CN112029460A - Preparation method of plasma graphene permeable adhesive - Google Patents
Preparation method of plasma graphene permeable adhesive Download PDFInfo
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- CN112029460A CN112029460A CN202010913030.7A CN202010913030A CN112029460A CN 112029460 A CN112029460 A CN 112029460A CN 202010913030 A CN202010913030 A CN 202010913030A CN 112029460 A CN112029460 A CN 112029460A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/309—Sulfur containing acids
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Abstract
The invention relates to a preparation method of a plasma graphene permeable adhesive, which is characterized by comprising the following steps: the preparation method of the plasma graphene permeable adhesive comprises the following steps of preparing an adhesive base material: EA 9396 epoxy resin; reinforcing materials: the purity of the single-layer graphene stripped by a physical method is 99.9%; catalytic material: argon in plasma state, oxygen elements Ar and O2(ii) a Stabilizing material: NaOH, HNO3Sulfuric acid H2SO4Is prepared from the raw materials. According to the invention, the preparation method of the plasma graphene permeable adhesive is adopted to excite the activity of graphene atoms and the stability of the specific hexagonal atomic structure thereof, improve the physical properties, enhance the physical strength and permeability thereof, and overcome the problems of poor fusion and precipitation of the graphene atoms. Improve the fusibility of graphene in liquid without precipitation. The physical property and the permeability of the graphene permeable adhesive after use are improved.
Description
The invention relates to the technical field of chemical industry, belongs to a preparation technology of a plasma graphene permeable adhesive, is applied to the fields of aviation, ocean engineering, metallurgy, mines, vehicle traffic and the like, and particularly relates to a preparation method of the plasma graphene permeable adhesive.
Background
Graphene is used as the thinnest 'two-dimensional material', and high-purity graphene has extremely strong material strength and toughness. High thermal and electrical conductivity. Due to the excellent improvement of mechanical properties, the related graphene glue and various glue coating products are widely applied. However, graphene is poor in compatibility in epoxy resin and other similar gels, is very easy to precipitate, is quickly oxidized, and the practical effect of the product is not improved or reduced. Conventional epoxy resins and related gel-like products have long been used in the prior art for the preparation of composite materials or for adhesive bonding materials. However, the adhesive property thereof is seriously deteriorated under high temperature, high pressure or complicated environment. In recent years, the problem of dissolving-in property of the nano material of the adhesive prepared by adding the nano material catalyst is not solved, so that the nano material forms precipitates in a short time, the adhesive is forced to be used at present, and the storage period is extremely short. The application development of the graphene is subjected to bottleneck. The plasma graphene permeable adhesive prepared by the method has a storage life of 24 months at normal temperature without precipitates, and the shear force test is consistent with the data of the initial agent. The graphene is used as the strongest two-dimensional material, the permeability of the graphene is far higher than that of other nano materials, the problem of the compatibility and the stability of the graphene and epoxy resin is solved, and the method is a key for preparing the graphene permeable adhesive.
Disclosure of Invention
The invention overcomes the defects, aims to solve the problems that a nano material forms a precipitate in a short time, the storage period of an adhesive is short and the like, can greatly improve the mechanical shearing property of the adhesive, and provides a preparation method of a plasma graphene permeable adhesive.
The preparation method of the plasma graphene permeable adhesive is briefly described as follows:
the preparation method of the plasma graphene permeable adhesive is characterized by comprising the following steps:
the preparation method of the plasma graphene permeable adhesive comprises the following steps of preparing an adhesive base material: EA 9396 epoxy resin; reinforcing materials: the purity of the single-layer graphene stripped by a physical method is 99.9%; catalytic material: argon Ar in plasma state and oxygen element O2(ii) a Stabilizing material: NaOH, HNO3Sulfuric acid H2SO4；
The raw material ratio is as follows:
graphene and epoxy resin: 1: 1000 or 2: 1000; the ratio of the graphene epoxy resin to the stabilizing material is 1: 0.07; the catalytic material proportion is as follows: argon Ar oxygen O2The element ratio is 1: 1; the proportion of the stabilizing material is as follows: according to the ratio of sodium hydroxide NaOH to nitric acid HNO3 Sulfuric acid H2SO4In a ratio of 1: 0.5: 0.5.
The plasma graphene permeable adhesive is prepared by the following process steps:
1. preparing plasma coating graphene, and using a plasma coating generator to mix argon Ar and oxygen element O2The graphene is attached to the outer surface of graphene in a plasma state so as to enhance the activity of the graphene and the stability of the specific hexagonal atomic structure of the graphene; placing graphene powder in a containing groove of a plasma generator by adopting a plasma coating generator; argon Ar and oxygen O2The elements are sprayed out from the top microwave oscillation nozzle in a microwave mode, when the bottom tray rotates, graphene powder floats in the containing tank in a suspension mode, and all powder in the tank is sprayed by microwaves in a uniform mode;
according to the ratio of argon Ar to oxygen O2Mixing according to the proportion of 1: 1, pressurizing 1.5mbar in a plasma chamber, setting the gas flow rate to be 200sccm, setting the microwave energy to be 500w, and setting the operation setting time to be 10 minutes or 1 hour;
argon Ar and oxygen O2Elements are stabilized on the surface of the graphene so as to enhance the activity of the graphene and the stability of the specific hexagonal atomic structure of the graphene;
2. preparing a mixed solution of plasma graphene and epoxy resin, adopting a vacuum shearing and melting method and a vacuum shearing machine, melting the plasma graphene into the epoxy resin according to the proportion of 1: 1000 or 2: 1000, and adopting a vacuum high-strength shearing machine to stir the graphene solution at the shearing force of 2000rpm for 1 hour so as to uniformly distribute the plasma graphene powder in the epoxy resin;
3. adopting a plasma dielectric barrier discharge method and a plasma dielectric barrier discharge device to remove NaOH and HNO3Sulfuric acid H2SO4And (2) proportionally: 1: 0.5: 0.5, storing the media in a channel, sequentially releasing the media into a prepared plasma graphene epoxy resin mixture according to the channel numbering sequence, electrifying the media in the releasing process to enable the media to surround argon and oxygen elements at the periphery of the plasma graphene to generate a superimposed plasma layer, and mutually connecting the media through the plasma layer to stabilize the uniform distribution state of the graphene materials in the epoxy resin without generating stacked precipitates; each timeDischarging for 10 minutes, wherein the peak value proportion of the medium release amount is not more than 7wt% of the epoxy resin solution, and the structural integrity of the plasma graphene is ensured;
the dose and energy of the generated plasma are calculated according to the formula: plasma release dose = N × P/V × W;
n is channel quantity, P is energy, v is release rate, and w is release width 1 m;
the plasma dose and energy per release parameters were obtained as follows:
sequence 1: the power is not released;
sequence 2: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 1, and the dosage is 600;
sequence 3: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 2, and the dosage is 1200;
sequence 4: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 6, and the dosage is 3600;
sequence 5: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 9, and the dosage is 5400;
4. and (3) stabilizing the catalyzed plasma graphene epoxy resin by using an ultrasonic machine, and vibrating the graphene solution subjected to dielectric barrier discharge for 30 minutes in an ultrasonic vibration mode with the frequency of 40Khz to prepare the plasma graphene permeable adhesive.
According to the invention, the preparation method of the plasma graphene permeable adhesive is adopted to excite the activity of graphene atoms and the stability of the specific hexagonal atomic structure thereof, improve the physical properties, enhance the physical strength and permeability thereof, and overcome the problems of poor fusion and precipitation of the graphene atoms. Improve the fusibility of graphene in liquid without precipitation. The physical property and the permeability of the graphene permeable adhesive after use are improved.
Drawings
FIG. 1 is a schematic diagram of a plasma coating generator;
FIG. 2 is a schematic diagram of a plasma dielectric barrier discharge device;
in the figure: 1 is a plasma coating generator, 2 is a plasma microwave oscillation nozzle3 is argon Ar and oxygen O2Plasma microwave, 4 holding tank, 5 graphene powder, 6 rotating tray, 7 high-frequency alternating current power supply, 8 electrode, 9 plasma graphene epoxy resin mixture and 10 medium release channel.
Detailed Description
The preparation method of the plasma graphene penetrating adhesive is realized in this way, and is specifically described below with reference to an embodiment.
Examples
The preparation method of the plasma graphene permeable adhesive comprises the following steps of: EA 9396 epoxy resin; reinforcing materials: the purity of the single-layer graphene stripped by a physical method is 99.9%; catalytic material: argon Ar in plasma state and oxygen element O2(ii) a Stabilizing material: NaOH, HNO3Sulfuric acid H2SO4；
The raw material ratio is as follows:
graphene and epoxy resin: 1: 1000 or 2: 1000; the ratio of the graphene epoxy resin to the stabilizing material is 1: 0.07; the catalytic material proportion is as follows: argon Ar oxygen O2The element ratio is 1: 1; the proportion of the stabilizing material is as follows: according to the ratio of sodium hydroxide NaOH to nitric acid HNO3 Sulfuric acid H2SO4In a ratio of 1: 0.5: 0.5.
The method comprises the following steps:
the plasma graphene permeable adhesive is prepared by the following process steps:
1. preparing plasma coating graphene, and using a plasma coating generator to mix argon Ar and oxygen element O2The graphene is attached to the outer surface of graphene in a plasma state so as to enhance the activity of the graphene and the stability of the specific hexagonal atomic structure of the graphene; placing graphene powder in a containing groove of a plasma generator by adopting a plasma coating generator; argon Ar and oxygen O2The elements are sprayed out from the top microwave oscillation nozzle in a microwave mode, when the bottom tray rotates, graphene powder floats in the containing tank in a suspension mode, and all powder in the tank is sprayed by microwaves in a uniform mode;
according to the ratio of argon Ar to oxygen O2Mixing according to the proportion of 1: 1, pressurizing 1.5mbar in a plasma chamber, setting the gas flow rate to be 200sccm, setting the microwave energy to be 500w, and setting the operation setting time to be 10 minutes or 1 hour;
argon Ar and oxygen O2Elements are stabilized on the surface of the graphene so as to enhance the activity of the graphene and the stability of the specific hexagonal atomic structure of the graphene;
2. preparing a mixed solution of plasma graphene and epoxy resin, adopting a vacuum shearing and melting method and a vacuum shearing machine, melting the plasma graphene into the epoxy resin according to the proportion of 1: 1000 or 2: 1000, and adopting a vacuum high-strength shearing machine to stir the graphene solution at the shearing force of 2000rpm for 1 hour so as to uniformly distribute the plasma graphene powder in the epoxy resin;
3. adopting a plasma dielectric barrier discharge method and a plasma dielectric barrier discharge device to remove NaOH and HNO3Sulfuric acid H2SO4And (2) proportionally: 1: 0.5: 0.5, storing the media in a channel, sequentially releasing the media into a prepared plasma graphene epoxy resin mixture according to the channel numbering sequence, electrifying the media in the releasing process to enable the media to surround argon and oxygen elements at the periphery of the plasma graphene to generate a superimposed plasma layer, and mutually connecting the media through the plasma layer to stabilize the uniform distribution state of the graphene materials in the epoxy resin without generating stacked precipitates; discharging for 10 minutes each time, wherein the peak value proportion of the medium release amount is not more than 7wt% of the epoxy resin solution, and the structural integrity of the plasma graphene is ensured;
the dose and energy of the generated plasma are calculated according to the formula: plasma release dose = N × P/V × W;
n is channel quantity, P is energy, v is release rate, and w is release width 1 m;
the plasma dose and energy per release parameters were obtained as follows:
sequence 1: the power is not released;
sequence 2: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 1, and the dosage is 600;
sequence 3: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 2, and the dosage is 1200;
sequence 4: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 6, and the dosage is 3600;
sequence 5: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 9, and the dosage is 5400;
4. and (3) stabilizing the catalyzed plasma graphene epoxy resin by using an ultrasonic machine, and vibrating the graphene solution subjected to dielectric barrier discharge for 30 minutes in an ultrasonic vibration mode with the frequency of 40Khz to prepare the plasma graphene permeable adhesive.
The use method of the plasma graphene permeable adhesive comprises the following steps:
the standard method of use for epoxy resins was followed. The invention can be uniformly coated on the surface of an object to be bonded, the thickness is not more than 0.76mm, the thickness is the thickness of a standard adhesive, and the object to be bonded is a composite material or a metal material.
The preparation method of the plasma graphene permeable adhesive is proved by production experiments that:
enhancing the water solubility of graphene: and pouring the graphene powder subjected to plasma spraying into a water bottle, and standing for 30 days to observe the water-solubility effect. Through observation, the solubility of the graphene in water is greatly enhanced after plasma spraying, and stacking precipitates are not generated.
Enhancing the structural stability of graphene: the test is to measure the polarity energy of the plasma graphene epoxy resin after each plasma dielectric barrier discharge, and the measurement result shows that the structural stability of the plasma graphene epoxy resin is greatly enhanced.
Through the test: after the first dielectric barrier discharge, the electrode performance is 0.3 mJ/m2;
The second order polarity performance is 58.89 mJ/m2;
The third order polarity performance is 109.20 mJ/m2;
The fourth order polarity property is 114.91 mJ/m2;
The fifth order polar property is 119.95 mJ/m2。
Enhancing the fusion degree of graphene: the observation of a microscope shows that the plasma graphene is uniformly distributed in the epoxy resin, the graphene forms corrugated connection, and the connection mechanism keeps the solubility of the graphene and does not precipitate.
Enhancing the permeability of graphene: the plasma graphene permeable adhesive is uniformly coated on the surface of an adhesive composite material plate, the composite material plate is a carbon fiber 8-layer vacuum pressing plate, the thickness is 2mm, and the permeability of the composite material plate can be truly reflected.
Tests show that when the composite material plate bonded by the plasma graphene permeable adhesive is broken, the plate material on one side of the composite material plate is broken. The fracture part is 4-5 layers of the material, so that the penetrating adhesive can be seen to have been penetrated into the surface layer and the inner layer of the composite material board, and the tensile fracture strength is the strength of the composite material itself. The original epoxy resin can not permeate into the composite material, the fracture mode is that the adhesive is fractured, the adhesive material is orderly dropped off, and the surface is not adhered with the base material of the composite material. Under an electron microscope, the original epoxy resin fracture surface adhesive is fractured and falls off in a large area, and a composite material substrate is arranged below the falling-off part. The fracture part of the fracture surface of the composite board bonded by the graphene permeable adhesive is 4-5 layers of the composite material, and the graphene permeable adhesive permeates into the composite material carbon fiber, so that the permeability is obviously enhanced.
Uniformly coating the plasma graphene permeable adhesive on the surface of the adhesive aluminum alloy material plate. The same result is obtained through test detection. The middle bonding part of the test material plate coated with the plasma graphene permeable adhesive is not broken, and the broken part is the test material which is broken. The fracture of the test material plate coated with the original epoxy resin is the fracture of the bonding part.
Enhancing the mechanical property of graphene: the mechanical property of the plasma graphene permeable adhesive is far higher than that of a common epoxy resin adhesive. The highest shear force performance of the reinforced material graphene is improved to 99.8% by adopting 10-minute plasma treatment and 1-hour plasma treatment tests.
According to the invention, the preparation method of the plasma graphene permeable adhesive is adopted to excite the activity of graphene atoms and the stability of the specific hexagonal atomic structure thereof, improve the physical properties, enhance the physical strength and permeability thereof, and overcome the problems of poor fusion and precipitation of the graphene atoms. Improve the fusibility of graphene in liquid without precipitation. The physical property and the permeability of the graphene permeable adhesive after use are improved.
Claims (2)
1. A preparation method of a plasma graphene permeable adhesive is characterized by comprising the following steps: the preparation method of the plasma graphene permeable adhesive comprises the following steps of preparing an adhesive base material: EA 9396 epoxy resin; reinforcing materials: the purity of the single-layer graphene stripped by a physical method is 99.9%; catalytic material: argon Ar in plasma state and oxygen element O2(ii) a Stabilizing material: NaOH, HNO3Sulfuric acid H2SO4；
The raw material ratio is as follows:
graphene and epoxy resin: 1: 1000 or 2: 1000; the ratio of the graphene epoxy resin to the stabilizing material is 1: 0.07; the catalytic material proportion is as follows: argon Ar oxygen O2The element ratio is 1: 1; the proportion of the stabilizing material is as follows: according to the ratio of sodium hydroxide NaOH to nitric acid HNO3 Sulfuric acid H2SO4In a ratio of 1: 0.5: 0.5.
2. The method for preparing the plasma graphene infiltrated binder of claim 1, wherein: the plasma graphene permeable adhesive is prepared by the following process steps:
(1) preparing plasma coating graphene, and using a plasma coating generator to mix argon Ar and oxygen element O2The graphene is attached to the outer surface of graphene in a plasma state so as to enhance the activity of the graphene and the stability of the specific hexagonal atomic structure of the graphene; placing graphene powder in a containing groove of a plasma generator by adopting a plasma coating generator; argon Ar and oxygen O2The elements are sprayed out from the top microwave oscillation nozzle in a microwave mode, when the bottom tray rotates, graphene powder floats in the containing tank in a suspension mode, and all powder in the tank is sprayed by microwaves in a uniform mode;
according to the ratio of argon Ar to oxygen O2Mixing at a ratio of 1: 1, pressurizing in a plasma chamber by 1.5mbar, setting gas flow rate of 200sccm, and controllingSetting wave energy to be 500w, and setting operation time to be 10 minutes or 1 hour;
argon Ar and oxygen O2Elements are stabilized on the surface of the graphene so as to enhance the activity of the graphene and the stability of the specific hexagonal atomic structure of the graphene;
(2) preparing a mixed solution of plasma graphene and epoxy resin, adopting a vacuum shearing and melting method and a vacuum shearing machine, melting the plasma graphene and the epoxy resin into the epoxy resin according to the proportion of 1: 1000 or 2: 1000, and adopting a vacuum high-strength shearing machine to shear the graphene solution at 2000rpm for high-strength stirring for 1 hour so as to uniformly distribute the plasma graphene powder in the epoxy resin;
(3) adopting a plasma dielectric barrier discharge method and a plasma dielectric barrier discharge device to remove NaOH and HNO3Sulfuric acid H2SO4And (2) proportionally: 1: 0.5: 0.5, storing the media in a channel, sequentially releasing the media into a prepared plasma graphene epoxy resin mixture according to the channel numbering sequence, electrifying the media in the releasing process to enable the media to surround argon and oxygen elements at the periphery of the plasma graphene to generate a superimposed plasma layer, and mutually connecting the media through the plasma layer to stabilize the uniform distribution state of the graphene materials in the epoxy resin without generating stacked precipitates; discharging for 10 minutes each time, wherein the peak value proportion of the medium release amount is not more than 7wt% of the epoxy resin solution, and the structural integrity of the plasma graphene is ensured;
the dose and energy of the generated plasma are calculated according to the formula: plasma release dose = N × P/V × W;
n is channel quantity, P is energy, v is release rate, and w is release width 1 m;
the plasma dose and energy per release parameters were obtained as follows:
sequence 1: the power is not released;
sequence 2: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 1, and the dosage is 600;
sequence 3: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 2, and the dosage is 1200;
sequence 4: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 6, and the dosage is 3600;
sequence 5: electrifying to release stable catalytic materials, wherein the speed is 5 m/min, the energy is 3000W, the channel number is 9, and the dosage is 5400;
(4) and stabilizing the catalyzed plasma graphene epoxy resin by using an ultrasonic machine, and vibrating the graphene solution subjected to dielectric barrier discharge for 30 minutes in an ultrasonic vibration mode with the frequency of 40Khz to prepare the plasma graphene permeable adhesive.
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| CN111100587A (en) * | 2019-12-31 | 2020-05-05 | 苏州桐力光电股份有限公司 | Graphene AB adhesive and preparation method thereof |
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| CN102993751A (en) * | 2012-12-03 | 2013-03-27 | 鹤山丽得电子实业有限公司 | High-thermal-conductivity and high-strength insulating PPS (polyphenylene sulfite) composite material and preparation method for same |
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