CN111863341A - Method for inducing fusion sintering of liquid metal micro-nano droplets by solvent evaporation - Google Patents
Method for inducing fusion sintering of liquid metal micro-nano droplets by solvent evaporation Download PDFInfo
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Abstract
The invention relates to the technical field of liquid metal sintering and fusing, in particular to a method for inducing liquid metal micro-nano liquid drop fusion and sintering by using solvent evaporation. And (3) evaporating and drying the liquid metal micro-nano droplet dispersion liquid or the liquid metal micro-nano droplet dispersion liquid containing the auxiliary agent, and realizing sintering and fusion by using the capillary force generated in the evaporation and drying process. The method for sintering the liquid metal micro-nano droplets has the advantages of simplicity and convenience in operation, low cost, realization at normal temperature and normal pressure and the like, and can be used in the fields of packaging circuits, 3D printing electronic technology, sensors, drivers, electromagnetic shielding and the like.
Description
Technical Field
The invention relates to the technical field of liquid metal sintering and fusing, in particular to a method for inducing liquid metal micro-nano liquid drop fusion and sintering by using solvent evaporation.
Background
Liquid metal generally refers to a simple metal or an alloy with a melting point below 200 ℃, and perfectly combines the conductivity of the metal and the fluidity of liquid. The liquid metal is a gallium-based alloy (e.g., a eutectic gallium indium alloy of 74.5 wt% Ga and 24.5 wt% In, melting point-15.8 deg.C; a eutectic gallium indium tin alloy of 62.5 wt% Ga, 21.5 wt% In, and 16 wt% Sn, melting point-13.2 deg.C; etc.). Liquid metals have excellent mechanical, thermal and electrical properties. In addition, due to the characteristics of low toxicity, low viscosity and the like, the composite material has wide application prospects in the fields of wearable sensing electronic devices, conductive composite materials, flexible display screens, intelligent electronic equipment and the like. The research on the liquid metal has important theoretical significance and practical value.
The surface tension of the liquid metal is high (the surface tension of the eutectic gallium-indium alloy is 624mN m–1) And the composite material is difficult to be compounded with other materials to form the composite material, so that the application range of the liquid metal is limited. The liquid metal is dispersed into the solvent to form micro-nano liquid drops, the surface modifier is easily modified on the surfaces of the liquid drops in the solvent system, and the method is favorable for improving the affinity of the liquid metal on different substrates and widening the application range of the liquid metal. However, since the dispersed micro-nano liquid drops of liquid metal are easily oxidized by air or solvent environment (such as oxidizing agents like water and oxygen), and the surface of the micro-nano liquid drops is provided with a layer of oxide shell, the electron conductivity between the liquid metal micro-nano liquid drops which are contacted with each other is also poor, and the conductivity of the micro-nano liquid drops can be recovered only by destroying the oxide shell of the micro-nano liquid drops through pressure, laser or high-temperature sintering. For example, the literature (advanced materials, 2015, 27: 2355) discloses liquid metal droplets dispersed in ethanol, which, after drying, can be brought back to the conductive state by means of mechanical pressure sintering; literature (ACS Applied Materials)&Interfaces, 2018, 10: 28232) The method is characterized in that the oxide layer shell of the liquid metal drop is damaged by a laser sintering or high-temperature sintering method to make the liquid metal drop conductive. However, the operation under the conditions of external pressure, laser, high temperature and the like is more complicated, the cost is higher, the energy consumption is higher, and certain limitations exist, for example, the high-temperature sintering has higher requirement on the heat resistance of a base material for bearing liquid metal droplets; the pressure sintering has higher requirements on the mechanical properties of the base material; potential safety hazards exist in laser sintering and the like.
Disclosure of Invention
The invention aims to provide a method for inducing fusion sintering of liquid metal micro-nano liquid drops by using solvent evaporation.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for inducing fusion sintering of liquid metal micro-nano droplets by solvent evaporation is characterized in that liquid metal micro-nano droplet dispersion liquid or liquid metal micro-nano droplet dispersion liquid containing an auxiliary agent is subjected to evaporation drying, and the sintering fusion is realized by using capillary force generated in the evaporation drying process.
Further, the following steps are carried out:
1) adding liquid metal into a dispersion solvent, and uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid;
or adding liquid metal into a dispersing solvent containing an auxiliary agent, and uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid;
or adding liquid metal into a dispersion solvent, uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid, adding an auxiliary agent into the dispersion liquid, and uniformly mixing for later use;
or adding liquid metal into a dispersing solvent containing an auxiliary agent, uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid, then adding the auxiliary agent into the dispersion liquid, and uniformly mixing for later use;
2) placing the dispersion liquid obtained in the step 1) on a substrate, evaporating the dispersion liquid, and drying to obtain the fused and sintered liquid metal and restore the conductivity of the fused and sintered liquid metal.
All methods reported or later reported for ultrasonication (Nano Letters,2011, 11: 5104), milling (Proceedings of the National Academy of Science of the United States of America, 2017, 114: 2143), microchannel extrusion (Advanced Functional Materials, 2012, 22: 2624), and the like can be utilized in the above process of obtaining the dispersion.
For example, ultrasonic methods (Advanced Functional Materials, 2018, 39: 1804197), are simple to operate, low in cost, and can produce liquid metal dispersions with particle sizes down to the nanometer level,
preferably, the power used for the ultrasound is more than or equal to 200W, such as 200W, 300W and 400W; the ultrasonic, stirring and oscillating ultrasonic time is more than 30s, preferably 10-60 min, such as 10min, 30min, 45min and 60 min; the time of sonication is preferably 60 min. The stirring speed is 100-3000 rpm, such as 500 rpm, 2000 rpm, 3000 rpm.
Obtained in the above step 1)An auxiliary agent can be added in the process of the liquid metal micro-nano liquid drop dispersion liquid, the auxiliary agent can achieve the effect of nano dispersion at the moment, the colloid stability is improved, the particle size is smaller in the nano process, the nano is promoted, the auxiliary agent is added in a form of dispersing to a dispersion solvent, and the final concentration of the auxiliary agent is generally 0.5-2 mg mL –1Preferably 0.5mg mL–1，0.8mg mL–1，1mgmL–1，1.5mg mL–1，1.7mg mL–1，2mg mL–1Etc.;
meanwhile, the auxiliary agent can be added after the ultrasonic treatment is finished, the addition form can be directly added or dispersed in a dispersion solvent for further complement, so that the capillary force generated by solvent evaporation can be increased in the evaporation sintering process, and the sintering and fusion of the liquid metal micro-nano liquid drops are promoted.
Furthermore, the auxiliary agent in the step 1) can be added before the ultrasonic treatment, after the ultrasonic treatment, or both before and after the ultrasonic treatment; the mass ratio of the liquid metal to the auxiliary agent is 50:1-5: 1; and it plays two roles of reducing the particle size and increasing the colloid stability; secondly, the capillary force in the evaporation process is increased, and sintering is promoted.
The dispersion solvent is water or a mixed solvent, and the mixed solvent is ethanol, acetone, methanol, dimethylformamide, tert-butanol or dimethyl sulfoxide and water; wherein the volume fraction of water in the mixed solvent is more than or equal to 40 percent.
Preferably water or a mixed solvent having a water content of 50% or more, for example, 90% by volume of water + 10% by volume of ethanol, 95% by volume of water + 5% by volume of acetone, 98% by volume of water + 2% by volume of dimethylsulfoxide, etc.; more preferably water.
The liquid metal can be added into an excessive amount of dispersion solvent, and the concentration range of the liquid metal is 5-100 mg mL–1；。
The auxiliaries in the dispersion solvent in the step 1) or the auxiliaries added after the formation of the nano-droplet dispersion liquid can be the same or different (the auxiliaries added before or after the ultrasound in the step 1) can be the same or different), and are selected from 2,2,6, 6-tetramethylpiperidine oxide (TEMPO) oxidized cellulose, Sodium Alginate (SA), Hyaluronic Acid (HA), sodium carboxymethylcellulose (CMC), quaternized chitosan (Qch), carboxylated Cellulose Nanofibers (CNF), Quaternized Cellulose Nanofibers (QCNF) or Silk Nanofibers (SNF).
The mass ratio of the liquid metal to the auxiliary agent is 50:1-5: 1; e.g., 20:1, 10:1, 5:1, etc.
The evaporation drying process is carried out under the pressure of-0.1-1 Mpa and at the temperature from the melting point of the alloy to the boiling point of the dispersion solvent. The temperature is preferably 0-100 ℃, such as 10 ℃, 30 ℃, 45 ℃, 60 ℃ and the like; the pressure is preferably-0.05 to 0.05MPa, for example-0.05 MPa, -0.025MPa, 0MPa, 0.05MPa, 0.05MPa or the like;
the liquid metal micro-nano liquid drop has the particle size of 5-100000 nm; wherein the liquid metal is selected from gallium (Ga), gallium and low melting point alloy, indium (In) or indium (In) and low melting point alloy.
The melting point of the low-melting-point alloy is less than or equal to 200 ℃.
The substrate is glass, quartz, mica, silicon chip, macromolecule or biological tissue; such as glass, quartz, mica sheets, silicon wafers, elastomers, biological tissues, microscopic tunnels and the like, all materials capable of carrying the evaporation of the liquid metal dispersion can be used as substrates;
the preparation method of the liquid metal micro-nano liquid drop can be all reported methods such as ultrasonic crushing, grinding, micro-channel extrusion and the like or reported later. If a dispersing aid is added during the dispersing process, and the dispersing aid and the evaporation sintering aid are superposed or play a similar role, the adding amount of the dispersing aid is taken into consideration and calculated when the evaporation sintering aid is added.
Compared with the prior art, the method for sintering the liquid metal micro-nano liquid drops by utilizing natural evaporation has the following advantages:
compared with the method for sintering the liquid metal by external force (such as mechanical pressure and laser sintering) after the ultrasonic treatment, the method has the unexpected effects of simplicity, good sintering effect, multiple purposes and the like.
The method has the advantages of simple operation, low energy consumption, low cost, good environment and practical and effective sintering of the liquid metal micro-nano droplets, and increases the capillary action force in the evaporation process by evaporating and drying the liquid metal micro-nano droplet dispersion liquid or further adding a chemical additive into the dispersion liquid and then evaporating and drying, so that the oxide layer on the surface of the micro-nano droplets is stressed and broken in the natural evaporation process, the sintering and fusion of the liquid metal micro-nano droplets are promoted, and the conductivity of the liquid metal micro-nano droplets is recovered.
The invention utilizes the chemical auxiliary agent to increase the capillary action in the evaporation process, so that the liquid metal droplets can be spontaneously fused and sintered under mild conditions to form a conductive path. The idea of adding the auxiliary agent into the liquid metal dispersion liquid to promote sintering is ingenious in design, simple to operate, low in cost, suitable for large-scale production, extremely low in substrate requirement, capable of being widely applied to the fields of printed circuits, packaging circuits, 3D printing electronic technology and the like, and conductive liquid metal (thin film) obtained through evaporation sintering can be used in the fields of optics, electronics, electromagnetic shielding, sensing, soft robots and the like.
Description of the drawings:
FIG. 1 is a view showing that the liquid metal film obtained in example 1 is used as an optical mirror material;
FIG. 2 is a scanning electron microscope image of a cross section of the sintered material obtained in example 2;
FIG. 3 is a scanning electron micrograph of a liquid metal droplet obtained in example 2;
FIG. 4 is a graph showing the effect of the sintered liquid metal material obtained in example 2 on electromagnetic shielding (different electromagnetic wave frequency band shielding);
FIG. 5 shows the sintered liquid metal of example 2 used as a package circuit;
FIG. 6 is a graph of the evaporative sintering of liquid metal on styrene-butadiene block copolymer (SEBS) as a stress sensor in example 3;
FIG. 7 shows the sintered liquid metal/cellulose bilayer film material obtained in example 4 used as an electric driver (the sintered liquid metal film is peeled off from the glass substrate to prepare a "U" shaped film, and a voltage of 0.5-2.0V is applied across the "U" shaped film to obtain an electric driver);
FIG. 8 shows the sintered liquid metal/cellulose bilayer film material obtained in example 4 used as an optical actuator.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
According to the method, the aim of sintering and fusing the micro-nano droplets is achieved by utilizing the capillary force generated by the liquid metal micro-nano droplet dispersion liquid in the solvent evaporation and drying process, and the size of the capillary force can be controlled by regulating and controlling the evaporation pressure and changing the composition and content of the dispersion liquid auxiliary agent in the process, so that the sintering process is regulated and controlled.
Example 1
1) 100mg of gallium-indium alloy (74.5 wt% of Ga and 24.5 wt% of In) is added into 10mL of deionized water, and ultrasonic treatment is carried out for 60min under the condition of ice-water bath by using an ultrasonic crusher with the power of 300W;
2) the gray solution obtained in step 1) was drop-coated onto a glass substrate and dry-sintered under vacuum (-0.1MPa) at room temperature (25 ℃) (see fig. 1).
By observing figure 1, the micro-nano liquid drops formed by adopting the water dispersion liquid metal are naturally dried at room temperature (25 ℃) under vacuum condition (-0.1MPa), the surface tension formed under the vacuum condition is increased, the capillary force generated in the drying process is further increased, the liquid metal liquid drops are promoted to be fused and sintered, a layer of liquid metal film is formed on the glass substrate, the upper side of the film presents dark gray, and the lower side close to the glass substrate presents bright silvery white, and the material can be used as a mirror surface material.
Example 2
1) Adding 100mg of gallium-indium alloy into 10mL of deionized water, and carrying out ultrasonic treatment for 60min under the condition of ice-water bath by using an ultrasonic crusher with the power of 300W;
2) adding 5mL of solution obtained in the step 1) with the concentration of 2mg mL–1TEMPO oxidized cellulose (carboxyl content 1.4mmol g)-1) Stirring the nanofiber solution for 30min to uniformly mix the nanofiber solution;
3) the gray solution obtained in step 2) was applied dropwise to a glass substrate and dried and sintered at room temperature (25 ℃) and atmospheric pressure (0.1MPa) (see fig. 2 to 4).
2-4, the micro-nano liquid drops are formed by adopting water dispersion liquid metal, then the cellulose nano-fibers oxidized by the aid of TEMPO are added, the average diameter of the uniformly mixed particles is 100nm, fiber winding is arranged outside the particles, and the added cellulose nano-fibers can increase capillary force in the evaporation process and promote fusion sintering of the liquid metal liquid drops. The liquid metal has shielding effect and can be used as an electromagnetic shielding material in military.
Example 3
1) 100mg of gallium-indium alloy is added into 10mL of gallium-indium alloy with the concentration of 1mg mL–1In the ethanol aqueous solution of the silk nano-fibers (the volume ratio of water to ethanol in the ethanol aqueous solution is 9:1), performing ultrasonic treatment for 60min under the condition of ice water bath by using an ultrasonic crusher with the power of 300W;
The preparation method of the silk nanofiber is disclosed in the literature (ACS Nano,2017,11, 8178).
2) After the ultrasonic treatment, magnetic stirring is carried out for 30min at the stirring speed of 1000 rpm, so that the silk nano-fibers and the liquid metal micro-nano particles are fully and uniformly mixed;
3) the resulting gray solution was drop-coated onto a polyethylene terephthalate (PET) film with a pattern, and dried under a vacuum of 0Mpa at a temperature of 30 c to form conductive paths on the PET film (see fig. 5).
It knows through scanning electron microscope analysis, adopt the disperse solvent dispersion liquid metal that contains auxiliary agent silk nanofiber to form and receive a little liquid drop, the particle diameter can be reduced through the nanocrystallization in the supersound process and promote stability, the average particle diameter size of the liquid metal that forms is 150nm, can increase the capillary force in its evaporation process through silk nanofiber simultaneously, and then promote the liquid metal sintering, form the double faced membrane, the membrane that forms belongs to the heterogeneous membrane of difference of upper and lower structure, the upper strata is the higher insulating layer of cellulose content, the lower floor is the conducting layer that liquid metal content is high. This material can be used as a self-sintered formed package circuit (fig. 5).
Example 4
1) 100mg of gallium-indium alloy is added into 10mL of alloy with the concentration of 1mg mL –1The TEMPO oxidized cellulose acetone aqueous solution (the volume ratio of water to acetone in the acetone aqueous solution is 9.5:0.5) is subjected to ultrasonic treatment for 60min under the condition of ice-water bath by using an ultrasonic crusher with the power of 200W;
2) adding 5mL of solution with the concentration of 1mg mL after the ultrasonic treatment–1The TEMPO oxidized cellulose water/acetone dispersion (volume ratio of water to acetone in acetone aqueous solution is 9.5:0.5) is magnetically stirred for 30min at a stirring speed of 2000 rpm to fully and uniformly mix the cellulose and the solvent;
3) the resulting gray solution was drop-coated onto a SEBS film with patterning and dried under a vacuum of-0.1 MPa to form a conductive film on the SEBS elastomer (see FIG. 6).
The observation shows that the dispersion solvent containing the auxiliary agent is adopted to disperse the liquid metal to form micro-nano droplets, and then TEMPO oxidized cellulose dispersion liquid is added, the first addition of the auxiliary agent dispersion liquid is beneficial to the nanocrystallization of the liquid metal to form droplets with the particle size of about 100nm, and the second addition of the auxiliary agent dispersion liquid can further increase the capillary force generated by the evaporation action through a separation liquid bridge to promote the sintering of the liquid metal; two layers of films are formed on the SEBS elastomer, wherein the upper layer is a heterogeneous film and the lower layer is a liquid metal coating, and the heterogeneous film on the upper layer contains an insulating layer with higher cellulose content and a conductive layer with high liquid metal content. The upper heterogeneous film can fall off in the stretching process, a uniform liquid metal coating is left on the SEBS elastomer, and the conductivity of the SEBS elastomer is regularly changed in the stretching process. This material can be used as a stress sensor (fig. 6).
Example 5
1) 150mg of gallium-indium alloy is added into 15mL of alloy with the concentration of 1.5mg mL–1The sodium alginate dimethyl sulfoxide aqueous solution (water in the dimethyl sulfoxide aqueous solution: dimethyl sulfoxide is 9.8:0.2) is subjected to ultrasonic treatment for 30min under the condition of ice-water bath by using an ultrasonic crusher with the power of 300W;
2) the obtained gray solution is dripped on a glass substrate and dried under the condition that the vacuum degree is minus 0.05 Mpa;
3) after drying, the film was peeled off from the glass substrate to form heterogeneous films having different gloss on both sides (see fig. 7 and 8).
Analysis shows that the dispersion liquid containing sodium alginate is adopted to disperse liquid metal to form micro-nano liquid drops, then the auxiliary agent is added, so that liquid drops with uniform particle size (about 150nm) can be formed firstly, and then the fibers and the liquid metal are combined more tightly in the evaporation process through the viscosity action of the sodium alginate, so that the capillary force in the evaporation process is further increased, and the sintering of the liquid metal is promoted; the front and back surfaces of the heterogeneous film formed on the glass substrate have great difference, one surface has higher cellulose content and is gray, the other surface has higher liquid metal content and is silver white, the surface with higher gray cellulose content is electrically insulated, and the other surface of the silver white liquid metal has metal conductivity. Such heterogeneous membranes can be used as actuators, humidity sensors, and the like.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (9)
1. A method for inducing fusion sintering of liquid metal micro-nano liquid drops by solvent evaporation is characterized by comprising the following steps: and (3) evaporating and drying the liquid metal micro-nano droplet dispersion liquid or the liquid metal micro-nano droplet dispersion liquid containing the auxiliary agent, and realizing sintering and fusion by using the capillary force generated in the evaporation and drying process.
2. The method for inducing fusion sintering of liquid metal micro-nano droplets by using solvent evaporation according to claim 1, wherein the method comprises the following steps:
1) adding liquid metal into a dispersion solvent, and uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid;
or adding liquid metal into a dispersing solvent containing an auxiliary agent, and uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid;
Or adding liquid metal into a dispersion solvent, uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid, adding an auxiliary agent into the dispersion liquid, and uniformly mixing for later use;
or adding liquid metal into a dispersing solvent containing an auxiliary agent, uniformly mixing and dispersing to obtain a liquid metal micro-nano droplet dispersion liquid, then adding the auxiliary agent into the dispersion liquid, and uniformly mixing for later use;
2) placing the dispersion liquid obtained in the step 1) on a substrate, evaporating the dispersion liquid, and drying to obtain the fused and sintered liquid metal and restore the conductivity of the fused and sintered liquid metal.
3. The method according to claim 1, wherein the dispersing solvent is water or a mixed solvent, and the mixed solvent is ethanol, acetone, methanol, dimethylformamide, t-butanol or dimethylsulfoxide mixed with water; wherein the volume fraction of water in the mixed solvent is more than or equal to 40 percent.
4. The method of claim 1 or 2, wherein the auxiliary agent in the dispersion solvent of step 1) or the auxiliary agent added after forming the nanoparticle dispersion may be the same or different and is selected from the group consisting of 2,2,6, 6-tetramethylpiperidine oxide (TEMPO) -oxidized cellulose, Sodium Alginate (SA), Hyaluronic Acid (HA), sodium carboxymethylcellulose (CMC), quaternized chitosan (qcch), carboxylated Cellulose Nanofibers (CNF), Quaternized Cellulose Nanofibers (QCNF) and Silk Nanofibers (SNF).
5. The method of claim 4, wherein the mass ratio of liquid metal to adjuvant is from 50:1 to 5: 1.
6. The method according to claim 1 or 2, wherein the evaporation drying process is an evaporation drying process performed at a pressure of-0.1 to 1MPa and at a temperature within a range from a melting point of the alloy to a boiling point of the dispersion solvent.
7. The method of claim 1 or 2, wherein the liquid metal micro-nano droplet has a particle size of 5-100000 nm; wherein the liquid metal is selected from gallium (Ga), gallium and low melting point alloy, indium (In) or indium (In) and low melting point alloy.
8. The method of claim 7, wherein said low melting point alloy has a melting point of 200 ℃ or less.
9. The method of claim 2, wherein the substrate is glass, quartz, mica, a silicon wafer, a polymer, or a biological tissue.
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