Method for manufacturing light-transmitting material

Abstract

Disclosed is a manufacturing method for a ternary alloy material comprising nickel, carbon, and graphene. The manufacturing method for the corresponding material is as follows: A conductive material is subjected to the steps of ultrasonic cleaning, sulfuric acid activation, and washing, and then is put into a nickel-carbon-graphene alloy electrolyte to start electrolysis, followed by washing with pure water and drying. Afterwards, through a high-temperature heating conductive carbonization treatment,a ternary alloy material comprising nickel, carbon, and graphene, of 50-100 micrometers is obtained. The ternary alloy material of the present invention is mainly applied to high-quality electromagnetic shielding and absorbing materials and to the reduction of electric arc generation of a large contact terminal, and a product manufactured by the process of the present invention has excellent electromagnetic shielding and absorbance performance and heat dissipation performance, and thus the performance of the product may be improved in a well-balanced manner.

Description

Method for manufacturing light-transmitting materials

[0001] The present invention relates to a method for manufacturing a light-transmitting material, and in particular to a method for manufacturing a nickel, carbon, and graphene ternary alloy light-transmitting material.

[0002] Conductive cloths can be classified into: fiber cloths (commonly used polysound fiber cloths) that are pretreated with electroplating metal plating to acquire metallic properties and become conductive fiber cloths; nickel-plated conductive cloths, gold-plated conductive cloths, carbon-plated conductive cloths, and aluminum foil fiber composite cloths; appearances that differ between general and mesh types; and ternary alloy translucent materials primarily used for defense, military, and industrial high-grade electromagnetic shielding and large contacts. Terminals often used in conjunction with conductive cloths can reduce arc generation.

[0003] While the electromagnetic shielding effect of existing ternary alloy translucent materials is poor, the heat dissipation performance is low. The types of metal transparent electromagnetic shielding materials and their manufacturing methods, such as Chinese patent document CN112930100B, are provided using gold, silver, copper, alloys, and other nano-metal materials with excellent conductivity as the main body for electromagnetic shielding of electromagnetic waves, and organic glass and other transparent substrates as supports for inorganic and inorganic composite transparent films. As a result, it is difficult to achieve improved electromagnetic shielding effect and heat dissipation control, and the use of the product's efficiency is limited.

[0004] The objective of the present invention is to provide a method for manufacturing a ternary alloy of nickel, carbon, and graphene as a light-transmitting material in order to address the defects of the prior art and solve the problems raised in the background art.

[0005] The technical problems to be solved by the present invention are not limited to those mentioned above, and other technical problems not mentioned will be clearly understood by those skilled in the art to which the present invention belongs from the description below.

[0006] The method for manufacturing a light-transmitting material according to the present invention to achieve the above technical problem comprises the following steps: the present invention provides a method for manufacturing a light-transmitting material from a ternary alloy of nickel, carbon, and graphene:

[0007] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0008] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electroplating. After electroplating, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a nickel, carbon, and graphene ternary alloy transparent material with a thickness of 50-100 micrometers.

[0009] Preferably, the complexing agent is polyethylene glycol and the amount added is 0.1g.

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

[0011] The stirring ultrasonic conditions may be a stirring speed of 450-550 r / min and an ultrasonic power of 300-400 KW. Fiber carbonization treatment may be performed at a temperature of 350°C for 4 hours.

[0012] The light-transmitting material of the present invention may be in powder form. In such case, it may be heat-treated at 700 to 950°C for powder processing. A conveyor-type heat treatment furnace may be used for the heat treatment. The heat treatment time may be, for example, 1 to 8 hours, 2 to 6 hours, 3 to 5 hours, etc.

[0013] After heat treatment, it can be turned into powder through mechanical grinding.

[0014] In the case of a powder form, the particle size may be, for example, 100 to 800 mesh, 100 to 700 mesh, 100 to 600 mesh, 100 to 500 mesh, 100 to 400 mesh, 200 to 300 mesh, etc.

[0015] The inventors of the present invention have discovered that the product of the present invention possesses excellent electromagnetic shielding efficacy and thermal conductivity coefficients, and that the electromagnetic shielding and heat dissipation performance of the product can be harmoniously improved. The nanographene modifier of the present invention is used to directly replace nanographene raw materials, and without using the method of the present invention, the product performance is significantly degraded. Furthermore, in the manufacturing process of the nanographene modifier, S01 treatment is not used, modifier treatment is not used, lanthanum nitrate solution is not added during the preparation of the modifier, and silica sol is not added, all of which showed a tendency for the product performance to degrade. The product performance effect was most pronounced only through the nanographene modifier manufactured using the method of the present invention.

[0016] Preferably, the graphene dispersant is prepared by the following:

[0017] A graphene modifier with a diameter of 50 to 100 micrometers and a thickness of 3 to 5 nm is placed in a 1000 ml beaker, and a suitable surfactant, wetting agent, dispersant, and transport agent are added. The mixture is then stirred using ultrasound for 48 hours, and bubbles are removed using a vacuum cleaner to prepare a graphene dispersant.

[0018] Preferably, the surfactant may be 0.5 g / L of polyethylene glycol, the wetting agent may be 0.1 g / L of mannitol, the transfer agent may be 0.1 g / L of sodium saccharin, and the dispersant may be 0.1 g of sodium dodecyl sulfate.

[0019] Preferably, the output of the corresponding ultrasound can be 750-850 KW.

[0020] Preferably, the nanographene modifier can be prepared as follows:

[0021] S01: After heat-treating nanographene at 310-320℃ for 5-10 min, cool it to 45-50℃ at a rate of 1-3℃ / min;

[0022] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass 5-10 times the total amount of the S01 product, then washed with water and dried;

[0023] S03: Add a modifier of 5-10% of the total amount of S02 product to the S02 product, ball mill treatment, washing, and drying to obtain the nanographene modifier.

[0024] Preferably, the ball mill treatment may be performed at a rotational speed of 1000-1500 r / min and for 20-30 min.

[0025] Preferably, the modifier comprises the following components by weight: 2-4 parts of a 2 wt% lanthanum nitrate solution, 2-5 parts of silica sol, 1-3 parts of a 6 wt% chitosan solution, and 0.2-0.4 parts of sodium dodecylbenzenesulfonate.

[0026] The above embodiments of the present invention are merely some of the preferred embodiments of the present invention, and various embodiments reflecting the technical features of the present invention can be derived and understood by those skilled in the art based on the detailed description of the present invention to be described below.

[0027] Compared to existing technology, the beneficial effects of the present invention are as follows:

[0028] The ternary alloy light-transmitting material of the present invention is primarily applied to high-grade electromagnetic shielding materials and large contact terminals in the defense and military industries, and can reduce the generation of electric arcs. Products manufactured using the process of the present invention possess excellent electromagnetic shielding and heat dissipation performance, and product performance can be harmoniously improved. It is manufactured using nickel, carbon, and graphene as raw materials through a specific process of the present invention, and the graphene dispersant utilizes a combination of a nanographene modifier, surfactant, wetting agent, dispersant, and transporter. Furthermore, the nanographene modifier enhances the dispersion and activity of the nanographene raw material through hydrochloric acid dispersion following heat treatment, and the graphene dispersant manufactured by improving and optimizing with the specific regulator of the present invention harmonizes with the nickel and carbon raw materials to exhibit better effects. The electromagnetic shielding and heat dissipation performance of the manufactured product can be harmoniously improved.

[0029] The effects obtainable from the present invention are not limited to those mentioned above, and other unmentioned effects will be clearly understood by those skilled in the art from the description below.

[0030] Figure 1 is a schematic diagram of the EDS composition analysis report of the present invention.

[0031] The following describes the technical methods included in the embodiments of the present invention clearly and completely, together with the drawings included in the embodiments of the present invention. Clearly, the described embodiments are only some embodiments of the present invention and do not include all embodiments. Based on the embodiments of the present invention, all other embodiments that a person skilled in the art can obtain without creative effort fall within the scope of protection of the present invention.

[0032] The method for manufacturing a nickel, carbon, and graphene ternary alloy light-transmitting material of the present embodiment comprises the following steps:

[0033] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0034] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a nickel, carbon, and graphene ternary alloy transparent material with a thickness of 50-100 micrometers.

[0035] In this embodiment, the complexing agent is polyethylene glycol, and the amount added is 0.1g.

[0036] In this embodiment, the electrolysis temperature is 45-50℃ and the current is 30-40A.

[0037] In this embodiment, the stirring ultrasonic conditions are a stirring speed of 450-550 r / min and an ultrasonic output of 300-400 KW, and the fiber carbonization treatment is 4 hours at 350°C.

[0038] The light-transmitting material of the present invention may be in powder form. In such case, it may be heat-treated at 700 to 950°C for powder processing. A conveyor-type heat treatment furnace may be used for the heat treatment. The heat treatment time may be, for example, 1 to 8 hours, 2 to 6 hours, 3 to 5 hours, etc.

[0039] After heat treatment, it can be turned into powder through mechanical grinding.

[0040] In the case of a powder form, the particle size may be, for example, 100 to 800 mesh, 100 to 700 mesh, 100 to 600 mesh, 100 to 500 mesh, 100 to 400 mesh, 200 to 300 mesh, etc.

[0041] The graphene dispersant of this embodiment can be prepared as follows:

[0042] A graphene modifier with a diameter of 50-100 micrometers and a thickness of 3-5 nanometers is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, ultrasonic and rotary stirring are performed for 48 hours, and bubbles are removed with a vacuum to obtain the graphene dispersant.

[0043] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the moving agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0044] In this embodiment, the output of the ultrasound is 750-850 KW.

[0045] The method for preparing the nanographene modifier of this embodiment is as follows:

[0046] S01: Heat-treat nanographene at 310-320℃ for 5-10 min, then cool to 45-50℃ at a rate of 1-3℃ / min

[0047] S02: Stir the S01 product in a 2% hydrochloric acid solution at a mass 5-10 times the total amount of the S01 product, then wash with water and dry.

[0048] S03: Add a modifier of 5-10% of the total amount of S02 product to the S02 product, ball mill treatment, washing, and drying to obtain the nanographene modifier.

[0049] In the ball milling process of this embodiment, the ball milling speed is 1000-1500 r / min and the ball milling time is 20-30 minutes.

[0050] The modifier of the present embodiment comprises the following components:

[0051] The modifier is 2-4 parts of 2 wt% lanthanum nitrate solution, 2-5 parts of silica sol, 1-3 parts of 6 wt% chitosan solution, and 0.2-0.4 parts of sodium dodecylbenzenesulfonate.

[0052]

[0053] Example 1

[0054] The method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene according to the present embodiment comprises the following steps:

[0055] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0056] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a nickel, carbon, and graphene ternary alloy transparent material with a thickness of 80 micrometers.

[0057] In this embodiment, the complexing agent is polyethylene glycol, and the amount of complexing agent added is 0.1g.

[0058] In this embodiment, the electrolysis temperature is 45°C and the current is 30A.

[0059] In this embodiment, the stirring ultrasonic conditions are: stirring rotation speed 450 r / min, ultrasonic output 300 KW, and carbonization is treated at 350°C for 4 hours.

[0060] The graphene dispersant of this embodiment is prepared as follows:

[0061] A graphene modifier with a diameter of 50 micrometers and a thickness of 3 nm is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, and the mixture is rotated and stirred using ultrasound for 48 hours, after which bubbles are removed using a vacuum cleaner to produce the graphene dispersant in-house.

[0062] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the transfer agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0063] In this embodiment, the output of the ultrasound is 750KW.

[0064] The method of modifying the nanographene modifier of this embodiment is as follows:

[0065] S01: Graphene nanoparticles are first heat-treated at 310°C for 5 minutes, then cooled to 45°C at a rate of 1°C / min;

[0066] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass 5 times the total amount of the S01 product, then washed with water and dried;

[0067] S03: Add a modifier of 5% of the total amount of S02 product to the S02 product, ball mill treatment, washing, and drying to obtain the nanographene modifier.

[0068] The ball mill treatment of this embodiment is performed at a rotational speed of 1000 r / min and for 20 minutes.

[0069] The regulator of the present embodiment comprises the following components on a weight basis:

[0070] 2 parts of 2wt% lanthanum nitrate solution, 2 parts of silica sol, 1 part of 6wt% chitosan solution, 0.2 parts of sodium dodecylbenzenesulfonate

[0071]

[0072] Example 2

[0073] The method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene according to the present embodiment comprises the following steps:

[0074] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0075] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a 90-micrometer nickel, carbon, and graphene ternary alloy transparent material.

[0076] In this embodiment, the complexing agent is polyethylene glycol, and the amount of complexing agent added is 0.1g.

[0077] In this embodiment, the electrolysis temperature is 50°C and the current is 40A.

[0078] In this embodiment, the stirring ultrasonic conditions are: stirring rotation speed 550 r / min, ultrasonic output 400 KW, and carbonization is performed at 350°C for 4 hours.

[0079] The graphene dispersant of this embodiment is prepared as follows:

[0080] A graphene modifier with a diameter of 70 micrometers and a thickness of 3 nm is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, and the mixture is stirred using ultrasound for 48 hours, after which bubbles are removed using a vacuum cleaner to produce a graphene dispersant.

[0081] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the transfer agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0082] In this embodiment, the output of the ultrasound is 850KW.

[0083] The method of modifying the nanographene modifier of this embodiment is as follows:

[0084] S01: Graphene nanoparticles are first heat-treated at 320°C for 10 minutes, then cooled to 50°C at a rate of 3°C / min;

[0085] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass 10 times the total amount of the S01 product, then washed with water and dried;

[0086] S03: A modifier of 10% of the total amount of S02 product is added to the S02 product, ball milled, washed, and dried to obtain the nanographene modifier.

[0087] The ball mill treatment of this embodiment is performed at a rotational speed of 1500 r / min and for 30 minutes.

[0088] The regulator of the present embodiment comprises the following components on a weight basis:

[0089] 4 parts of 2wt% lanthanum nitrate solution, 5 parts of silica sol, 3 parts of 6wt% chitosan solution, 0.4 parts of sodium dodecylbenzenesulfonate

[0090]

[0091] Example 3

[0092] The method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene according to the present embodiment comprises the following steps:

[0093] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0094] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a 30-micrometer nickel, carbon, and graphene ternary alloy transparent material.

[0095] In this embodiment, the complexing agent is polyethylene glycol, and the amount of complexing agent added is 0.1g.

[0096] In this embodiment, the electrolysis temperature is 50°C and the current is 40A.

[0097] In this embodiment, the stirring ultrasonic conditions are: stirring rotation speed 550 r / min, ultrasonic output 400 KW, and carbonization is performed at 350°C for 4 hours.

[0098] The graphene dispersant of this embodiment is prepared as follows:

[0099] A graphene modifier with a diameter of 30 micrometers and a thickness of 3 nm is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, and the mixture is rotated and stirred using ultrasound for 48 hours, after which bubbles are removed using a vacuum cleaner to produce a graphene dispersant.

[0100] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the transfer agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0101] In this embodiment, the output of the ultrasound is 850KW.

[0102] The method of modifying the nanographene modifier of this embodiment is as follows:

[0103] S01: Graphene nanoparticles are first heat-treated at 320°C for 10 minutes, then cooled to 50°C at a rate of 3°C / min;

[0104] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass 10 times the total amount of the S01 product, then washed with water and dried;

[0105] S03: A modifier of 10% of the total amount of S02 product is added to the S02 product, ball milled, washed, and dried to obtain the nanographene modifier.

[0106] The ball mill treatment of this embodiment is performed at a rotational speed of 1500 r / min and for 30 minutes.

[0107] The regulator of the present embodiment comprises the following components on a weight basis:

[0108] 4 parts of 2wt% lanthanum nitrate solution, 5 parts of silica sol, 3 parts of 6wt% chitosan solution, 0.4 parts of sodium dodecylbenzenesulfonate

[0109]

[0110] Example 3

[0111] The method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene according to the present embodiment comprises the following steps:

[0112] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0113] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a 60-micrometer nickel, carbon, and graphene ternary alloy transparent material.

[0114] In this embodiment, the complexing agent is polyethylene glycol, and the amount of complexing agent added is 0.1g.

[0115] In this embodiment, the electrolysis temperature is 47°C and the current is 35A.

[0116] In this embodiment, the stirring ultrasonic conditions are: a stirring rotation speed of 500 r / min and an ultrasonic output of 350 KW, and carbonization is performed at 350°C for 4 hours.

[0117] The graphene dispersant of this embodiment is prepared as follows:

[0118] A graphene modifier with a diameter of 60 micrometers and a thickness of 3 nm is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, and the mixture is rotated and stirred using ultrasound for 48 hours, after which bubbles are removed using a vacuum cleaner to produce the graphene dispersant in-house.

[0119] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the transfer agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0120] In this embodiment, the output of the ultrasound is 800KW.

[0121] The method of modifying the nanographene modifier of this embodiment is as follows:

[0122] S01: Graphene nanoparticles are first heat-treated at 315°C for 7.5 minutes, then cooled to 47.5°C at a rate of 2°C / min;

[0123] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass 7.5 times the total amount of the S01 product, then washed with water and dried;

[0124] S03: A modifier of 7.5% of the total amount of S02 product is added to the S02 product, ball milled, washed, and dried to obtain the nanographene modifier.

[0125] The ball mill treatment of this embodiment is performed at a rotational speed of 1250 r / min and for 25 minutes.

[0126] The regulator of the present embodiment comprises the following components on a weight basis:

[0127] 3 parts of 2wt% lanthanum nitrate solution, 3.5 parts of silica sol, 2 parts of 6wt% chitosan solution, 0.3 parts of sodium dodecylbenzenesulfonate

[0128]

[0129] Example 4

[0130] The method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene according to the present embodiment comprises the following steps:

[0131] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0132] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a 56-micrometer nickel, carbon, and graphene ternary alloy transparent material.

[0133] In this embodiment, the complexing agent is polyethylene glycol, and the amount of complexing agent added is 0.1g.

[0134] In this embodiment, the electrolysis temperature is 46°C and the current is 32A.

[0135] In this embodiment, the stirring ultrasonic conditions are: a stirring rotation speed of 460 r / min and an ultrasonic output of 320 KW, and carbonization is performed at 350°C for 4 hours.

[0136] The graphene dispersant of this embodiment is prepared as follows:

[0137] A graphene modifier with a diameter of 22 micrometers and a thickness of 2 nm is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, and the mixture is rotated and stirred using ultrasound for 48 hours, after which bubbles are removed using a vacuum cleaner to produce the graphene dispersant in-house.

[0138] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the transfer agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0139] In this embodiment, the output of the ultrasound is 760KW.

[0140] The method of modifying the nanographene modifier of this embodiment is as follows:

[0141] S01: Graphene nanoparticles are first heat-treated at 312°C for 6 minutes, then cooled to 46°C at a rate of 2°C / min;

[0142] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass six times the total amount of the S01 product, then washed with water and dried;

[0143] S03: Add a modifier of 6% of the total amount of S02 product to the S02 product, ball mill treatment, washing, and drying to obtain the nanographene modifier.

[0144] The ball milling process of this embodiment is performed at a rotational speed of 1200 r / min and for 22 minutes.

[0145] The regulator of the present embodiment comprises the following components on a weight basis:

[0146] 3 parts 2wt% lanthanum nitrate solution, 3 parts silica sol, 2 parts 6wt% chitosan solution, 0.3 parts sodium dodecylbenzenesulfonate

[0147]

[0148] Example 5

[0149] The method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene according to the present embodiment comprises the following steps:

[0150] First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte.

[0151] Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a 65-micrometer nickel, carbon, and graphene ternary alloy transparent material.

[0152] In this embodiment, the complexing agent is polyethylene glycol, and the amount of complexing agent added is 0.1g.

[0153] In this embodiment, the electrolysis temperature is 48°C and the current is 38A.

[0154] In this embodiment, the stirring ultrasonic conditions are: a stirring rotation speed of 520 r / min and an ultrasonic output of 380 KW, and carbonization is performed at 350°C for 4 hours.

[0155] The graphene dispersant of this embodiment is prepared as follows:

[0156] A graphene modifier with a diameter of 70 micrometers and a thickness of 4.2 nm is placed in a 1000 ml beaker, a surfactant, a wetting agent, a dispersant, and a transport agent are added, and the mixture is rotated and stirred using ultrasound for 48 hours, after which bubbles are removed using a vacuum cleaner to produce a graphene dispersant.

[0157] In this embodiment, the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the moving agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

[0158] In this embodiment, the output of the ultrasound is 810KW.

[0159] The method of modifying the nanographene modifier of this embodiment is as follows:

[0160] S01: Graphene nanoparticles are first heat-treated at 318°C for 8 minutes, then cooled to 48°C at a rate of 2°C / min;

[0161] S02: The S01 product is stirred in a 2% hydrochloric acid solution at a mass 8 times the total amount of the S01 product, then washed with water and dried;

[0162] S03: Add a modifier of 8% of the total amount of S02 product to the S02 product, ball mill treatment, washing, and drying to obtain the nanographene modifier.

[0163] The ball milling process of this embodiment is performed at a rotational speed of 1400 r / min and for 28 minutes.

[0164] The regulator of the present embodiment comprises the following components on a weight basis:

[0165] 3 parts of 2wt% lanthanum nitrate solution, 4 parts of silica sol, 2 parts of 6wt% chitosan solution, 0.35 parts of sodium dodecylbenzenesulfonate

[0166]

[0167] Comparative Example 1

[0168] The nanographene modifier was replaced with nanographene, which is different from Example 3.

[0169] Comparative Example 2

[0170] It differs from Example 3 in that S01 treatment was not performed when manufacturing the nanographene modifier.

[0171] Comparative Example 3

[0172] It differs from Example 3 in that no modifier treatment was performed when manufacturing the nanographene modifier.

[0173] Comparative Example 4

[0174] It differs from Example 3 in that lanthanum nitrate solution was not added when preparing the regulator.

[0175] Comparative Example 5

[0176] It differs from Example 3 in that silica sol was not added when manufacturing the regulator.

[0177] Performance tests were conducted on the products of Examples 1 to 5 and Comparative Examples 1 to 5, and the test results are as follows.

[0178]

[0179] Electromagnetic Shielding Effect Value (dB) Thermal Conductivity (W / mk) Example 1962500 Example 2972535 Example 3982550 Example 4972540 Example 5972548 Ratio 1872035 Ratio 2942350 Ratio 3902120 Ratio 4922210 Ratio 5942275

[0180] As can be seen in Comparative Examples 1-5 and Examples 1-5;

[0181] The product of Example 3 possesses excellent electromagnetic shielding and absorption efficiency values ​​and thermal conductivity, and the electromagnetic shielding and heat dissipation performance of the product can be harmoniously improved. As can be seen in Comparative Examples 1-5 and Example 3, replacing the nanographene modifier of the present invention with nanographene significantly degrades the performance of the product. At the same time, if S01 treatment is not performed during the preparation of the nanographene modifier, if a modifier treatment is not performed, if a lanthanum nitrate solution is not added during the preparation of the modifier, or if silica sol is not added during the preparation of the modifier, the performance of the product tends to degrade. Only the nanographene modifier prepared by the method of the present invention exhibits the most superior product performance effect.

[0182] To those skilled in the art, it is evident that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention may be embodied in other specific forms without departing from the spirit or basic features of the invention. Accordingly, the embodiments should be regarded as exemplary and non-limiting in any respect, and the scope of the invention is defined by the appended claims, not by the description above. Accordingly, all variations within the meaning and scope of the equivalents of the claims are intended to be included in the invention.

[0183] In addition, it should be understood that while this specification is described according to embodiments, each embodiment does not contain only a single independent technical solution. This manner of description in the specification is merely for clarity, and a person skilled in the art should view the specification as a whole and the technical solutions of each embodiment may be appropriately combined to form other embodiments that a person skilled in the art can understand.

Claims

1. First step: Dissolve 300g of nickel-aminosulfonate, 5g of hydrochloric acid, and 1000g of water in the appropriate ratio to dissolve the nickel-aminosulfonate, then slowly add a complexing agent to completely dissolve it. After the temperature is lowered to room temperature, slowly add 150ml of nickel acetate dissolved in 1000g of water to completely dissolve it. After the temperature is lowered to room temperature, stir for another 24 hours, then add water up to 1000ml and complex for another 12 hours. After complexing, slowly add 0.001g of graphene dispersant and stir with ultrasound for 12 hours to obtain a nickel, carbon, and graphene alloy electrolyte. Second step: The conductive fiber is cleaned with ultrasound, activated with sulfuric acid, and then placed in a nickel, carbon, and graphene alloy electrolyte to start electrolysis. After electrolysis, it is washed with water and dried. Subsequently, the fiber is carbonized to obtain a nickel, carbon, and graphene ternary alloy transparent material with a thickness of 50-100 micrometers. A method for manufacturing a ternary alloy light-transmitting material of nickel, carbon, and graphene comprising 2. The method of claim 1, wherein the complexing agent is polyethylene glycol and the amount added is 0.1g.

3. The method of claim 1, wherein the electrolysis temperature is 45-50℃ and the current is 30-40A.

4. A method according to claim 1, wherein the stirring ultrasonic conditions are a stirring speed of 450-550 r / min and an ultrasonic output of 300-400 KW, and the fiber carbonization treatment is performed at 350℃ for 4 hours.

5. A method according to claim 1, further comprising the step of adding a graphene modifier with a diameter of 50-100 micrometers and a thickness of 3-5 nanometers to a 1000 ml beaker, adding a surfactant, a wetting agent, a dispersant, and a transport agent, performing ultrasonic and rotary stirring for 48 hours, and removing bubbles with a vacuum to obtain the graphene dispersant.

6. The method of claim 5, wherein the surfactant is polyethylene glycol 0.5 g / L, the wetting agent is mannitol 0.1 g / L, the transfer agent is sodium saccharin 0.1 g / L, and the dispersant is sodium dodecyl sulfate 0.1 g.

7. The method of claim 5, wherein the ultrasonic output is 750-850KW.

8. In Claim 5, S01: Heat-treat nanographene at 310-320℃ for 5-10 min, then cool to 45-50℃ at a rate of 1-3℃ / min S02: Stir the S01 product in a 2% hydrochloric acid solution at a mass 5-10 times the total amount of the S01 product, then wash with water and dry. S03: A method further comprising the step of obtaining the nanographene modifier by adding a modifier of 5-10% of the total amount of the S02 product to the S02 product, ball milling, washing, and drying.

9. The method of claim 8, wherein the ball mill treatment is performed at a rotational speed of 1000-1500 r / min and a time of 20-30 min.

10. The method of claim 8, wherein the modifier comprises 2-4 parts of a 2% lanthanum nitrate solution, 2-5 parts of a silica sol, 1-3 parts of a 6% chitosan solution, and 0.2-0.4 parts of sodium dodecylbenzenesulfonate.

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