CN115458314A - Organic material coated microcapsule composite carbonyl iron powder and preparation method thereof - Google Patents

Organic material coated microcapsule composite carbonyl iron powder and preparation method thereof Download PDF

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CN115458314A
CN115458314A CN202210853647.3A CN202210853647A CN115458314A CN 115458314 A CN115458314 A CN 115458314A CN 202210853647 A CN202210853647 A CN 202210853647A CN 115458314 A CN115458314 A CN 115458314A
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iron powder
carbonyl iron
mixture
coated
microcapsule composite
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张林博
高浩宇
张澎
侯明慧
梁迪飞
邓龙江
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University of Electronic Science and Technology of China
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/06—Making microcapsules or microballoons by phase separation
    • B01J13/14—Polymerisation; cross-linking
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01Q—ANTENNAS, i.e. RADIO AERIALS
    • H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding

Abstract

The invention belongs to the technical field of electromagnetic microwave absorbers, relates to corrosion protection of carbonyl iron powder, and particularly relates to organic material-coated microcapsule composite carbonyl iron powder and a preparation method thereof. The invention adopts an in-situ polymerization method, a layer of modifier and preservative is coated on carbonyl iron powder, then a layer of resin is coated through a cross-linking curing reaction, and finally a double-shell structure of the resin @ preservative @ carbonyl iron powder is formed. The materials used in the invention are all organic materials and all low dielectric materials, so that the dielectric property of carbonyl iron powder can be reduced, impedance matching is optimized, and reflection loss is improved. Finally, under the condition that the electromagnetic performance of the powder is not greatly deteriorated, the acid resistance, electrochemical corrosion resistance and salt spray resistance of the modified powder are obviously improved, the carbonyl iron powder with various shapes can be coated, and a new scheme is provided for improving the corrosion resistance of the carbonyl iron powder.

Description

Organic material coated microcapsule composite carbonyl iron powder and preparation method thereof
Technical Field
The invention belongs to the technical field of electromagnetic microwave absorbers, and relates to corrosion protection of carbonyl iron powder. Carbonyl iron powder can be applied to high-humidity and high-salt-spray environments as a microwave absorbent, and particularly relates to microcapsule composite carbonyl iron powder coated by an organic material and a preparation method thereof.
Background
Carbonyl iron powder is a traditional magnetic absorbent, has the advantages of high magnetic conductivity, high saturation magnetization and the like, and is widely applied to the field of microwave absorption. Because of the large specific surface area, the atoms on the surface of the material are relatively increased, so that the area of the region which interacts with the electromagnetic wave is increased, and the electromagnetic wave is favorably converted into heat energy or other forms of energy to be lost. The carbonyl iron powder is obtained by thermally decomposing a carbonyl iron compound in a preheated nitrogen atmosphere, is in a unique onion sphere layered structure, has higher resistivity, is beneficial to inhibiting the eddy current effect and reducing the adverse effect caused by the skin effect. Therefore, the carbonyl iron powder is a common microwave absorbent material of the thin-layer wave-absorbing coating and is widely applied to important fields of military and the like.
In recent years, in the field of application of microwave absorbers to marine environments, carbonyl iron powder is not favorable for application thereof because the powder itself has a small particle size and a high surface activity, and is easily oxidized to form substances such as iron oxide and the like, thereby losing its physical structure and characteristics. Therefore, the research on the corrosion resistance of the carbonyl iron powder is receiving extensive attention, and the long-term stability of the electromagnetic performance of the carbonyl iron powder in a salt-fog humid environment needs to be realized.
In the current research, most researchers modify the surface of carbonyl iron powder by inorganic or organic modification to form a continuous layer,A uniform and dense inorganic or organic protective layer. Inorganic materials, such as an Ag layer, a Co layer, and a Ni layer, are coated on the surface of carbonyl iron powder, and a common research is to coat a layer of SiO 2 Materials, etc.; organic materials, such as a layer of polyaniline and cholesteryl chloroformate coated on the surface of carbonyl iron powder. The inorganic and organic materials can provide protection for carbonyl iron powder in a salt-fog humid environment and isolate corrosive media such as oxygen.
In patent CN113388231a, after a silane coupling agent is used to modify the surface of carbonyl iron powder, the treated carbonyl iron powder and epoxy resin are mixed, stirred and cured to obtain an epoxy resin coated carbonyl iron powder wave-absorbing material. According to the method, carbonyl iron powder is treated by using a silane coupling agent, the electromagnetic performance of the carbonyl iron powder is deteriorated to a certain extent, and meanwhile, the surface of the epoxy resin coated powder obtained by the preparation method is rough and uneven, corrosive media such as water vapor, oxygen, chloride ions and the like cannot be completely isolated, and the modified carbonyl iron powder has general corrosion resistance.
In patent CN112563010A, a compact silicon dioxide thick coating layer is coated on the surface of iron powder by a hydrolysis-pyrolysis method, so that the iron powder has good salt water/salt spray corrosion resistance. The method adopts silicon dioxide to coat the powder, and has the problem of serious deterioration of electromagnetic performance.
CN110722153B provides an antioxidant absorbent and a preparation method thereof, wherein aluminum powder is uniformly attached to the surface of spherical carbonyl iron powder, and is controlled to be oxidized to form compact Al 2 O 3 The coated carbonyl iron powder antioxidant absorbent has compact and continuous powder coating layer, improves the corrosion resistance, but also has the problem that the electromagnetic performance of the modified powder is seriously deteriorated.
Disclosure of Invention
Aiming at the problems or defects in the research, the invention aims to solve the problem that the current carbonyl iron powder has excellent electromagnetic performance and corrosion resistance. The invention provides an organic material coated microcapsule composite carbonyl iron powder and a preparation method thereof, which are used for ensuring that the electromagnetic property of the carbonyl iron powder is not deteriorated and simultaneously have excellent corrosion resistance.
A preparation method of microcapsule composite carbonyl iron powder coated by organic materials comprises the following steps:
step 1, dissolving a preservative and a modifier in an organic solvent at room temperature to obtain a mixture A. In the mixture A, the preservative accounts for 12-24 percent, the modifier accounts for 12-24 percent and the organic solvent accounts for 52-76 percent by mass, and the sum of the three is 1.
The preservative is one or more of 2-amino-4-methylpyridine, N' -di (diphenylphosphino) -1-phenylethylamine and N-hexadecylamine;
the modifier is one or two of diethylamine propylamine, triethylene tetramine and hexamethylene diamine;
and 2, adding carbonyl iron powder into the mixture A obtained in the step 1, and uniformly dispersing to obtain a mixture B. In the mixture B, the carbonyl iron powder accounts for 30-50% by mass, the mixture A accounts for 50-70% by mass, and the sum of the proportions of the carbonyl iron powder and the mixture A is 1.
And 3, filtering the mixture B obtained in the step 2, sequentially washing with deionized water, and drying in vacuum to obtain carbonyl iron powder coated with a layer of modifier and preservative.
And 4, dissolving the resin in an organic solvent to obtain a mixture C. In the mixture C, the mass fraction of the resin is 2-8%, the mass fraction of the organic solvent is 92-98%, and the sum of the mass fraction of the resin and the organic solvent is 1.
And 5, adding a crosslinking assistant, an emulsifier and the carbonyl iron powder obtained in the step 3 into the mixture C obtained in the step 4, and then heating and stirring the mixture C until the crosslinking reaction is complete to obtain a mixture D.
In the mixture D, the mass fraction of the crosslinking assistant is 1-4%, the mass fraction of the emulsifier is 1-4%, the mass fraction of the carbonyl iron powder is 7-14%, the mass fraction of the mixture C is 78-91%, and the sum of the four is 1.
The crosslinking assistant is one or two of phthalic anhydride, tetrahydrophthalic anhydride and N, N-dimethyl piperazine; the emulsifier is one or two of sorbitan monooleate, sorbitan monooleate and sodium dodecyl sulfate.
And 6, cooling the mixture D obtained in the step 5 to room temperature, and sequentially performing suction filtration, deionized water washing and vacuum drying to obtain the organic material coated microcapsule composite carbonyl iron powder.
Further, the organic solvent is acetone, xylene, n-butanol or ethanol.
Furthermore, the carbonyl iron powder is spherical, so that the finally obtained organic material-coated microcapsule composite carbonyl iron powder has better corrosion resistance.
Furthermore, the carbonyl iron powder is flaky, so that the finally obtained microcapsule composite carbonyl iron powder coated by the organic material has better electromagnetic performance.
A microcapsule composite carbonyl iron powder coated by organic materials is prepared by the method.
The invention adopts an in-situ polymerization method, wherein the in-situ polymerization method is characterized in that a reaction monomer generates copolymerization reaction on the surface of a coated core material with the aid of a catalyst to generate a prepolymer, and the prepolymer continuously reacts with the reaction to form a high-molecular-weight copolymer to cover the surface of the core material. The modifier and the preservative are adsorbed on the surface of carbonyl iron powder, belonging to chemical adsorption. Researchers generally believe that transition metal atoms such as iron and nickel have an empty d-orbital and are susceptible to electron acceptance. Most organic molecules contain polar groups with nitrogen, oxygen, sulfur and phosphorus as central atoms, and have certain electron donating capability, and the polar groups and the organic molecules can form coordinate bonds to generate chemisorption. The chemical adsorption has large acting force and high adsorption heat, the required activation energy is larger than that of physical adsorption and is about 41.8 multiplied by 102kJ/mol, the chemical adsorption is carried out slowly, and once the chemical adsorption is difficult to desorb, the adsorption has irreversibility. Step 1, coating a layer of modifier and preservative on carbonyl iron powder, wherein the modifier is adsorbed on the surface of the carbonyl iron powder and simultaneously has a chemical reaction with the epoxy resin in step 5, so that the adhesive force between the epoxy resin and the surface of the powder is improved; the preservative has the function of adsorbing on the surface of the carbonyl iron powder and effectively preventing the carbonyl iron powder from being corroded. In the step 5, the epoxy resin and the crosslinking assistant are subjected to crosslinking reaction on the carbonyl iron powder coated with a layer of modifier and preservative, and finally a double-shell structure of the resin @ preservative @ carbonyl iron powder is formed. The double-shell structure can separate corrosive media such as water vapor, oxygen, chlorine ions and the like in a long-term salt mist environment. If the resin is aged and shed in long-term use, the preservative adsorbed on the surface of the carbonyl iron powder is exposed to the salt spray environment, and the carbonyl iron powder is continuously protected from corrosion. And the adopted materials are all organic materials and low dielectric materials, so that the dielectric property of the carbonyl iron powder can be reduced, the impedance matching is optimized, and the reflection loss is improved.
In conclusion, the preparation process is mature and simple, the raw materials are low in price, and the preparation method is suitable for mass production. Firstly preparing a layer of modifier and preservative on the surface layer of carbonyl iron powder, and then coating a layer of resin; so that the finally prepared microcapsule composite carbonyl iron powder has less electromagnetic property deterioration and excellent salt spray corrosion resistance; and can coat carbonyl iron powder with various shapes.
Drawings
Fig. 1 is an SEM image of uncoated and examples one to three.
FIG. 2 is a polarization curve of the tests of uncoated and example one to three powders in 3.5% NaCl solution.
Fig. 3 shows the results of the acid resistance test of the uncoated powder and the powder of examples one to three.
FIG. 4 is a simplified flow diagram of the preparation of the present invention.
Detailed Description
The technical solutions of the present invention will be described in further detail below with reference to the embodiments and the drawings, but the present invention is not limited thereto.
Example 1
Step 1, dissolving 4g of 2-amino-4-methylpyridine and 8g of triethylene tetramine in 200ml of xylene at room temperature of 25 ℃ to obtain a mixture A.
And 2, dispersing 8g of spherical carbonyl iron powder E in the mixture A obtained in the step 1, and stirring for 24H at the room temperature of 25 ℃ at the rotating speed of 400RPM to obtain a mixture B.
And 3, filtering the mixture B obtained in the step 2, washing the mixture B for a plurality of times by deionized water, and drying the mixture B in vacuum to obtain spherical carbonyl iron powder E coated with a layer of 2-amino-4-methylpyridine and triethylene tetramine.
Step 4, 2.4g of epoxy resin was dissolved in 100ml of xylene to give mixture C.
And 5, adding 0.5g of phthalic anhydride, 0.1g of sorbitan monooleate and the spherical carbonyl iron powder E obtained in the step 3 into the mixture C obtained in the step 4, and then carrying out crosslinking reaction for 8 hours until the reaction is completed under the stirring conditions of 80 ℃ and 550RPM to obtain a mixture D.
And 6, cooling the mixture D obtained in the step 5 to room temperature, and then sequentially carrying out magnetic separation, deionized water washing and vacuum drying on the mixture D to obtain the organic material coated microcapsule composite flaky carbonyl iron powder E.
Example 2
Step 1, under the condition of room temperature of 25 ℃, 8g of N, N' -di (diphenylphosphino) -1-phenylethylamine and 16g of triethylene tetramine are dissolved in 400ml of xylene to obtain a mixture A.
And 2, dispersing 16g of flaky carbonyl iron powder F in the mixture A obtained in the step 1, and stirring for 24H at the room temperature of 25 ℃ at the rotating speed of 500RPM to obtain a mixture B.
And 3, filtering the mixture B obtained in the step 2, washing the mixture B for a plurality of times by deionized water, and drying the mixture in vacuum to obtain the flaky carbonyl iron powder F coated with a layer of N, N' -di (diphenylphosphino) -1-phenylethylamine and triethylene tetramine.
Step 4, 4.8g of epoxy resin was dissolved in 200ml of xylene to give mixture C.
And 5, adding 0.6g of N, N-dimethylpiperazine, 0.3g of sodium dodecyl sulfate and the flaky carbonyl iron powder F obtained in the step 3 into the mixture C obtained in the step 4, and then carrying out crosslinking reaction for 8 hours until the reaction is completed under the stirring conditions of 75 ℃ and 650RPM to obtain a mixture D.
And 6, cooling the mixture D obtained in the step 5 to room temperature, and then sequentially carrying out magnetic separation, deionized water washing and vacuum drying on the mixture D to finally obtain the organic material coated microcapsule composite flaky carbonyl iron powder F.
Example 3
Step 1, 8.5g of n-hexadecylamine and 14g of diethylaminopropylamine were dissolved in 400ml of xylene at room temperature of 25 ℃ to obtain a mixture A.
And 2, dispersing 16G of spherical carbonyl iron powder G in the mixture A in the step 1, and stirring for 24H at the room temperature of 25 ℃ at the rotating speed of 500RPM to obtain a mixture B.
And 3, filtering the mixture B obtained in the step 2, washing the mixture B for a plurality of times by deionized water, and drying the mixture B in vacuum to obtain spherical carbonyl iron powder G coated with a layer of n-hexadecylamine and diethylaminopropylamine.
Step 4, 4.8g of epoxy resin was dissolved in 200ml of xylene to give mixture C.
And 5, adding 0.4G of tetrahydrophthalic anhydride, 0.3G of sodium dodecyl sulfate and the spherical carbonyl iron powder G obtained in the step 3 into the mixture C obtained in the step 4, and then carrying out crosslinking reaction for 8 hours until the reaction is completed under the conditions of stirring at the temperature of 90 ℃ and the RPM of 550 to obtain a mixture D.
And 6, cooling the mixture D obtained in the step 5 to room temperature, and then sequentially carrying out magnetic separation, deionized water washing and vacuum drying on the mixture D to finally obtain the microcapsule composite flaky carbonyl iron powder G coated with the organic material.
For the results of the three groups of samples, the corrosion resistance of the prepared corrosion-resistant magnetic metal powder is characterized in 3 ways: (1) testing the electrochemical corrosion resistance of the corrosion-resistant magnetic metal powder in a 3.5-percent NaCl solution by adopting an electrochemical workstation; (2) the corrosion-resistant magnetic metal powder was placed in a hydrochloric acid solution with PH =1 while stirring the hydrochloric acid solution, and the change in PH of the solution was measured. (3) Adding the corrosion-resistant magnetic metal powder into a resin coating formula to prepare a coating, carrying out salt spray test, and regularly observing the surface change condition of the coating.
Table 1 shows the electromagnetic parameters measured by a vector grid analyzer in the range of 1-18GHz after the powder is added with coaxial samples according to a standard machine before, after and after the first, second and third coatings of the example. The electromagnetic parameter change before and after coating is compared, so that the influence of the coating on the electromagnetic performance of the powder is small, and the process has feasibility.
Table 1: electromagnetic parameters of samples prepared from the powder before and after coating of each example were compared.
Figure BDA0003739697410000051
Figure BDA0003739697410000061
Figure BDA0003739697410000071
Table 2 is a table comparing salt spray resistance of the coating prepared from the powder before, after, and after the first, second, and third coating, and the test results show that the corrosion resistance of the coated powder is significantly improved and has excellent corrosion resistance.
Table 2: the salt spray resistant time of the coatings prepared from the powder before and after coating of each example was compared.
Figure BDA0003739697410000072
FIG. 4 is a simple schematic of the preparation process of the present invention. FIG. 1 is SEM images of powders before and after coating in examples I, II and III, and a tight and continuous organic layer is obviously present on the surface of the coated powder, so that the powder can be protected for a long time. The process is suitable for spherical powder or flaky powder. FIG. 2 is a polarization curve of the test of the powders in 3.5% NaCl solution before, after, and after the first, second, and third coating in examples, showing a significant decrease in corrosion current and an increase in corrosion potential after all three powders were modified. FIG. 3 shows the results of the acid resistance test before and after coating in examples I, II and III, which shows that the acid resistance of the three coated powders is improved. FIG. 4 is a simple schematic of the preparation process of the present invention.
The above examples show that the present invention adopts an in-situ polymerization method, in which a layer of modifier and preservative is coated on carbonyl iron powder, and then a layer of resin is coated through a cross-linking curing reaction, so as to finally form a double-shell structure of resin @ preservative @ carbonyl iron powder. The adopted materials are all organic materials and low dielectric materials, so that the dielectric property of carbonyl iron powder can be reduced, impedance matching is optimized, and reflection loss is improved. Finally, under the condition that the electromagnetic performance of the powder is not greatly deteriorated, the acid resistance, electrochemical corrosion resistance and salt spray resistance of the modified powder are obviously improved, the carbonyl iron powder with various shapes can be coated, and a new scheme is provided for improving the corrosion resistance of the carbonyl iron powder.

Claims (5)

1. A preparation method of microcapsule composite carbonyl iron powder coated by organic materials is characterized by comprising the following steps:
step 1, dissolving a preservative and a modifier in an organic solvent at room temperature to obtain a mixture A; in the mixture A, the preservative accounts for 12-24 percent, the modifier accounts for 12-24 percent and the organic solvent accounts for 52-76 percent by mass, and the sum of the three is 1;
the preservative is one or more of 2-amino-4-methylpyridine, N' -di (diphenylphosphino) -1-phenylethylamine and N-hexadecylamine;
the modifier is one or two of diethylaminopropylamine, triethylene tetramine and hexamethylene diamine;
step 2, adding carbonyl iron powder into the mixture A obtained in the step 1, and uniformly dispersing to obtain a mixture B; in the mixture B, the carbonyl iron powder accounts for 30-50% by mass, the mixture A accounts for 50-70% by mass, and the sum of the proportions of the carbonyl iron powder and the mixture A is 1;
step 3, filtering the mixture B obtained in the step 2, sequentially washing the mixture B by deionized water, and then drying the mixture B in vacuum to obtain carbonyl iron powder coated with a layer of modifier and preservative;
step 4, dissolving the resin in an organic solvent to obtain a mixture C; in the mixture C, the mass fraction of the resin is 2-8%, the mass fraction of the organic solvent is 92-98%, and the sum of the mass fraction of the resin and the organic solvent is 1;
step 5, adding a crosslinking auxiliary agent, an emulsifying agent and the carbonyl iron powder obtained in the step 3 into the mixture C obtained in the step 4, and then heating and stirring the mixture C until the crosslinking reaction is complete to obtain a mixture D;
in the mixture D, the mass fraction of the crosslinking assistant is 1-4%, the mass fraction of the emulsifier is 1-4%, the mass fraction of the carbonyl iron powder is 7-14%, the mass fraction of the mixture C is 78-91%, and the sum of the four mass fractions is 1;
the crosslinking assistant is one or two of phthalic anhydride, tetrahydrophthalic anhydride and N, N-dimethyl piperazine; the emulsifier is one or two of sorbitan monooleate, sorbitan monooleate and sodium dodecyl sulfate;
and 6, cooling the mixture D obtained in the step 5 to room temperature, and then sequentially performing suction filtration, deionized water washing and vacuum drying to obtain the organic material coated microcapsule composite carbonyl iron powder.
2. The method for preparing the organic material coated microcapsule composite carbonyl iron powder as claimed in claim 1, wherein: the organic solvent is acetone, xylene, n-butanol or ethanol.
3. The method for preparing the organic material coated microcapsule composite carbonyl iron powder as claimed in claim 1, wherein: the carbonyl iron powder is spherical, so that the finally obtained microcapsule composite carbonyl iron powder coated by the organic material has better corrosion resistance.
4. The method for preparing the organic material coated microcapsule composite carbonyl iron powder according to claim 1, wherein the method comprises the following steps: the carbonyl iron powder is flaky, so that the finally obtained organic material coated microcapsule composite carbonyl iron powder has better electromagnetic performance.
5. A microcapsule composite carbonyl iron powder coated by organic materials is characterized in that: prepared by the process of claim 1.
CN202210853647.3A 2022-07-11 2022-07-11 Organic material coated microcapsule composite carbonyl iron powder and preparation method thereof Pending CN115458314A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117467294A (en) * 2023-11-23 2024-01-30 哈尔滨工业大学 Preparation method of carbonyl iron wave-absorbing coating with corrosion prevention and self-repairing functions

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117467294A (en) * 2023-11-23 2024-01-30 哈尔滨工业大学 Preparation method of carbonyl iron wave-absorbing coating with corrosion prevention and self-repairing functions

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