Silver, nickel and graphene ternary alloy light-transmitting material
By using whisker-adjusted graphene agent in silver, nickel, and graphene ternary alloy light-transmitting materials, the problem of poor conductivity of existing materials is solved, and the coordinated improvement of conductivity and electromagnetic shielding performance is achieved, and the overall performance of the product is improved.
Patent Information
- Application Number
- CN202510313444.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-17
- Publication Date
- 2025-06-13
AI Technical Summary
When existing silver, nickel and graphene ternary alloy light-transmitting materials optimize the electromagnetic shielding performance, the conductivity is poor and difficult to coordinate and improve, which affects the efficiency of the product.
Silver, nickel and graphene are used as raw materials to prepare ternary alloy light-transmitting materials, and the graphene agent is improved by whisker adjustment, including activation of graphene potassium permanganate solution, heat treatment and immersion treatment of zinc oxide whiskers, to optimize the interface and activity performance between the raw materials.
The conductive performance and electromagnetic shielding performance of the product are significantly optimized, so that the two are coordinated and improved, and the overall performance and effect of the system are improved.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of alloy light-transmitting materials, and specifically to a silver, nickel, and graphene ternary alloy light-transmitting material. Background Art
[0002] Conductive cloth is based on fiber cloth (usually polyester fiber cloth), and after pre-treatment, an electroplated metal coating is applied to make it have metal characteristics and become conductive fiber cloth; it can be divided into: nickel-plated conductive cloth, gold-plated conductive cloth, carbon-plated conductive cloth, and aluminum foil fiber composite cloth.
[0003] In order to optimize the electromagnetic shielding efficiency of the existing silver, nickel, and graphene ternary alloy light-transmitting materials, it is easy to cause poor electrical conductivity of the products, and it is very difficult to coordinately improve the electrical conductivity and electromagnetic shielding performance of the products. For example, Chinese Patent Document CN105788703B discloses an antioxidant silver copper paste for electromagnetic shielding and its preparation method. The raw material combination used in this document is relatively large, which instead affects the electromagnetic shielding and electrical conductivity of the products and limits the use efficiency of the products. Summary of the Invention
[0004] Aiming at the defects of the existing technology, the purpose of the present invention is to provide a silver, nickel, and graphene ternary alloy light-transmitting material to solve the problems raised in the above background art.
[0005] The present invention adopts the following technical solutions to solve the technical problems:
[0006] The present invention provides a silver, nickel, and graphene ternary alloy light-transmitting material, and the preparation method of the light-transmitting material is as follows:
[0007] Step 1: Dissolve 400 grams of nickel sulfate, 10 g of hydrochloric acid, and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add 0.2 g of diethylenetriamine and dissolve it completely. Wait for the temperature to drop to room temperature, and slowly add 150 ml of silver nitrate dissolved in 1000 g of pure water and dissolve it completely;
[0008] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring for complexation for 12 hours. After sufficient complexation, slowly add 0.001 g of whisker-adjusted graphene agent, and carry out stirring and ultrasonic treatment simultaneously for 12 hours. The stirring speed is 450 - 550 r / min, and the ultrasonic power is 300 - 400 KW; to obtain a silver, nickel, and graphene alloy electroplating solution;
[0009] Step 2: Use conductive fibers to be ultrasonically cleaned, sulfuric acid activated, cleaned, and put into the silver, nickel, and graphene alloy electroplating solution for electroplating. After electroplating, clean with pure water and dry; then obtain a 20 - 30 micron silver, nickel, and graphene ternary alloy light-transmitting material after high-temperature heating and fiber carbonization treatment.
[0010] Preferably, the preparation method of the whisker regulating graphene agent is:
[0011] S01: placing the graphene in a potassium permanganate solution 3-5 times the total weight of the graphene and stirring evenly, then washing and drying to obtain pretreated graphene;
[0012] S02: heat-treating the zinc oxide whisker at 45-50° C. for 5-10 minutes, then keeping the temperature, immersing the whisker in an immersion agent, filtering, and drying to obtain a zinc oxide whisker agent;
[0013] S03: 4-7 parts of zinc oxide whisker agent, 1-3 parts of silane coupling agent, 2-4 parts of glycolic acid and 10-15 parts of deionized water are stirred and mixed, and finally 1-2 parts of phosphate buffer solution are added and stirred sufficiently to obtain a zinc oxide whisker conditioning solution;
[0014] S04: ball milling the pretreated graphene and zinc oxide whisker conditioning liquid in a weight ratio of 5:2, with a ball milling speed of 1000-1500r / min, for 1-2h. After the ball milling is completed, washing and drying are performed to obtain a whisker conditioning graphene agent.
[0015] Preferably, the mass fraction of the potassium permanganate solution is 4-8%.
[0016] Preferably, the specific operation steps of immersing in the immersion agent are:
[0017] The heat-insulated zinc oxide whiskers are immersed in the immersion agent at a weight ratio of 1:5, the immersion pressure is 10-15 MPa, the immersion time is 10-20 minutes, and the immersion is completed.
[0018] Preferably, the impregnating agent is yttrium nitrate solution.
[0019] Preferably, the mass fraction of the yttrium nitrate solution is 4-7%.
[0020] Preferably, the pH value of the phosphate buffer solution is 4.5-5.0.
[0021] Preferably, the electroplating temperature is 48-52° C., and the electroplating current is 35-40A.
[0022] Preferably, the carbonization treatment is carried out at 350-370° C. for 3-5 hours.
[0023] Compared with the prior art, the present invention has the following beneficial effects:
[0024] The ternary alloy light-transmitting material of the present invention is prepared by using silver, nickel, and graphene as raw materials. The innovative improvement is made by using whisker-adjusted graphene agent to optimize the electrical conductivity and electromagnetic shielding performance of the product system, and to coordinately improve the two performances. The whisker-adjusted graphene agent is prepared by activating graphene with potassium permanganate solution to optimize its activity efficiency. Zinc oxide whiskers are first heat-treated at 45-50 °C for 5-10 minutes, and then immersed in yttrium nitrate solution for improvement. The immersed zinc oxide whiskers are doped with yttrium element, which can better cooperate with graphene for improvement, and improve the electrical conductivity and electromagnetic shielding efficiency of the system. At the same time, zinc oxide whisker agent, silane coupling agent, glycolic acid, and phosphate buffer solution are combined with each other. The interface between raw materials is improved by silane coupling agent, and glycolic acid and phosphate buffer solution are used as raw materials to improve the interface activity efficiency. The synergistic effect between the prepared zinc oxide whisker adjustment liquid and graphene is enhanced, so that the whisker-adjusted graphene agent obtained in the system further optimizes and improves the performance effect of the product. Detailed implementation mode
[0025] The technical solutions in the embodiments of the present invention are clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.
[0026] The silver, nickel, and graphene ternary alloy light-transmitting material of this embodiment, the preparation method of the light-transmitting material is as follows:
[0027] Step 1: Dissolve 400 grams of nickel sulfate, 10 g of hydrochloric acid, and 1000 g of water in proportion to dissolve nickel sulfate, and then slowly add 0.2 g of diethylenetriamine and dissolve completely. Wait for the temperature to drop to room temperature, and slowly add 150 ml of silver nitrate dissolved in 1000 g of pure water and dissolve completely;
[0028] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring and complexing for 12 hours. After sufficient complexing, slowly add 0.001 g of whisker-adjusted graphene agent, and carry out stirring and ultrasonic treatment simultaneously for 12 hours. The stirring speed is 450-550 r / min, and the ultrasonic power is 300-400 KW; to obtain a silver, nickel, and graphene alloy electroplating solution;
[0029] Step 2: Use conductive fiber to be ultrasonically cleaned, sulfuric acid activated, cleaned, and put into the silver, nickel, and graphene alloy electroplating solution for electroplating. After electroplating, clean with pure water and dry; then heat the fiber at high temperature for carbonization treatment to obtain a 20-30 micron silver, nickel, and graphene ternary alloy light-transmitting material.
[0030] The preparation method of the whisker-adjusted graphene agent in this embodiment is as follows:
[0031] S01: placing the graphene in a potassium permanganate solution 3-5 times the total weight of the graphene and stirring evenly, then washing and drying to obtain pretreated graphene;
[0032] S02: heat-treating the zinc oxide whisker at 45-50° C. for 5-10 minutes, then keeping the temperature, immersing the whisker in an immersion agent, filtering, and drying to obtain a zinc oxide whisker agent;
[0033] S03: 4-7 parts of zinc oxide whisker agent, 1-3 parts of silane coupling agent, 2-4 parts of glycolic acid and 10-15 parts of deionized water are stirred and mixed, and finally 1-2 parts of phosphate buffer solution are added and stirred sufficiently to obtain a zinc oxide whisker conditioning solution;
[0034] S04: ball milling the pretreated graphene and zinc oxide whisker conditioning liquid in a weight ratio of 5:2, with a ball milling speed of 1000-1500r / min, for 1-2h. After the ball milling is completed, washing and drying are performed to obtain a whisker conditioning graphene agent.
[0035] The mass fraction of the potassium permanganate solution in this embodiment is 4-8%.
[0036] The specific operation steps of immersing in the immersion agent in this embodiment are:
[0037] The heat-insulated zinc oxide whiskers are immersed in the immersion agent at a weight ratio of 1:5, the immersion pressure is 10-15 MPa, the immersion time is 10-20 minutes, and the immersion is completed.
[0038] The immersion agent in this embodiment is yttrium nitrate solution.
[0039] The mass fraction of the yttrium nitrate solution in this embodiment is 4-7%.
[0040] The pH value of the phosphate buffer solution of this embodiment is 4.5-5.0.
[0041] The electroplating temperature of this embodiment is 48-52° C., and the electroplating current is 35-40A.
[0042] The carbonization treatment conditions of this embodiment are 350-370° C. for 3-5 hours.
[0043] Example 1.
[0044] The silver, nickel, and graphene ternary alloy light-transmitting material of this embodiment is prepared by:
[0045] Step 1: Dissolve 400 g of nickel sulfate, 10 g of hydrochloric acid and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add 0.2 g of diethylenetriamine and dissolve it completely. Wait for the temperature to drop to room temperature and add it slowly. Dissolve 150 ml of silver nitrate in 1000 g of pure water and dissolve it completely;
[0046] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring for complexation for 12 hours. After sufficient complexation, slowly add 0.001 g of whisker-adjusted graphene agent and carry out stirring and ultrasonic treatment simultaneously for 12 hours. The stirring speed is 450 r / min and the ultrasonic power is 300 KW; obtain silver, nickel, graphene alloy electroplating solution;
[0047] Step 2: Use conductive fiber, after ultrasonic cleaning, sulfuric acid activation, cleaning, put it into the silver, nickel, graphene alloy electroplating solution for electroplating, and after electroplating, wash it with pure water and dry it; then heat the fiber at high temperature for carbonization treatment to obtain a 20-micron silver, nickel, graphene ternary alloy light-transmitting material.
[0048] The preparation method of the whisker-adjusted graphene agent in this embodiment is as follows:
[0049] S01: First place graphene in a potassium permanganate solution with a mass multiple of 3 times the total weight of graphene and stir evenly, then wash it with water and dry it to obtain pretreated graphene;
[0050] S02: First heat-treat zinc oxide whiskers at 45 °C for 5 min, then keep warm and immerse them in an immersion agent for immersion treatment, filter by suction and dry to obtain zinc oxide whisker agent;
[0051] S03: Stir and mix 4 parts of zinc oxide whisker agent, 1 part of silane coupling agent, 2 parts of glycolic acid and 10 parts of deionized water evenly, and finally add 1 part of phosphate buffer solution and stir well to obtain zinc oxide whisker adjustment liquid;
[0052] S04: Ball-mill and improve the pretreated graphene and zinc oxide whisker adjustment liquid according to a weight ratio of 5:2. The ball-milling speed is 1000 r / min and the ball-milling time is 1 h. After the ball-milling is finished, wash it with water and dry it to obtain the whisker-adjusted graphene agent.
[0053] The mass fraction of the potassium permanganate solution in this embodiment is 4%.
[0054] The specific operation steps of the immersion treatment in this embodiment are as follows:
[0055] Immerse the heat-preserved zinc oxide whiskers in the immersion agent according to a weight ratio of 1:5, the immersion pressure is 10 MPa, and the immersion time is 10 min. After the immersion is finished, it is ok.
[0056] The immersion agent in this embodiment is yttrium nitrate solution.
[0057] The mass fraction of the yttrium nitrate solution in this embodiment is 4%.
[0058] The pH value of the phosphate buffer solution in this example is 4.5.
[0059] The electroplating temperature of this embodiment is 48° C., and the electroplating current is 35A.
[0060] The carbonization treatment conditions of this embodiment are 350° C. for 3 hours.
[0061] Example 2
[0062] The silver, nickel, and graphene ternary alloy light-transmitting material of this embodiment is prepared by:
[0063] Step 1: Dissolve 400 g of nickel sulfate, 10 g of hydrochloric acid and 1000 g of water in proportion to the nickel sulfate, then slowly add 0.2 g of diethylenetriamine until it is completely dissolved, wait for the temperature to drop to room temperature, slowly add 150 ml of silver nitrate dissolved in 1000 g of pure water until it is completely dissolved;
[0064] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring for 12 hours, after sufficient complexation, slowly add 0.001 g of whisker adjustment graphene agent, stir ultrasonically for 12 hours at the same time, the stirring speed is 550 r / min, and the ultrasonic power is 400 KW; obtain silver, nickel, graphene alloy electroplating solution;
[0065] Step 2: Use the conductive fiber to undergo ultrasonic cleaning, sulfuric acid activation, cleaning, and then put it into the silver, nickel, and graphene alloy plating solution to start electroplating. After electroplating, it is washed with pure water and dried; then the fiber is heated at high temperature for carbonization to obtain a 30-micron silver, nickel, and graphene ternary alloy translucent material.
[0066] The preparation method of the whisker-adjusting graphene agent of this embodiment is:
[0067] S01: placing the graphene in a potassium permanganate solution 5 times the total weight of the graphene and stirring evenly, then washing with water and drying to obtain pretreated graphene;
[0068] S02: heat-treating the zinc oxide whisker at 50° C. for 10 min, then keeping the temperature, immersing the whisker in an immersion agent, filtering, and drying to obtain a zinc oxide whisker agent;
[0069] S03: 7 parts of zinc oxide whisker agent, 3 parts of silane coupling agent, 4 parts of glycolic acid and 15 parts of deionized water are stirred and mixed, and finally 2 parts of phosphate buffer solution are added and stirred sufficiently to obtain a zinc oxide whisker conditioning solution;
[0070] S04: Adjust and improve the pre-treated graphene and zinc oxide whisker solution by ball milling at a weight ratio of 5:2. The ball milling speed is 1500 r / min for 2 h. After ball milling, wash with water and dry to obtain the whisker-adjusted graphene agent.
[0071] In this example, the mass fraction of the potassium permanganate solution is 4 - 8%.
[0072] The specific operation steps of the immersion treatment in this example by immersing in the immersion agent are as follows:
[0073] Immerse the heat-insulated zinc oxide whiskers into the immersion agent at a weight ratio of 1:5. The immersion pressure is 15 MPa and the immersion time is 20 min. After immersion, it is completed.
[0074] The immersion agent in this example is a yttrium nitrate solution.
[0075] In this example, the mass fraction of the yttrium nitrate solution is 7%.
[0076] In this example, the pH value of the phosphate buffer solution is 5.0.
[0077] In this example, the electroplating temperature is 52 °C and the electroplating current is 40 A.
[0078] The conditions for the carbonization treatment in this example are treatment at 370 °C for 5 h.
[0079] Example 3
[0080] For the silver, nickel, graphene ternary alloy light-transmitting material in this example, the preparation method of the light-transmitting material is as follows:
[0081] Step 1: Dissolve 400 g of nickel sulfate, 10 g of hydrochloric acid and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add 0.2 g of diethylenetriamine and dissolve completely. Wait for the temperature to drop to room temperature and slowly add. Dissolve 150 ml of silver nitrate with 1000 g of pure water and dissolve completely;
[0082] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring and complexing for 12 hours. After sufficient complexing, slowly add 0.001 g of the whisker-adjusted graphene agent and carry out stirring and ultrasonic treatment simultaneously for 12 hours. The stirring speed is 500 r / min and the ultrasonic power is 350 KW; obtain the silver, nickel, graphene alloy electroplating solution;
[0083] Step 2: Use the conductive fiber to be ultrasonically cleaned, sulfuric acid activated, washed, and put into the silver, nickel, graphene alloy electroplating solution for electroplating. After electroplating, wash with pure water and dry; then heat the fiber at high temperature for carbonization treatment to obtain a 25-micron silver, nickel, graphene ternary alloy light-transmitting material.
[0084] The preparation method of the whisker-adjusted graphene agent in this embodiment is as follows:
[0085] S01: First, place the graphene in a potassium permanganate solution that is 3 - 5 times the total weight of the graphene by mass, stir evenly, then wash with water and dry to obtain pretreated graphene;
[0086] S02: First, heat-treat the zinc oxide whiskers at 47 °C for 7.5 min, then keep warm, immerse them in an immersion agent for immersion treatment, filter by suction and dry to obtain the zinc oxide whisker agent;
[0087] S03: Stir 5.5 parts of the zinc oxide whisker agent, 2 parts of the silane coupling agent, 3 parts of glycolic acid, and 12.5 parts of deionized water evenly, and finally add 1.5 parts of the phosphate buffer solution and stir thoroughly to obtain the zinc oxide whisker adjustment liquid;
[0088] S04: Ball-mill and improve the pretreated graphene and the zinc oxide whisker adjustment liquid according to a weight ratio of 5:2, with a ball-milling speed of 1250 r / min for 1.5 h. After the ball-milling is completed, wash with water and dry to obtain the whisker-adjusted graphene agent.
[0089] The mass fraction of the potassium permanganate solution in this embodiment is 6%.
[0090] The specific operation steps of the immersion treatment in this embodiment are as follows:
[0091] Immerse the heat-preserved zinc oxide whiskers in the immersion agent according to a weight ratio of 1:5, with an immersion pressure of 12.5 MPa and an immersion time of 15 min. After the immersion is completed, it is okay.
[0092] The immersion agent in this embodiment is a yttrium nitrate solution.
[0093] The mass fraction of the yttrium nitrate solution in this embodiment is 5.5%.
[0094] The pH value of the phosphate buffer solution in this embodiment is 4.7.
[0095] The temperature of electroplating in this embodiment is 50 °C, and the electroplating current is 37.5 A.
[0096] The conditions for carbonization treatment in this embodiment are treatment at 360 °C for 4 h.
[0097] Example 4.
[0098] The silver, nickel, graphene ternary alloy light-transmitting material in this embodiment, and the preparation method of the light-transmitting material is as follows:
[0099] Step 1: Dissolve 400 g of nickel sulfate, 10 g of hydrochloric acid and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add 0.2 g of diethylenetriamine and dissolve it completely. Wait for the temperature to drop to room temperature and add it slowly. Dissolve 150 ml of silver nitrate in 1000 g of pure water and dissolve it completely;
[0100] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring for complexation for 12 hours. After sufficient complexation, slowly add 0.001 g of whisker-adjusted graphene agent, and carry out stirring and ultrasonic treatment simultaneously for 12 hours. The stirring speed is 460 r / min and the ultrasonic power is 320 KW; Obtain a silver, nickel, graphene alloy electroplating solution;
[0101] Step 2: Use conductive fibers to carry out ultrasonic cleaning, sulfuric acid activation, cleaning, put them into the silver, nickel, graphene alloy electroplating solution for electroplating, and wash and dry them with pure water after electroplating; After high-temperature heating and fiber carbonization treatment, a 22-micron silver, nickel, graphene ternary alloy light-transmitting material is obtained.
[0102] The preparation method of the whisker-adjusted graphene agent in this embodiment is as follows:
[0103] S01: First place graphene in a potassium permanganate solution 4 times the total weight of graphene and stir evenly, then wash with water and dry to obtain pretreated graphene;
[0104] S02: First heat-treat zinc oxide whiskers at 46 °C for 6 min, then keep warm, immerse them in an immersion agent for immersion treatment, filter and dry to obtain zinc oxide whisker agent;
[0105] S03: Stir and mix 5 parts of zinc oxide whisker agent, 2 parts of silane coupling agent, 3 parts of glycolic acid and 12 parts of deionized water evenly, and finally add 1.2 parts of phosphate buffer solution and stir well to obtain zinc oxide whisker adjustment solution;
[0106] S04: Ball-mill and improve the pretreated graphene and zinc oxide whisker adjustment solution according to a weight ratio of 5:2. The ball-mill speed is 1200 r / min, ball-mill for 1.2 h, after the ball-milling is finished, wash with water and dry to obtain the whisker-adjusted graphene agent.
[0107] The mass fraction of the potassium permanganate solution in this embodiment is 5%.
[0108] The specific operation steps of the immersion treatment in this embodiment are as follows:
[0109] Immerse the heat-preserved zinc oxide whiskers in the immersion agent according to a weight ratio of 1:5, the immersion pressure is 12 MPa, the immersion time is 12 min, and after the immersion is finished, it is ok.
[0110] The immersion agent in this embodiment is yttrium nitrate solution.
[0111] The mass fraction of the yttrium nitrate solution in this embodiment is 5%.
[0112] The pH value of the phosphate buffer solution in this example is 4.6.
[0113] The electroplating temperature of this embodiment is 49° C., and the electroplating current is 36A.
[0114] The carbonization treatment conditions of this embodiment are 355° C. for 4 hours.
[0115] Example 5.
[0116] The silver, nickel, and graphene ternary alloy light-transmitting material of this embodiment is prepared by:
[0117] Step 1: Dissolve 400 g of nickel sulfate, 10 g of hydrochloric acid and 1000 g of water in proportion to the nickel sulfate, then slowly add 0.2 g of diethylenetriamine until it is completely dissolved, wait for the temperature to drop to room temperature, slowly add 150 ml of silver nitrate dissolved in 1000 g of pure water until it is completely dissolved;
[0118] After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring for 12 hours, after sufficient complexation, slowly add 0.001 g of whisker adjustment graphene agent, stir ultrasonically for 12 hours at the same time, the stirring speed is 510 r / min, and the ultrasonic power is 3800 KW; obtain silver, nickel, graphene alloy electroplating solution;
[0119] Step 2: Use the conductive fiber to undergo ultrasonic cleaning, sulfuric acid activation, and cleaning, and then put it into the silver, nickel, and graphene alloy plating solution to start electroplating. After electroplating, it is washed with pure water and dried; then the fiber is heated at high temperature for carbonization to obtain a 28-micron silver, nickel, and graphene ternary alloy translucent material.
[0120] The preparation method of the whisker-adjusting graphene agent of this embodiment is:
[0121] S01: placing the graphene in a potassium permanganate solution 4 times the total weight of the graphene and stirring evenly, then washing with water and drying to obtain pretreated graphene;
[0122] S02: heat-treating the zinc oxide whisker at 48° C. for 8 minutes, then keeping the temperature, immersing the whisker in an immersion agent, filtering, and drying to obtain a zinc oxide whisker agent;
[0123] S03: 6 parts of zinc oxide whisker agent, 2 parts of silane coupling agent, 3 parts of glycolic acid and 14 parts of deionized water are stirred and mixed, and finally 1.8 parts of phosphate buffer solution are added and stirred sufficiently to obtain a zinc oxide whisker conditioning solution;
[0124] S04: Adjust the pre-treated graphene and zinc oxide whisker regulating solution by ball milling with a weight ratio of 5:2. The ball milling speed is 1400 r / min, and the ball milling time is 1.8 h. After the ball milling is completed, wash with water and dry to obtain the whisker-regulated graphene agent.
[0125] In this example, the mass fraction of the potassium permanganate solution is 7%.
[0126] The specific operation steps of the immersion treatment in this example by immersing into the immersion agent are as follows:
[0127] Immerse the heat-preserved zinc oxide whiskers into the immersion agent according to a weight ratio of 1:5. The immersion pressure is 14 MPa, and the immersion time is 18 min. After the immersion is completed, it is okay.
[0128] The immersion agent in this example is a yttrium nitrate solution.
[0129] In this example, the mass fraction of the yttrium nitrate solution is 6%.
[0130] In this example, the pH value of the phosphate buffer solution is 4.8.
[0131] In this example, the electroplating temperature is 50 °C, and the electroplating current is 38 A.
[0132] In this example, the carbonization treatment conditions are treatment at 360 °C for 4 h.
[0133] Comparative Example 1.
[0134] The difference from Example 3 is that the whisker-regulated graphene agent is replaced by nano-graphene.
[0135] Comparative Example 2.
[0136] The difference from Example 3 is that S01 treatment is not used in the preparation of the whisker-regulated graphene agent.
[0137] Comparative Example 3.
[0138] The difference from Example 3 is that the zinc oxide whisker agent is replaced by zinc oxide whiskers.
[0139] Comparative Example 4.
[0140] The difference from Example 3 is that the zinc oxide whisker regulating solution in the preparation of the whisker-regulated graphene agent is composed of 5 parts of zinc oxide whisker regulating solution and 12 parts of deionized water.
[0141] Perform performance tests on the products of Examples 1 to 5 and Comparative Examples 1 to 4. Use a shielding effectiveness tester to test, the test frequency is 30 MHz, test the effectiveness value, and at the same time use a conductivity meter to measure the conductivity value. The test results are as follows
[0142]
[0143]
[0144] It can be seen from Comparative Examples 1-4 and Examples 1-5 that;
[0145] The product of Example 3 has excellent electromagnetic shielding efficiency value and conductivity, and the electromagnetic shielding and conductivity of the product can be coordinately improved; at the same time, it can be seen from Comparative Examples 1-4 that when the whisker-adjusted graphene agent is replaced by nano-graphene, the performance of the product changes significantly, and for the whisker-adjusted graphene prepared by different methods, the performance effect of the product shows a deteriorating trend. Only the whisker-adjusted graphene agent prepared by the method of the present invention has the most significant performance effect.
[0146] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention.
[0147] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. Silver, nickel, graphene ternary alloy light-transmitting material, characterized in that: The preparation method of the light-transmitting material is as follows: Step 1: Dissolve 400 g of nickel sulfate, 10 g of hydrochloric acid and 1000 g of water in proportion to the nickel sulfate, then slowly add 0.2 g of diethylenetriamine until it is completely dissolved, wait for the temperature to drop to room temperature, slowly add 150 ml of silver nitrate dissolved in 1000 g of pure water until it is completely dissolved; After the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 ml and continue stirring for 12 hours, after sufficient complexation, slowly add 0.001 g of whisker adjustment graphene agent, stir ultrasonically for 12 hours at the same time, the stirring speed is 450-550r / min, and the ultrasonic power is 300-400KW; obtain silver, nickel, graphene alloy electroplating solution; Step 2: Use the conductive fiber to undergo ultrasonic cleaning, sulfuric acid activation, cleaning, and then put it into a silver, nickel, and graphene alloy plating solution to start electroplating. After electroplating, it is washed with pure water and dried; then the fiber is heated at high temperature for carbonization to obtain a 20-30 micron silver, nickel, and graphene ternary alloy translucent material.
2. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The preparation method of the whisker regulating graphene agent is: S01: placing the graphene in a potassium permanganate solution 3-5 times the total weight of the graphene and stirring evenly, then washing and drying to obtain pretreated graphene; S02: heat-treating the zinc oxide whisker at 45-50° C. for 5-10 minutes, then keeping the temperature, immersing the whisker in an immersion agent, filtering, and drying to obtain a zinc oxide whisker agent; S03: 4-7 parts of zinc oxide whisker agent, 1-3 parts of silane coupling agent, 2-4 parts of glycolic acid and 10-15 parts of deionized water are stirred and mixed, and finally 1-2 parts of phosphate buffer solution are added and stirred sufficiently to obtain a zinc oxide whisker conditioning solution; S04: ball milling the pretreated graphene and zinc oxide whisker conditioning liquid in a weight ratio of 5:2, with a ball milling speed of 1000-1500r / min, for 1-2h. After the ball milling is completed, washing and drying are performed to obtain a whisker conditioning graphene agent.
3. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 2, characterized in that: The mass fraction of the potassium permanganate solution is 4-8%.
4. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 2, characterized in that: The specific operation steps of the immersion treatment in the immersion agent are: The heat-insulated zinc oxide whiskers are immersed in the immersion agent at a weight ratio of 1:5, the immersion pressure is 10-15 MPa, the immersion time is 10-20 minutes, and the immersion is completed.
5. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 4, characterized in that: The immersion agent is yttrium nitrate solution.
6. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 5, characterized in that: The mass fraction of the yttrium nitrate solution is 4-7%.
7. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 2, characterized in that: The pH value of the phosphate buffer solution is 4.5-5.
0.
8. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The electroplating temperature is 48-52° C., and the electroplating current is 35-40A.
9. The silver, nickel, graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The carbonization treatment conditions are 350-370° C. for 3-5 hours.
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Patent Citations
An antioxidant silver-copper paste for electromagnetic shielding and its preparation method
CN105788703B