and chemical performance makes graphene in the sub- device of nano photoelectric
There is extremely wide application prospect in the fields such as part, sensor, catalysis, composite material, energy storage and biological medicine stent.Greatly
Scope assembles two-dimensional graphene nanometer sheet, and retaining its original physical and chemical performance while forming it into three-dimensional (3D) structure is
Further expand prerequisite of the grapheme material in the various applications of macro-scale.
Redox graphene (RGO) aeroge based on chemical synthesis is a kind of most common three-dimensional grapheme structure.
3D porous graphenes network structure is prepared mainly by hydrothermal reduction, electronation and directly friendship using graphene oxide presoma
The methods of connection, realizes the self assembly or gelation of graphene film, and the shaping of aeroge is limited to the shape of template, and structure is excessively single
One and simple.Developing the 3D grapheme materials that a kind of controllable, easy-operating method preparation structure accurately controls, there are still great
Challenge.
In recent years, one kind be called ink direct write shaping (direct ink writing) extruded type 3D printing technique by with
In constructing the labyrinths such as porous elastomers structure.At ambient temperature, held using the mechanical arm cooperation micro-nozzle of three-axis moving
It is continuous to squeeze out " ink " silk, and assemble 3D structures by designed shape stacked in multi-layers.Ink direct write forming technique, which needs to have, to be cut
The dilute and quick pseudoplastic viscoplasticity glue ink of shear, is presented mobility, is expanded rapidly after removing pressure deposition under stress
Recover and retain the shape being pre-designed.Research shows graphene oxide water solution at high concentrations, due to graphene oxide two
The tightly packed and good water-retaining property of nanometer sheet is tieed up, extraordinary shear shinning property, quick pseudoplastic behavior can be showed and is glued
Elasticity is highly suitable for ink direct write forming technique.But using the 3D grapheme materials of graphene oxide ink printed micro-
The closelypacked state of graphene two-dimensional nano piece is in sight, it is suppressed that excellent physico in graphene two-dimensional nano piece
Learn performance.In order to solve the problems, such as that this is fatal, a kind of 3D graphite built using ink direct write shaping 3D printing technique of exploitation
The method that alkene material possesses porous structure on microcosmic seems particularly important.
The content of the invention
A kind of 3D printing the invention aims to overcome the deficiencies in the prior art is provided and surpasses poroelasticity graphene gas
The method of gel.
In order to achieve the above objectives, the technical solution adopted by the present invention is：A kind of 3D printing surpasses poroelasticity graphene airsetting
The method of glue, it comprises the following steps：
(a) graphene oxide, ascorbic acid and deionized water are mixed to form graphene hydrogel ink, the oxidation stone
The mass ratio 1 of black alkene and the ascorbic acid：1~10；
(b) by the graphene hydrogel ink as 40~80 DEG C heating 1~3 it is small when obtain micropore graphene hydrogel ink
Water；
(c) the micropore graphene hydrogel ink is transferred in 3D printer, with glass after setting 3D printer parameter
Glass piece carries out 3D printing for substrate and obtains 3D graphene oxide hydrogels；
(d) the 3D graphene oxides hydrogel is freeze-dried, then heating makes graphene oxide and Vitamin C
Acid reaction, in deionized water soaked overnight removal soluble impurity, then be freeze-dried to obtain redox graphene aeroge；
(e) the redox graphene aeroge is subjected to high-temperature calcination under inert gas conditions.
Optimally, in step (c), by the syringe of micropore graphene hydrogel ink transfer 3D printer, it is equipped with
A diameter of 100~500 μm of printing syringe needle drives the printing syringe needle to move by mechanical arm.
Optimally, in step (d), the high-temperature calcination is to be heated up in tube furnace with the heating rate of 5~20 DEG C/min
To 900~1200 DEG C of calcinings.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：3D printing of the present invention surpasses
The method of poroelasticity graphene aerogel, by carrying out graphene oxide and ascorbic acid to mix to obtain graphene hydrogel ink
Water heats to obtain different microscopic apertures, then through 3D printing, reduction and calcining, you can while acquisition with compared with low-density
3D printing graphene aerogel with outstanding elasticity, anti-fatigue performance and crushing resistance.
Description of the drawings
Fig. 1 is during 3D printing of the present invention：(a) 3D printing process photo；(b) 3D printing macroscopic view program porous structure shows
It is intended to；(c) graphene hydrogel ink is extruded into the microcosmic porous schematic diagram of silk；
Fig. 2 is the SEM figures that 3D printing of the present invention surpasses poroelasticity graphene aerogel：(a, b) surface texture, (c, d) are cut
Face structure；
Fig. 3 is that 3D printing in different embodiments of the invention surpasses the SEM figures of poroelasticity graphene aerogel (engineer's scale is
10μm)：(a) embodiment 1, (b) embodiment 2.
Fig. 4 is the performance test that 3D printing surpasses poroelasticity graphene aerogel in embodiment 1：(a) 10 Xun Huan compressions
Stress-strain diagram；(b) 10 Xun Huan maximum pressures and energy dissipation index variation profiles；(c) 10 Xun Huan compressions recover bent
Line；
Fig. 5 is the performance test that 3D printing surpasses poroelasticity graphene aerogel in embodiment 1：(a) 10 Xun Huan compressions
Stress-strain diagram；(b) 10 Xun Huan maximum pressures and energy dissipation index variation profiles；(c) 10 Xun Huan compressions recover bent
Line；And 3D printing surpasses the performance test of poroelasticity graphene aerogel in embodiment 2：(d) 10 cyclic compressive stress should
Varied curve；(e) 10 Xun Huan maximum pressures and energy dissipation index variation profiles；(f) 10 Xun Huan compression recovery curves.
Specific embodiment
The graphene oxide that the present invention uses may be employed commercially available, can also be made using following methods：(1) in ice bath
Under the conditions of, 0.5~2g sodium nitrate is added in the three-neck flask equipped with the 23mL concentrated sulfuric acids, is stirred with the speed of 800~2000rpm
It mixes to sodium nitrate and is completely dissolved；(2) rotating speed is turned down as 300~500rpm, and 1g graphite powders are slowly added into three-neck flask, treat stone
Ink powder adds in the potassium permanganate that total amount is 5~10g, 0~10 DEG C of the temperature of control system after uniformly dispersing；(3) by above-mentioned reaction
Solution is warming up to 40 DEG C, and adjustment rotating speed is 400rpm, 1~4h of reaction is kept after system temperature reaches 40 DEG C, solution is by blackish green
Discoloration is into taupe；(4) 70 DEG C are warming up to, 46mL deionized waters is added in, reacts 10-50min after being warming up to 95 DEG C；(5) stop
Heating adds in 140mL deionized waters, 1~2mL, 30% hydrogen peroxide is added dropwise；(6) filter while hot, with 10% salt acid elution
Twice, then filter cake is dispersed in 400mL deionizations, 300W ultrasounds 3h；(7) by the graphene oxide solution after ultrasound with
Upper solution is taken after the rotating speed centrifugation 10min of 3000-8000rpm, graphene oxide powder is obtained after freeze-drying.
The present invention is further described below in conjunction with embodiment.
Embodiment 1
The present embodiment provides a kind of methods that 3D printing surpasses poroelasticity graphene aerogel, it comprises the following steps：
(a) 180mg graphene oxide powders, 420mg ascorbic acid and 3mL deionized waters is taken uniformly to mix, you can prepare
It obtains with shear shinning property, quick pseudoplastic behavior and viscoelastic graphene hydrogel ink；
(b) micropore graphene hydrogel ink will be heated 20 minutes to obtain at 50 DEG C of graphene hydrogel ink；
(c) micropore graphene hydrogel ink will be obtained to be transferred in the 5mL syringes for 3D printing, selection is fitted with syringe
Match somebody with somebody and a diameter of 100~1000 μm of printing syringe needle, pre-set mechanical arm mobile process, and select 100~400kpa gas
Pressure, the mechanical arm translational speed (printer model F5200N) of 1~20mm/s；Adjustment printing starting point syringe needle and glass chip bottom it
Between spacing be 0.75 millimeter of needle diameter, directly carry out ink writing 3D printing at normal temperatures and obtain 3D graphene oxide water-settings
Glue (shown in such as Fig. 1 (a) to Fig. 1 (c))；I.e. this example provides a kind of graphite for being suitable for ink direct write shaping 3D printing technique
Alkene ink, and based on the ink, it is prepared for that there is the porous and microcosmic super porous graphite of macroscopical sequencing using 3D printing technique
Alkene aeroge sample.Fig. 1 (a) illustrates optical photograph during 3D printing Microscopic order graphene aerogel under normal temperature and pressure, can
Seeing the graphene hydrogel ink of 3D printing has extraordinary self-supporting energy, can be parallel in bottom as " crossbeam " sample rack
In the graphene-structured at interval, by upper and lower two layers vertical orientated stacked in multi-layers, the Microscopic order that can be pre-designed
Porous structure (Fig. 1 (b)).The graphene hydrogel not only has Microscopic order porous structure, and has micro-nano on microcosmic
The porous structure of scale is filled (Fig. 1 (c)) by water among hole.By freeze-drying, moisture removal can be successfully removed, is kept microcosmic
With the porous structure of Microscopic order.
(d) the graphene 3D hydrogels that printing obtains are freeze-dried, then heat 6h in 80 DEG C of baking ovens, make oxygen
Graphite alkene and ascorbic acid react completely, then the soaked overnight in a large amount of deionized waters, removal graphene aerogel surface
Then soluble impurity is freeze-dried, obtain redox graphene aeroge；
(e) in tube furnace under nitrogen atmosphere with the heating rate of 30 DEG C/min, 3h is pyrolyzed with further at 1050 DEG C
Reduced graphene；As shown in Fig. 2 (a)-Fig. 2 (d), there is the graphene aerogel of 3D printing very regular size to exist
500 μm or so of macropore, and with the microcellular structure of abundant micro-meter scale.For surface, internal graphite
Alkene nanometer sheet preferably remains ultra-thin characteristic, is cross-linked with each other and forms very abundant microcellular structure together, with hydro-thermal
Graphene aerogel microstructure prepared by the conventional methods such as method is consistent.This result shows that, using new graphene oxide
Hydrogel ink, 3D printing graphene aerogel can not only obtain the unavailable Microscopic order porous structure of conventional method, moreover it is possible to
Keep microcosmic relatively rich pore property.
Embodiment 2
The present embodiment provides a kind of method that 3D printing surpasses poroelasticity graphene aerogel, it and the base in embodiment 1
This is consistent, unlike：Micropore graphene hydrogel ink is heated 40 minutes to obtain in step (b), at 50 DEG C.
SEM tests are carried out respectively to graphene aerogel made from embodiment 1, embodiment 2, it can be found that by controlling stone
The time of black alkene hydrogel heating ink can regulate and control reducing degree of the ascorbic acid to graphene nanometer sheet, so as to control stone
The crosslinking degree of black alkene hydrogel ink, crosslinking degree is higher, and aperture is smaller.The adjustable characteristic of this microscopic aperture, beats for 3D
Print graphene aerogel provides wider application prospect.Fig. 3 (a) to Fig. 3 (c) illustrates the increase with crosslinking degree,
The size of 3D printing graphene aerogel micropore constantly reduces.
The mechanical measuring and calculation method of 3D printing graphene aerogel：Use following for universal testing machine (Instron 3365)
Ring compact model tests the elasticity of the microcosmic porous graphene aeroge of 3D printing.Quality, ruler are weighed using a ten thousandth balance
It measures size, calculates density.Excellent elasticity assigns 3D printing graphene aerogel and is widely applied occasion.Fig. 4 illustrates reality
Stress-strain diagram of the 3D graphene aerogels by 10 Xun Huan compressions in example 1 is applied, in the case where compression ratio reaches 80%,
The figure of loss cycled for the first time is only 55.1%, and figure of loss is basically unchanged after 5 Xun Huans, less than 50%, exhibition
Reveal extraordinary anti-fatigue performance.Maximum pressure is for the first time 82% after 10 Xun Huans, has fully demonstrated 3D printing graphene
The outstanding crushing resistance of aeroge.Graphene aerogel deformation quantity is less than 5% after 10 Xun Huans, embodies the elasticity of its superelevation.3D
The density of print routine porous graphene aeroge is only 11.7mg/cm3, while density is well below other elastomers,
Elasticity, anti-fatigue performance and many traditional materials of crushing resistance ratio are outstanding, have huge application prospect.Fig. 5 illustrates embodiment 1
50% Xun Huan compression performance figure of (Fig. 5 (a-c)) and embodiment 2 (Fig. 5 (d-f)), with extending heating time, aperture becomes smaller,
It cycles compressive stability and certain decline occurs, the ratio of maximum pressure and initial maximum pressure is declined by 90.7% after cycling 9 times
To 87.9%, graphene aerogel volume deformation amount increases to 6% by 2.9%.And existing 3D printing graphene aerogel is
Product deformation quantity substantially 15-35%.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, it is all according to the present invention
The equivalent change or modification that Spirit Essence is made, should be covered by the protection scope of the present invention.
Claims (3)
1. a kind of 3D printing surpasses the method for poroelasticity graphene aerogel, which is characterized in that it comprises the following steps：
(a) graphene oxide, ascorbic acid and deionized water are mixed to form graphene hydrogel ink, the graphene oxide
With the mass ratio 1 of the ascorbic acid:1~10；
(b) by the graphene hydrogel ink as 40~80 DEG C heating 1~3 it is small when obtain micropore graphene hydrogel ink；
(c) the micropore graphene hydrogel ink is transferred in 3D printer, with sheet glass after setting 3D printer parameter
3D printing, which is carried out, for substrate obtains 3D graphene oxide hydrogels；
(d) the 3D graphene oxides hydrogel is freeze-dried, then heating makes graphene oxide and ascorbic acid anti-
Should, soluble impurity is removed with soaked overnight in deionized water, then is freeze-dried to obtain redox graphene aeroge；
(e) the redox graphene aeroge is subjected to high-temperature calcination under inert gas conditions.
2. 3D printing according to claim 1 surpasses the method for poroelasticity graphene aerogel, it is characterised in that：Step
(c) in, by the syringe of micropore graphene hydrogel ink transfer 3D printer, a diameter of 100~500 μm is equipped with and is beaten
Syringe needle is printed, by mechanical arm the printing syringe needle is driven to move.
3. 3D printing according to claim 1 surpasses the method for poroelasticity graphene aerogel, it is characterised in that：Step
(d) in, the high-temperature calcination is to be warming up to 900~1200 DEG C of calcinings in tube furnace with the heating rate of 5~20 DEG C/min.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108424533A (en) * | 2018-05-30 | 2018-08-21 | 中国科学院兰州化学物理研究所 | A kind of 3D printing bio-medical hydrogel and preparation method thereof |
| CN109534320A (en) * | 2018-10-15 | 2019-03-29 | 上海交通大学 | A kind of preparation method and composite aerogel of 3D printing graphene composite aerogel |
| CN111005034A (en) * | 2019-12-02 | 2020-04-14 | 苏州大学 | Method for 3D printing of high-strength graphene-carbon nanotube electrode, graphene-carbon nanotube electrode and application of graphene-carbon nanotube electrode |
| CN111220314A (en) * | 2020-03-09 | 2020-06-02 | 苏州大学 | Preparation method of zero-power-consumption pressure sensor |
| CN111232959A (en) * | 2020-03-12 | 2020-06-05 | 浙江大学 | Preparation method of miniature graphene aerogel device |
| CN111682801A (en) * | 2020-06-22 | 2020-09-18 | 苏州大学 | 3D printing graphene-based water evaporation power generation device and preparation method and application thereof |
| CN111973568A (en) * | 2020-08-28 | 2020-11-24 | 广东药科大学 | 3D printing-based preparation floatable drug sustained-release carrier with micro air bags and preparation method and application thereof |
| CN112151255A (en) * | 2019-12-17 | 2020-12-29 | 中山大学·深圳 | Magnetic control deformation memory material and manufacturing method thereof |
| CN112337434A (en) * | 2020-11-25 | 2021-02-09 | 兰州理工大学 | 3D printing-based graphene composite material preparation method and sewage purification device |
| CN112408366A (en) * | 2020-12-07 | 2021-02-26 | 南通第六元素材料科技有限公司 | Method for printing and in-situ reduction of graphene |
| CN112430094A (en) * | 2020-11-25 | 2021-03-02 | 中国科学院上海硅酸盐研究所 | Macrostructure ordered graphene aerogel and preparation method thereof |
| CN113120884A (en) * | 2021-04-16 | 2021-07-16 | 北京理工大学 | Graphene aerogel with sound absorption and audio recognition functions and application thereof |
| CN114103125A (en) * | 2021-09-30 | 2022-03-01 | 哈尔滨工业大学（威海） | Preparation method of high-thermal-conductivity micro device |
| CN114195136A (en) * | 2022-01-05 | 2022-03-18 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108424533A (en) * | 2018-05-30 | 2018-08-21 | 中国科学院兰州化学物理研究所 | A kind of 3D printing bio-medical hydrogel and preparation method thereof |
| CN109534320A (en) * | 2018-10-15 | 2019-03-29 | 上海交通大学 | A kind of preparation method and composite aerogel of 3D printing graphene composite aerogel |
| CN109534320B (en) * | 2018-10-15 | 2022-07-01 | 上海交通大学 | Preparation method of 3D printing graphene composite aerogel and composite aerogel |
| CN111005034A (en) * | 2019-12-02 | 2020-04-14 | 苏州大学 | Method for 3D printing of high-strength graphene-carbon nanotube electrode, graphene-carbon nanotube electrode and application of graphene-carbon nanotube electrode |
| CN112151255A (en) * | 2019-12-17 | 2020-12-29 | 中山大学·深圳 | Magnetic control deformation memory material and manufacturing method thereof |
| CN111220314A (en) * | 2020-03-09 | 2020-06-02 | 苏州大学 | Preparation method of zero-power-consumption pressure sensor |
| CN111220314B (en) * | 2020-03-09 | 2021-10-22 | 苏州大学 | Preparation method of zero-power-consumption pressure sensor |
| CN111232959A (en) * | 2020-03-12 | 2020-06-05 | 浙江大学 | Preparation method of miniature graphene aerogel device |
| CN111232959B (en) * | 2020-03-12 | 2021-04-13 | 浙江大学 | Preparation method of miniature graphene aerogel device |
| CN111682801A (en) * | 2020-06-22 | 2020-09-18 | 苏州大学 | 3D printing graphene-based water evaporation power generation device and preparation method and application thereof |
| CN111682801B (en) * | 2020-06-22 | 2021-11-26 | 苏州大学 | 3D printing graphene-based water evaporation power generation device and preparation method and application thereof |
| CN111973568A (en) * | 2020-08-28 | 2020-11-24 | 广东药科大学 | 3D printing-based preparation floatable drug sustained-release carrier with micro air bags and preparation method and application thereof |
| CN111973568B (en) * | 2020-08-28 | 2022-12-02 | 广东药科大学 | 3D printing-based preparation-based floatable drug sustained-release carrier with micro air bags and preparation method and application thereof |
| CN112430094A (en) * | 2020-11-25 | 2021-03-02 | 中国科学院上海硅酸盐研究所 | Macrostructure ordered graphene aerogel and preparation method thereof |
| CN112337434A (en) * | 2020-11-25 | 2021-02-09 | 兰州理工大学 | 3D printing-based graphene composite material preparation method and sewage purification device |
| CN112408366A (en) * | 2020-12-07 | 2021-02-26 | 南通第六元素材料科技有限公司 | Method for printing and in-situ reduction of graphene |
| CN113120884A (en) * | 2021-04-16 | 2021-07-16 | 北京理工大学 | Graphene aerogel with sound absorption and audio recognition functions and application thereof |
| CN114103125A (en) * | 2021-09-30 | 2022-03-01 | 哈尔滨工业大学（威海） | Preparation method of high-thermal-conductivity micro device |
| CN114103125B (en) * | 2021-09-30 | 2022-06-28 | 哈尔滨工业大学（威海） | Preparation method of high-thermal-conductivity micro device |
| CN114195136A (en) * | 2022-01-05 | 2022-03-18 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
| CN114195136B (en) * | 2022-01-05 | 2023-07-07 | 郑州大学 | Preparation method and application of 3D printing nitrogen-doped high-pyrrole graphene aerogel |
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