CN112876731A - Method for constructing anisotropic conductive hydrogel based on bidirectional freezing - Google Patents
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Abstract
The invention discloses a method for constructing anisotropic conductive hydrogel based on two-way freezing, which comprises the steps of firstly uniformly mixing sodium alginate and silver nanowires, then forming a long-range ordered silver nanowire-sodium alginate aerogel substrate with a layered structure by the two-way freezing method, and then adding a monomer and a cross-linking agent into the aerogel to construct the hydrogel with the layered structure.
Description
Technical Field
The invention relates to a method for constructing anisotropic conductive hydrogel based on bidirectional freezing, belonging to the technical field of nano materials.
Background
With the increasing demand for environmental protection, hydrogels containing water as the main component are becoming excellent candidates for sustainable materials, and hydrogels are water-containing materials with three-dimensional network structure and strong competitors of future artificial biomaterials due to their natural flexibility and excellent mechanical properties. Meanwhile, with the increasing requirements of people on electronic products, the development of flexible bendable electronic devices has become a mainstream consensus, the combination of conductive materials and materials with excellent mechanical properties such as hydrogel is an important direction for developing flexible conductive materials, silver nanowires are conductive nano materials with excellent conductivity, and the combination of silver nanowires and hydrogel is an important way for solving the problem of flexible conductive materials.
The structure of biological tissues such as muscles and tendons in the biological tissues has a highly ordered anisotropic structure, so that the biological tissues have more excellent performance, and meanwhile, the requirement of anisotropy is provided for conductive materials in some fields. The anisotropy of the material is a basic way to realize from the construction of an ordered structure, and the bidirectional freezing orientation is an effective method for constructing the ordered structure. The silver nanowire-sodium alginate aerogel with long-range order and excellent conductivity is obtained by bidirectional freezing, and the aerogel is filled to obtain the conductive hydrogel with anisotropy, so that the conductive hydrogel is applied to some special environment requirements.
Disclosure of Invention
The invention aims to provide a method for constructing anisotropic conductive hydrogel based on bidirectional freezing. According to the invention, a long-range ordered three-dimensional layered network structure is formed by a method of bidirectionally freezing silver nanowires and sodium alginate, and then a hydrogel network is introduced by filling hydrogel, so that the obtained conductive hydrogel has excellent performances such as electrical conductivity, compressive stress anisotropy and the like.
The invention relates to a method for constructing anisotropic conductive hydrogel based on bidirectional freezing, which comprises the steps of firstly uniformly mixing sodium alginate and silver nanowires, then forming a long-range ordered silver nanowire-sodium alginate aerogel substrate with a layered structure by a bidirectional freezing method, and then adding a monomer and a cross-linking agent into the aerogel substrate to construct the hydrogel with the layered structure. Due to the fact that silver nanowires exist in aerogel walls and the structure of the initial aerogel is not damaged after hydrogel is filled subsequently, the prepared hydrogel has good conductivity, and due to the fact that the hydrogel has a long-range ordered layered structure, stress parallel to the layered direction and stress perpendicular to the layered direction are different, and anisotropy performance is further shown.
The invention relates to a method for constructing anisotropic conductive hydrogel based on bidirectional freezing, which comprises the following steps:
step 1: and synthesizing the silver nanowires. Firstly 5.86g MwAdding 40000 parts of polyvinylpyrrolidone into 190ml of glycerol solution, uniformly stirring, and heating in a microwave for 10min to completely dissolve the polyvinylpyrrolidone; then cooling to room temperature, pouring into a 250ml three-neck flask, sequentially adding a mixed solution of 1.58g of silver nitrate, 10ml of glycerol and prepared 0.5ml of deionized water 59mg of sodium chloride, and then heating to 210 ℃ within 20min while controlling the stirring speed to be 50 rpm; after the reaction is finished, pouring the mixture into a 500ml beaker, adding deionized water with the same volume, cooling, centrifuging twice, and dispersing and fixing the volume.
In the step 1, the length of the synthesized silver nanowire is 7-15 μm, and the diameter is 60-100 nm;
step 2: putting 1.2g of sodium alginate powder into a 50ml beaker, adding 30ml of deionized water, and then carrying out magnetic stirring for 8 hours to obtain a 40mg/ml uniform sodium alginate solution.
And step 3: taking 20ml of silver nanowire with the mass concentration of 40mg/ml and 20ml of sodium alginate solution with the mass concentration of 40mg/ml, mixing the two solutions, magnetically stirring for 30min, placing the uniformly mixed solution in a bidirectional freezing mould, adjusting the freezing rate to be 14 mu m/min, and freeze-drying the solution in a freeze-drying machine for 48h after the solution is completely frozen, wherein the freezing temperature is-40 ℃. And taking out to obtain the silver nanowire-sodium alginate aerogel substrate.
And 4, step 4: sequentially and respectively dissolving 1g of monomer N-isopropyl acrylamide, 2mg of cross-linking agent methylene bisacrylamide and 20mg of initiator potassium persulfate in 5ml of deionized water, carrying out ice bath for 30min, and then adding 20 mu l of catalyst tetramethyl ethylenediamine into the mixed solution in the ice bath; and (3) placing the silver nanowire-sodium alginate aerogel substrate obtained in the step (3) in a hydrogel precursor solution, and standing for 48 hours (keeping the ice bath state for the first two hours and then taking out at room temperature) to obtain the conductive hydrogel with the anisotropic property.
The hydrogel precursor solution is a mixed solution consisting of a monomer, an initiator, a cross-linking agent, a catalyst and deionized water. The mass added by the catalyst addition is not counted in the total mass of the hydrogel precursor solution.
The invention has the beneficial effects that:
when the conductive hydrogel is prepared, based on a bidirectional freezing preparation method, firstly, a long-range ordered aerogel support is formed by bidirectional freezing silver nanowires-sodium alginate; the hydrogel precursor solution is then soaked to introduce the aqueous polymer network. Therefore, through the interaction between sodium alginate and polymer chains, the anisotropic conductive hydrogel constructed based on bidirectional freezing has excellent compressive stress anisotropy and conductive performance, namely, at the compressive strain of 30%, the stress in the direction vertical to the laminated structure is about 3 times of the stress in the direction parallel to the laminated structure, and the conductivity in the direction parallel to the laminated structure (92S/m) is about 2.6 times of the conductivity in the direction vertical to the laminated structure (35S/m).
In conclusion, the invention provides a preparation method of a brand-new anisotropic conductive hydrogel, and the method provides a brand-new thought and theoretical basis for the synthesis and special performance of conductive hydrogel materials.
Drawings
Fig. 1 is a transmission electron microscope photograph of silver nanowires prepared according to the present invention. It can be seen from fig. 1 that the silver nanowires prepared by the present invention are uniformly distributed.
Fig. 2 is a scanning electron microscope photograph of the silver nanowire-sodium alginate aerogel substrate prepared according to the present invention. It can be seen from fig. 2 that the aerogel support has a long-range ordered layered structure, which facilitates the realization of anisotropic properties of the material from both directions parallel to the layer and perpendicular to the layer.
FIG. 3 is a scanning electron micrograph of an aerogel substrate prepared according to the present invention after being filled with a hydrogel. It can be seen from figure 3 that the original aerogel scaffold in the filled hydrogel remained intact, which gives a structural basis for the excellent conductivity of the hydrogel, which is a surface topography map of the sample prepared in example 2.
FIG. 4 is an optical diagram showing the electrical conductivity of the hydrogel prepared in accordance with the present invention. It can be seen from fig. 4 that the hydrogel has good electrical conductivity.
FIG. 5 is a graph showing the anisotropy of compressive stress in the direction parallel to the layered structure and in the direction perpendicular to the layered structure of the hydrogel prepared according to the present invention, from which it can be seen that the compressive stress in the direction perpendicular to the layered structure is about 3 times that in the direction parallel to the layered structure, which corresponds to the sample prepared in example 1 below.
FIG. 6 is a graph showing the anisotropy of compressive stress in the direction parallel to the layered structure and in the direction perpendicular to the layered structure of the hydrogel prepared according to the present invention, from which it can be seen that the compressive stress in the direction perpendicular to the layered structure is about 1.9 times the compressive stress in the direction parallel to the layered structure, which corresponds to the sample prepared in example 2 below. Since the sample prepared in example 1 has a more excellent layered structure than the sample prepared in example 2, the compressive stress anisotropy performance is more pronounced.
FIG. 7 is a scan of the hydrogel prepared in example 1, from which it can be seen that the layered structure of the aerogel remains intact after filling with the hydrogel.
Fig. 8 is a graph of performance when applied as a sensor, from which it can be seen that the sample has different relative resistance changes at different compressive strains.
Detailed Description
The following examples illustrate the invention in detail. The reagent raw materials and equipment used in the invention are all commercially available products and can be purchased in the market.
Example 1:
1. firstly 5.86g Mw190ml of glycerol were added to 40000 g of polyvinylpyrrolidoneStirring the solution uniformly, heating the solution in a microwave for 10min to completely dissolve the polyvinylpyrrolidone. Then the temperature is reduced to room temperature, the mixture is poured into a 250ml three-neck flask, 1.58g of silver nitrate is sequentially added into the three-neck flask, 10ml of glycerol and prepared mixed solution of 0.5ml of deionized water and 59mg of sodium chloride are added into the three-neck flask, the temperature is increased to 210 ℃ along with 20min, and the stirring speed is controlled to be 50 rpm. After the reaction is finished, pouring the mixture into a 500ml beaker, adding deionized water with the same volume, cooling, then carrying out 6000rpm, centrifuging twice for 10min, and dispersing and fixing the volume.
2. Putting 1.2g of sodium alginate powder into a 50ml beaker, adding 30ml of deionized water, and then carrying out magnetic stirring for 8 hours to obtain a 40mg/ml uniform sodium alginate solution.
3. And taking 20ml of 50mg/ml silver nanowires, adding 20ml of sodium alginate dispersion liquid with the mass concentration of 40mg/ml, uniformly stirring by magnetic force, taking a small part of mixed liquid by a suction pipe, dripping the small part of mixed liquid into a mould, adjusting the freezing speed to be 14 mu m/min, putting the mixed liquid into a freeze dryer for freeze drying after complete freezing, wherein the freezing temperature is-40 ℃, and taking out the mixed liquid after 48 hours to obtain the silver nanowire-sodium alginate aerogel substrate.
4. 1g N-isopropyl acrylamide, 2mg methylene bisacrylamide and 20mg potassium persulfate are sequentially and respectively dissolved in 5ml deionized water, then ice bath is carried out for 30min, and then 20 mu l tetramethyl ethylenediamine is added into the mixed solution after the ice bath. And (3) placing the aerogel obtained in the step (3) in a hydrogel precursor solution, and standing for 48 hours (keeping the ice bath state for the first two hours, and then taking out at room temperature) to obtain the conductive hydrogel with anisotropic performance.
Example 2:
1. firstly 5.86g MwThe polyvinylpyrrolidone (40000) is added into 190ml of glycerol solution, stirred uniformly and heated in a microwave for 10min to completely dissolve the polyvinylpyrrolidone. Then the temperature is reduced to room temperature, the mixture is poured into a 250ml three-neck flask, 1.58g of silver nitrate is sequentially added into the three-neck flask, 10ml of glycerol and prepared mixed solution of 0.5ml of deionized water and 59mg of sodium chloride are added into the three-neck flask, the temperature is increased to 210 ℃ along with 20min, and the stirring speed is controlled to be 50 rpm. After the reaction was completed, the mixture was poured into a 500ml beaker, and addedAnd (3) carrying out centrifugation twice at 6000rpm for 10min after the temperature is reduced by using deionized water with the volume, and dispersing and fixing the volume.
2. Putting 1.2g of sodium alginate powder into a 50ml beaker, adding 30ml of deionized water, and then carrying out magnetic stirring for 8 hours to obtain a 40mg/ml uniform sodium alginate solution.
3. And taking 20ml of 20mg/ml silver nanowires, adding 20ml of sodium alginate dispersion liquid with the mass concentration of 40mg/ml, uniformly stirring by magnetic force, taking a small part of mixed liquid by a straw, dripping the small part of mixed liquid into a mold, adjusting the freezing speed to be 14 mu m/min, putting the mixed liquid into a freeze dryer for freeze drying after complete freezing, wherein the freezing temperature is-40 ℃, and taking out the mixed liquid after 48 hours to obtain the silver nanowire-sodium alginate aerogel substrate.
4. 1g N-isopropyl acrylamide, 2mg methylene bisacrylamide and 20mg potassium persulfate are sequentially and respectively dissolved in 5ml deionized water, then ice bath is carried out for 30min, and then 20 mu l tetramethyl ethylenediamine is added into the mixed solution after the ice bath. And (3) placing the aerogel obtained in the step (3) in a hydrogel precursor solution, and standing for 48 hours (keeping the ice bath state for the first two hours, and then taking out at room temperature) to obtain the conductive hydrogel with anisotropic performance.
Example 3:
1. firstly 5.86g MwThe polyvinylpyrrolidone (40000) is added into 190ml of glycerol solution, stirred uniformly and heated in a microwave for 10min to completely dissolve the polyvinylpyrrolidone. Then the temperature is reduced to room temperature, the mixture is poured into a 250ml three-neck flask, 1.58g of silver nitrate is sequentially added into the three-neck flask, 10ml of glycerol and prepared mixed solution of 0.5ml of deionized water and 59mg of sodium chloride are added into the three-neck flask, the temperature is increased to 210 ℃ along with 20min, and the stirring speed is controlled to be 50 rpm. After the reaction is finished, pouring the mixture into a 500ml beaker, adding deionized water with the same volume, cooling, then carrying out 6000rpm, centrifuging twice for 10min, and dispersing and fixing the volume.
2. And (3) putting 0.6g of sodium alginate powder into a 50ml beaker, adding 30ml of deionized water, and then carrying out magnetic stirring for 8 hours to obtain a uniform sodium alginate solution of 20 mg/ml.
3. And taking 20ml of 60mg/ml silver nanowire, adding 20ml of sodium alginate dispersion liquid with the mass concentration of 20mg/ml, uniformly stirring by magnetic force, taking a small part of mixed liquid by a straw, dripping the small part of mixed liquid into a mould, adjusting the freezing speed to be 14 mu m/min, putting the mixed liquid into a freeze dryer for freeze drying after complete freezing, wherein the freezing temperature is-40 ℃, and taking out the mixed liquid after 48 hours to obtain the silver nanowire-sodium alginate aerogel substrate.
4. 1g N-isopropyl acrylamide, 2mg methylene bisacrylamide and 20mg potassium persulfate are sequentially and respectively dissolved in 5ml deionized water, then ice bath is carried out for 30min, and then 20 mu l tetramethyl ethylenediamine is added into the mixed solution after the ice bath. And (3) placing the aerogel obtained in the step (3) in a hydrogel precursor solution, and standing for 48 hours (keeping the ice bath state for the first two hours, and then taking out at room temperature) to obtain the conductive hydrogel with anisotropic performance.
When the anisotropic conductive hydrogel is prepared, the silver nanowires and sodium alginate are constructed into the aerogel with an ordered layered structure by adopting two-way freezing, and then the aerogel is filled with the hydrogel by taking the aerogel as a support, so that the hydrogel has excellent conductivity and compressive stress anisotropy, and meanwhile, the hydrogel is applied to a sensing direction, so that the anisotropic conductive hydrogel prepared by the invention has huge application in the field of flexible electronic devices.
Claims (8)
1. A method for constructing anisotropic conductive hydrogel based on bidirectional freezing is characterized in that:
firstly, sodium alginate and silver nanowires are uniformly mixed, then a long-range ordered silver nanowire-sodium alginate aerogel substrate with a layered structure is formed by a two-way freezing method, and then a monomer and a cross-linking agent are added into the aerogel substrate to construct hydrogel with the layered structure.
2. The method according to claim 1, characterized by comprising the steps of:
step 1: synthesizing silver nanowires;
step 2: preparing a sodium alginate solution;
and step 3: mixing and dispersing the silver nanowires and the sodium alginate solution uniformly;
and 4, step 4: freezing the dispersion liquid obtained in the step 3 into a solid by a bidirectional freezing method, and then freezing and drying to obtain the silver nanowire-sodium alginate aerogel substrate;
and 5: and (4) adding a monomer, an initiator, a cross-linking agent and a catalyst into the aerogel substrate obtained in the step (4) to construct the anisotropic conductive hydrogel.
3. The method of claim 2, wherein:
in step 1, the length of the synthesized silver nanowire is 7-15 μm, and the diameter is 60-100 nm.
4. The method of claim 2, wherein:
in the step 3, the content of the silver nanowires in the dispersion liquid obtained after uniform mixing and dispersion is 20mg/ml, and the content of the sodium alginate is 20 mg/ml.
5. The method of claim 2, wherein:
in the step 5, the monomer is N-isopropyl acrylamide, and the adding mass of the monomer is 14.32-16.6% of the total mass of the hydrogel precursor solution.
6. The method of claim 2, wherein:
in the step 5, the initiator is potassium persulfate, and the adding mass of the initiator is 0.11-0.33% of the total mass of the hydrogel precursor solution.
7. The method of claim 2, wherein:
in the step 5, the cross-linking agent is methylene bisacrylamide, and the addition mass of the cross-linking agent is 0.01-0.03% of the total mass of the hydrogel precursor solution.
8. The method of claim 2, wherein:
in the step 5, the catalyst is tetramethylethylenediamine, the adding volume of the catalyst is based on 1g of the monomer in the hydrogel precursor solution, and the adding volume of the catalyst is 15-20 mul.
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| US20090252800A1 (en) * | 2003-08-13 | 2009-10-08 | Wan-Kei Wan | Anisotropic nanocomposite hydrogel |
| CN109851816A (en) * | 2019-01-28 | 2019-06-07 | 合肥工业大学 | A kind of preparation method of the binary hydrogel of orientation freezing silver nanowires cooperative reinforcing |
| CN110064347A (en) * | 2019-05-23 | 2019-07-30 | 中国石油大学(华东) | Porous aerogel and its preparation method and application based on bionical vascular bundle micro-structure |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090252800A1 (en) * | 2003-08-13 | 2009-10-08 | Wan-Kei Wan | Anisotropic nanocomposite hydrogel |
| CN109851816A (en) * | 2019-01-28 | 2019-06-07 | 合肥工业大学 | A kind of preparation method of the binary hydrogel of orientation freezing silver nanowires cooperative reinforcing |
| CN110064347A (en) * | 2019-05-23 | 2019-07-30 | 中国石油大学(华东) | Porous aerogel and its preparation method and application based on bionical vascular bundle micro-structure |
Non-Patent Citations (1)
| Title |
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| 宋品: ""基于冰模板法构筑三维有序纳米自组装材料与性能研究"", 《中国优秀博硕士学位论文全文数据库(博士) 工程科技Ⅰ辑》 * |
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