CN113529075A - Liquid metal composite porous membrane and preparation method and application thereof - Google Patents
Liquid metal composite porous membrane and preparation method and application thereof Download PDFInfo
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- G01N31/005—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods investigating the presence of an element by oxidation
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Abstract
The invention discloses a liquid metal composite porous membrane and a preparation method thereof, wherein a metal porous material is used as a negative electrode, a counter electrode is used as a positive electrode, a strong acid solution with the concentration of pH being less than or equal to 0 is used as a conductive liquid, liquid metal is dripped on the negative electrode, a voltage of 0.5-5V is applied to fill pore channels of the metal porous material with the liquid metal, and the voltage is continuously applied for stabilization for 1-5 min after the filling is completed. The invention also discloses a responsive gating system, wherein the liquid metal composite porous membrane is arranged in the flow channel and used as a gating unit for the fluid to pass through the flow channel, the responder enables the liquid metal to be in a first flowing state or a second flowing state by enabling the solid oxide layer to exist or not exist on the surface of the liquid metal, so as to control the state of the fluid in the pore channel of the liquid metal composite porous membrane, the responsive gating system has the properties of pore channel memory and recovery, and has wide application prospect in intelligent pore channel switches and substance responsiveness detection.
Description
Technical Field
The invention belongs to the field of new material preparation and new material device design and application, and particularly relates to a liquid metal composite porous membrane and a preparation method and application thereof.
Background
Liquid metal refers to a metal consisting of a single or multiple metals having a low melting point in a flowable liquid state at normal temperature. It possesses the properties of ordinary liquid, such as viscosity, flowability and deformability. But also has specificity such as high electrical conductivity, high density, high surface tension, high thermal conductivity, low volatility, no toxicity and good biocompatibility. Due to these excellent characteristics, liquid metals have become an important research focus and hot spot for emerging materials in recent years.
The promotion of novel materials cannot be separated from the combination with additional materials and the optimized design of the structure. The research focus of liquid metal mainly centers on the properties of liquid metal at present, shows that the preparation of specific liquid metal taking the components of the liquid metal as the focus and the research on the physicochemical properties of related single composite materials are mainly applied to micro-fluidics, flexible circuits and wearing equipment based on stretchable composite soft materials, energy utilization, biochemical materials, motors, intelligent novel robots and the like. The research on the liquid metal interface, such as the research on the composite material with high interfacial energy, adhesion and interface thin oxide layer, is very rare, especially the research and utilization of the oxide layer. The formation of the oxide layer is mainly present in liquid metal containing components such as gallium which are easily oxidized by air. This property is currently used mainly to control the deformation and selective wetting of the liquid metal. Therefore, how to develop a new liquid metal material and further improve the specific advantages of liquid metal is another novel subject in the field of liquid metal material design. The development of the research also provides possibility for the application development of the novel liquid metal material.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a liquid metal composite porous membrane and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a preparation method of a liquid metal composite porous membrane, which adopts an electrochemical method, takes a metal porous material as a negative electrode, takes a counter electrode as a positive electrode, takes a strong acid solution with the concentration of pH less than or equal to 0 as a conductive liquid, dropwise adds liquid metal on the negative electrode, applies a voltage of 0.5-5V to enable the liquid metal to fill pore channels of the metal porous material, continuously applies the voltage for stabilization for 1-5 min after the filling is finished, takes out the negative electrode, cleans the negative electrode and dries the liquid metal composite porous membrane to obtain the liquid metal composite porous membrane. The term "complete filling" as used herein means that the upper and lower (front and back) surfaces of the porous metal material have silvery-white luster after being filled with the liquid metal.
Optionally, the strong acid solution with the pH value less than or equal to 0 is a hydrochloric acid solution with the concentration more than or equal to 1M.
Optionally, the pore size of the metal porous material ranges from 5 μm to 30 μm.
Optionally, the liquid metal is an alloy of gallium and at least one element selected from indium and selenium, and the liquid metal is in a liquid state at normal temperature. The normal temperature mentioned here means the indoor temperature under the normal climatic conditions, and is defined as 10-30 ℃.
Optionally, the counter electrode can be a standard electrode, such as a saturated calomel electrode, an Ag/AgCl electrode; or chemically inactive but good conductivity electrodes such as: glassy carbon electrodes, and the like.
Optionally, the drying method includes drying, blow-drying, airing and the like.
Wherein, the concentration of the hydrochloric acid solution is more than or equal to 1M, which can ensure that no oxide layer is formed on the surface of the liquid metal.
Wherein, the voltage can not be lower than 0.5V, and the liquid metal can quickly and effectively fill the pore channels of the metal porous material only when the voltage is higher than the voltage; above 5V, the electric energy utilization efficiency will be reduced.
The invention also provides a liquid metal composite porous membrane prepared by the method, wherein the liquid metal composite porous membrane is prepared by the method of any one of claims 1 to 3; the liquid metal composite porous membrane comprises a metal porous material and liquid metal, wherein the liquid metal fills the pore channels of the metal porous material and covers the surface of the metal porous material, and an alloy layer is formed at the contact interface of the liquid metal and the metal porous material.
The invention also provides a responsive gating system, which comprises a flow channel, a responder and the liquid metal composite porous membrane, wherein the liquid metal composite porous membrane is arranged in the flow channel and is used as a gating unit for allowing fluid to pass through the flow channel; the responder enables the liquid metal to be in a first flowing state or a second flowing state by enabling a solid oxide layer to exist or not exist on the surface of the liquid metal, so that the state of a channel of the liquid metal composite porous membrane through which fluid passes is controlled.
Optionally, the fluid contains the responder.
Optionally, the liquid metal composite porous membrane further comprises a responsive substance unit, wherein the responsive substance unit is in contact with the liquid metal composite porous membrane and contains the responder.
Optionally, in the first flow state, the liquid metal opens the pore channel after the fluid passes through the liquid metal composite porous membrane, and in the second flow state, the liquid metal closes the pore channel after the fluid passes through the liquid metal composite porous membrane.
Optionally, the responder changes the flowing state of the liquid metal by generating or ablating a solid oxide layer on the surface of the liquid metal so as to change the channel state of the liquid metal composite porous membrane.
Optionally, the responder is an oxidizing substance or a reducing substance, and a solid oxide layer on the surface of the liquid metal is generated or ablated through an oxidation-reduction reaction.
The invention has the beneficial effects that:
the invention combines the solid material of the rigid porous network metal with the flowing gallium-containing liquid metal, develops a novel liquid metal composite porous membrane, and provides a new idea for the development of the novel liquid metal material. The porous and rigid structure of the porous network metal solid material and the characteristics of fluid, interface high surface energy and an oxidation layer of liquid metal are combined, the porous membrane material with the change from the shape memory of the pore channel to the state recovery is designed, and the application in a responsive gating system is realized. The system is simple in principle and easy to implement, and can be widely applied to intelligent controllable gate control systems, especially to research and development in the fields of intelligent gate control switches, substance responsiveness detection and the like.
Drawings
FIG. 1 is a schematic view of the production process of example 1;
FIG. 2 is a schematic structural view of a liquid metal composite porous membrane prepared in example 1;
fig. 3 is an apparatus schematic diagram of a responsive gating system of example 2;
FIG. 4 is a graph of the gating pressure of fluids containing different responders through the gate unit in example 2;
FIG. 5 is a schematic diagram showing the response process and result of the gate control unit to different respondents in example 2;
fig. 6 is an apparatus schematic diagram of a responsive gating system of embodiment 3;
FIG. 7 is a pressure diagram illustrating the gating of air through a gating system containing units of different responsive substances in example 3;
FIG. 8 is a schematic diagram showing the response results of the gate control unit to different respondents in example 3;
FIG. 9 is a graph showing the results of the effect of different responsive substance units on the gate unit in example 4;
FIG. 10 is a graph showing the results of the effect of different constituent responsive substance units on the gate unit in example 5;
FIG. 11 is a graph showing the results of the effect of different concentrations of responsive substance units on the gating cell in example 6.
Detailed Description
The invention is further explained below with reference to the figures and the specific embodiments.
Example 1
Referring to fig. 1, a method for preparing a liquid metal composite porous membrane includes the steps of:
s1, selecting liquid metal (Ga) capable of reacting with Ga-in-SexInySez) A copper porous film (selected here) in which Ga as the main component interacts withRepresented by copper foam) as a rigid base material of the liquid metal composite porous film;
s2, adopting a two-electrode system, taking the prepared material as a working electrode, taking a glassy carbon electrode as a counter electrode, taking 1M HCl as a conductive liquid, taking the working electrode as a negative electrode and taking the counter electrode as a positive electrode, and assembling according to the figure 1;
s3, dripping gallium indium selenium liquid metal on the working electrode in a ventilation environment, and applying 1V voltage until the liquid metal covers the copper porous film and then stabilizing for 2 min;
and S3, taking out the working electrode, washing with clean water, and drying.
Referring to fig. 2, the obtained liquid metal composite porous film, the gallium indium selenium liquid metal filled the pore channels of the copper porous film and covered the upper surface of the copper porous film (the surface on which the liquid metal was dropped), and CuGa was formed on the surface where copper and the liquid metal were in contact2The alloy layer increases the bonding force of the two, so that the liquid metal can be easily recovered in the pore channel under the action of the reducing responder.
Example 2
Referring to fig. 3, the responsive gating system of the present embodiment includes a gating cell 1 formed of the liquid metal composite porous film of example 1, a sealing cell 2, a fluid input channel 3, and a fluid output channel 3'. The fluid input channel 3 and the fluid output channel 3 'form a fluid flow channel, the fluid in the fluid input channel 3 needs to pass through the gate control unit 1 to enter the fluid output channel 3', and the sealing unit 2 plays a role in sealing and can be used for carrying high-pressure fluid in the fluid input channel 3. The liquid metal composite porous membrane is placed in an oxidation environment before assembly, wherein gallium is easy to oxidize to generate gallium oxide, the thickness of the solid oxide layer is about dozens of nanometers, the formation of the solid oxide layer can limit partial fluidity of the liquid metal, but the solid oxide layer can also change along with the state of the bulk liquid metal, and the oxidation interface and the bulk component of the liquid metal belong to a dynamic equilibrium state. In the initial state of application, the surface of the liquid metal composite porous membrane is formed with a solid oxide layer, and the liquid metal fills (closes) the pore channel.
Gas (here air), NaOH solution and NaCl solution were passed through the liquid metal composite porous membrane as fluids, and as a result, it was found that these fluids all required overcoming a high gating pressure to pass through for the first time through the gate unit, but two cases occurred for the second and third times: for gases (here air) and NaCl solutions, very low pressures are required to pass; while for NaOH solutions, very high pressures are still required, the data are detailed in fig. 4.
Referring to fig. 5, when the fluid contains a responder (air, NaCl solution) that is a substance that can hold the oxide layer: referring to fig. 5a-i, when fluid passes through the pore channels, a liquid/solid/liquid (gas) interface composition form is formed, wherein solid is an oxide layer formed by liquid metal, referring to fig. 5b-i, the oxide layer on the surface of the liquid metal limits the fluidity of the liquid metal (presents a first flowing state), so that the liquid metal is molded into various shapes, the action of external force on the liquid metal is shown, therefore, traces of the fluid flowing through can be preserved in the pore channels of the liquid metal composite porous membrane, and the open state of the pore channels is maintained after the fluid passes through; when the fluid contains a responder (NaOH solution) that is a substance that can reduce (ablate) the liquid metal oxide layer: referring to fig. 5a-ii, a liquid/liquid (gas) interface is formed when the fluid flows through the cell, and referring to fig. 5b-ii, the liquid metal is fully in a flowing state (second flowing state), and no trace is left when the fluid flows through, and the liquid metal fills the cell under the capillary force of the pores and the high surface energy of the liquid metal in the cell, and returns to the initial state, maintaining the initialized "closed" shape of the cell.
In this embodiment, the flow-through behavior of the substance can be selectively memorized as it passes through the channels of the membrane. In use, the system may be used for intelligent switching or detection of substances by monitoring the performance of liquid metal in terms of oxidation or reduction. The system provides an intelligent gate control switch design, and can realize whether a gate control system is opened or closed through controlling the components of a transmission fluid: the switch is in a closed state by using NaOH solution, and single-pass action of the substance is realized, namely large gating pressure needs to be overcome when the substance passes through each time; the valve is opened by air or NaCl solution only once, so that the fluid can be easily passed through the gate control system. It is also possible to detect whether the fluid contains an oxidizing component by this action.
Example 3
Referring to fig. 6, the responsive gating system of the present embodiment includes a gating cell 1 formed of the liquid metal composite porous film of example 1, a sealing cell 2, a fluid input channel 3, a fluid output channel 3', and a responsive substance cell 4. The fluid input channel 3 and the fluid output channel 3 'form a fluid flow channel, the fluid in the fluid input channel 3 needs to pass through the gate control unit 1 to enter the fluid output channel 3', and the sealing unit 2 plays a role in sealing and can be used for carrying high-pressure fluid in the fluid input channel 3. The responsive substance unit 4 is disposed in contact with the door control unit 1. In the initial state of application, the surface of the liquid metal composite porous membrane is formed with a solid oxide layer, and the liquid metal fills (closes) the pore channel.
The responsive substance unit 4 is formed by using a gas (air here), which is a fluid passing flow channel, as a responder, a NaOH solution and a NaCl solution, respectively. It was found that these gases, on the first pass through the gate unit 1, all need to overcome a high gate pressure to pass, but on the second and third passes, both cases occur. For the responsive substance units of gas (air here) and NaCl solution, very low pressure is required to pass; while for NaOH solutions, very high pressures are still required, the data are detailed in fig. 7. Thus, when air flows from the side of the fluid input channel 3 through the gate unit 1 to the fluid output channel 3' under the action of the responsive substance unit 4, two states will also occur, with reference to fig. 8, 1) a trace of the fluid flow will be preserved in the channel of the gate unit 1, see in detail fig. 8 i; or 2) after the fluid flows through, the gate unit 1 will stay in the initial state under the action of the responsive substance unit, and the liquid metal fills the pore channel, as shown in detail in FIG. 8 ii.
In application, the system is used for intelligent switching or detecting substances by monitoring whether liquid metal is oxidized or reduced, and can also be realized by other modes. By replacing the components of the responsive substance unit, the intelligent switch of the gating system is turned on or off: the switch is in a closed state by using NaOH solution, and single-pass action of the substance is realized, namely large gating pressure needs to be overcome when the substance passes through each time; by utilizing air or NaCl solution, the switch can be in an open state only by opening once, and fluid can pass through the door control system easily. It is also possible to detect whether or not the responsive substance unit contains an oxidizing component by such a behavior.
Example 4
With the device of example 3, for a gate unit in which the pore channel is maintained in a shape "memory" state (herein, considered as a pore that retains a fluid passing state, i.e., a pore channel open state), under the action of the responsive substance unit 4, two states are assumed, 1) the pore channel is still maintained in a state in which the fluid flows, and the gas is still maintained in the "open" state when passing, and the gas can pass through the liquid metal composite porous membrane gate unit with only a small pressure; or 2) return to the initial liquid metal filled state upon stimulation by the responsive substance unit, at which time it is necessary to overcome the significant gating pressure to pass through the gate unit. The detailed data are shown in FIG. 9. For the first state, the switch is in the open state, and the response substance can be judged to contain the oxidation component; in the second state, the switch is closed, and the responsive substance is judged to contain a reducing component.
Example 5
With the device of example 3, the state of the channel of the gate unit was regulated by changing the substance component of the responsive substance unit 4. Referring to fig. 10, the opening-continuous opening-closing-reopening process of the intelligent switch formed by the responsive gating system is realized by first retaining the shape information (1a-3a) of the gas flowing through the channel and maintaining the shape information (1b-3b) of the channel under the NaCl solution, so that the channel can be restored to the initial closed filling state (1c-3c) under the NaOH solution, and the information (1d-3d) of the gas flowing through the channel is retained again when the NaCl solution is changed.
Example 6
With the apparatus of example 3, how much of the responsive substance unit contained the oxidation component was detected by observing the gating behavior. If the shape memory state of the liquid metal can be left by utilizing whether the gas passes through the pore channel, the behavior can be regulated and controlled by the concentration of the effective ingredients in the substances of the responsive substance unit. Referring to fig. 11, after the information (1a-3a) on the shape of the gas flowing through the cell channels is retained, HCl solutions and NaOH solutions of different concentrations are used as the responsive substance unit 4 to adjust the concentrations of HCl and NaOH (1b-3b, 0.001M; 1c-3c, 0.01M; 1d-3d, 0.1M; 1e-3e,1M), and the gas passes through the cell channels of the liquid metal composite porous membrane to gradually restore the information from the gas flowing through the cell channels to the original closed filling state. When air as a fluid was passed through the gate unit by high pressure, it was judged that the HCl concentration had been higher than 1M or the NaOH concentration had been higher than 0.1M in the solution at that time.
The above examples are only used to further illustrate the liquid metal composite porous membrane of the present invention, the preparation method and the application thereof, but the present invention is not limited to the examples, and any simple modification, equivalent change and modification made to the above examples according to the technical spirit of the present invention fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a liquid metal composite porous membrane is characterized by comprising the following steps: the method comprises the steps of adopting an electrochemical method, taking a metal porous material as a negative electrode, taking a counter electrode as a positive electrode, taking a strong acid solution with the concentration of pH being less than or equal to 0 as a conductive liquid, dropwise adding liquid metal on the negative electrode, applying a voltage of 0.5-5V to enable the liquid metal to fill pore channels of the metal porous material, continuously applying the voltage for stabilization for 1-5 min after filling, taking out the negative electrode, cleaning and drying to obtain the liquid metal composite porous membrane.
2. The method of claim 1, wherein: the pore diameter range of the metal porous material is 5-30 mu m.
3. The method of claim 1, wherein: the liquid metal is an alloy of gallium and at least one element of indium and selenium, and the liquid metal is liquid at normal temperature.
4. A liquid metal composite porous membrane characterized by: the liquid metal composite porous membrane is prepared by the method of any one of claims 1 to 3; the liquid metal composite porous membrane comprises a metal porous material and liquid metal, wherein the liquid metal fills the pore channels of the metal porous material and covers the surface of the metal porous material, and an alloy layer is formed at the contact interface of the liquid metal and the metal porous material.
5. A responsive gating system, characterized by: a gate control unit comprising a flow channel, a responder, and the liquid metal composite porous membrane of claim 4 disposed in the flow channel and passing through the flow channel as a fluid; the responder enables the liquid metal to be in a first flowing state or a second flowing state by enabling a solid oxide layer to exist or not exist on the surface of the liquid metal, so that the state of a channel of the liquid metal composite porous membrane through which fluid passes is controlled.
6. The responsive gating system of claim 5, wherein: the fluid contains the responder.
7. The responsive gating system of claim 5, wherein: the liquid metal composite porous membrane further comprises a responsive substance unit, wherein the responsive substance unit is in contact with the liquid metal composite porous membrane and contains the responder.
8. The responsive gating system of claim 5, wherein: and in the first flow state, after the fluid passes through the liquid metal composite porous membrane, the liquid metal opens the pore channel, and in the second flow state, after the fluid passes through the liquid metal composite porous membrane, the liquid metal closes the pore channel.
9. The responsive gating system of claim 5, wherein: the responder changes the flowing state of the liquid metal by generating or ablating a solid oxide layer on the surface of the liquid metal so as to change the channel state of the liquid metal composite porous membrane.
10. The responsive gating system of claim 9, wherein: the response substance is an oxidizing substance or a reducing substance, and a solid oxide layer on the surface of the liquid metal is generated or ablated through an oxidation-reduction reaction.
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| CN114836799A (en) * | 2022-05-13 | 2022-08-02 | 北京航空航天大学 | Preparation method of liquid metal with electric field induced multilevel structure |
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