CN112588331A - Method for synthesizing composite conductive material by droplet microfluidics and microfluidic synthesis chip - Google Patents
Method for synthesizing composite conductive material by droplet microfluidics and microfluidic synthesis chip Download PDFInfo
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- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention provides a method for synthesizing a composite conductive material by droplet microfluidics and a microfluidics synthetic chip, wherein the microfluidics synthetic chip comprises a polymer soft rubber tube, a parallel double-channel steel needle and a heating layer; the first end of the polymer flexible glue pipe forms a continuous phase inlet, and the second end forms an outlet; the parallel double-channel steel needle comprises a first dispersed phase channel for introducing graphite dispersion liquid and a second dispersed phase channel for introducing a nickel source, an ammonium source and an alkali source water phase; the first dispersed phase channel is located between the first end and the second dispersed phase channel, and the heating layer is located between the second dispersed phase channel and the second end. The graphite/nickel hydroxide nanosheet composite material prepared by the method has the advantages of controllable reaction process, adjustable components, controllable appearance, high conductivity and the like.
Description
Technical Field
The invention relates to a preparation method of a composite conductive material synthesized by droplet microfluidics, in particular to a preparation method of a composite conductive material synthesized by the droplet microfluidics in situ and graphite/nickel hydroxide nanosheets and a microfluidic synthesis chip for realizing the preparation method.
Background
Microfluidics is the science and technology of studying devices and methods for controlling fluids in microchannels on the scale of from a hundred nanometers to hundreds of micrometers. Microfluidics has been the focus of attention over the last two decades because of its low chemical consumption, short analysis time, high throughput, better control of mass and heat transfer, and the scaling down of the laboratory to one chip. Graphite is a natural two-dimensional material, has good chemical stability, high temperature resistance and excellent conductivity, and is widely applied to catalytic materials, battery cathode materials, refractory materials and lubricants. The nickel hydroxide is a petal-shaped nano material, and among various metal hydroxides, the nickel hydroxide nanosheet has the advantages of large specific surface area, promotion of electron and hole separation and the like. The graphite/nickel hydroxide nanosheet composite material with high conductivity and rich oxidation-reduction active sites can be obtained by compounding the two materials by using a droplet microfluidic technology, so that the graphite/nickel hydroxide nanosheet composite material has important application prospects in the fields of preparation of high-performance electrocatalytic materials, nano energy storage and the like.
Disclosure of Invention
The invention aims to provide a preparation method for in-situ synthesizing a graphite/nickel hydroxide nanosheet composite material by droplet microfluidics and a microfluidic synthesis chip for realizing the preparation method.
In order to achieve the above object, the present invention provides the following technical solutions.
The technical scheme of the invention is as follows: a three-phase microfluidic synthesis chip is used as a microreactor, graphite dispersion liquid and nickel hydroxide precursor (a nickel source, an ammonium source and an alkali source) dispersion liquid are introduced into a microchannel of the microfluidic synthesis chip as dispersed phases, and the graphite dispersion liquid forms micro-droplets under the action of continuous phase (oil phase) shearing force. Under the heating condition, due to efficient mass and heat transfer in a confined space, a nickel source, an ammonium source and an alkali source in a nickel hydroxide precursor react rapidly on the surface of graphite to generate a nickel hydroxide nanosheet, and the graphite/nickel hydroxide nanosheet composite material is obtained. The nickel hydroxide nanosheets grown in situ on the graphite surface can improve the conductivity, the specific surface area and the redox active sites of the composite material, so that the composite material has stronger charge storage capacity.
The microfluidic synthesis chip of the embodiment of the invention comprises: the device comprises a polymer soft rubber pipe, a parallel double-channel steel needle which is arranged on the polymer soft rubber pipe and communicated with the polymer soft rubber pipe through an adapter, and a heating layer which is wrapped outside the polymer soft rubber pipe; a continuous phase inlet into which an oil supply continuous phase is introduced is formed at the first end of the polymer flexible rubber pipe, and an outlet for outputting the graphite sheet/nickel hydroxide nanosheet composite material is formed at the second end of the polymer flexible rubber pipe; the parallel double-channel steel needle comprises a first dispersed phase channel for introducing graphite dispersion liquid and a second dispersed phase channel for introducing a nickel source, an ammonium source and an alkali source water phase; the first dispersed phase channel is located between the first end and the second dispersed phase channel; the heating layer is located between the second dispersed phase channel and the second end.
The microfluidic synthesis chip of the invention has the further technical scheme that: the microfluidic synthesis chip adopts photoetching or soft lithography micromachining technology to establish a microchannel network or a multi-T-shaped channel; the T-shaped channel comprises four openings, two of which are inlets of the first and second dispersed phase channels, one of which is a continuous phase inlet and the other of which is an outlet.
The microfluidic synthesis chip of the invention has the further technical scheme that: the polymer soft rubber tube is one of a polydimethylsiloxane tube, a polyvinyl chloride tube or a polytetrafluoroethylene tube; the micro-channel network is made of polymethyl methacrylate or polydimethylsiloxane micro-fluid chip.
The method for synthesizing the composite conductive material by utilizing the liquid drop microfluidic comprises the following steps: introducing an oil continuous phase into the polymer soft rubber pipe from the continuous phase inlet, introducing a graphite dispersion liquid into the first dispersion phase channel, and forming micro-droplets by the graphite dispersion liquid under the action of the shearing force of the oil continuous phase; introducing a nickel hydroxide precursor dispersion liquid into the second dispersion phase channel, wherein the nickel hydroxide precursor dispersion liquid comprises a nickel source, an ammonium source andan alkali source water phase is mixed with the micro-droplets; under the condition of heating, NH in the mixed liquid drops4 +、Ni2+With OH-Generating nickel hydroxide on graphite in situ to obtain a graphite flake/nickel hydroxide nanosheet composite material; and centrifuging, washing and drying the prepared graphite/nickel hydroxide composite material to obtain a target product.
The preparation method of the drop microfluidic in-situ synthesis graphite/nickel hydroxide nanosheet composite material has the further technical scheme that: the graphite dispersion liquid is preferably a graphite powder aqueous solution; the ammonium source water phase is preferably ammonium chloride water solution; the nickel source water phase is preferably one of nickel sulfate water solution, nickel chloride water solution and nickel nitrate water solution; the alkali source water phase is preferably one of sodium hydroxide and potassium hydroxide aqueous solution; the oil continuous phase is preferably one of methyl silicone oil, paraffin oil and toluene.
The preparation method of the drop microfluidic in-situ synthesis graphite/nickel hydroxide nanosheet composite material has the further technical scheme that: controlling the reaction time by adjusting the flow rate of each phase, wherein the flow rate of the oil continuous phase is 0.1-30 mL.h-1The flow rate of the graphite dispersion is 0.1-10 mL/h-1The flow rate of the nickel source, the ammonium source and the alkali source water phase is 0.1-10 mL.h-1。
The preparation method of the drop microfluidic in-situ synthesis graphite/nickel hydroxide nanosheet composite material has the further technical scheme that: the concentration of the graphite dispersion liquid is 0.1-20 mg/mL-1The molar ratio of the ammonium source to the nickel source to the alkali source in the nickel hydroxide precursor dispersion liquid is 6: 1.15: 2.
the preparation method of the drop microfluidic in-situ synthesis graphite/nickel hydroxide nanosheet composite material has the further technical scheme that: the heating temperature is preferably 50-100 ℃.
The preparation method of the drop microfluidic in-situ synthesis graphite/nickel hydroxide nanosheet composite material has the further technical scheme that: the drying temperature is preferably 10-80 ℃, and the drying time is preferably 1-24 h.
The invention has the following beneficial effects:
1. the graphite/nickel hydroxide composite material can be rapidly prepared in the micro-fluidic reaction channel due to the small micro-reaction space with high-efficiency mass and heat transfer.
2. The components, morphology, conductivity and the like of the graphite/nickel hydroxide composite material can be regulated and controlled by regulating and controlling microfluidic synthesis parameters, such as microchannel size, fluid flow rate, precursor components and the like.
3. The nickel hydroxide nanosheets grown in situ on the graphite surface can improve the conductivity, the specific surface area and the redox active sites of the composite material, so that the composite material has stronger charge storage capacity.
Specific embodiments of the present invention are disclosed in detail with reference to the following description and drawings, indicating the manner in which the principles of the invention may be employed. It should be understood that the embodiments of the invention are not so limited in scope.
Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.
Drawings
The drawings described herein are for illustration purposes only and are not intended to limit the scope of the present disclosure in any way. In addition, the shapes, the proportional sizes, and the like of the respective members in the drawings are merely schematic for facilitating the understanding of the present invention, and do not specifically limit the shapes, the proportional sizes, and the like of the respective members of the present invention. Those skilled in the art, having the benefit of the teachings of this invention, may choose from the various possible shapes and proportional sizes to implement the invention as a matter of case. In the drawings:
fig. 1 is a schematic diagram of a preparation method for performing droplet microfluidic in-situ synthesis on a graphite/nickel hydroxide nanosheet composite material by using a microfluidic synthesis chip according to an embodiment of the present invention.
Detailed Description
The following examples illustrate the preparation of the graphite sheet/nickel oxide graphite/nickel hydroxide composite material for microfluidic synthesis of nickel hydroxide according to the present invention, but the present invention is not limited to these examples.
The microfluidic synthesis chip in the embodiment of the invention is prepared by the following method: adopts a steel needle, a polymer soft rubber pipe and an adapter. There are four access ports: two dispersed phases, one continuous phase, one outlet. The two-phase microfluidic system generates uniform mixed liquid drops containing two dispersed phases through the actions of interfacial tension between two phases, shearing force of continuous relative dispersed phases and the like, and the flow rate of fluid is controlled through a numerical control micro-injection pump.
As shown in fig. 1, the microfluidic composite chip includes a polymer soft rubber tube 1, a parallel double-channel steel needle disposed on the polymer soft rubber tube 1 and communicated with the polymer soft rubber tube 1 through an adapter, and a heating layer 4 wrapped on the polymer soft rubber tube 1. The first end of the polymer flexible glue pipe 1 forms a continuous phase inlet 11 for introducing the oil supply continuous phase, and the second end forms an outlet 12 for outputting the graphite sheet/nickel hydroxide nano sheet composite material. The parallel double-channel steel needle comprises a first dispersed phase channel 2 for introducing graphite dispersion liquid and a second dispersed phase channel 3 for introducing a nickel source, an ammonium source and an alkali source water phase. The first dispersed phase channel 2 is located between the first end and the second dispersed phase channel 3, and the heating layer 4 is located between the second dispersed phase channel 3 and the second end.
In specific implementation, an oil continuous phase is introduced into the polymer soft rubber hose 1 from the continuous phase inlet 11, a graphite dispersion liquid is introduced into the first dispersed phase channel 2, and the graphite dispersion liquid forms micro-droplets under the shearing force action of the oil continuous phase. And (3) introducing a nickel hydroxide precursor dispersion liquid containing a nickel source, an ammonium source and an alkali source water phase into the second dispersion phase channel 3, and mixing the nickel hydroxide precursor dispersion liquid with the micro-droplets. Under the condition of heating, NH in the mixed liquid drops4 +、Ni2+With OH-And (3) generating nickel hydroxide on the graphite in situ to obtain the graphite flake/nickel hydroxide nanosheet composite material. Compounding the prepared graphite/nickel hydroxideAnd centrifuging, washing and drying the material to obtain a target product.
Example 1
1. Dispersing 30mg graphite powder in 30mL water, ultrasonically dispersing for 60min to obtain a first dispersion phase, sucking the first dispersion into a syringe, connecting with a micro-injection pump, and setting flow rate at 0.1 mL.h-1。
2. Dispersing 1.0g ammonium chloride, 0.46g nickel chloride hexahydrate and 0.2g sodium hydroxide in 30mL water, ultrasonically dispersing for 30min to obtain a second dispersion phase, sucking the second dispersion into a syringe, connecting with a micro-injection pump, and setting the flow rate at 0.1 mL-h-1。
3. Selecting methyl silicone oil as continuous phase solution, sucking into an injector, connecting with a micro-injection pump, and setting the flow rate at 0.2 mL.h-1。
4. Starting the micro-fluidic device: after the polymer soft rubber tube 1 is completely filled with the oil continuous phase methyl silicone oil, simultaneously starting the injection pumps of the two dispersed phases, heating the liquid drops for 2 hours at 50 ℃ after the flow rate is stable, and carrying out in-situ reaction on the precursor in microliter liquid drops to generate the graphite/nickel hydroxide composite material of nickel hydroxide.
5. Centrifuging the collected graphite flake/nickel hydroxide composite material in the oil phase, washing the graphite flake/nickel hydroxide composite material with ethanol for three times, and drying the graphite flake/nickel hydroxide composite material at 50 ℃ for 15 hours to obtain the graphite/nickel hydroxide nanocomposite material with uniform particle size.
Example 2
1. Dispersing 60mg graphite powder in 30mL water, ultrasonically dispersing for 60min to obtain a first dispersion phase, sucking the first dispersion liquid into an injector, connecting with a micro-injection pump, and setting the flow rate at 3 mL.h-1。
2. Dispersing 2.4g ammonium sulfate, 0.93g nickel sulfate and 0.28g potassium hydroxide in 30mL water, ultrasonically dispersing for 30min to obtain a second dispersion phase, sucking the second dispersion into a syringe, connecting with a micro-injection pump, and setting the flow rate at 3 mL. h-1。
3. Selecting methyl silicone oil as continuous phase solution, sucking into an injector, connecting with a micro-injection pump, and setting the flow rate at 5 mL.h-1。
4. Starting the micro-fluidic device: and after the soft rubber tube is completely filled with the continuous-phase methyl silicone oil, simultaneously starting the injection pumps of the two dispersed phases, heating the liquid drop at 60 ℃ for 10 hours after the flow rate is stable, and carrying out in-situ reaction on the precursor in microliter liquid drops to generate the graphite/nickel hydroxide composite material of nickel hydroxide.
5. Centrifuging the collected graphite/nickel hydroxide composite material in the oil phase, washing the graphite/nickel hydroxide composite material with ethanol for three times, and drying the graphite/nickel hydroxide composite material at the temperature of 60 ℃ for 5 hours to obtain the graphite/nickel hydroxide nano composite material with uniform particle size.
Example 3
1. Dispersing 3mg graphite powder in 30mL water, ultrasonically dispersing for 60min to obtain a first dispersion phase, sucking the first dispersion liquid into an injector, connecting with a micro-injection pump, and setting the flow rate at 8 mL.h-1。
2. Dispersing 1.0g ammonium chloride, 1.03g nickel nitrate and 0.28g potassium hydroxide in 30mL water, ultrasonically dispersing for 30min to obtain a second dispersion phase, sucking the second dispersion into a syringe, connecting with a micro-injection pump, and setting the flow rate at 8 mL. h-1。
3. Selecting methyl silicone oil as continuous phase solution, sucking into an injector, and connecting with a micro-injection pump at a set flow rate of 10mL & h-1。
4. Starting the micro-fluidic device: and after the soft rubber tube is completely filled with the continuous-phase methyl silicone oil, simultaneously starting the injection pumps of the two dispersed phases, heating the liquid drop for 8 hours at 70 ℃ after the flow rate is stable, and carrying out in-situ reaction on the precursor in the microliter liquid drop to generate the graphite/nickel hydroxide composite material of nickel hydroxide.
5. Centrifuging the collected graphite/nickel hydroxide composite material in the oil phase, washing the graphite/nickel hydroxide composite material with ethanol for three times, and drying the graphite/nickel hydroxide composite material at 70 ℃ for 15 hours to obtain the graphite/nickel hydroxide nano composite material with uniform particle size.
Example 4
1. Dispersing 200mg graphite powder in 30mL water, ultrasonically dispersing for 60min to obtain a first dispersion phase, sucking the first dispersion liquid into an injector, connecting with a micro-injection pump, and setting the flow rate at 10 mL.h-1。
2. Dispersing 1.0g ammonium chloride, 1.03g nickel nitrate and 0.28g potassium hydroxide in 30mL water, ultrasonically dispersing for 30min to obtain a second dispersion phase, and sucking and injecting the second dispersion liquidThe rear part of the device is connected with a micro-injection pump, and the flow rate is set to be 4 mL.h-1。
3. Selecting methyl silicone oil as continuous phase solution, sucking into an injector, connecting with a micro-injection pump, and setting the flow rate at 15 mL.h-1。
4. Starting the micro-fluidic device: and after the soft rubber tube is completely filled with the continuous-phase methyl silicone oil, simultaneously starting the injection pumps of the two dispersed phases, heating the liquid drop for 5 hours at 80 ℃ after the flow rate is stable, and carrying out in-situ reaction on the precursor in microliter liquid drop to generate the graphite/nickel hydroxide composite material of nickel hydroxide.
5. Centrifuging the collected graphite/nickel hydroxide composite material in the oil phase, washing the graphite/nickel hydroxide composite material with ethanol for three times, and drying the graphite/nickel hydroxide composite material at the temperature of 80 ℃ for 24 hours to obtain the graphite/nickel hydroxide nano composite material with uniform particle size.
Example 5
1. Dispersing 400mg graphite powder in 30mL water, ultrasonically dispersing for 60min to obtain a first dispersion phase, sucking the first dispersion liquid into an injector, connecting with a micro-injection pump, and setting the flow rate at 10 mL.h-1。
2. Dispersing 1.0g ammonium chloride, 1.03g nickel nitrate and 0.28g potassium hydroxide in 30mL water, ultrasonically dispersing for 30min to obtain a second dispersion phase, sucking the second dispersion into a syringe, connecting with a micro-injection pump, and setting the flow rate at 10 mL. h-1。
3. Selecting methyl silicone oil as continuous phase solution, sucking into an injector, connecting with a micro-injection pump, and setting the flow rate at 30 mL.h-1。
4. Starting the micro-fluidic device: and after the soft rubber tube is completely filled with the continuous-phase methyl silicone oil, simultaneously starting the injection pumps of the two dispersed phases, heating the liquid drop at 950 ℃ for 2 hours after the flow rate is stable, and carrying out in-situ reaction on the precursor in the microliter liquid drop to generate the graphite/nickel hydroxide composite material of nickel hydroxide.
5. Centrifuging the collected graphite/nickel hydroxide composite material in the oil phase, washing the graphite/nickel hydroxide composite material with ethanol for three times, and drying the graphite/nickel hydroxide composite material at 65 ℃ for 2 hours to obtain the graphite/nickel hydroxide nano composite material with uniform particle size.
Any numerical value recited herein includes all values from the lower value to the upper value that are incremented by one unit, provided that there is a separation of at least two units between any lower value and any higher value. For example, if it is stated that the number of a component or a value of a process variable (e.g., temperature, pressure, time, etc.) is from 1 to 90, preferably from 21 to 80, and more preferably from 30 to 70, it is intended that equivalents such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 are also expressly enumerated in this specification. For values less than 1, one unit is suitably considered to be 0.0001, 0.001, 0.01, 0.1. These are only examples of what is intended to be explicitly recited, and all possible combinations of numerical values between the lowest value and the highest value that are explicitly recited in the specification in a similar manner are to be considered.
Unless otherwise indicated, all ranges include the endpoints and all numbers between the endpoints. The use of "about" or "approximately" with a range applies to both endpoints of the range. Thus, "about 20 to about 30" is intended to cover "about 20 to about 30", including at least the endpoints specified.
It should be noted that, in the description of the present invention, the terms "first", "second", and the like are used for descriptive purposes only and for distinguishing similar objects, and no precedence between the two is considered as indicating or implying relative importance. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
The above description is only a few embodiments of the present invention, and those skilled in the art can make various changes or modifications to the embodiments of the present invention according to the disclosure of the application document without departing from the spirit and scope of the present invention.
Claims (7)
1. A microfluidic synthesis chip, comprising: the device comprises a polymer soft rubber pipe, a parallel double-channel steel needle which is arranged on the polymer soft rubber pipe and communicated with the polymer soft rubber pipe through an adapter, and a heating layer which is wrapped outside the polymer soft rubber pipe; a continuous phase inlet into which an oil supply continuous phase is introduced is formed at the first end of the polymer flexible rubber pipe, and an outlet for outputting the graphite sheet/nickel hydroxide nanosheet composite material is formed at the second end of the polymer flexible rubber pipe; the parallel double-channel steel needle comprises a first dispersed phase channel for introducing graphite dispersion liquid and a second dispersed phase channel for introducing nickel hydroxide precursor dispersion liquid; the first dispersed phase channel is located between the first end and the second dispersed phase channel, and the heating layer is located between the second dispersed phase channel and the second end.
2. A method for microfluidic synthesis of a composite conductive material using droplets according to claim 1, comprising: introducing an oil continuous phase into the polymer soft rubber hose from the continuous phase inlet, introducing a graphite dispersion liquid into the first dispersion phase channel, wherein the graphite dispersion liquid forms micro-droplets under the action of the shearing force of the oil continuous phase; introducing a nickel hydroxide precursor dispersion liquid into the second dispersion phase channel, wherein the nickel hydroxide precursor dispersion liquid comprises a nickel source, an ammonium source and an alkali source water phase and is mixed with the micro-droplets; under the condition of heating, NH in the mixed liquid drops4 +、Ni2+With OH-Generating nickel hydroxide on graphite in situ to obtain a graphite flake/nickel hydroxide nanosheet composite material; and centrifuging, washing and drying the prepared graphite/nickel hydroxide composite material to obtain a target product.
3. The method of claim 2, wherein the graphite dispersion is an aqueous graphite powder solution; the ammonium source water phase is an ammonium chloride aqueous solution; the nickel source water phase is one of a nickel sulfate water solution, a nickel chloride water solution and a nickel nitrate water solution; the alkali source water phase is one of sodium hydroxide and potassium hydroxide water solution; the oil connecting phase is one of methyl silicone oil, paraffin oil and toluene.
4. The method of claim 2, wherein the reaction time is controlled by adjusting the flow rate of each phase, wherein the flow rate of the oil continuous phase is 0.1 to 30 mL-h-1The flow rate of the graphite dispersion liquid is 0.1-10 mL/h-1The flow rates of the nickel source, the ammonium source and the alkali source water phase are 0.1-10 mL.h-1。
5. The method of claim 2, wherein the graphite dispersion has a concentration of 0.1 to 20 mg-mL-1The molar ratio of the ammonium source to the nickel source to the alkali source in the nickel hydroxide precursor dispersion liquid is 6: 1.15: 2.
6. the method of claim 2, wherein the heating temperature is 50 to 100 ℃.
7. The method according to claim 2, wherein the drying temperature is 10 to 80 ℃ and the drying time is 1 to 24 hours.
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