CN113764741B - Flexible paper-based battery and preparation method thereof - Google Patents
Flexible paper-based battery and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a flexible paper-based battery and a preparation method thereof. The preparation method comprises the following steps: firstly, long metal nickel on filter paper is realized on the filter paper by an ion exchange method, and the binding force between the nickel and a paper-based substrate is strong, the flexibility is large, and the conductive capacity is good. Then, a layer of gold nano particles is electroless plated on the surface of the nickel layer, so that the chemical stability of the nickel layer prepared by electroless plating deposition can be improved, the interference of impurities such as phosphorus and the like is reduced, the conductivity of the nickel electrode is further improved, and the nickel/gold electrode is used as a current collector of the flexible paper-based battery. Next, silver and zinc electrodes are deposited on the current collector by electroplating, respectively. Finally, simple packaging is carried out, and the electrolyte is dripped to prepare the paper-based battery. The paper-based battery prepared by the invention belongs to a silver-zinc battery, and has the advantages of flexibility, portability, low cost, green and non-toxic manufacturing process.
Description
Technical Field
The invention relates to an energy device in the field of flexible electronics, comprising metal growth on a flexible substrate and patterning thereof. The invention discloses a flexible paper-based battery with large flexibility, simple process, non-toxic process and low cost and a preparation method thereof.
Background
With the development of flexible electronics technology, many flexible substrate-based devices, such as wearable flexible display screens, distributed sensors, flexible sensors, etc., are emerging. The battery is taken as an energy source of various electronic devices, has great research significance and wide application, and therefore, the flexible battery is generated. It is compatible with semiconductor manufacturing process, and has excellent mechanical property, bending property, and wearable and foldable characteristics, so that the market demand can be satisfied. In addition, the flexible paper-based electrode has the advantages of light weight, easiness in integration, environment friendliness and the like. Therefore, the application of the flexible paper battery is very wide.
In the preparation process of the paper-based battery, for example, chinese patent: 201821057988.5, although achieving high efficiency, is not flexible, environmentally friendly and cost-effective. This will limit the mass production and application of paper batteries.
Among various batteries, a silver-zinc battery is a mature secondary battery system, can keep stable voltage in the discharging process, has a typical working voltage of 1.5V, and can meet the requirements of most flexible devices. In addition, the silver-zinc battery is nontoxic and environment-friendly, the toxicity in the preparation process is low, the glove box is not needed for preparation, and the theoretical energy density is as high as 478Wh kg -1 The discharge voltage is higher, the requirements of portable and wearable electronic equipment are met, and the battery has greater potential in the field of flexible batteries.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides a flexible paper-based battery and a preparation method thereof, which can prepare electrodes on paper-based substrates such as common filter paper, A4 printing paper, sulfuric acid paper and the like, and can form the flexible paper-based battery by combining the electrodes with proper electrolyte, and has the advantages of high electrochemical stability, good adhesiveness, low dielectric constant, high thermal stability, simple process, low cost, environmental protection, degradability, light weight, recoverability, easy bending and the like.
The specific technical scheme for realizing the aim of the invention is as follows:
a method for preparing a flexible paper-based battery, comprising the following specific steps:
step 1: preparing a metal nickel layer at two ends of a substrate by an ion exchange method, which comprises the following steps:
(i) Respectively carrying out ultrasonic cleaning on the substrate for 25-35 min by using deionized water, ethanol and acetone to obtain a dust-free substrate, and drying;
(ii) Respectively soaking the two ends of the cleaned and dried substrate in nickel sulfate solution for 10-15 min to enable the surface of the substrate to be subjected to metal ion adsorption;
(iii) Washing and drying the substrate in the step (ii) by deionized water, and then placing the substrate in sodium borohydride solution for soaking for 3-5 min to enable metal ions adsorbed on the surface to react with the solution to generate a nickel seed layer;
(iv) Washing and drying the substrate in the step (iii) by deionized water, and then soaking the substrate in a commercial electroless nickel plating solution for 20-30 min to obtain a conductive and compact metal nickel layer;
step 2: washing and drying the metal nickel layer obtained in the step 1 by deionized water, soaking in commercial electroless gold plating solution for 20-30 min, and electroless plating a layer of gold nano particles on the surface of the nickel layer to obtain a nickel/gold electrode serving as a current collector of the flexible paper-based battery;
step 3: and (2) electroplating silver at one end of the nickel/gold current collector obtained in the step (2), which specifically comprises the following steps:
(i) preparing silver plating solution;
(ii) taking a current collector to be electroplated as a cathode, silver wires as an anode, putting silver plating solution into the current collector, electroplating for 10-20 min at-0.5V voltage, and performing electrodeposition to prepare a flexible silver electrode serving as a cathode;
step 4: and (2) electrogalvanizing the other end of the nickel/gold current collector obtained in the step (2), wherein the method specifically comprises the following steps of:
(i) preparing a galvanization solution;
(ii) a current collector to be electroplated is used as a working electrode, a platinum electrode is used as a counter electrode, a silver-silver chloride electrode is used as a reference electrode, a voltage of-0.8V is added into a galvanization solution, electroplating is carried out for 10-20 min, and a flexible zinc electrode is prepared by electrodeposition and is used as an anode;
step 5: leading out wires on the anode and the cathode obtained in the step 3 and the step 4, and dripping electrolyte to obtain the flexible paper-based battery; wherein:
the substrate is made of paper materials, including A4 paper, filter paper and parchment paper;
the concentration of the nickel sulfate solution is 80-100 mM, and the temperature is 80-100 ℃;
the concentration of the sodium borohydride solution is 0.03-0.05M, and the temperature is room temperature;
the temperature of the commercial electroless nickel plating solution is 90-120 ℃;
the temperature of the commercial electroless gold plating solution is 90-120 ℃.
The silver electroplating solution is prepared by mixing 0.4M silver nitrate solution and 0.4-0.8M sodium nitrate solution according to the volume ratio of 1:1.
The electrogalvanizing solution is prepared by mixing 0.6-0.8M zinc sulfate solution and 1M trisodium citrate solution according to the volume ratio of 1:1.
The electrolyte is 1-5M sodium chloride solution or lithium chloride solution; the zinc plating solution contains all zinc salts which can be used for electroplating, such as zinc chloride and the like; the electrolyte comprises all electrolytes suitable for silver-zinc batteries.
A flexible paper-based battery prepared by the method.
The invention has the beneficial effects that:
compared with other batteries, the invention has the advantages of flexibility, light weight, simple preparation process and low cost, and has application prospect in a plurality of fields. Paper-based batteries are an emerging field, and the invention is innovative.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
FIG. 2 is a schematic illustration of an electroless plating process of the present invention;
FIG. 3 is a graph of the discharge curve at 1mA for example 1;
FIG. 4 is a flow chart of the preparation of example 2.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Referring to fig. 1 and 2, the present invention includes:
s1, preparing metal nickel layers 12 at two ends of a substrate 11 by an ion exchange method, wherein the method specifically comprises the following steps:
s1.1, respectively ultrasonically cleaning a substrate for 25-35 min by using deionized water, ethanol and acetone to obtain a dust-free substrate 11, and drying for later use;
s1.2, respectively soaking two ends of the cleaned and dried substrate 11 in nickel sulfate solution for 10-15 min to enable the surface of the substrate to be adsorbed with metal ions;
s1.3, washing and drying by deionized water, and then soaking in sodium borohydride solution for 3-5 min, wherein surface adsorption ions react with the solution to generate a nickel seed layer 21;
s1.4, washing and drying by deionized water, and then soaking in a commercial electroless nickel plating solution for 20-30 min to obtain a conductive and compact metal nickel layer 12;
s2, washing and drying the metal nickel layer 12 obtained in the S1 by deionized water, soaking in commercial electroless gold plating solution for 20-30 min, and preparing a metal gold layer 13 on the surface of the nickel layer 12 to obtain a nickel/gold electrode serving as a current collector of the flexible paper-based battery;
s3, electroplating silver on one end of the nickel/gold current collector obtained in the S2, and preparing a flexible silver electrode by electrodeposition as a cathode 14, wherein the method specifically comprises the following steps:
s3.1, preparing silver plating solution;
s3.2, taking a current collector to be electroplated as a cathode, taking silver wires as an anode, putting silver plating solution into the silver plating solution, and electroplating for 10-20 min at-0.5V voltage;
s4, electrogalvanizing the other end of the nickel/gold current collector obtained in the S2, and taking the flexible zinc electrode prepared by electrodeposition as an anode 15, wherein the method specifically comprises the following steps:
s4.1, preparing a galvanization solution;
s4.2, a current collector to be electroplated is used as a working electrode, a platinum electrode is used as a counter electrode, a silver-silver chloride electrode is used as a reference electrode, and a voltage of-0.8V is added into a galvanization solution to be electroplated for 10-20 min;
and S5, leading out a lead 16 on the cathode 14 and the anode 15 obtained in the steps S3 and S4, and dripping an electrolyte 17 to obtain the flexible paper-based battery.
Example 1
S1, preparing metal nickel layers 12 at two ends of a substrate 11 by an ion exchange method, wherein the method specifically comprises the following steps:
s1.1, selecting rectangular filter paper with the thickness of 2cm x 5cm as a substrate, respectively ultrasonically cleaning the substrate for 30min by deionized water, ethanol and acetone to obtain a dust-free substrate 11, and drying for later use;
s1.2, respectively soaking two ends of a substrate 11 which is cleaned and dried in a nickel sulfate solution for 10min to enable the surface of the substrate to be adsorbed with metal ions;
s1.3, washing and drying with deionized water, then soaking in sodium borohydride solution for 3min, and reacting the ions adsorbed on the surface with the solution to generate a nickel seed layer;
s1.4, washing and drying by deionized water, and then soaking in a commercial electroless nickel plating solution for 20min to obtain a conductive and compact metal nickel layer 12;
s2, washing and drying the metal nickel layer 12 obtained in the S1 by deionized water, placing the metal nickel layer in a commercial electroless gold plating solution for soaking for 20min, and preparing a metal gold layer 13 on the surface of the nickel layer 12 to obtain a nickel/gold electrode serving as a current collector of the flexible paper-based battery;
s3, electroplating silver on one end of the nickel/gold current collector obtained in the S2, and preparing a flexible silver electrode by electrodeposition as a cathode 14, wherein the method specifically comprises the following steps:
s3.1, mixing 0.4M silver nitrate solution and 0.6M sodium nitrate solution according to the volume ratio of 1:1 to prepare silver plating solution;
s3.2, taking a current collector to be electroplated as a cathode, taking silver wires as an anode, putting silver plating solution into the silver plating solution, and electroplating for 10 minutes under the voltage of-0.5V;
s4, electrogalvanizing the other end of the nickel/gold current collector obtained in the S2, and taking the flexible zinc electrode prepared by electrodeposition as an anode 15, wherein the method specifically comprises the following steps:
s4.1, mixing a zinc sulfate solution with the concentration of 0.6M and a trisodium citrate solution with the concentration of 1M according to the volume ratio of 1:1 to prepare a zinc plating solution;
s4.2, a current collector to be electroplated is used as a working electrode, a platinum electrode is used as a counter electrode, a silver-silver chloride electrode is used as a reference electrode, and a voltage of-0.8V is added into a galvanization solution for electroplating for 10min;
and S5, leading out a lead 16 on the cathode 14 and the anode 15 obtained in the steps S3 and S4, and dripping 5M sodium chloride solution as an electrolyte 17 to obtain the flexible paper-based battery.
The prepared paper-based battery had an open circuit voltage of 0.7V and a short circuit current of about 4mA. FIG. 3 is a discharge curve at 1mA, setting the effective voltage to be greater than 0.3V, dropping the voltage from 0.65V to 0.3V for 230s.
Example 2
Paper-based batteries generally have two structures, the planar one shown in example 1, and a stacked structure as shown in fig. 4.
S1, preparing a metal nickel layer 12 on two substrates 11 by an ion exchange method, wherein the method specifically comprises the following steps:
s1.1, selecting two pieces of 1 cm-1 cm rectangular sulfuric acid paper as substrates, respectively ultrasonically cleaning the substrates for 30min by deionized water, ethanol and acetone to obtain two dust-free substrates 11, and drying for later use;
s1.2, respectively soaking the two cleaned and dried substrates 11 in nickel sulfate solution for 15min to enable the surfaces of the substrates to be adsorbed with metal ions;
s1.3, washing and drying with deionized water, then soaking in sodium borohydride solution for 5min, and reacting the ions adsorbed on the surface with the solution to generate a nickel seed layer;
s1.4, washing and drying by deionized water, and then soaking in a commercial electroless nickel plating solution for 20min to obtain two conductive and compact metal nickel layers 12;
s2, washing and drying the two metal nickel layers 12 obtained in the S1 by deionized water, respectively soaking the two metal nickel layers in commercial electroless gold plating solution for 20min, and preparing a metal gold layer 13 on the surface of the nickel layer 12 to obtain two nickel/gold electrodes serving as current collectors of the flexible paper-based battery;
s3, electroplating silver on the nickel/gold current collector obtained in the S2, and taking the flexible silver electrode obtained by electrodeposition as a cathode 14, wherein the method specifically comprises the following steps of:
s3.1, mixing 0.4M silver nitrate solution and 0.6M sodium nitrate solution according to the volume ratio of 1:1 to prepare silver plating solution;
s3.2, taking a current collector to be electroplated as a cathode, taking silver wires as an anode, putting silver plating solution into the silver plating solution, and electroplating for 20min at the voltage of-0.5V;
s4, electroplating zinc on the other nickel/gold current collector obtained in the S2, and taking the flexible zinc electrode prepared by electrodeposition as an anode 15, wherein the method specifically comprises the following steps of:
s4.1, mixing a zinc sulfate solution with the concentration of 0.6M and a trisodium citrate solution with the concentration of 1M according to the volume ratio of 1:1 to prepare a zinc plating solution;
s4.2, a current collector to be electroplated is used as a working electrode, a platinum electrode is used as a counter electrode, a silver-silver chloride electrode is used as a reference electrode, and a voltage of-0.8V is added into a galvanization solution for electroplating for 20min;
and S5, leading out leads 16 on the cathode 14 and the anode 15 obtained in the steps S3 and S4, isolating the cathode 14 and the anode 15 by using a piece of sulfuric acid paper 11, stacking, and dripping 2M sodium chloride solution as electrolyte 17 at the center of the obtained device after packaging to obtain the flexible paper-based battery with a stacked structure.
The working principle of the invention is as follows:
referring to fig. 1, the preparation method of the invention comprises the steps of firstly realizing long metal nickel on filter paper by an ion exchange method on the filter paper, wherein the nickel and paper-based substrate have strong binding force, large flexibility and good electric conductivity. Then, a layer of gold nano particles is electroless plated on the surface of the nickel layer, so that the chemical stability of the nickel layer prepared by electroless plating deposition can be improved, the interference of impurities such as phosphorus and the like is reduced, the conductivity of the nickel electrode is further improved, and the nickel/gold electrode is used as a current collector of the flexible paper-based battery. Then, silver and zinc are deposited on the nickel electrode by electroplating, respectively. Finally, simple encapsulation is carried out, and the electrolyte is dripped to realize the preparation of the paper-based battery. The paper-based battery prepared by the invention belongs to a silver-zinc battery, and has the advantages of flexibility, portability, low cost, green and non-toxic manufacturing process.
Claims (5)
1. The preparation method of the flexible paper-based battery is characterized by comprising the following specific steps of:
step 1: preparing a metal nickel layer at two ends of a substrate by an ion exchange method, which comprises the following steps:
(i) Respectively carrying out ultrasonic cleaning on the substrate for 25-35 min by using deionized water, ethanol and acetone to obtain a dust-free substrate, and drying;
(ii) Respectively soaking the two ends of the cleaned and dried substrate in nickel sulfate solution for 10-15 min to enable the surface of the substrate to be subjected to metal ion adsorption;
(iii) Washing and drying the substrate in the step (ii) by deionized water, and then placing the substrate in sodium borohydride solution for soaking for 3-5 min to enable metal ions adsorbed on the surface to react with the solution to generate a nickel seed layer;
(iv) Washing and drying the substrate in the step (iii) by deionized water, and then soaking the substrate in a commercial electroless nickel plating solution for 20-30 min to obtain a conductive and compact metal nickel layer;
step 2: washing and drying the metal nickel layer obtained in the step 1 by deionized water, soaking in commercial electroless gold plating solution for 20-30 min, and electroless plating a layer of gold nano particles on the surface of the nickel layer to obtain a nickel/gold electrode serving as a current collector of the flexible paper-based battery;
step 3: and (2) electroplating silver at one end of the nickel/gold current collector obtained in the step (2), which specifically comprises the following steps:
(i) Preparing silver plating solution;
(ii) The current collector to be electroplated is used as a cathode, silver wires are used as an anode, silver plating solution is put into the current collector, electroplating is carried out for 10-20 min under the voltage of-0.5V, and flexible silver electrodes are prepared by electrodeposition and used as the cathode;
step 4: and (2) electrogalvanizing the other end of the nickel/gold current collector obtained in the step (2), wherein the method specifically comprises the following steps of:
(i) Preparing a zinc plating solution;
(ii) A current collector to be electroplated is used as a working electrode, a platinum electrode is used as a counter electrode, a silver-silver chloride electrode is used as a reference electrode, a voltage of-0.8V is added into a galvanization solution, electroplating is carried out for 10-20 min, and a flexible zinc electrode is prepared by electrodeposition and is used as an anode;
step 5: leading out wires on the cathode and the anode obtained in the step 3 and the step 4, and dripping electrolyte to obtain the flexible paper-based battery; wherein:
the substrate is made of paper materials, including A4 paper, filter paper and parchment paper;
the concentration of the nickel sulfate solution is 80-100 mM, and the temperature is 80-100 ℃;
the concentration of the sodium borohydride solution is 0.03-0.05M, and the temperature is room temperature;
the temperature of the commercial electroless nickel plating solution is 90-120 ℃;
the temperature of the commercial electroless gold plating solution is 90-120 ℃.
2. The method for producing a flexible paper-based battery according to claim 1, wherein the electrolytic silver plating solution is formed by mixing a silver nitrate solution of 0.4M and a sodium nitrate solution of 0.4 to 0.8M in a volume ratio of 1:1.
3. The method for preparing a flexible paper-based battery according to claim 1, wherein the electrogalvanizing solution is prepared by mixing a zinc sulfate solution of 0.6-0.8M and a trisodium citrate solution of 1M in a volume ratio of 1:1.
4. The method for preparing the flexible paper-based battery according to claim 1, wherein the electrolyte is 1-5M sodium chloride solution or lithium chloride solution.
5. A flexible paper-based battery made by the method of claim 1.
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| CN115954431B (en) * | 2023-02-13 | 2023-10-20 | 起源智能科技(嘉兴)有限公司 | Zinc-silver battery and method for improving efficiency of zinc-silver battery |
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| CN111082147A (en) * | 2019-12-09 | 2020-04-28 | 上海交通大学 | Preparation method of photonic crystal lithium-sulfur battery based on large-area thick film controllable texture |
| WO2020093157A1 (en) * | 2018-11-06 | 2020-05-14 | Salient Energy Inc. | Systems, devices, and methods for electroplated zinc negative electrodes for zinc metal cells and batteries |
| CN111349934A (en) * | 2020-03-12 | 2020-06-30 | 华东师范大学 | Flexible silver electrode and preparation method thereof |
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| WO2020093157A1 (en) * | 2018-11-06 | 2020-05-14 | Salient Energy Inc. | Systems, devices, and methods for electroplated zinc negative electrodes for zinc metal cells and batteries |
| CN111082147A (en) * | 2019-12-09 | 2020-04-28 | 上海交通大学 | Preparation method of photonic crystal lithium-sulfur battery based on large-area thick film controllable texture |
| CN111349934A (en) * | 2020-03-12 | 2020-06-30 | 华东师范大学 | Flexible silver electrode and preparation method thereof |
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| 锌银蓄电池中镀银泡沫镍的电化学性能研究;张辉;朱立群;项民;;稀有金属材料与工程(第01期);全文 * |
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