Preparation method of nickel, manganese and graphene ternary alloy light-transmitting material

Abstract

The invention discloses a preparation method of a nickel, manganese and graphene ternary alloy light-transmitting material. The preparation method of the light-transmitting material comprises the following steps: carrying out ultrasonic cleaning, sulfuric acid activation and cleaning on conductive fibers, putting the conductive fibers into a nickel, manganese and graphene alloy electroplating solution, starting electroplating, cleaning with purified water after electroplating, and drying; and heating the fibers at a high temperature and carrying out carbonization treatment to obtain the nickel-manganese-graphene ternary alloy light-transmitting material with the thickness of 20-30 microns. The ternary alloy light-transmitting material is mainly applied to national defense military industry high-end electromagnetic shielding materials and large contact terminals and can reduce generation of electric arcs, products prepared through the technology have excellent electromagnetic shielding performance and heat dissipation performance, and the performance of the products can be improved in a coordinated mode.

Description

Technical Field

[0001] The present invention relates to the technical field of light-transmitting materials, and particularly to a preparation method of a nickel, manganese, 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, it is electroplated with a metal coating to make it have metal properties and become conductive fiber cloth; it can be divided into: nickel-plated conductive cloth, gold-plated conductive cloth, carbon-plated conductive cloth, aluminum foil fiber composite cloth; in appearance, there are plain weave and grid distinctions; while ternary alloy light-transmitting materials are mainly used in high-end electromagnetic shielding materials for national defense and military, and large contact terminals can reduce the generation of electric arcs, and are often used in combination with conductive cloth.

[0003] The existing ternary alloy light-transmitting materials have poor electromagnetic shielding efficiency and low heat dissipation performance at the same time, and it is difficult to achieve coordinated improvement of the electromagnetic shielding efficiency and heat dissipation of the products. For example, in the Chinese patent document CN112930100B, a metal transparent electromagnetic shielding material and its preparation method, which uses excellent conductive nano-metal materials such as gold, silver, copper, and alloys as the main body of electromagnetic wave shielding, and inorganic and organic glass as the support of the composite transparent film, it is difficult for the product to achieve coordinated improvement of electromagnetic shielding efficiency and heat dissipation, which limits the use efficiency of the product. Summary of the Invention

[0004] Aiming at the defects of the prior art, the purpose of the present invention is to provide a preparation method of a nickel, manganese, 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 preparation method of a nickel, manganese, and graphene ternary alloy light-transmitting material, including the following steps:

[0007] Step 1: Dissolve 300 grams of nickel sulfate, 5g of hydrochloric acid, and 1000g of water in proportion to dissolve nickel sulfate, then slowly add a matching complexing agent and dissolve it completely. Wait for the temperature to drop to room temperature, and slowly add 150 milliliters of manganese oxide dissolved in 1000g of pure water and dissolve it completely; after the temperature drops to room temperature, continue to stir for 24 hours, add pure water to 1000 milliliters and continue to stir and complex for 12 hours. After sufficient complexing, slowly add 0.001 grams of graphene dispersant, and stir and perform ultrasonic waves simultaneously for 12 hours to obtain a nickel, manganese, and graphene alloy electroplating solution;

[0008] Step 2: The conductive fiber is ultrasonically cleaned, sulfuric acid activated, cleaned, and then placed in a nickel, manganese, and graphene alloy electroplating solution for electroplating. After electroplating, it is cleaned with pure water and dried; then, it is heat-treated at a high temperature for fiber carbonization to obtain a nickel, manganese, and graphene ternary alloy light-transmitting material with a thickness of 20-30 microns.

[0009] Preferably, the complexing agent is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0010] Preferably, the electroplating temperature is 45-50 °C, and the electroplating current is 30-40 A.

[0011] Preferably, the conditions of the stirring ultrasonic wave are: the stirring speed is 450-550 r / min, and the ultrasonic power is 300-400 KW; the fiber carbonization temperature is 350 °C for 4 h.

[0012] The inventor of the present invention found that the product of the present invention has excellent electromagnetic shielding efficiency values and thermal conductivity coefficients, and the electromagnetic shielding and heat dissipation performances of the product can be coordinately improved; when the nano-graphene modifier of the present invention is directly replaced with nano-graphene raw materials, the performance of the product deteriorates significantly. At the same time, in the preparation of the nano-graphene modifier, S01 treatment is not adopted, regulator treatment is not adopted, lanthanum nitrate solution is not added in the preparation of the regulator, and silica sol is not added in the preparation of the regulator, and the performance of the product shows a deteriorating trend. Only when the nano-graphene modifier prepared by the method of the present invention is used, the performance effect of the product is the most significant.

[0013] Preferably, the preparation method of the graphene dispersant is as follows:

[0014] Take a 1000 ml beaker, add graphene modifiers with a sheet diameter of 20-30 microns and a thickness of 1-3 nanometers, then add a matching surfactant, wetting agent, dispersant, and leveling agent, use ultrasonic waves and rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0015] Preferably, the surfactant is polyethylene glycol at 0.5 g / L, the wetting agent is mannitol at 0.1 g / L, the leveling agent is saccharin sodium at 0.1 g / L; the dispersant is sodium dodecyl sulfate at 0.1 g.

[0016] Preferably, the ultrasonic power is 750-850 KW.

[0017] Preferably, the modification method of the nano-graphene modifier is as follows:

[0018] S01: First, heat-treat the nano-graphene at 310-320 °C for 5-10 min, and then cool it to 45-50 °C at a rate of 1-3 °C / min.

[0019] S02: The product of S01 is stirred evenly in a hydrochloric acid solution with a mass fraction of 2% that is 5 - 10 times the total mass of the product of S01, and then washed with water and dried.

[0020] S03: A regulator accounting for 5 - 10% of the total amount of the product of S02 is added to the product of S02, followed by ball milling. After the ball milling is completed, it is washed with water and dried to obtain a nano-graphene modifier.

[0021] Preferably, the ball milling speed for the ball milling treatment is 1000 - 1500 r / min, and the ball milling time is 20 - 30 min.

[0022] Preferably, the regulator comprises the following raw materials in parts by weight:

[0023] 2 - 4 parts of a lanthanum nitrate solution with a mass fraction of 2%, 2 - 5 parts of silica sol, 1 - 3 parts of a chitosan solution with a mass fraction of 6%, and 0.2 - 0.4 part of sodium dodecylbenzenesulfonate.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] The ternary alloy light-transmitting material of the present invention is mainly applied to high-end electromagnetic shielding materials for national defense and military industries and large contact terminals, which can reduce the generation of electric arcs. The product prepared by the process of the present invention has excellent electromagnetic shielding performance and heat dissipation performance, and the performance of the product can be coordinately improved; it is made of nickel, manganese, and graphene as raw materials through a specific process of the present invention. The graphene dispersant is prepared by mutually blending and coordinating a nano-graphene modifier, an interfacial active agent, a wetting agent, a dispersant, and a leveling agent. At the same time, the nano-graphene modifier is heat-treated with nano-graphene raw materials and then dispersed in hydrochloric acid to improve the dispersion degree and activity. Through the improvement and optimization of a specific regulator of the present invention, the prepared graphene dispersant has a better coordination effect with nickel and manganese raw materials, and the electromagnetic shielding performance and heat dissipation performance of the prepared product can be coordinately improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a schematic diagram of the EDS component analysis report of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0027] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0028] The preparation method of the nickel, manganese, and graphene ternary alloy light-transmitting material in this embodiment includes the following steps:

[0029] Step 1: Dissolve 300 grams of nickel sulfate, 5 grams of hydrochloric acid and 1000 grams of water in proportion to dissolve nickel sulfate, then slowly add a matching complexing agent and dissolve completely. Wait for the temperature to drop to room temperature, add it slowly, and dissolve 150 milliliters of manganese oxide dissolved in 1000 grams of pure water completely; after the temperature drops to room temperature, continue stirring for 24 hours, add pure water to 1000 milliliters and continue stirring and complexing for 12 hours. After sufficient complexing, slowly add 0.001 grams of graphene dispersant and carry out stirring and ultrasonic treatment simultaneously for 12 hours to obtain a nickel, manganese, graphene alloy electroplating solution;

[0030] Step 2: Use conductive fibers to be ultrasonically cleaned, sulfuric acid activated, cleaned, and put into the nickel, manganese, graphene alloy electroplating solution for electroplating. After electroplating, clean with pure water and dry; then heat the fibers at high temperature for carbonization treatment to obtain a 20-30 micron nickel, manganese, graphene ternary alloy light-transmitting material.

[0031] The complexing agent in this embodiment is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0032] The electroplating temperature in this embodiment is 45-50 °C, and the electroplating current is 30-40 A.

[0033] The conditions for stirring and ultrasonic treatment in this embodiment are: the stirring speed is 450-550 r / min, the ultrasonic power is 300-400 KW; the temperature for fiber carbonization is 350 °C for 4 h.

[0034] The preparation method of the graphene dispersant in this embodiment is:

[0035] Take a 1000-milliliter beaker and add graphene modifiers with a sheet diameter of 20-30 microns and a thickness of 1-3 nanometers, then add a matching surfactant, wetting agent, dispersant, and leveling agent, use ultrasonic waves, rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0036] The surfactant in this embodiment is polyethylene glycol at 0.5 grams per liter, the wetting agent is mannitol at 0.1 grams per liter, the leveling agent is saccharin sodium at 0.1 grams per liter; the dispersant is sodium dodecyl sulfate at 0.1 grams.

[0037] The ultrasonic power in this embodiment is 750-850 KW.

[0038] The modification method of the nano-graphene modifier in this embodiment is:

[0039] S01: First heat-treat the nano-graphene at 310-320 °C for 5-10 min, and then cool it to 45-50 °C at a rate of 1-3 °C / min;

[0040] S02: The product of S01 is first stirred evenly in a hydrochloric acid solution with a mass fraction of 2% that is 5 - 10 times its mass, then washed with water and dried.

[0041] S03: Add a regulator accounting for 5 - 10% of the total amount of the S02 product to the S02 product, conduct ball milling treatment. After the ball milling ends, wash with water and dry to obtain a nano-graphene modifier.

[0042] In this example, the ball milling speed for the ball milling treatment is 1000 - 1500 r / min, and the ball milling time is 20 - 30 min.

[0043] The regulator in this example includes the following raw materials in parts by weight:

[0044] 2 - 4 parts of lanthanum nitrate solution with a mass fraction of 2%, 2 - 5 parts of silica sol, 1 - 3 parts of chitosan solution with a mass fraction of 6%, and 0.2 - 0.4 part of sodium dodecylbenzenesulfonate.

[0045] Example 1.

[0046] The preparation method of the nickel, manganese, and graphene ternary alloy light-transmitting material in this example includes the following steps:

[0047] Step 1: Dissolve 300 grams of nickel sulfate, 5 g of hydrochloric acid, and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add a matching complexing agent and dissolve it completely. Wait for the temperature to drop to room temperature, then slowly add 150 ml of manganese oxide dissolved in 1000 g of pure water and dissolve it completely. 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 graphene dispersant and conduct stirring and ultrasonic treatment simultaneously for 12 hours to obtain a nickel, manganese, and graphene alloy electroplating solution.

[0048] Step 2: Use conductive fibers, clean them through ultrasonic cleaning, activate them with sulfuric acid, then clean them and put them into the nickel, manganese, and graphene alloy electroplating solution for electroplating. After electroplating, wash with pure water and dry. Then, after high-temperature heating and fiber carbonization treatment, a 20-micron nickel, manganese, and graphene ternary alloy light-transmitting material can be obtained.

[0049] The complexing agent in this example is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0050] The electroplating temperature in this example is 45 °C, and the electroplating current is 30 A.

[0051] The conditions for stirring and ultrasonic treatment in this example are: the stirring speed is 450 r / min, the ultrasonic power is 300 KW; the temperature for fiber carbonization is 350 °C for 4 h.

[0052] The preparation method of the graphene dispersant in this example is:

[0053] Take a 1000 ml beaker and add a graphene modifier with a diameter of 20 microns and a thickness of 1 nanometer. Then add matching surfactants, wetting agents, dispersants, and moving agents. Use ultrasound to rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0054] The surfactant in this embodiment is 0.5 g / L polyethylene glycol, the wetting agent is 0.1 g / L manna, the displacement agent is 0.1 g / L saccharin sodium; and the dispersant is 0.1 g sodium lauryl sulfate.

[0055] The power of the ultrasonic wave in this embodiment is 750KW.

[0056] The modification method of the nanographene modifier of this embodiment is:

[0057] S01: The nanographene was first heat treated at 310°C for 5 min, and then cooled to 45°C at a rate of 1°C / min;

[0058] S02: The S01 product is first stirred evenly in a 2% hydrochloric acid solution with a mass fraction of 5 times, then washed with water and dried;

[0059] S03: Add a regulator in an amount of 5% of the total amount of the S02 product to the S02 product, and perform ball milling. After the ball milling is completed, wash with water, and dry to obtain a nanographene modifier.

[0060] The ball milling speed of the ball milling treatment in this embodiment is 1000 r / min, and the ball milling time is 20 min.

[0061] The conditioning agent of this embodiment comprises the following raw materials in parts by weight:

[0062] 2 parts of 2% by mass lanthanum nitrate solution, 2 parts of silica sol, 1 part of 6% by mass chitosan solution, and 0.2 parts of sodium dodecylbenzene sulfonate.

[0063] Example 2

[0064] The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material of this embodiment comprises the following steps:

[0065] Step 1: Dissolve nickel sulfate in 300 g of nickel sulfate, 5 g of hydrochloric acid and 1000 g of water in proportion, then slowly add a matching complexing agent to completely dissolve, wait for the temperature to drop to room temperature, slowly add 150 ml of manganese oxide dissolved in 1000 g of pure water to completely dissolve; 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 graphene dispersant, stir and ultrasonicate for 12 hours, and obtain a nickel, manganese and graphene alloy electroplating solution;

[0066] Step 2: Use conductive fibers, which are ultrasonically cleaned, activated with sulfuric acid, cleaned again, and then placed in a nickel, manganese, and graphene alloy electroplating solution for electroplating. After electroplating, they are cleaned with pure water and dried. Then, they are heated at a high temperature for fiber carbonization treatment to obtain a 30-micron nickel, manganese, and graphene ternary alloy light-transmitting material.

[0067] The complexing agent in this example is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0068] The electroplating temperature in this example is 50 °C, and the electroplating current is 40 A.

[0069] The conditions of the stirring ultrasonic wave in this example are: the stirring speed is 550 r / min, and the ultrasonic power is 400 KW; the temperature for fiber carbonization is 350 °C for 4 h.

[0070] The preparation method of the graphene dispersant in this example is as follows:

[0071] Take a 1000-milliliter beaker, add graphene modifiers with a sheet diameter of 30 microns and a thickness of 3 nanometers, and then add a matching surfactant, wetting agent, dispersant, and leveling agent. Use ultrasonic waves and rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0072] The surfactant in this example is polyethylene glycol at 0.5 g per liter, the wetting agent is mannitol at 0.1 g per liter, the leveling agent is saccharin sodium at 0.1 g per liter; the dispersant is sodium dodecyl sulfate at 0.1 g.

[0073] The ultrasonic power in this example is 850 KW.

[0074] The modification method of the nano-graphene modifier in this example is as follows:

[0075] S01: First, place the nano-graphene at 320 °C for heat treatment for 10 min, and then cool it to 50 °C at a rate of 3 °C / min;

[0076] S02: The product of S01 is first stirred evenly in a 2% hydrochloric acid solution with a mass fraction of 10 times, and then washed with water and dried;

[0077] S03: Add a regulator accounting for 10% of the total amount of the product of S02 to the product of S02, and perform ball milling treatment. After the ball milling is completed, wash with water and dry to obtain the nano-graphene modifier.

[0078] The ball milling speed of the ball milling treatment in this example is 1500 r / min, and the ball milling time is 30 min.

[0079] The regulator in this example includes the following raw materials in parts by weight:

[0080] 4 parts of lanthanum nitrate solution with a mass fraction of 2%, 5 parts of silica sol, 3 parts of chitosan solution with a mass fraction of 6%, and 0.4 part of sodium dodecylbenzenesulfonate.

[0081] Example 3

[0082] The preparation method of the nickel, manganese, and graphene ternary alloy light-transmitting material in this example includes the following steps:

[0083] Step 1: Dissolve 300 grams of nickel sulfate, 5 g of hydrochloric acid, and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add a matching complexing agent and dissolve it completely. Wait for the temperature to drop to room temperature, and slowly add 150 ml of manganese oxide dissolved in 1000 g of pure water and dissolve it completely. 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 graphene dispersant, and carry out stirring and ultrasonic treatment simultaneously for 12 hours to obtain a nickel, manganese, and graphene alloy electroplating solution;

[0084] Step 2: Use conductive fibers to undergo ultrasonic cleaning, sulfuric acid activation, and cleaning, then put them into the nickel, manganese, and graphene alloy electroplating solution for electroplating. After electroplating, wash with pure water and dry. Then, after high-temperature heating and fiber carbonization treatment, a 20 - 30 - micron nickel, manganese, and graphene ternary alloy light-transmitting material can be obtained.

[0085] The complexing agent in this example is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0086] The electroplating temperature in this example is 47°C, and the electroplating current is 35 A.

[0087] The conditions for stirring and ultrasonic treatment in this example are: the stirring speed is 500 r / min, and the ultrasonic power is 350 KW; the temperature for fiber carbonization is 350°C for 4 h.

[0088] The preparation method of the graphene dispersant in this example is:

[0089] Take a 1000 - ml beaker, add graphene modifiers with a sheet diameter of 25 microns and a thickness of 2 nanometers, then add a matching surfactant, wetting agent, dispersant, and leveling agent, use ultrasonic waves, and rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0090] The surfactant in this example is polyethylene glycol at 0.5 g / L, the wetting agent is mannitol at 0.1 g / L, the leveling agent is saccharin sodium at 0.1 g / L; the dispersant is sodium dodecyl sulfate at 0.1 g.

[0091] The ultrasonic power in this example is 800 KW.

[0092] The modification method of the nano-graphene modifier in this embodiment is as follows:

[0093] S01: First, heat-treat the nano-graphene at 315 °C for 7.5 min, and then cool it to 47.5 °C at a rate of 2 °C / min;

[0094] S02: The product of S01 is first stirred evenly in a hydrochloric acid solution with a mass fraction of 2% that is 7.5 times the mass, and then washed with water and dried;

[0095] S03: Add a regulator accounting for 7.5% of the total amount of the product of S02 to the product of S02, perform ball milling treatment. After the ball milling ends, wash with water and dry to obtain the nano-graphene modifier.

[0096] The ball milling speed of the ball milling treatment in this embodiment is 1250 r / min, and the ball milling time is 25 min.

[0097] The regulator in this embodiment includes the following raw materials in parts by weight:

[0098] 3 parts of lanthanum nitrate solution with a mass fraction of 2%, 3.5 parts of silica sol, 2 parts of chitosan solution with a mass fraction of 6%, and 0.3 part of sodium dodecylbenzenesulfonate.

[0099] Example 4.

[0100] The preparation method of the nickel, manganese, and graphene ternary alloy light-transmitting material in this embodiment includes the following steps:

[0101] Step 1: Dissolve 300 g of nickel sulfate, 5 g of hydrochloric acid, and 1000 g of water in proportion to dissolve nickel sulfate, and then slowly add a matching complexing agent and dissolve it completely. Wait for the temperature to drop to room temperature, and slowly add 150 ml of manganese oxide dissolved in 1000 g of pure water and dissolve it completely. After the temperature drops to room temperature, continue to stir for 24 hours, add pure water to 1000 ml and continue to stir and complex for 12 hours. After sufficient complexing, slowly add 0.001 g of graphene dispersant and perform stirring and ultrasonic treatment simultaneously for 12 hours to obtain a nickel, manganese, and graphene alloy electroplating solution;

[0102] Step 2: Use conductive fibers to be ultrasonically cleaned, sulfuric acid-activated, cleaned, put into the nickel, manganese, and graphene alloy electroplating solution for electroplating, and after electroplating, wash with pure water and dry; then perform high-temperature heating and fiber carbonization treatment to obtain a 22-micron nickel, manganese, and graphene ternary alloy light-transmitting material.

[0103] The complexing agent in this embodiment is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0104] The electroplating temperature in this embodiment is 46 °C, and the electroplating current is 32 A.

[0105] The conditions of the stirring ultrasonic wave in this embodiment are as follows: the stirring speed is 460 r / min, and the ultrasonic power is 320 KW; the temperature for fiber carbonization is 350 °C for 4 h.

[0106] The preparation method of the graphene dispersant in this embodiment is as follows:

[0107] Take a 1000 - milliliter beaker, add graphene modifiers with a sheet diameter of 22 microns and a thickness of 2 nanometers, then add a matching surfactant, wetting agent, dispersant, and leveling agent. Use ultrasonic waves and rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0108] The surfactant in this embodiment is polyethylene glycol at 0.5 g / L, the wetting agent is mannitol at 0.1 g / L, the leveling agent is sodium saccharin at 0.1 g / L; the dispersant is sodium dodecyl sulfate at 0.1 g.

[0109] The ultrasonic power in this embodiment is 760 KW.

[0110] The modification method of the nano - graphene modifier in this embodiment is as follows:

[0111] S01: First, place the nano - graphene at 312 °C for heat treatment for 6 min, and then cool it to 46 °C at a rate of 2 °C / min;

[0112] S02: The product of S01 is first stirred evenly in a hydrochloric acid solution with a mass fraction of 2% six times the mass, and then washed with water and dried;

[0113] S03: Add a regulator accounting for 6% of the total amount of the product of S02 to the product of S02, and perform ball - milling treatment. After the ball - milling ends, wash with water and dry to obtain the nano - graphene modifier.

[0114] The ball - milling speed of the ball - milling treatment in this embodiment is 1200 r / min, and the ball - milling time is 22 min.

[0115] The regulator in this embodiment includes the following raw materials in parts by weight:

[0116] 3 parts of lanthanum nitrate solution with a mass fraction of 2%, 3 parts of silica sol, 2 parts of chitosan solution with a mass fraction of 6%, and 0.3 part of sodium dodecyl benzene sulfonate.

[0117] Example 5.

[0118] The preparation method of the nickel, manganese, graphene ternary alloy light - transmitting material in this embodiment includes the following steps:

[0119] Step 1: Dissolve 300 g of nickel sulfate, 5 g of hydrochloric acid and 1000 g of water in proportion to dissolve nickel sulfate, then slowly add a matching complexing agent and dissolve completely. Wait for the temperature to drop to room temperature, then slowly add 150 ml of manganese oxide dissolved in 1000 g of pure water and dissolve completely. 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 graphene dispersant and carry out stirring and ultrasonic treatment simultaneously for 12 hours to obtain a nickel, manganese, graphene alloy electroplating solution;

[0120] Step 2: Use conductive fibers, which are ultrasonically cleaned, sulfuric acid activated, and then cleaned, and then put into the nickel, manganese, graphene alloy electroplating solution for electroplating. After electroplating, clean with pure water and dry; then heat the fibers at high temperature for carbonization treatment to obtain a 28-micron nickel, manganese, graphene ternary alloy light-transmitting material.

[0121] The complexing agent in this example is diethylenetriamine, and the addition amount of the complexing agent is 0.1 g.

[0122] The electroplating temperature in this example is 48 °C, and the electroplating current is 38 A.

[0123] The conditions for stirring and ultrasonic treatment in this example are: the stirring speed is 520 r / min, and the ultrasonic power is 380 KW; the temperature for fiber carbonization is 350 °C for 4 h.

[0124] The preparation method of the graphene dispersant in this example is:

[0125] Take a 1000-ml beaker, add graphene modifiers with a sheet diameter of 28 microns and a thickness of 2.8 nanometers, then add a matching surfactant, wetting agent, dispersant, and leveling agent, use ultrasonic waves and rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

[0126] The surfactant in this example is polyethylene glycol at 0.5 g / L, the wetting agent is mannitol at 0.1 g / L, the leveling agent is saccharin sodium at 0.1 g / L; the dispersant is sodium dodecyl sulfate at 0.1 g.

[0127] The ultrasonic power in this example is 810 KW.

[0128] The modification method of the nano-graphene modifier in this example is:

[0129] S01: First heat-treat the nano-graphene at 318 °C for 8 min, and then cool it to 48 °C at a rate of 2 °C / min;

[0130] S02: The product of S01 is first stirred evenly in a hydrochloric acid solution with a mass fraction of 2% that is 8 times its mass, then washed with water and dried;

[0131] S03: Add a regulator accounting for 8% of the total amount of the S02 product to the S02 product, conduct ball milling treatment, and after the ball milling is completed, wash with water and dry to obtain a nano-graphene modifier.

[0132] In this example, the ball milling speed for the ball milling treatment is 1400 r / min, and the ball milling time is 28 min.

[0133] The regulator in this example includes the following raw materials in parts by weight:

[0134] 3 parts of lanthanum nitrate solution with a mass fraction of 2%, 4 parts of silica sol, 2 parts of chitosan solution with a mass fraction of 6%, and 0.35 part of sodium dodecylbenzenesulfonate.

[0135] Comparative Example 1.

[0136] The difference from Example 3 is that the nano-graphene modifier is replaced with nano-graphene.

[0137] Comparative Example 2.

[0138] The difference from Example 3 is that S01 treatment is not used in the preparation of the nano-graphene modifier.

[0139] Comparative Example 3.

[0140] The difference from Example 3 is that regulator treatment is not used in the preparation of the nano-graphene modifier.

[0141] Comparative Example 4.

[0142] The difference from Example 3 is that lanthanum nitrate solution is not added in the preparation of the regulator.

[0143] Comparative Example 5.

[0144] The difference from Example 3 is that silica sol is not added in the preparation of the regulator.

[0145] Conduct performance tests on the products of Examples 1 - 5 and Comparative Examples 1 - 5, and the test results are as follows

[0146] Electromagnetic shielding effectiveness value (dB) Thermal conductivity (W / mk) Example 1 96 2500 Example 2 97 2535 Example 3 98 2550 Example 4 97 2540 Example 5 97 2548 Comparative Example 1 87 2035 Comparative Example 2 94 2350 Comparative Example 3 90 2120 Comparative Example 4 92 2210 Comparative Example 5 94 2275

[0147] It can be seen from Comparative Examples 1 - 5 and Examples 1 - 5;

[0148] The product of Example 3 has excellent electromagnetic shielding efficiency value and thermal conductivity, and the electromagnetic shielding and heat dissipation performance of the product can be coordinately improved. It can be seen from Comparative Examples 1-5 and Example 3 that when the nano-graphene modifier of the present invention is replaced by nano-graphene, the performance of the product deteriorates significantly. At the same time, when the nano-graphene modifier is not treated with S01, not treated with a regulator, lanthanum nitrate solution is not added during the preparation of the regulator, and silica sol is not added during the preparation of the regulator, the performance of the product shows a deteriorating trend. Only when the nano-graphene modifier prepared by the method of the present invention is used, the performance effect of the product is the most significant.

[0149] 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.

[0150] 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. A method for preparing a nickel, manganese, and graphene ternary alloy light-transmitting material, characterized in that: The following steps are involved: Step 1: Dissolve nickel sulfate in 300 g of nickel sulfate, 5 g of hydrochloric acid and 1000 g of water in proportion, then slowly add a matching complexing agent to completely dissolve, wait for the temperature to drop to room temperature, slowly add 150 ml of manganese oxide dissolved in 1000 g of pure water to completely dissolve; 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 graphene dispersant, stir and ultrasonicate for 12 hours, and obtain a nickel, manganese and graphene alloy electroplating solution; Step 2: Use the conductive fiber to undergo ultrasonic cleaning, sulfuric acid activation, and cleaning, and then put it into the nickel, manganese, and graphene alloy plating solution to start electroplating. After electroplating, it is washed with pure water and dried; after high-temperature heating and fiber carbonization treatment, a 20-30 micron nickel, manganese, and graphene ternary alloy translucent material can be obtained.

2. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The complexing agent is diethylenetriamine, and the amount of the complexing agent added is 0.1 g.

3. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The electroplating temperature is 45-50° C., and the electroplating current is 30-40A.

4. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The stirring ultrasonic conditions are: stirring speed of 450-550 r / min, ultrasonic power of 300-400 KW; fiber carbonization temperature of 350° C. for 4 hours.

5. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 1, characterized in that: The preparation method of the graphene dispersant is: Take a 1000 ml beaker and add a graphene modifier with a sheet diameter of 20-30 microns and a thickness of 1-3 nanometers, then add matching surfactants, wetting agents, dispersants, and moving agents, use ultrasound to rotate and stir for 48 hours, and then use a vacuum machine to extract the bubbles to prepare the graphene dispersant.

6. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 5, characterized in that: The surfactant is 0.5 g / L polyethylene glycol, the wetting agent is 0.1 g / L manna, the displacement agent is 0.1 g / L saccharin sodium; and the dispersant is 0.1 g sodium dodecyl sulfate.

7. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 5, characterized in that: The power of the ultrasonic wave is 750-850KW.

8. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 5, characterized in that: The modification method of the nanographene modifier is: S01: heat treating the nanographene at 310-320°C for 5-10 min, and then cooling to 45-50°C at a rate of 1-3°C / min; S02: The S01 product is first stirred evenly in a 2% hydrochloric acid solution with a mass fraction of 5-10 times the total amount of the S01 product, then washed with water and dried; S03: Add 5-10% of the total amount of the S02 product to the S02 product, perform ball milling, and after the ball milling is completed, wash with water and dry to obtain a nanographene modifier.

9. The nickel, manganese, graphene ternary alloy light-transmitting material according to claim 8, characterized in that: The ball milling speed of the ball milling treatment is 1000-1500r / min, and the ball milling time is 20-30min.

10. The method for preparing the nickel, manganese and graphene ternary alloy light-transmitting material according to claim 8, characterized in that: The regulator comprises the following raw materials in parts by weight: 2-4 parts of 2% by mass lanthanum nitrate solution, 2-5 parts of silica sol, 1-3 parts of 6% by mass chitosan solution, and 0.2-0.4 parts of sodium dodecylbenzene sulfonate.

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