阅读说明：本技术 一种提纯多维纳米材料的方法及其装置 (Method and device for purifying multidimensional nano material ) 是由 唐宏浩 叶怀宇 张国旗 于 2020-03-06 设计创作，主要内容包括：本发明提供了一种提纯多维纳米材料的方法及其装置,装置包括过滤缸、搅拌装置、溶液注入系统、滤液流出收集系统,所述过滤缸由过滤底座、过滤骨架以及附着在过滤骨架上的滤膜组成,所述滤膜通过过滤缸上的骨架固定在过滤缸上,与过滤底座垂直；该提纯方法,步骤简单、条件温和、高效快速,可应用于对纳米线、纳米片的提纯。(The invention provides a method and a device for purifying multidimensional nano materials, wherein the device comprises a filter cylinder, a stirring device, a solution injection system and a filtrate outflow and collection system, the filter cylinder consists of a filter base, a filter framework and a filter membrane attached to the filter framework, and the filter membrane is fixed on the filter cylinder through the framework on the filter cylinder and is vertical to the filter base; the purification method has the advantages of simple steps, mild conditions, high efficiency and high speed, and can be applied to the purification of the nano wires and the nano sheets.)

1. The utility model provides a device of purification multidimension nano-material, its characterized in that includes filter tank, agitating unit, solution injection system, filtrating outflow collecting system, filter tank comprises filtration base, filtration skeleton and the filter membrane of attached to on filtering the skeleton, the filter membrane passes through the filtration skeleton to be fixed on filtering the base, and is perpendicular with filtering the base.

2. The apparatus for purifying multidimensional nanomaterial of claim 1, wherein the size of the filtration pores of the filter membrane is 100nm to 10 μm.

3. The apparatus for purifying multidimensional nanomaterials of claim 1 wherein the agitation device comprises an electric motor and an agitator paddle connected to the electric motor.

4. The apparatus for purifying multidimensional nano materials of claim 3, wherein the stirring paddle is selected from one of a single screw propeller, a double screw propeller, and a perforated stirring paddle.

5. The apparatus for purifying multidimensional nano materials as recited in claim 3, wherein the electric motor is connected to the stirring paddle to stir and generate a centrifugal force during the purification, providing a filtering pressure for the nano materials to filter out by-products on the filtering membrane.

6. The apparatus for purifying multidimensional nano material as recited in claim 1, wherein the solution injection system injects the displacing solvent during the agitation filtration to ensure that the concentration of the multidimensional nano material in the agitation centrifugal filtration cylinder is relatively stable during the filtration, and the filtrate flows out of the collection system to collect the filtered by-products.

7. A method for purifying multi-dimensional nanomaterial using the apparatus for purifying multi-dimensional nanomaterial of any one of claims 1 to 6, comprising the steps of:

s1, diluting the nano material mother liquor by using a diluent, and injecting the diluted nano material mother liquor into a filter vat through a solution injection system;

s2, starting stirring at a fixed stirring speed; while stirring, the leaching solvent continuously flows in through the solution injection system to compensate the loss of the filter liquor flowing away;

s3, stirring for 60-180min, stopping adding the leaching solvent, and continuing to stir the concentrated solution;

s4 when the concentration of the concentrated solution reaches 1mg m L^-1-15mg mL^-1After that, the purified concentrate was collected at the bottom of the filtration cylinder.

8. The method for purifying multidimensional nano materials as recited in claim 7, wherein the diluent is one or more selected from the group consisting of water, isopropanol, ethanol, ethyl acetate, and petroleum ether.

9. The method of purifying multi-dimensional nanomaterials of claim 7, wherein the eluting solvent is selected from the group consisting of: one or more of water, isopropanol, ethanol, ethyl acetate and petroleum ether.

10. The method of purifying multi-dimensional nanomaterials of claim 7, wherein the fixed stirring speed is 80rpm to 1000 rpm.

Technical Field

The invention relates to the field of preparation of multidimensional nano metal powder and packaging and interconnection of semiconductor chips, in particular to a method and a device for preparing a pure multidimensional nano material.

Background

The chemical preparation and synthesis of the nano material are mainly divided into a top-down method and a bottom-up method, wherein the top-down method comprises the following steps: the nano structure required by people is prepared by a substance with larger size (from micron level to centimeter level) through various etching technologies, and the nano structure has the advantages that various exotic three-dimensional structures can be conveniently prepared; the 'from bottom to top' is that some small structural units (such as atoms, molecules, nano particles and the like) are self-assembled through weak interaction to form a relatively large and complex structural system on the nano scale, and the structural system has the advantages of saving materials, controlling the appearance, controlling the thickness of the materials and the like and has the defect of difficult synthesis. However, the production of the multi-dimensional nano material from top to bottom or from bottom to top is accompanied by the production of byproducts. For example, taking the preparation of silver nanowires as an example, the formation of nanoparticles and nanoprobes as byproducts is inevitable during the preparation of silver nanowires because the formation of crystal nuclei is not instantaneous, and when the oriented growth of silver atoms on the surface of the crystal nuclei is limited, the crystal nuclei grow along multiple paths and thus the formation of byproducts is caused. In addition, some surfactants such as PVP and metal salts are also present in the reaction product, which can greatly degrade the performance of the materials in the device if used directly without purification treatment. Taking the transparent conductive network of the silver nanowires as an example, the existence of PVP can obviously improve the contact resistance between the nanowires and the square resistance of the conductive network, thereby reducing the electrical property of the nanowires; the nanoparticles cannot provide effective conductive paths, so that the improvement of the electrical properties is very limited, and the existence of the nanoparticles can cause light scattering in a visible light range to reduce the optical properties of the transparent conductive film. The two-dimensional material takes boron nitride nanosheets as an example, and at present, common literature reports that hexagonal boron nitride is generally prepared by mechanical ball milling or alkali etching on the boron nitride nanosheets, but a large amount of boron nitride nanoparticle byproducts are generated in the mechanical ball milling or etching process, so that the separation of particles and the nanosheets becomes a difficult point.

At present, the post-treatment purification of the multi-dimensional nano material comprises methods such as centrifugation, filtration, selective sedimentation, electrophoresis, dialysis and the like, but all the methods have limitations, mainly comprising complex and complicated steps, low efficiency and long time consumption, and are not beneficial to large-scale and repeatable preparation in the actual production process. Therefore, in order to further improve the quality of multi-dimensional nanomaterials and reduce production costs for commercial applications, it is necessary to develop an industrially scalable, high-performance, cost-controllable process for large-scale purification of multi-dimensional nanomaterials.

Disclosure of Invention

Aiming at the technical problems in the prior art, the invention provides a device for purifying multidimensional nanomaterials, which comprises a filter cylinder, a stirring device, a solution injection system and a filtrate outflow and collection system, wherein the filter cylinder consists of a filter base, a filter framework and a filter membrane attached to the filter framework, and the filter membrane is fixed on the filter base through the filter framework and is vertical to the filter base.

Preferably, the size of the filter pores of the filter membrane is 100 nm-10 μm.

Preferably, the stirring device comprises a stirring paddle connected to an electric motor.

Preferably, the stirring paddle is selected from one of a single screw propeller, a double screw propeller and a porous stirring paddle.

Preferably, the electric motor is connected with a stirring paddle, and stirring is carried out to generate centrifugal force in purification so as to provide filtering pressure for the nano material to filter out byproducts.

Preferably, the solution injection system is responsible for injecting a replacement solvent during stirring and filtering so as to ensure that the concentration of the multidimensional nanomaterial in the stirring centrifugal filter cylinder is relatively stable during filtering, and the filtrate outflow collection system is responsible for collecting filtered byproducts.

The method for purifying multi-dimensional nanomaterials by the device for purifying multi-dimensional nanomaterials comprises the following steps:

s1, diluting the nano material mother liquor by a diluent, and injecting the diluted nano material mother liquor into a filter cylinder through a solution injection system;

s2, starting stirring at a fixed stirring speed, and enabling the leaching solvent to continuously flow in through the solution injection system during stirring so as to compensate the loss of the filter liquor flowing away;

s3, stirring for 60-180min, stopping adding the leaching solvent, and continuing to stir the concentrated solution;

s4 when the concentration of the concentrated solution reaches 1mg m L^-1-15mg mL^-1After that, the purified concentrate was collected at the bottom of the filtration cylinder.

The nanowire mother liquor contains synthesis byproducts such as nano short rods, a surfactant, a surface coating agent, unreacted reactants and the like, the mother liquor solvent is determined according to a method for synthesizing the nano material, and the diluting solvent comprises water, isopropanol, ethanol, ethyl acetate, petroleum ether and the like.

Preferably, the diluent is selected from water, isopropanol, ethanol, ethyl acetate, petroleum ether.

Preferably, the leaching solvent is selected from: selected from water, isopropanol, ethanol, ethyl acetate, petroleum ether.

Preferably, the fixed stirring speed is 80rpm to 1000 rpm.

The beneficial effects of the invention at least comprise:

(1) the invention discloses a method for purifying a nano material based on dynamic stirring centrifugation, which has the advantages of simple steps, mild conditions, high efficiency and high speed, and can be applied to the purification of nano wires and nano sheets.

(2) Compared with the traditional filtration and purification method, the set of dynamic stirring centrifugal filter device has many advantages: firstly, accurately regulating and controlling the filtering pressure based on stirring, wherein the filtering pressure is derived from a centrifugal force generated when liquid is stirred, the filtering pressure is controlled by the stirring rotating speed, the filtering pressure is high when the rotating speed is high, the filtering speed is relatively accelerated, and the filtering speed is low when the rotating speed is not high; the filter membrane is fixed on the filter cylinder through a framework on the filter cylinder, is vertical to the filter base, and has a larger filter area compared with the traditional bottom filtration; thirdly, the shearing force generated by stirring can clean the surface of the filter membrane, so that the nano by-products are prevented from being accumulated and blocking filter holes of the filter membrane, the subsequent filtration efficiency and the continuous filtration capacity are reduced, meanwhile, the repeated utilization of the filter membrane is realized, and the cost is reduced; fourthly, the solvent can be replaced by various target solvents after the nano material is concentrated through a solution injection system, for example, the undesirable high boiling point solvent is replaced; fifthly, the purification, concentration and solvent phase change of the nano material can be realized in one step in stirring, and the post-treatment process is simplified.

Drawings

Fig. 1 is a schematic structural diagram of an apparatus for purifying multi-dimensional nanomaterials according to an embodiment of the invention.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of the present invention.