CN116924408A - Preparation of ultrathin Ti by rotation/revolution induced convection shearing 3 C 2 Method of making a microchip - Google Patents
Preparation of ultrathin Ti by rotation/revolution induced convection shearing 3 C 2 Method of making a microchip Download PDFInfo
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Abstract
Description
技术领域Technical field
本发明属于纳米材料制备技术领域，具体涉及一种自转/公转诱导对流剪切制备超薄Ti3C2微米片的方法。The invention belongs to the technical field of nanomaterial preparation, and specifically relates to a method for preparing ultra-thin Ti 3 C 2 micron sheets through rotation/revolution-induced convection shearing.
背景技术Background technique
Ti3C2导电材料作为MXene材料家族中最重要的一个分支，由于其优异的光电性能、电化学性能、高导电性和良好的机械柔性，在柔性电子领域中的智能传感、无线通信、便携电源和电磁屏蔽等应用中，展现了令人兴奋的应用前景。Ti3C2的电荷传输由片内传输主导(Nature Electronics,2021,4,893)，简而言之，单层或少层Ti3C2的尺寸是影响Ti3C2薄膜导电性的主要因素。现有的大尺寸超薄Ti3C2微米片的研究展示了Ti3C2薄膜优异的导电性，而在柔性透明电子领域展现了巨大的应用前景。As the most important branch of the MXene material family, Ti 3 C 2 conductive materials are widely used in smart sensing, wireless communications, and flexible electronics due to their excellent photoelectric properties, electrochemical properties, high conductivity, and good mechanical flexibility. It shows exciting application prospects in applications such as portable power supply and electromagnetic shielding. The charge transport of Ti 3 C 2 is dominated by intra-chip transport (Nature Electronics, 2021, 4, 893). In short, the size of a single or few layers of Ti 3 C 2 is the main factor affecting the conductivity of the Ti 3 C 2 film. Existing research on large-size ultra-thin Ti 3 C 2 micron sheets has demonstrated the excellent conductivity of Ti 3 C 2 films, and has shown great application prospects in the field of flexible and transparent electronics.
随着研究的不断深入，已经发展了数十种制备手风琴Ti3C2的方法和二维超薄Ti3C2的制备技术。二维超薄Ti3C2的制备技术是限制Ti3C2薄膜展示其优异导电性的主要因素。常见超声辅助的分层制备技术，所制备单层Ti3C2的横向尺寸大多在1μm以下，这将制约Ti3C2导电性能的进一步提升。而手摇法制备的单层Ti3C2能够得到较大尺寸的单层Ti3C2，但其可重复性较差，这些因素都极大了限制了二维超薄Ti3C2应用前景。采用更温和的和可重复的分层方式是制备高导电性大尺寸二维超薄Ti3C2的具有前景的研究方向。With the continuous deepening of research, dozens of methods for preparing accordion Ti3C2 and two-dimensional ultrathin Ti3C2 preparation technology have been developed. The preparation technology of two-dimensional ultra-thin Ti 3 C 2 is the main factor that limits the Ti 3 C 2 film to exhibit its excellent conductivity. With the common ultrasonic-assisted layered preparation technology, the lateral dimensions of the single-layer Ti 3 C 2 prepared are mostly below 1 μm, which will restrict the further improvement of the conductive properties of Ti 3 C 2 . The single-layer Ti 3 C 2 prepared by the hand-cranking method can produce larger-sized single-layer Ti 3 C 2 , but its repeatability is poor. These factors have greatly limited the application of two-dimensional ultra-thin Ti 3 C 2 prospect. Adopting a gentler and reproducible layering approach is a promising research direction for the preparation of highly conductive large-scale two-dimensional ultrathin Ti3C2 .
发明内容Contents of the invention
本发明的目的在于解决现有技术中的不足，提供一种自转/公转诱导对流剪切制备超薄Ti3C2微米片的方法，解决现有手风琴Ti3C2通过超声辅助分层技术或手摇法制备的二维超薄Ti3C2尺寸较小，或可复性较差的问题。The purpose of the present invention is to solve the deficiencies in the existing technology, provide a method for preparing ultra-thin Ti 3 C 2 micron sheets through rotation/revolution-induced convection shearing, and solve the problem of existing accordion Ti 3 C 2 through ultrasonic-assisted layering technology or The two-dimensional ultra-thin Ti 3 C 2 prepared by the hand-cranking method has the problem of small size or poor reproducibility.
为了达到上述目的，本发明是通过以下技术方案实现的：一种自转/公转诱导对流剪切制备超薄Ti3C2微米片的方法，其特征在于，所述方法包括以下步骤：In order to achieve the above objects, the present invention is achieved through the following technical solutions: a method for preparing ultra-thin Ti 3 C 2 micron sheets through rotation/revolution-induced convection shearing, which is characterized in that the method includes the following steps:
步骤S1：通过LiF/HCl刻蚀液去除Ti3AlC2中Al层，制备手风琴状多层Ti3C2；Step S1: Remove the Al layer in Ti 3 AlC 2 using LiF/HCl etching solution to prepare accordion-shaped multi-layer Ti 3 C 2 ;
步骤S2：用去离子水分散步骤S1制备得到的多层Ti3C2，得到多层Ti3C2溶液；Step S2: Disperse the multilayer Ti 3 C 2 prepared in step S1 with deionized water to obtain a multilayer Ti 3 C 2 solution;
步骤S3：将多层Ti3C2溶液置于同时自转和公转的容器中，利用自转和公转诱导产生对流剪切和驱动多层Ti3C2相互对撞，然后公转离心将水和Ti3C2微米片分离，得到大尺寸二维超薄Ti3C2微米片。Step S3: Place the multi-layer Ti 3 C 2 solution in a container that rotates and revolves at the same time. Use the rotation and revolution to induce convective shear and drive the multi-layer Ti 3 C 2 solution to collide with each other. Then, the revolution and centrifugation will separate the water and Ti 3 C 2 micron sheets are separated to obtain large-size two-dimensional ultra-thin Ti 3 C 2 micron sheets.
优选的，步骤S1所述的通过LiF/HCl刻蚀液去除Ti3AlC2中Al层，制备手风琴状多层Ti3C2，具体步骤如下：Preferably, the Al layer in Ti 3 AlC 2 is removed through LiF/HCl etching solution in step S1 to prepare accordion-shaped multi-layer Ti 3 C 2 . The specific steps are as follows:
按每克LiF溶于20～50mL HCl，称取LiF于HCl溶液中，搅拌至LiF完全溶解，然后缓慢加入Ti3AlC2，LiF与Ti3AlC2的质量比为1:3～3:1；将混合物在反应釜中进行加热反应，加热温度为45～70℃，加热时间为72～96h；将产物于转速为3000～8000rpm的条件下离心10min，并用去离子水洗涤，直到pH为5～7，用乙醇洗涤，之后在50～80℃的温度下真空干燥16～36h得到多层Ti3C2。Dissolve each gram of LiF in 20~50mL HCl, weigh LiF into the HCl solution, stir until LiF is completely dissolved, then slowly add Ti 3 AlC 2 , the mass ratio of LiF to Ti 3 AlC 2 is 1:3~3:1 ; The mixture is heated in a reaction kettle at a heating temperature of 45 to 70°C and a heating time of 72 to 96 hours; the product is centrifuged at a speed of 3000 to 8000 rpm for 10 minutes and washed with deionized water until the pH is 5 ~7, wash with ethanol, and then vacuum dry at a temperature of 50~80°C for 16~36h to obtain multi-layer Ti 3 C 2 .
优选的，所述Ti3AlC2选用200目，并将其经过尺寸分离后横向尺寸为10～75μm作为制备多层Ti3C2的原料。Preferably, the Ti 3 AlC 2 is selected as 200 mesh, and its lateral size after size separation is 10-75 μm as the raw material for preparing multi-layer Ti 3 C 2 .
优选的，分离得到10～75μm的Ti3AlC2方法如下：将5～20g 200目Ti3AlC2分散于30～60mL去离子水中进行混合均匀，将混合溶液静置5～15min，取下层10～75μm的Ti3AlC2为制备多层Ti3C2的原料。Preferably, the method for isolating Ti 3 AlC 2 of 10 to 75 μm is as follows: Disperse 5 to 20 g of 200 mesh Ti 3 AlC 2 in 30 to 60 mL of deionized water and mix evenly, let the mixed solution stand for 5 to 15 minutes, and remove the layer 10 ~75μm Ti 3 AlC 2 is the raw material for preparing multi-layer Ti 3 C 2 .
优选的，所述HCl溶液的浓度为9M。Preferably, the concentration of the HCl solution is 9M.
优选的，步骤S2中所述多层Ti3C2溶液的浓度为1～25mg/mL。Preferably, the concentration of the multilayer Ti 3 C 2 solution in step S2 is 1 to 25 mg/mL.
优选的，步骤S3中所述自转转速为公转转速的40％，公转转速为400～2000rpm，搅拌时间为0.1～3h；公转离心转速为500～2200rpm，时间为0.01～1h。Preferably, the rotation speed in step S3 is 40% of the revolution speed, the revolution speed is 400-2000 rpm, and the stirring time is 0.1-3h; the revolution centrifugal speed is 500-2200 rpm, and the time is 0.01-1 h.
优选的，步骤S3所述容器采用行星式离心搅拌机，其型号为THINKY AR-100。Preferably, the container in step S3 uses a planetary centrifugal mixer, whose model is THINKY AR-100.
本发明具有以下有益效果：(1)本发明提供一种自转/公转诱导对流剪切制备超薄Ti3C2微米片的方法，首先通过LiF/HCl刻蚀液去除大尺寸Ti3AlC2中的Al层制备大尺寸手风琴状多层Ti3C2，然后将多层Ti3C2溶于去离子水中配制成Ti3C2溶液，通过高速自转和公转产生最大400g的离心力形成压紧力作用于容器中的多层Ti3C2溶液，使溶液产生旋涡状的上下对流。这种连续不断地对流诱导产生剪切作用于多层Ti3C2，并且对流能够驱动多层Ti3C2相互运动发生对撞，最终对流剪切作用和对撞运动协同作用于多层Ti3C2，将其分散为大尺寸超薄二维Ti3C2微米片溶液。同时，多层Ti3C2的质量是超薄Ti3C2的数十倍，制备的大尺寸超薄二维Ti3C2微米片由于其产生更小的重力，在公转作用下能够分散于溶液的上层，而下层较大质量的多层Ti3C2会持续发生对流剪切作用直到多层Ti3C2完全分层为超薄Ti3C2微米片。由于大尺寸的手风琴状多层Ti3C2往往存在较少的缺陷点位，同时自转/公转诱导的相对更弱的对流剪切作用，最后公转产生的离心力使多层Ti3C2沉降于溶液下层，产生的大尺寸二维超薄Ti3C2分散于溶液上层。多种因素协同作用减弱了对超薄Ti3C2的尺寸破坏，最终得到大尺寸二维超薄Ti3C2。The present invention has the following beneficial effects: (1) The present invention provides a method for preparing ultra-thin Ti 3 C 2 micron sheets through rotation/revolution-induced convection shearing. First, the large-sized Ti 3 AlC 2 is removed through LiF/HCl etching solution. A large-sized accordion-shaped multi-layer Ti 3 C 2 is prepared from the Al layer, and then the multi-layer Ti 3 C 2 is dissolved in deionized water to prepare a Ti 3 C 2 solution. Through high-speed rotation and revolution, a maximum centrifugal force of 400g is generated to form a compacting force. It acts on the multi-layer Ti 3 C 2 solution in the container to cause the solution to produce vortex-like up-and-down convection. This continuous convection induces shearing on the multi-layer Ti 3 C 2 , and the convection can drive the multi-layer Ti 3 C 2 to move and collide with each other. Finally, the convection shearing and collision motion act synergistically on the multi-layer Ti 3 C 2 and disperse it into a solution of large-sized ultra-thin two-dimensional Ti 3 C 2 micron sheets. At the same time, the mass of multi-layer Ti 3 C 2 is dozens of times that of ultra-thin Ti 3 C 2. The prepared large-size ultra-thin two-dimensional Ti 3 C 2 micron sheets can be dispersed under the action of revolution due to the smaller gravity they generate. in the upper layer of the solution, while the larger-mass multi-layer Ti 3 C 2 in the lower layer will continue to undergo convective shearing until the multi-layer Ti 3 C 2 is completely stratified into ultra-thin Ti 3 C 2 micron sheets. Since large-sized accordion-shaped multi-layer Ti 3 C 2 tends to have fewer defect points, and at the same time the relatively weaker convective shear effect induced by rotation/revolution, the centrifugal force generated by the final revolution causes the multi-layer Ti 3 C 2 to settle in In the lower layer of the solution, the large-sized two-dimensional ultra-thin Ti 3 C 2 produced is dispersed in the upper layer of the solution. The synergistic effect of multiple factors weakens the size damage to ultra-thin Ti 3 C 2 , and finally obtains large-size two-dimensional ultra-thin Ti 3 C 2 .
(2)本发明使用高速自转/公转诱导溶液形成对流剪切，辅助多层Ti3C2制备大尺寸超薄二维Ti3C2微米片，使用该方法可实现超薄二维Ti3C2微米片的大规模加工。同时，采用相比与超声、震荡更加温和的分层技术，利用强力的离心加速度诱导溶液产生对流剪切作用，制备的大尺寸二维Ti3C2微米片将具有高导电性、优异的机械柔性和更少的缺陷位点，在柔性透明电子产品和智能可穿戴等领域有很大的应用前景。(2) The present invention uses high-speed rotation/revolution to induce the solution to form convective shear, and assists multi-layer Ti 3 C 2 to prepare large-sized ultra-thin two-dimensional Ti 3 C 2 micron sheets. This method can be used to achieve ultra-thin two-dimensional Ti 3 C Large-scale processing of 2- micron flakes. At the same time, using a layering technology that is gentler than ultrasound and vibration, and using strong centrifugal acceleration to induce convective shearing in the solution, the large-size two-dimensional Ti 3 C 2 micron sheets prepared will have high conductivity and excellent mechanical properties. Flexibility and fewer defect sites have great application prospects in fields such as flexible transparent electronics and smart wearables.
附图说明Description of the drawings
图1为本发明所采用的流体剪切辅助制备大尺寸二维超薄Ti3C2的流程图。Figure 1 is a flow chart for the fluid shear-assisted preparation of large-size two-dimensional ultra-thin Ti 3 C 2 used in the present invention.
图2为本发明制备得到的大尺寸手风琴状多层Ti3C2的SEM照片。Figure 2 is an SEM photo of the large-size accordion-shaped multilayer Ti 3 C 2 prepared by the present invention.
图3为本发明制备得到的大尺寸二维超薄Ti3C2的TEM照片。Figure 3 is a TEM photo of large-size two-dimensional ultra-thin Ti 3 C 2 prepared by the present invention.
图4为本发明制备得到的大尺寸二维超薄Ti3C2溶液的丁达尔效应。Figure 4 shows the Tyndall effect of the large-size two-dimensional ultra-thin Ti 3 C 2 solution prepared by the present invention.
图5为本发明制备得到的大尺寸手风琴状多层Ti3C2(M-Ti3C2)、大尺寸二维超薄Ti3C2(L-Ti3C2)和大尺寸Ti3AlC2的XRD图。Figure 5 shows the large-size accordion-shaped multilayer Ti 3 C 2 (M-Ti 3 C 2 ), large-size two-dimensional ultra-thin Ti 3 C 2 (L-Ti 3 C 2 ) and large-size Ti 3 prepared by the present invention. XRD pattern of AlC 2 .
图6为本发明对比例采用超声辅助制备得到的Ti3C2的TEM照片。Figure 6 is a TEM photo of Ti 3 C 2 prepared using ultrasound assistance in the comparative example of the present invention.
具体实施方式Detailed ways
下面结合实施例对本发明作进一步的说明，但并不作为对本发明限制的依据。The present invention will be further described below with reference to the examples, but they are not used as a basis for limiting the present invention.
大尺寸手风琴状多层Ti3C2 Large accordion-shaped multi-layer Ti 3 C 2
为了阐述本发明的大尺寸二维超薄Ti3C2的制备原理，制作了如图1所示的制备流程图。将多层Ti3C2分散于去离子水中，通过行星式离心搅拌机的搅拌模式160～800rpm自转和400～2000rpm公转产生最大400g的离心力形成压紧力作用于容器中的多层Ti3C2，从而溶液产生旋涡状的上下对流并且伴随溶液的自流。连续不断地对流和自流能够诱导Ti3C2混合溶液流体产生剪切作用并作用于多层Ti3C2上，同时对流还能驱动多层Ti3C2相互运动发生多层Ti3C2之间的对撞，最终对流剪切作用和对撞运动协同作用于多层Ti3C2将其分散为大尺寸超薄二维Ti3C2微米片溶液。同时，更大质量的多层Ti3C2在高速公转离心作用下沉积在溶液体系的下层继续发生分层作用，而大尺寸超薄二维Ti3C2微米片由于更小的重力，在公转作用下能够分散于溶液的上层起到了保护大尺寸二维超薄Ti3C2微米片尺寸不被破坏。由于大尺寸的手风琴状多层Ti3C2存在更少的缺陷点位和诱导的相对更弱的对流剪切作用以及公转离心保护超薄Ti3C2微米片，从而减弱了对超薄Ti3C2的尺寸破坏，最终得到大尺寸二维超薄Ti3C2。In order to illustrate the preparation principle of large-size two-dimensional ultra-thin Ti 3 C 2 of the present invention, a preparation flow chart as shown in Figure 1 was produced. Disperse the multi-layer Ti 3 C 2 in deionized water, and use the planetary centrifugal mixer's stirring mode of 160 to 800 rpm rotation and 400 to 2000 rpm rotation to generate a maximum centrifugal force of 400 g to form a compressive force that acts on the multi-layer Ti 3 C 2 in the container. , so that the solution generates vortex-like up-and-down convection and is accompanied by the self-flow of the solution. Continuous convection and self-flow can induce Ti 3 C 2 mixed solution fluid to produce shear and act on multi-layer Ti 3 C 2. At the same time, convection can also drive multi-layer Ti 3 C 2 to move with each other to produce multi-layer Ti 3 C 2. The collision, final convective shear action and collision motion synergistically act on the multi-layer Ti 3 C 2 to disperse it into a large-sized ultra-thin two-dimensional Ti 3 C 2 micron sheet solution. At the same time, the larger-mass multi-layer Ti 3 C 2 is deposited in the lower layer of the solution system under the action of high-speed revolution centrifugal force and continues to stratify, while the large-sized ultra-thin two-dimensional Ti 3 C 2 micron sheets are deposited in the lower layer of the solution system due to the smaller gravity. The upper layer that can be dispersed in the solution under the action of revolution protects the large-size two-dimensional ultra-thin Ti 3 C 2 micron sheets from being destroyed. Since the large-sized accordion-shaped multi-layer Ti 3 C 2 has fewer defect sites and induces relatively weaker convective shear effects, as well as the revolution and centrifugal protection of ultra-thin Ti 3 C 2 micron sheets, the impact on ultra-thin Ti 3 C 2 is weakened. The size of 3 C 2 is destroyed, and finally large-size two-dimensional ultra-thin Ti 3 C 2 is obtained.
一种自转/公转诱导对流剪切制备超薄Ti3C2微米片的方法，所述步骤如下：A method for preparing ultra-thin Ti 3 C 2 micron sheets by rotation/revolution-induced convection shearing. The steps are as follows:
步骤S1：按每克LiF溶于20～50mL 9M HCl，称取LiF于HCl溶液中，搅拌至LiF完全溶解，然后缓慢加入横向尺寸为10～75μm的Ti3AlC2，LiF与Ti3AlC2的质量比为1:3～3:1；将混合物在反应釜中进行加热反应，加热温度为45～70℃，加热时间为72～96h；将产物于转速为3000～8000rpm的条件下离心10min，并用去离子水洗涤，直到pH在5～7，用乙醇洗涤，之后在50～80℃的温度下真空干燥16～36h得到手风琴状多层Ti3C2。Step S1: Dissolve each gram of LiF in 20 to 50 mL of 9M HCl, weigh the LiF in the HCl solution, stir until the LiF is completely dissolved, and then slowly add Ti 3 AlC 2 with a lateral size of 10 to 75 μm, LiF and Ti 3 AlC 2 The mass ratio is 1:3~3:1; the mixture is heated in the reaction kettle, the heating temperature is 45~70°C, and the heating time is 72~96h; the product is centrifuged at 3000~8000 rpm for 10 minutes , and washed with deionized water until the pH is between 5 and 7, washed with ethanol, and then vacuum dried at a temperature of 50 to 80°C for 16 to 36 hours to obtain an accordion-shaped multilayer Ti 3 C 2 .
步骤S2：取50～500mg多层Ti3C2溶于20～50mL去离子水中，得到浓度为1～25mg/mL多层Ti3C2溶液；Step S2: Dissolve 50 to 500 mg of multilayer Ti 3 C 2 in 20 to 50 mL of deionized water to obtain a multilayer Ti 3 C 2 solution with a concentration of 1 to 25 mg/mL;
步骤S3：将多层Ti3C2溶液放置于行星式离心搅拌机中，其型号为THINKY AR-100，采用400～2000rpm的公转转速下，160～800rpm自转转速下搅拌0.1～3h；然后用500～2200rpm的转速离心0.01～1h；得到大尺寸二维超薄Ti3C2微米片。Step S3: Place the multi-layer Ti 3 C 2 solution in a planetary centrifugal mixer, the model is THINKY AR-100, stir for 0.1 to 3 hours at a revolution speed of 400 to 2000 rpm and a rotation speed of 160 to 800 rpm; then stir with 500 Centrifuge at ~2200rpm for 0.01~1h; obtain large-size two-dimensional ultra-thin Ti 3 C 2 micron sheets.
进一步，分离得到10～75μm的Ti3AlC2方法如下：将5～20g 200目Ti3AlC2分散于30～60mL去离子水中进行混合均匀，将混合溶液静置5～15min，取下层10～75μm的Ti3AlC2为制备多层Ti3C2的原料Further, the method of separating Ti 3 AlC 2 with a thickness of 10 to 75 μm is as follows: disperse 5 to 20 g of 200 mesh Ti 3 AlC 2 in 30 to 60 mL of deionized water and mix evenly, let the mixed solution stand for 5 to 15 minutes, and remove the layer 10 to 75μm Ti 3 AlC 2 is the raw material for preparing multi-layer Ti 3 C 2
实施例1Example 1
大尺寸手风琴状多层Ti3C2的制备，具体步骤如下：Preparation of large-size accordion-shaped multi-layer Ti 3 C 2 , the specific steps are as follows:
将1g LiF分散于20mL 9M HCl，搅拌至LiF完全溶解，缓慢加入0.5g尺寸为10～75μm的Ti3AlC2；将混合物在反应釜45℃条件下反应96h；将产物于3000rpm，10min条件下进行离心，取粘土状沉淀并用去离子水洗涤9次，直到pH为6，再乙醇洗涤2次。在80℃下真空干燥24h，得到大尺寸手风琴状多层Ti3C2粉末。所得的手风琴状多层Ti3C2如图2所示，横向尺寸为5～15μm。图5中M-Ti3C2为所得手风琴状多层Ti3C2的XRD曲线，证明Ti3AlC2被完全去除和LiF被清洗干净。Disperse 1g LiF in 20mL 9M HCl, stir until LiF is completely dissolved, slowly add 0.5g Ti 3 AlC 2 with a size of 10 to 75 μm; react the mixture in the reactor at 45°C for 96 hours; incubate the product at 3000 rpm for 10 min. Centrifuge, take out the clay-like precipitate and wash it 9 times with deionized water until the pH is 6, and then wash it 2 times with ethanol. After vacuum drying at 80°C for 24 hours, large-sized accordion-shaped multi-layer Ti 3 C 2 powder was obtained. The obtained accordion-shaped multilayer Ti 3 C 2 is shown in Figure 2, with a lateral size of 5 to 15 μm. In Figure 5, M-Ti 3 C 2 is the XRD curve of the obtained accordion-shaped multilayer Ti 3 C 2 , which proves that Ti 3 AlC 2 is completely removed and LiF is cleaned.
高速自转/公转诱导对流剪切制备大尺寸二维超薄Ti3C2微米片的制备，具体步骤如下：Preparation of large-size two-dimensional ultra-thin Ti 3 C 2 micron sheets by high-speed rotation/revolution-induced convective shear. The specific steps are as follows:
将400mg大尺寸手风琴状多层Ti3C2分散于20mL去离子水中，制得20mg/mL的多层Ti3C2溶液置于行星式离心搅拌机中，采用1000rpm的公转转速和400rpm的自转速度下搅拌2h，然后用1500rpm的转速离心0.5h，通过对流剪切和对撞运动辅助制备得到大尺寸二维超薄Ti3C2微米片。所得的大尺寸的二维超薄Ti3C2纳米片如图3所示，横向尺寸为2～15μm。从图4中大尺寸二维超薄Ti3C2溶液的丁达尔效应可以证明多层Ti3C2被成功分层并且形成了均一的胶体溶液。图5中S-Ti3C2为所得大尺寸二维超薄Ti3C2的XRD曲线，证明通过高速自转/公转诱导对流剪切作用辅助制备方法成功制备了大尺寸二维超薄Ti3C2。Disperse 400 mg of large-size accordion-shaped multi-layer Ti 3 C 2 in 20 mL of deionized water to prepare a 20 mg/mL multi-layer Ti 3 C 2 solution. Place it in a planetary centrifugal mixer, using a revolution speed of 1000 rpm and a rotation speed of 400 rpm. Stir for 2 hours at high temperature, and then centrifuge at 1500 rpm for 0.5 hours. Large-size two-dimensional ultra-thin Ti 3 C 2 micron sheets are prepared through convective shearing and collision motion. The obtained large-sized two-dimensional ultra-thin Ti 3 C 2 nanosheets are shown in Figure 3, with a lateral size of 2 to 15 μm. From the Tyndall effect of the large-scale two-dimensional ultrathin Ti 3 C 2 solution in Figure 4, it can be proven that the multilayer Ti 3 C 2 is successfully layered and a uniform colloidal solution is formed. In Figure 5, S-Ti 3 C 2 is the XRD curve of the obtained large-size two-dimensional ultra-thin Ti 3 C 2 , which proves that large-size two-dimensional ultra-thin Ti 3 has been successfully prepared through the high-speed rotation/revolution-induced convection shear assisted preparation method. C2 .
对比例1Comparative example 1
采用实施例1中的大尺寸手风琴状多层Ti3C2的制备方法和超声辅助二维超薄Ti3C2纳米片的制备。The preparation method of large-size accordion-shaped multilayer Ti 3 C 2 and the ultrasound-assisted preparation of two-dimensional ultra-thin Ti 3 C 2 nanosheets in Example 1 were used.
离心辅助二维超薄Ti3C2纳米片的制备，具体步骤如下：Centrifugation-assisted preparation of two-dimensional ultrathin Ti 3 C 2 nanosheets, the specific steps are as follows:
将400mg大尺寸手风琴状多层Ti3C2分散于20mL去离子水中，制得20mg/mL的多层Ti3C2溶液置于400W功率的超声机中，超声90min，制备得到二维超薄Ti3C2纳米片。所得的二维超薄Ti3C2纳米片如图6所示，横向尺寸小于1μm。Disperse 400 mg of large-size accordion-shaped multi-layer Ti 3 C 2 in 20 mL of deionized water to prepare a 20 mg/mL multi-layer Ti 3 C 2 solution. Place it in a 400 W power ultrasonic machine and ultrasonic for 90 minutes to prepare a two-dimensional ultra-thin Ti 3 C 2 nanosheets. The resulting two-dimensional ultrathin Ti 3 C 2 nanosheets are shown in Figure 6, with a lateral size of less than 1 μm.
以上显示和描述了本发明的基本原理、主要特征及优点。但是以上所述仅为本发明的具体实施例，本发明的技术特征并不局限于此，任何本领域的技术人员在不脱离本发明的技术方案下得出的其他实施方式均应涵盖在本发明的专利范围之中。The basic principles, main features and advantages of the present invention have been shown and described above. However, the above are only specific embodiments of the present invention, and the technical features of the present invention are not limited thereto. Any other implementations derived by those skilled in the art without departing from the technical solutions of the present invention shall be covered by this invention. within the patent scope of the invention.
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