CN110655827A - Micron or nano-scale liquid metal water-based dispersion liquid and preparation method thereof - Google Patents
Micron or nano-scale liquid metal water-based dispersion liquid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of liquid metal dispersion liquid, in particular to a micron or nano liquid metal water-based dispersion liquid which is prepared and stably stored by using microgel as a protective layer and a preparation method thereof. Adding liquid metal into the soluble natural polymer dispersion liquid, uniformly mixing, and performing low-temperature ultrasonic cavitation to obtain a uniformly dispersed dispersion liquid with uniform particle size; wherein the soluble natural polymer dispersion liquid consists of soluble polymer and water-based solution; wherein the soluble polymer is one or more of Sodium Alginate (SA), Hyaluronic Acid (HA), sodium carboxymethylcellulose (CMC), and quaternized chitosan (Qch). The liquid metal dispersion liquid prepared by the method has the characteristics of high preparation efficiency, adjustable particle size, stable dispersion, long-term storage, high biocompatibility and the like. Can be used as conductive "ink" and used in the fields of printed electronics, wearable sensors, actuators, or biomedical conductive parts.
Description
Technical Field
The invention relates to a preparation method of liquid metal dispersion liquid, in particular to a micron or nano liquid metal water-based dispersion liquid which is prepared and stably stored by using microgel as a protective layer and a preparation method thereof.
Background
The liquid metal is a pure metal or an alloy which is in a liquid state at normal temperature, and the liquid metal is widely applied to the field of flexible electronics because the liquid metal is easy to deform under the action of external force and has good fluidity. In addition, liquid metal has a series of excellent characteristics, such as low vapor pressure, low toxicity, high conductivity, low viscosity, etc., so that it has wide applications in stretchable electronics, chemical sensors, micro-switches, 3D printed structures, conductive composites, ink-jet printing inks, 3D micro-electrodes, etc., and is one of the research hotspots of current new material science.
Because the surface tension of the liquid metal is higher (for example, the surface tension of the gallium-indium alloy is 624mN m-1) The affinity on different substrates is low and a continuous conductive path cannot be formed. Therefore, the method of preparing metal particle micro-nano and then preparing conductive ink is a method for developing printing electrons. For example, the document (Advanced Materials,2015,27(14): 2355) discloses that conductive functional gloves are prepared by dispersing liquid gallium indium alloy in ethanol solution containing surfactant (ethyl 3-mercaptopropionate) by an ultrasonic method and then by a pressure sintering method. However, the prepared liquid metal dispersion is unstable and undergoes physical sedimentation and chemical deterioration when stored in air for a long time; the used dispersion liquid contains an organic solvent with high toxicity, so that the use process is dangerous; and a film prepared by the drop coating method may have minute cracks therein.
According to the search and discovery of the prior art, patent document No. CN 103068939A published as 2013-04-24 discloses a preparation method of liquid metal emulsion, which comprises the following steps: introducing liquid metal into a solvent, heating, adding a surfactant, and performing ultrasonic reaction to obtain a liquid metal emulsion, wherein the liquid metal is gallium, indium and an alloy thereof, and the solvent is a solvent of alkyl mercaptan. However, the prior art has the defects and disadvantages that the solvent is high in toxicity and poor in stability, and is not easy to further process and use subsequently.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the micron or nano-scale liquid metal water-based dispersion which is prepared and stably stored by using the microgel as the protective layer, has simple operation and low cost, can be stored for a long time and is convenient for industrial production, and the preparation thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing micron or nanometer liquid metal water-based dispersion liquid comprises adding liquid metal into soluble natural polymer dispersion liquid, mixing, and subjecting to low temperature ultrasonic cavitation to obtain uniform dispersion liquid with uniform particle size; wherein the soluble natural polymer dispersion liquid consists of soluble polymer and water-based solution; wherein the soluble polymer is one or more of Sodium Alginate (SA), Hyaluronic Acid (HA), sodium carboxymethylcellulose (CMC), and quaternized chitosan (Qch); when mixing, the polymer with the same charge is mixed and used in any proportion; or, polymers with different charges are mixed, and when the polymers with any one charge are mixed, the polymers with any one charge are added in excess.
Furthermore, gel (crosslinking) factors can be added into the soluble natural polymer dispersion liquid in the ultrasonic dispersion process, so that the gel crosslinking is more compact; wherein the gel factor is one or more of gallium ion, indium ion, tin ion, calcium ion, iron ion, glutaraldehyde, formaldehyde, epichlorohydrin, ethylenediamine and phytic acid; the addition amount of the gelator is 0.001-10 wt% of the addition amount of the natural high polymer;
the preparation method comprises the following steps:
1) dispersing the soluble natural polymer in a water-based solution to obtain a dispersion having a mass concentration of 0.001 wt% to 20 wt%, for example, 0.005%, 0.01%, 0.05%, 0.1%, 0.3%, 0.6%, 0.9%, 1%, 3%, 10%, etc.;
2) adding liquid metal into the dispersion liquid obtained in the step 1) and uniformly mixing; wherein the mass ratio of the state metal to the soluble polymer is 100:1-2: 1;
3) splitting the liquid metal in the uniformly mixed solution obtained in the step 2) at a low temperature by an ultrasonic cavitation method to form micro or nano spheres;
4) removing larger particles from the dispersion liquid obtained by the ultrasonic treatment in the step 3) through centrifugation to obtain the dispersion liquid with uniform particle size and uniform dispersion.
In the invention, soluble natural polymers and water or a mixed solvent thereof are uniformly mixed, and then liquid metal is added for ultrasonic dispersion, so that the natural polymers are uniformly dispersed as much as possible to obtain a uniformly distributed solution, in the dispersion process, the liquid metal can be subjected to ultrasonic cavitation to form nano particles, and the natural polymers can form crosslinking with metal ions escaping from the liquid metal to form a protective layer in a microgel mode, so that the nano particles are prevented from further reacting with the water and oxygen in the water, and the effect of protecting the liquid metal micro-nano particles is achieved. The effect of the natural polymer can be seen: one itself can form a stable solution; and the second one can cross-link with metal ion in solution to form protecting microgel layer.
The dispersion liquid which is obtained after larger particles are removed by centrifugation and has uniform particle size and uniform dispersion and can be stored for a long time under the inert gas is filled with the inert gas in a container, and the dispersion liquid is sealed for long-term storage after oxygen is discharged; wherein, the inert gas is one or two of nitrogen, helium or argon.
The water-based solution is a mixed solution of water, water and an organic solvent, and the pH value of the water-based solution is controlled to be between 4 and 10; wherein the organic solvent is one or more of ethanol, glycerol, ethylene glycol, acetone, dimethyl sulfoxide, dimethylformamide, dimethylacetamide and the like; preferably pure water or a mixed solution having a water volume fraction of 50% or more (for example, 90% water by volume + 10% ethanol by volume, 95% water by volume + 5% acetone by volume, 98% water by volume + 2% dimethylsulfoxide by volume, etc.).
The low temperature and ultrasonic cavitation are 0-70 ℃, the ultrasonic power is more than or equal to 100W (such as 200W, 250W, 300W, 400W and the like), and the ultrasonic time is more than or equal to 30s, preferably 10-60 min (such as 10min, 45min, 60min and the like).
The liquid metal is a liquid metal simple substance or an alloy of the liquid metal, and the melting point of the liquid metal is 0-100 ℃.
The liquid metal is selected from gallium (Ga), indium (In), mercury (Hg) or alloys of the metals, wherein the alloys may be gallium indium alloy (Ga 75%, In 25%), gallium indium tin alloy (Ga 68.5%, In 21.5%, tin 10%) and the like.
The centrifugation is performed at a rotation speed of 1-2000 rpm (e.g. 1500 rpm, 1000 rpm, 500 rpm, etc.), and the centrifugation time is 5-10min (e.g. 5min, 10min, etc.).
The micron or nanometer liquid metal water-based dispersion liquid is prepared according to the recording mode, and the internal particle parameters of the micron or nanometer liquid metal water-based dispersion liquid are characterized as follows: the particle size is 5nm-50 μm, and the shell thickness is 0.01nm-500 nm.
Wherein the metal water-based dispersion liquid with the particle size of 5-100nm can be applied to ink for ink-jet printing.
The metal water-based dispersion liquid with the particle size of 100nm-1 mu m can be applied to the preparation of conductive fillers and is used in the fields of sensing and the like.
The metal water-based dispersion with the particle size of 1-50 mu m can be applied to dielectric elastomer fillers.
Compared with the prior art, the method for preparing the liquid metal dispersion liquid has the following advantages:
the invention utilizes the soluble natural polymer solution as the dispersant, plays a role in solvent dispersion and a role in protecting a microgel shell layer, and combines dispersion and protection together to obtain the liquid metal dispersion liquid which has the characteristics of controllable metal particles, good stability, long-term preservation and good biocompatibility.
Drawings
FIG. 1 is a scanning electron micrograph of nanoparticles in a liquid metal dispersion obtained in example 1;
FIG. 2 is a magnified scanning electron microscope image of nanoparticles in the liquid metal dispersion obtained in example 1;
FIG. 3 is a projection electron microscope (TEM) image of nanoparticles of the liquid metal dispersion obtained in example 1;
FIG. 4 is an X-ray diffraction (XRD) pattern of the liquid metal dispersion obtained in example 1 during storage for various periods of time, showing no significant chemical change during long-term storage;
FIG. 5 is a graph showing the rate of change in resistance at different degrees of compression after the polyurethane foam is impregnated with the liquid metal dispersion obtained in example 1 and dried;
FIG. 6 is an exemplary view of the liquid metal dispersion obtained in example 1 after being impregnated with polyurethane foam and dried for use as a finger bend sensor;
FIG. 7 is a scanning electron micrograph of nanoparticles in a liquid metal dispersion obtained in example 2;
FIG. 8 shows the liquid metal dispersion obtained in example 1 used as an ink for ink jet printing: a example commercial printer (Canon iP 1188); b, printed characters;
FIG. 9 is a scanning electron micrograph of nanoparticles in the liquid metal dispersion obtained in example 3.
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.
The invention relates to a method for coating the surface of liquid metal by utilizing natural polymers so as to disperse and stabilize a solvent, which is characterized in that gallium-indium alloy or other liquid metals are subjected to ultrasonic treatment in water or a composite solvent thereof, and the surface of the liquid metal is coated by the gelation of the natural polymers so as to protect dispersed microscopic liquid metal particles. The liquid metal dispersion liquid prepared by the method has the characteristics of high preparation efficiency, adjustable particle size, stable dispersion, long-term storage, high biocompatibility and the like. Can be used as conductive "ink" and used in the fields of printed electronics, wearable sensors, actuators, or biomedical conductive parts.
Example 1
A method of preparing a shelf-stable liquid metal dispersion comprising the steps of:
1) dissolving 90mg of sodium alginate in 15mL of water, and shaking to uniformly mix the sodium alginate and the water to obtain a sodium alginate water solution with the mass fraction of 0.6%;
2) adding 150mg of gallium-indium alloy into the sodium alginate aqueous solution, and carrying out ultrasonic treatment for 15min in a water bath at 20 ℃ by using an ultrasonic crusher with the power of 200W;
3) putting the gray solution obtained in the step 2) into a centrifugal tube, and centrifuging for 10min under the condition that the rotating speed is 1000 r/min;
4) putting the supernatant obtained in the step 3) into a sample bottle, introducing nitrogen for 15min, discharging oxygen inside, and sealing for storage (see fig. 1-4).
Analysis by scanning electron microscopy, transmission electron microscopy and XRD from figures 1-4 shows that: the liquid metal dispersion obtained in this example had an average particle diameter of 200nm and a microgel protective layer (. about.20 nm) on the outside, and it was possible to prevent the deterioration of the metal inside by reaction with oxygen and water and to stably store it for 2 months under an inert gas (Ar). The material with smaller particle size can be filled into a microporous elastomer (such as sponge), metal nano-droplets are fused by external pressure, and the material shows resistance property which changes along with the difference of the magnitude of the external pressure, and is further used as a sensor material (figures 5 and 6).
In the ultrasonic process, an additional cross-linking agent (such as divalent or polyvalent metal ions Ca2+) can be added to ensure that the alginate on the outer layer is more firmly cross-linked, thereby achieving a similar dispersion effect.
Example 2
A method of preparing a shelf-stable liquid metal dispersion comprising the steps of:
1) dissolving 15mg of sodium alginate in 15mL of water, and shaking to uniformly mix the sodium alginate and the water to obtain a sodium alginate water solution with the mass fraction of 0.1%;
2) adding 150mg of gallium-indium alloy into the sodium alginate aqueous solution, and carrying out ultrasonic treatment for 30min in a water bath at 20 ℃ by using an ultrasonic crusher with the power of 300W;
3) putting the gray solution obtained in the step 2) into a centrifugal tube, and centrifuging for 10min under the condition that the rotating speed is 1000 r/min;
4) putting the supernatant obtained in the step 3) into a sample bottle, introducing nitrogen for 15min, and discharging oxygen inside to perform sealed storage.
Analysis by scanning electron microscopy fig. 7 shows: the liquid metal dispersion obtained in this example had an average diameter of 100nm and a microgel protective layer on the outside, and was able to prevent the metal inside from being deteriorated by reaction with oxygen and water and to be used in an inert gas (N is an inert gas)2) The product can be stored stably for 2 months. The material has particle size in nanometer range, uniform dispersibility and solution dispersion stability, and can be used as electronic ink for printing various patterns or characters, and can be further sintered under pressure for use as circuit (FIG. 8).
Sodium alginate in the above examples can be mixed with hyaloplasm (a substance having the same charge) in any ratio and added to water, and then the metal is added thereto, and a dispersion having the same effects as described above can be obtained.
Example 3
A method of preparing a shelf-stable liquid metal dispersion comprising the steps of:
1) dissolving 45mg of sodium carboxymethylcellulose in 15mL of water, and shaking to uniformly mix the sodium carboxymethylcellulose and the water to obtain a sodium carboxymethylcellulose aqueous solution with the mass fraction of 0.3%;
2) adding 150mg of gallium-indium alloy into the sodium carboxymethylcellulose aqueous solution, and carrying out ultrasonic treatment for 30min in an ice-water mixed bath by using an ultrasonic crusher with the power of 200W;
3) putting the gray solution obtained in the step 2) into a centrifugal tube, and centrifuging for 10min under the condition that the rotating speed is 1000 r/min;
4) putting the supernatant obtained in the step 3) into a sample bottle, introducing nitrogen for 15min, and discharging oxygen inside to perform sealed storage.
Analysis by scanning electron microscopy fig. 9 shows: the liquid metal dispersion obtained in this example had an average diameter of 150nm and a microgel protective layer (. about.10 nm) on the outside, and was stable under an inert gas atmosphere (Ar) for 3 months while preventing the deterioration of the metal in the interior due to the reaction with oxygen and water. Because the gel protective layer is thin, the material can be doped in the elastomer, the modulus of the matrix material is less influenced, and therefore the dielectric elastomer material can be prepared.
Example 4
A method of preparing a shelf-stable liquid metal dispersion comprising the steps of:
1) dissolving 450mg of sodium carboxymethylcellulose in 15mL of water, and shaking to uniformly mix the sodium carboxymethylcellulose and the water to obtain a sodium carboxymethylcellulose aqueous solution with the mass fraction of 3%;
2) adding 150mg gallium metal into the sodium carboxymethylcellulose water solution, and performing ultrasonic treatment in a water bath at 60 ℃ for 1min by using an ultrasonic crusher with the power of 200W;
3) putting the gray solution obtained in the step 2) into a centrifugal tube, and centrifuging for 10min under the condition that the rotating speed is 1000 r/min;
4) and (4) putting the supernatant obtained in the step (3) into a sample bottle, introducing nitrogen for 15min, and discharging oxygen inside to perform sealed storage.
Analysis by scanning electron microscopy fig. 9 shows: the liquid metal dispersion obtained in this example had an average diameter of 2 μm and a microgel protective layer (. about.10 nm) on the outside, and was stable under an inert gas atmosphere (Ar) for 6 months while preventing the deterioration of the metal in the interior due to the reaction with oxygen and water. Because the particle size is larger, the gel protective layer is relatively thinner and has more droplet properties, and the material can be doped in an elastomer to prepare a low-modulus dielectric elastomer material.
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 (10)
1. A method for preparing micron or nano-scale liquid metal water-based dispersion liquid is characterized by comprising the following steps: adding liquid metal into the soluble natural polymer dispersion liquid, uniformly mixing, and performing low-temperature ultrasonic cavitation to obtain a uniformly dispersed dispersion liquid with uniform particle size; wherein the soluble natural polymer dispersion liquid consists of soluble polymer and water-based solution; wherein the soluble polymer is one or more of Sodium Alginate (SA), Hyaluronic Acid (HA), sodium carboxymethylcellulose (CMC), and quaternized chitosan (Qch).
2. The method of preparing a micro-or nano-sized aqueous liquid metal dispersion according to claim 1, wherein: the soluble natural polymer dispersion liquid is the mixture of soluble polymer and gelator; wherein the gelator is one or more of gallium ion, indium ion, tin ion, calcium ion, iron ion, glutaraldehyde, formaldehyde, epichlorohydrin, ethylenediamine and phytic acid.
3. The process for the preparation of aqueous micro-or nano-sized liquid metal dispersions according to claim 1 or 2, characterized in that:
1) dispersing soluble natural macromolecules into a water-based solution to obtain a dispersion liquid with the mass concentration of 0.001-20 wt%;
2) adding liquid metal into the dispersion liquid obtained in the step 1) and uniformly mixing; wherein the mass ratio of the liquid metal to the soluble polymer is 100:1-2: 1;
3) splitting the liquid metal in the uniformly mixed solution obtained in the step 2) at a low temperature by an ultrasonic cavitation method to form micro or nano spheres;
4) removing larger particles from the dispersion liquid obtained by the ultrasonic treatment in the step 3) through centrifugation to obtain the dispersion liquid with uniform particle size and uniform dispersion.
4. A method for preparing a micro-or nano-sized aqueous liquid metal dispersion according to claim 3, wherein: and after larger particles are removed by centrifugation, the obtained dispersion liquid has uniform particle size and uniform dispersion, can be stored for a long time under the inert gas, and is sealed for long-term storage after oxygen is discharged.
5. A method for preparing a micro-or nano-sized aqueous liquid metal dispersion according to claim 1 or 3, characterized in that: the water-based solution is a mixed solution of water, water and an organic solvent, and the pH value of the water-based solution is controlled to be between 4 and 10; wherein the organic solvent is one or more of ethanol, glycerol, ethylene glycol, acetone, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, etc.
6. A method for preparing a micro-or nano-sized aqueous liquid metal dispersion according to claim 1 or 3, characterized in that: the low-temperature ultrasonic cavitation is 0-70 ℃, the ultrasonic power is more than or equal to 100W, and the ultrasonic time is more than or equal to 30 s.
7. A method for preparing a micro-or nano-sized aqueous liquid metal dispersion according to claim 1 or 3, characterized in that: the liquid metal is a liquid metal simple substance or an alloy of the liquid metal, and the melting point of the liquid metal is 0-100 ℃.
8. The method of preparing a micro-or nano-scale aqueous liquid metal dispersion according to claim 7, wherein: the liquid metal is selected from gallium (Ga), indium (In), mercury (Hg) or alloys of said metals.
9. A method for preparing a micro-or nano-sized aqueous liquid metal dispersion according to claim 3, wherein: the rotation speed of the centrifugation is 1-2000 r/min, and the centrifugation time is 5-10 min.
10. The micro-or nano-sized liquid metal water-based dispersion prepared according to claim 1, wherein: a micro-or nano-sized aqueous dispersion of a liquid metal, prepared in the manner described in claim 1, having internal particle parameters characterized by: the particle size is 5nm-50 μm, and the shell thickness is 0.01nm-500 nm.
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| CN117866484A (en) * | 2024-03-12 | 2024-04-12 | 成都先进金属材料产业技术研究院股份有限公司 | Liquid metal printing ink and preparation method thereof |
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