CN112563010A - Anti-corrosion treatment method for iron powder - Google Patents
Anti-corrosion treatment method for iron powder Download PDFInfo
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- CN112563010A CN112563010A CN202010964553.4A CN202010964553A CN112563010A CN 112563010 A CN112563010 A CN 112563010A CN 202010964553 A CN202010964553 A CN 202010964553A CN 112563010 A CN112563010 A CN 112563010A
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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
- H01F41/0253—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 for manufacturing permanent magnets
- H01F41/026—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 for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
Abstract
The invention provides an anti-corrosion treatment method for iron powder, belonging to the field of coating materials. According to the invention, a compact silicon dioxide thick coating layer is coated on the surface of the iron powder by a hydrolysis-pyrolysis method, so that the iron powder has good salt water/salt spray corrosion resistance. The treatment steps comprise uniformly dispersing iron powder into a solution containing an organic modifier, stirring and separating to obtain surface-modified iron powder; adding the surface modified iron powder into a solution containing organosilane, slowly stirring and adding a hydrolytic agent to form a uniform silicon-containing coating layer on the surface of the iron powder, and then carrying out high-temperature heat treatment on the uniform silicon-containing coating layer to further pyrolyze the surface coating layer to obtain the dense silicon dioxide thick-coated iron powder material. The invention has the advantages that the uniform dense thick coating of the surface of spherical or flaky iron powder can be realized, the electromagnetic specificity of the iron powder is kept, and the invention has better salt mist resistance and salt water corrosion resistance, and has important application prospect in the fields of functional coatings, soft magnetic materials and the like.
Description
Technical Field
The invention relates to corrosion-resistant iron powder and a preparation method thereof, belonging to the field of coating materials.
Background
Carbonyl iron powder is a kind of soft magnetic material with wide application, the granularity is generally micron-sized or nano-sized, and the carbonyl iron powder has the advantages of high magnetic conductivity, good stability and the like, and has important application in the fields of functional coatings, electromagnetic rheological materials, microwave absorbing materials, powder metallurgy, medical biology and the like. However, carbonyl iron powder has high activity and poor corrosion resistance, and particularly when the carbonyl iron powder is used in a humid and hot environment and an ocean zone, severe powder corrosion and powder oxidation often occur, so that the performance of the material is reduced and even the material is invalid, and the application range and the service life of the material are severely limited. Therefore, the development of effective iron powder corrosion prevention methods is urgently needed.
The addition of corrosion inhibitors to coatings or composite materials is a common metal corrosion protection means at present. However, in the case of a functional coating using iron powder as a filler, although the corrosion inhibitor can slow down the corrosion degree of the iron powder in the coating to a certain extent, the corrosion inhibitor is easy to interact with a film-forming material, the overall mechanical property of the coating is affected, and the effective life of the corrosion inhibitor is also reduced. Therefore, the research on corrosion prevention of the powder aiming at the carbonyl iron powder has important prospect and application value.
Powder coating is an effective way to improve the dispersibility and stability of the iron powder. Patent CN100409979C provides a method for physically adsorbing nano SiO on the surface of carbonyl iron powder2The coating method of the particles is adopted, but the coating layer is loose, so that the water and oxygen can not be blocked, and the corrosion of the iron powder is prevented. Patent CN103007845B adopts liquid phase method to synthesize nano-scale hydrophilic Fe @ SiO2The coating layer of the microsphere is thin and uneven in thickness, and the powder is easy to agglomerate. The patent CN105798291A generates SiO with 0-30nm on the surface of iron powder2However, since only a single liquid phase coating method is used, local aggregation of hydrolysis products is likely to occur when a thick coating layer is prepared, and it is difficult to prepare a dense thick coating layer, which is not favorable for long-term corrosion resistance of the material. In summary, the coating layer prepared by the physical adsorption or pure liquid phase method commonly used at present is often thin or loose, has poor uniformity, poor water and oxygen blocking capability, and does not have the capability of resisting salt water or salt mist corrosion, so that the practical use requirement of the marine environment is difficult to meet.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide an efficient carbonyl iron powder anti-corrosion treatment method aiming at the difficulties in the prior art.
The technical scheme of the invention is as follows:
a method for the anti-corrosion treatment of iron powder, said method comprising the steps of:
(1) uniformly dispersing iron powder into a solution containing an organic modifier, fully stirring to enable the surface of the iron powder to adsorb the modifier, and separating the iron powder adsorbing the modifier from the solution containing the organic modifier to obtain surface-modified iron powder;
(2) adding the surface-modified iron powder obtained in the step (1) into absolute ethyl alcohol, continuously stirring, dropwise adding an organosilane solution and a hydrolyzing agent to hydrolyze the organosilane, and forming a uniform silicon-containing coating layer on the surface of the iron powder to obtain coated iron powder;
(3) and (3) carrying out high-temperature heat treatment on the coated iron powder obtained in the step (2) in vacuum or inert atmosphere to further pyrolyze the coating layer on the surface of the coated iron powder to obtain the dense silicon dioxide coated iron powder.
The organosilane in the step (2) is one or more of methyl orthosilicate, ethyl orthosilicate, n-propyl silicate, aminopropyl triethoxysilane, vinyl trimethoxysilane and trifluoropropyl triethoxysilane, and the concentration of the organosilane is 0.01-10 g/mL.
And (3) the hydrolytic agent in the step (2) is ammonia water or diethanol amine.
The temperature of the high-temperature heat treatment in the step (3) is 200-1000 ℃, and the treatment time is 0.5-10 hours.
The organic modifier selected in the step (1) is one or more of sodium dodecyl benzene sulfonate, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and the concentration of the organic modifier is 0.01-1 g/mL.
The stirring time of the step (1) is 5-24 hours.
And (2) separating the iron powder adsorbing the modifier from the solution containing the organic modifier in the step (1) by a centrifugal or suction filtration mode.
The surface of the corrosion-resistant iron powder is provided with a compact pyrolytic coating layer, and the shell layer of the corrosion-resistant iron powder contains silicon dioxide with the thickness of 10-500 nm.
The invention has the beneficial effects that:
the invention provides a corrosion-resistant coated iron powder material and a preparation method thereof, which improve the traditional powder coating process and overcome the defects of the prior art, and adopt an organic modifier to modify the surface of carbonyl iron powder, and further form a dense SiO2 thick coating layer on the surface of the carbonyl iron powder through two steps of hydrolysis-pyrolysis. Different from physical adsorption or a simple liquid phase coating method adopted by other technologies, the coating layer prepared by the technology has the advantages of large thickness, good compactness, good water and oxygen blocking capacity and stability, and further improves the long-term salt water and salt spray corrosion resistance of the iron powder material.
Detailed Description
The invention provides an anti-corrosion treatment method of iron powder, which comprises the steps of firstly, uniformly dispersing the iron powder into a solution containing an organic modifier, fully stirring to ensure that the surface of the iron powder adsorbs the modifier to obtain surface-modified iron powder, and adopting the organic modifier to perform adsorption modification on the surface of the iron powder, so that the surface energy of the iron powder can be effectively optimized; secondly, dispersing the surface modified iron powder into an absolute ethyl alcohol solution, and dropwise adding an organosilane solution and a hydrolytic agent to hydrolyze the organic silicon silane and form a uniform silicon-containing coating on the surface of the iron powder. Because the surface of the iron powder is organically modified, the dispersion of the iron powder is more uniform and stable in the hydrolysis coating process, and hydrolysis coating products can be more uniformly deposited on the surface of the powder to form a uniform thick coating layer. Finally, the obtained coated iron powder is subjected to high-temperature heat treatment in vacuum or inert atmosphere, the hydrolysis coating layer can be further densified in the heat treatment process, the water and oxygen blocking capacity of the coating layer is improved, and the long-time salt water and salt mist corrosion resistance of the coated iron powder is improved.
The method comprises the following specific steps:
(1) uniformly dispersing iron powder into a solution containing an organic modifier, fully stirring to enable the surface of the iron powder to adsorb the modifier, and separating the iron powder adsorbing the modifier from the solution containing the organic modifier to obtain surface-modified iron powder;
(2) adding the surface-modified iron powder obtained in the step (1) into absolute ethyl alcohol, continuously stirring, dropwise adding an organosilane solution and a hydrolyzing agent to hydrolyze the organosilane, and forming a uniform silicon-containing coating layer on the surface of the iron powder to obtain coated iron powder;
(3) and (3) carrying out high-temperature heat treatment on the coated iron powder obtained in the step (2) in vacuum or inert atmosphere to further pyrolyze the coating layer on the surface of the coated iron powder to obtain the dense silicon dioxide coated iron powder.
The organosilane in the step (2) is one or more of methyl orthosilicate, ethyl orthosilicate, n-propyl silicate, aminopropyl triethoxysilane, vinyl trimethoxysilane and trifluoropropyl triethoxysilane, and the concentration of the organosilane is 0.01-10 g/mL.
And (3) the hydrolytic agent in the step (2) is ammonia water or diethanol amine.
The temperature of the high-temperature heat treatment in the step (3) is 200-1000 ℃, and the treatment time is 0.5-10 hours.
The organic modifier selected in the step (1) is one or more of sodium dodecyl benzene sulfonate, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and the concentration of the organic modifier is 0.01-1 g/mL.
The stirring time of the step (1) is 5-24 hours.
And (2) separating the iron powder adsorbing the modifier from the solution containing the organic modifier in the step (1) by a centrifugal or suction filtration mode.
The surface of the corrosion-resistant iron powder is provided with a compact pyrolytic coating layer, and the shell layer of the corrosion-resistant iron powder contains silicon dioxide with the thickness of 10-800 nm.
The technical solution of the present invention will be described in detail below with reference to specific examples, but the present invention is not limited thereto.
Example 1
Dissolving 10g of sodium dodecyl benzene sulfonate in 300mL of absolute ethyl alcohol, adding 30g of spherical carbonyl iron powder after full dissolution, dispersing for 10min by using ultrasonic (the ultrasonic power is 450W), then mechanically stirring for 3h (the rotating speed is 400r/min), separating the iron powder from the solution by using a centrifugal mode, and removing the supernatant to obtain the surface modified iron powder. The mixture is re-dispersed into 300mL of absolute ethyl alcohol, 10mL of concentrated ammonia water is added into the mixture in a dropwise adding mode, stirring is continued (400r/min), 40mL of ethyl orthosilicate ethanol solution (with the concentration of 10%) is slowly dropwise added, and stirring is continued for 3 hours after the dropwise adding is finished. And separating the iron powder from the solution in a centrifugal mode, drying the solution in a 60 ℃ oven for 24 hours, putting the powder into a nitrogen atmosphere furnace, and carrying out heat treatment at 500 ℃ for 1 hour (the heating rate is 10 ℃/min) to obtain the final coated iron powder. Scanning electron microscope shows that the thickness of the coating layer on the surface of the iron powder is about 600 nm. The energy spectrum analysis shows that the main component of the coating layer is silicon dioxide. The obtained coated iron powder is prepared into a functional coating test piece to be subjected to a salt spray corrosion experiment, and no rust spots appear on the surface in 1500 hours.
Example 2
Dissolving 5g of polyethylene glycol in 300mL of absolute ethyl alcohol, adding 10g of sheet carbonyl iron powder after full dissolution, dispersing for 20min (ultrasonic power 450W) by using ultrasonic, then mechanically stirring for 3h (rotating speed 400r/min), separating the iron powder from the solution by using a centrifugal mode, and removing supernatant to obtain the surface modified iron powder. The mixture is re-dispersed into 300mL of absolute ethyl alcohol, 10mL of concentrated ammonia water is added into the mixture in a dropwise adding mode, stirring is continued (400r/min), 40mL of mixed solution of tetraethoxysilane and aminopropyltriethoxysilane (the concentration is 10 percent, and the proportion of tetraethoxysilane and aminopropyltriethoxysilane is 1:1) is slowly added dropwise, and stirring is continued for 5 hours after the dropwise adding is finished. And separating the iron powder from the solution in a centrifugal mode, drying the solution in a 60 ℃ oven for 24 hours, putting the powder into an argon atmosphere furnace, and carrying out heat treatment at 400 ℃ for 1 hour (the temperature rise speed is 10 ℃/min) to obtain the final coated iron powder. Scanning electron microscope shows that the thickness of the coating layer on the surface of the iron powder is about 300nm, and the edge coating is complete. The obtained coated iron powder is prepared into a functional coating test piece to be subjected to a salt spray corrosion experiment, and no rust spots appear on the surface within 500 hours.
Example 3
Dissolving 8g of polyvinylpyrrolidone in 300mL of deionized water, adding 30g of ellipsoidal carbonyl iron powder after fully dissolving, dispersing for 15min (ultrasonic power of 450W) by using ultrasonic, then mechanically stirring for 3h (rotating speed of 400r/min), separating the iron powder from the solution by using a suction filtration mode, and removing the filtrate to obtain the surface modified iron powder. The mixture is re-dispersed into 300mL of absolute ethyl alcohol, 8mL of diethanolamine and 4mL of deionized water are added into the mixture in a dropwise manner, stirring is continued (400r/min), 80mL of mixed solution of tetraethoxysilane and aminopropyltriethoxysilane (the concentration is 10 percent, and the proportion of tetraethoxysilane and aminopropyltriethoxysilane is 1:1) is slowly added dropwise, and stirring is continued for 3 hours after the dropwise addition is finished. And separating the iron powder from the solution in a centrifugal mode, drying the solution in a 60 ℃ oven for 24 hours, putting the powder into an argon atmosphere furnace, and carrying out heat treatment at 450 ℃ for 1 hour (the heating rate is 10 ℃/min) to obtain the final coated iron powder. Scanning electron microscope shows that the thickness of the coating layer on the surface of the iron powder is 300-400 nm, and the coating layer structure is intact. The obtained coated iron powder is prepared into a functional coating test piece to be subjected to a salt spray corrosion experiment, and no rust spots appear on the surface within 1000 hours.
Example 4
Dissolving 20g of polyvinylpyrrolidone in 600mL of deionized water, adding 150g of spherical carbonyl iron powder after fully dissolving, dispersing for 30min (ultrasonic power of 450W) by using ultrasonic, then mechanically stirring for 6h (rotating speed of 400r/min), separating the iron powder from the solution by using a suction filtration mode, and removing the filtrate to obtain the surface modified iron powder. The mixture is redispersed in 800mL of absolute ethyl alcohol, 15mL of diethanol amine and 8mL of deionized water are added into the mixture in a dropwise manner, stirring is continued (400r/min), 80mL of ethyl orthosilicate solution (with the concentration of 10%) is slowly added dropwise, and stirring is continued for 6 hours after the dropwise addition is finished. And separating the iron powder from the solution in a centrifugal mode, drying the solution in a 60 ℃ oven for 24 hours, putting the powder into an argon atmosphere furnace, and carrying out heat treatment at 450 ℃ for 2 hours (the heating rate is 10 ℃/min) to obtain the final coated iron powder. Scanning electron microscope shows that the thickness of the coating layer on the surface of the iron powder is 400-500 nm, and the coating layer structure is intact. The obtained coated iron powder is prepared into a functional coating test piece to be subjected to a salt spray corrosion experiment, and no rust spots appear on the surface within 1000 hours.
Claims (8)
1. An anti-corrosion treatment method of iron powder is characterized in that: the method comprises the following steps:
(1) uniformly dispersing iron powder into a solution containing an organic modifier, fully stirring to enable the surface of the iron powder to adsorb the organic modifier, and separating the iron powder adsorbed with the organic modifier from the solution containing the organic modifier to obtain surface-modified iron powder;
(2) adding the surface-modified iron powder obtained in the step (1) into absolute ethyl alcohol, continuously stirring, dropwise adding an organosilane solution and a hydrolyzing agent to hydrolyze organosilane, and forming a uniform silicon-containing coating layer on the surface of the iron powder to obtain coated iron powder;
(3) and (3) carrying out high-temperature heat treatment on the coated iron powder obtained in the step (2) in vacuum or inert atmosphere to further pyrolyze the coating layer on the surface of the coated iron powder to obtain the dense silicon dioxide coated iron powder.
2. The method for the anti-corrosion treatment of iron powder according to claim 1, characterized in that: the organosilane in the step (2) is one or more of methyl orthosilicate, ethyl orthosilicate, n-propyl silicate, aminopropyl triethoxysilane, vinyl trimethoxysilane and trifluoropropyl triethoxysilane, and the concentration of the organosilane is 0.01-10 g/mL.
3. The method for the anti-corrosion treatment of iron powder according to claim 1, characterized in that: and (3) the hydrolytic agent in the step (2) is ammonia water or diethanol amine.
4. The method for the anti-corrosion treatment of iron powder according to claim 1, characterized in that: the temperature of the high-temperature heat treatment in the step (3) is 200-1000 ℃, and the treatment time is 0.5-10 hours.
5. The method for the anti-corrosion treatment of iron powder according to claim 1, characterized in that: the organic modifier selected in the step (1) is one or more of sodium dodecyl benzene sulfonate, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone and sodium dodecyl sulfate, and the concentration of the organic modifier is 0.01-1 g/mL.
6. The method for the anti-corrosion treatment of iron powder according to claim 1, characterized in that: the stirring time of the step (1) is 5-24 hours.
7. The method for the anti-corrosion treatment of iron powder according to claim 1, characterized in that: and (2) separating the iron powder adsorbing the modifier from the solution containing the organic modifier in the step (1) by a centrifugal or suction filtration mode.
8. A corrosion-resistant iron powder obtainable by the method for the corrosion-resistant treatment of iron powder according to any one of claims 1 to 7, characterized in that: the surface of the corrosion-resistant iron powder is provided with a compact pyrolytic coating layer, and the shell layer of the corrosion-resistant iron powder contains silicon dioxide with the thickness of 10-800 nm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114082943A (en) * | 2021-11-23 | 2022-02-25 | 成都佳驰电子科技股份有限公司 | Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system |
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| CN104078182A (en) * | 2014-07-24 | 2014-10-01 | 武汉科技大学 | Iron-based soft magnetic composite magnetic powder core and preparation method thereof |
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| CN111087032A (en) * | 2018-10-24 | 2020-05-01 | 中国石油化工股份有限公司 | Silicon oxide and magnesium oxide composite material and synthesis method thereof |
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2020
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| CN1225047A (en) * | 1996-06-10 | 1999-08-04 | 日铁矿业株式会社 | Powder coated with multilayer film and process for preparing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114082943A (en) * | 2021-11-23 | 2022-02-25 | 成都佳驰电子科技股份有限公司 | Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system |
| CN114082943B (en) * | 2021-11-23 | 2024-01-05 | 成都佳驰电子科技股份有限公司 | Method for coating carbonyl iron powder with silicon dioxide in ethanol-free system |
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