CN108941543A - A kind of alumina-coated crome metal raw powder's production technology - Google Patents
A kind of alumina-coated crome metal raw powder's production technology Download PDFInfo
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- CN108941543A CN108941543A CN201811141562.2A CN201811141562A CN108941543A CN 108941543 A CN108941543 A CN 108941543A CN 201811141562 A CN201811141562 A CN 201811141562A CN 108941543 A CN108941543 A CN 108941543A
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- crome metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
Abstract
The invention discloses a kind of preparation methods of alumina-coated crome metal powder, this method prepares a kind of powder of shell-nutty structure using sol-gal process, realizes that method and step of the invention is as follows: step 1): it is modified to carry out silane coupling agent surface to crome metal powder；Step 2): alumina sol is prepared using aluminium secondary butylate；Step 3): step 1) and step 2) products therefrom are mixed and stirred for, and make its gel；Step 4): it repeats to be mixed with colloidal sol obtained by step 2) after gel obtained by step 3) is dried and is dispersed to carry out gel；Step 5): after multiple gel, drying and sintering obtains nucleocapsid structure composite granule.It is characterized in that, by the way that control of the gel process realization to shell thickness is repeated several times before powder sintering.The present invention realizes the characteristics of cladding shell thickness is uniform, shell is fine and close, surface is smooth, free from admixture, also has simple process, low in cost, steady performance.
Description
Technical field
The invention belongs to thermal spraying and field of powder metallurgy, and in particular to a kind of preparation of alumina-coated crome metal powder
Method.
Background technique
With the high speed development of military surveillance technology, military installations and the hidden of weaponry become increasingly difficult, " it was found that
Destroy " have become one of modern war important feature.And the stealthy position of weaponry can be divided into room temperature according to operating temperature
With high temperature two types.Stealthy demand of the high temperature microwave absorbing coating primarily directed to high-temperature components such as engine, smoke exhaust pipes.Due to exhausted
Most of electromagnetic consumable type absorbent Curie temperature is lower, and the condition of high temperature can demagnetize, and decline absorbing property, lead to material function
It loses, therefore equip the stealthy of high temperature position to use high temperature absorbing material.Cermet is that one kind is common, is answered both at home and abroad
With more high-power attenuating ceraics are obtained, their preparation method is mostly with W powder and A12O3It is compound in proportion to prepare mechanical strength
It is high, thermal conductivity is good, the cermet that can metallize and weld, be easily machined into required shape.Metal powder removes W, outside Mo,
Cr, Ni or other alloyed powders can also be used.Ceramic matrix removes A12O3Outside, it is also possible to sapphire, quartz and high A12O3、BN、
It is prepared by the ceramic powders such as BeO.But at present in the world using such material as absorbent, grinding for microwave absorbing coating is prepared by thermal spraying
Study carefully relatively fewer.Further, since ceramic coatings metal powder has metal and nonmetallic performance concurrently, also obtained extensively in various fields
General application.
Summary of the invention
The purpose of the present invention is to provide a kind of alumina-coated crome metal raw powder's production technologies.
The present invention adopts the following technical scheme that realize:
A kind of alumina-coated crome metal raw powder's production technology, comprising the following steps:
1) be 1:(50~150 than ethyl alcohol volume ratio according to deionized water by deionized water and ethyl alcohol) carry out mix, so
Silane coupling agent is added in ethyl alcohol and the mixed liquor of deionized water afterwards, and is sufficiently stirred and makes to be uniformly mixed；Add 2~
6mL glacial acetic acid adjusts the pH value of mixed liquor to 3~5, adds 10~20g crome metal powder, mechanical constant speed stirring keeps mixing equal
0.5~1.5h of even stirring；
2) sealing of mixed liquor that step 1) obtains is placed on 10~25h of stirring on magnetic stirring apparatus, then precipitate 1~
The cleaning of obtained solid formation, drying are obtained the modified crome metal powder in surface by 2h；
3) it is weighed by the volume ratio of ethyl acetoacetate, aluminium secondary butylate and deionized water for 1:3:21；Then by sec-butyl alcohol
Aluminium is first added drop-wise in deionized water dropwise, and 6~12min is stirred under 70~100 DEG C of water bath conditions, adds acetoacetate second
Ester continues 2~4h of stirring, then stands 10~13h of aging, obtains alumina sol, and wherein aluminium secondary butylate mass fraction is 98%；
4) the modified crome metal powder in the surface that step 2) obtains is added in the alumina sol of step 3) preparation, is added
Heat is stirred to 50~70 DEG C, while using mechanical agitator constant speed, and keeps the temperature 2~3h, obtains gel；
5) gel for obtaining step 4) is put into dry 24~36h in the drying box that temperature is 40~60 DEG C, obtains dry solidifying
Glue by gel dispersion and is sieved in such a way that glass bar is slightly ground in the process；
6) in the alumina sol for continuously adding step 3) preparation using scattered xerogel as initial powder, heating
To 50~60 DEG C, while mechanical stirring is used, and keep the temperature 2~4h, obtains two-step gelation；Putting it to temperature is 40~50 DEG C
Dry 20~36h, obtains xerogel in drying box, continues through the mode that glass bar is slightly ground in the process and divides gel
It dissipates and is sieved；
7) it repeats the above steps 6) up to carrying out 6~8 gel process, places into vacuum sintering furnace, rise after drying
Then temperature cools to room temperature with the furnace, obtains alumina-coated crome metal powder to 800~1200 DEG C of 2~6h of heat preservation.
A further improvement of the present invention lies in that, which is characterized in that in step 1), the volume ratio of silane coupling agent and ethyl alcohol is
1:(50~150).
A further improvement of the present invention lies in that, which is characterized in that in step 1), silane coupling agent KH550, hafnium metal powfer
Last partial size is 3~100 μm.
A further improvement of the present invention lies in that, which is characterized in that in step 1), revolving speed when mechanical constant speed stirs is 200
~300rpm.
A further improvement of the present invention lies in that, which is characterized in that in step 2), after the mixed liquor sealing that step 1) is obtained
Being placed in whipping temp on magnetic stirring apparatus is 60~80 DEG C, and obtained solid formation is cleaned 2 with ethyl alcohol for 150~250rpm by revolving speed
~4 times, 2~6h is then dried under conditions of temperature is 110~130 DEG C.
A further improvement of the present invention lies in that, which is characterized in that in step 5), the revolving speed of mechanical agitator constant speed stirring is
200~300rpm.
The present invention has following beneficial technical effect:
A kind of alumina-coated crome metal raw powder's production technology provided by the invention, the preparation method use collosol and gel
Method prepares cermet nucleocapsid structure composite phase-change material, is realized by the way that gel process is repeated several times to shell before powder sintering
The control of thickness.Wherein crome metal powder diameter is 3~100 μm, and shell thickness is 3~10 μm, and shell is fine and close, surface light
Sliding, free from admixture, thickness is uniform, effectively improves the microwave absorption capacity of material, and the present invention also have simple process, at
This cheap, performance stablizes the features such as adjustable, has wide practical use in various fields.The powder body material phase structure is cladded type
Composite powder is a kind of powder of shell-nutty structure, has many advantages, such as apparent density height, good dispersion, is suitble to thermal spraying.It should
Kind cermet cladded type composite powder is a kind of high temperature microwave absorbing material, and the microwave absorbing coating made of this absorbent can
To reach ideal wave-absorbing effect.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the stereoscan photograph of the crome metal of uncoated aluminium oxide；
Fig. 3 is by the stereoscan photograph of the core-shell structure of the alumina-coated crome metal of this method preparation；
Fig. 4 is by the stereoscan photograph of the core-shell structure of the alumina-coated crome metal of this method preparation.
Specific embodiment
The present invention is made further instructions below in conjunction with drawings and examples.
Embodiment 1:
A kind of alumina-coated crome metal raw powder's production technology of present embodiment includes the following steps progress:
1) ethyl alcohol, deionized water, silane coupling agent are measured, wherein the respectively 250mL and 3mL of ethyl alcohol and deionized water,
Silane coupling agent 2mL is added, ethyl alcohol is mixed with deionized water, then adds silane coupling agent, after mixing, with addition
It is 4 that 4mL glacial acetic acid, which adjusts pH value, adds crome metal powder 15g, is uniformly mixed, and mixed liquor is obtained, and mechanical constant speed stirring makes to mix
It closes uniform stirring 1h (revolving speed 250rpm)；
2) the mixed liquor sealing that step 1) obtains is placed on magnetic stirring apparatus and is stirred for 24 hours, temperature is 75 DEG C, and revolving speed is
Then 200rpm precipitates 1.5h, obtained solid formation is cleaned 3 times with ethyl alcohol, then dry under conditions of temperature is 120 DEG C
4h obtains the modified crome metal powder in surface；
It 3) is respectively that 1mL, 3mL, 21mL are measured by the volume of ethyl acetoacetate, aluminium secondary butylate and deionized water, then
Aluminium secondary butylate is added drop-wise in deionized water dropwise, 8min is stirred under 80 DEG C of water bath conditions, adds ethyl acetoacetate, after
Continue and stir 3h under water bath condition, then stand aging 11h, obtains alumina sol；
4) the modified crome metal powder in the surface that step 2) obtains is added in the alumina sol of step 3) preparation, is added
Heat is stirred to 60 DEG C, while using mechanical agitator constant speed 250rpm, and keeps the temperature 2.5h, obtains gel.
5) gel for obtaining step 4) is put into dry 30h in the baking oven that temperature is 55 DEG C, obtains xerogel.In this process
In by gel dispersion and be sieved by way of Glass rod grinding.
6) in the alumina sol for continuously adding step 3) preparation using scattered xerogel as initial powder, heating
To 55 DEG C, while mechanical stirring is used, and keep the temperature 3h, obtains two-step gelation；It puts it in the drying box that temperature is 45 DEG C and does
It is dry for 24 hours, obtain xerogel.It by gel dispersion and is sieved by way of Glass rod grinding in the process.
7) above-mentioned 6 step is repeated until carrying out 7 gel process, place into vacuum sintering furnace, be warming up to after drying
1100 DEG C of heat preservation 4h, then cool to room temperature with the furnace, obtain nucleocapsid structure composite granule.It is illustrated in figure 2 crome metal powder
Single-size shape is presented in shape appearance figure, powder granule, and size range is distributed between 20~80 μm.Fig. 3 is alumina-coated chromium powder
The shape appearance figure of body, chromium metal surface form uniformly complete alumina-coated layer, and the metal surface after powder cladding forms
Colloidal silica silicon fiml.Fig. 4 is alumina-coated crome metal powder Cross Section Morphology figure, by section it can be seen that chromium powder surface forms
Complete clad, coating thickness are probably distributed in 2~4 μm.
Embodiment 2:
A kind of alumina-coated crome metal raw powder's production technology of present embodiment includes the following steps progress:
1) ethyl alcohol, deionized water, silane coupling agent are measured, wherein the respectively 250mL and 3mL of ethyl alcohol and deionized water,
Silane coupling agent 2mL is added, ethyl alcohol is mixed with deionized water, then adds silane coupling agent, after mixing, with addition
It is 4 that 4mL glacial acetic acid, which adjusts pH value, adds crome metal powder 18g, is uniformly mixed, and mixed liquor is obtained, and mechanical constant speed stirring makes to mix
It closes uniform stirring 1h (revolving speed 250rpm)；
2) the mixed liquor sealing that step 1) obtains is placed on magnetic stirring apparatus and is stirred for 24 hours, temperature is 75 DEG C, and revolving speed is
Then 200rpm precipitates 1.5h, obtained solid formation is cleaned 3 times with ethyl alcohol, then dry under conditions of temperature is 120 DEG C
4h obtains the modified crome metal powder in surface；
It 3) is respectively 1.5mL, 4.5mL, 31.5mL amount by the volume of ethyl acetoacetate, aluminium secondary butylate and deionized water
It takes, is then added drop-wise to aluminium secondary butylate in deionized water dropwise, stir 8min under 80 DEG C of water bath conditions, add acetoacetate
Ethyl ester, 3h is stirred in continuation under 80 DEG C of water bath condition, then stands aging 11h, obtains alumina sol；
4) the modified crome metal powder in the surface that step 2) obtains is added in the alumina sol of step 3) preparation, is added
Heat is stirred to 60 DEG C, while using mechanical agitator constant speed 250rpm, and keeps the temperature 2.5h, obtains gel.
5) gel for obtaining step 4) is put into dry 30h in the baking oven that temperature is 55 DEG C, obtains xerogel.In this process
In by gel dispersion and be sieved by way of Glass rod grinding.
6) in the alumina sol for continuously adding step 3) preparation using scattered xerogel as initial powder, heating
To 55 DEG C, while mechanical stirring is used, and keep the temperature 3h, obtains two-step gelation；It puts it in the drying box that temperature is 45 DEG C and does
It is dry for 24 hours, obtain xerogel.It by gel dispersion and is sieved by way of Glass rod grinding in the process.
7) above-mentioned 6 step is repeated until carrying out 7 gel process, place into vacuum sintering furnace, be warming up to after drying
1100 DEG C of heat preservation 4h, then cool to room temperature with the furnace, obtain nucleocapsid structure composite granule.
Embodiment 3:
A kind of alumina-coated crome metal raw powder's production technology of present embodiment includes the following steps progress:
1) ethyl alcohol, deionized water, silane coupling agent are measured, wherein the respectively 250mL and 3mL of ethyl alcohol and deionized water,
Silane coupling agent 2mL is added, ethyl alcohol is mixed with deionized water, then adds silane coupling agent, after mixing, with addition
It is 4 that 4mL glacial acetic acid, which adjusts pH value, adds crome metal powder 20g, is uniformly mixed, and mixed liquor is obtained, and mechanical constant speed stirring makes to mix
It closes uniform stirring 1h (revolving speed 250rpm)；
2) the mixed liquor sealing that step 1) obtains is placed on magnetic stirring apparatus and is stirred for 24 hours, temperature is 75 DEG C, and revolving speed is
200rpm.Then 1.5h is precipitated, obtained solid formation is cleaned 3 times with ethyl alcohol, it is then dry under conditions of temperature is 120 DEG C
4h obtains the modified crome metal powder in surface；
It 3) is respectively that 2mL, 6mL, 42mL are measured by the volume of ethyl acetoacetate, aluminium secondary butylate and deionized water, then
Aluminium secondary butylate is added drop-wise in deionized water dropwise, 8min is stirred under 80 DEG C of water bath conditions, adds ethyl acetoacetate, after
Continue and stir 3h under water bath condition, then stand aging 11h, obtains alumina sol；
4) the modified crome metal powder in the surface that step 2) obtains is added in the alumina sol of step 3) preparation, is added
Heat is stirred to 60 DEG C, while using mechanical agitator constant speed 250rpm, and keeps the temperature 2.5h, obtains gel.
5) gel for obtaining step 4) is put into dry 30h in the baking oven that temperature is 55 DEG C, obtains xerogel.In this process
In by gel dispersion and be sieved by way of Glass rod grinding.
6) in the alumina sol for continuously adding step 3) preparation using scattered xerogel as initial powder, heating
To 55 DEG C, while mechanical stirring is used, and keep the temperature 3h, obtains two-step gelation；It puts it in the drying box that temperature is 45 DEG C and does
It is dry for 24 hours, obtain xerogel.It by gel dispersion and is sieved by way of Glass rod grinding in the process.
7) above-mentioned 6 step is repeated until carrying out 7 gel process, place into vacuum sintering furnace, be warming up to after drying
1100 DEG C of heat preservation 4h, then cool to room temperature with the furnace, obtain nucleocapsid structure composite granule.
The present invention prepares cermet nucleocapsid structure composite phase-change material using sol-gal process, which is characterized in that powder
By the way that control of the gel process realization to shell thickness is repeated several times before sintering.Wherein the partial size of crome metal powder is 3~100 μ
M, shell thickness can achieve 2~10 μm, and shell is fine and close, and surface is smooth, and free from admixture, thickness is uniform, effectively improves
The microwave absorption capacity of material, and the present invention also have the characteristics that simple process, low in cost, performance stablize it is adjustable, in crowd
It is multi-field to have wide practical use.
Claims (6)
1. a kind of alumina-coated crome metal raw powder's production technology, which comprises the following steps:
1) be 1:(50~150 than ethyl alcohol volume ratio according to deionized water by deionized water and ethyl alcohol) carry out mix, then will
Silane coupling agent is added in ethyl alcohol and the mixed liquor of deionized water, and is sufficiently stirred and is made to be uniformly mixed；Add 2~6mL ice
Acetic acid adjusts the pH value of mixed liquor to 3~5, adds 10~20g crome metal powder, mechanical constant speed stirring makes to be uniformly mixed stirring
0.5~1.5h；
2) the mixed liquor sealing that step 1) obtains is placed on 10~25h of stirring on magnetic stirring apparatus, then precipitates 1~2h, it will
Obtained solid formation cleaning, drying, obtains the modified crome metal powder in surface；
3) it is weighed by the volume ratio of ethyl acetoacetate, aluminium secondary butylate and deionized water for 1:3:21；Then by aluminium secondary butylate elder generation
It is added drop-wise in deionized water dropwise, 6~12min is stirred under 70~100 DEG C of water bath conditions, adds ethyl acetoacetate, after
2~4h of continuous stirring, then 10~13h of aging is stood, alumina sol is obtained, wherein aluminium secondary butylate mass fraction is 98%；
4) the modified crome metal powder in the surface that step 2) obtains is added in the alumina sol of step 3) preparation, is heated to
50~70 DEG C, while being stirred using mechanical agitator constant speed, and keep the temperature 2~3h, obtain gel；
5) gel for obtaining step 4) is put into dry 24~36h in the drying box that temperature is 40~60 DEG C, obtains xerogel,
It by gel dispersion and is sieved during this in such a way that glass bar is slightly ground；
6) in the alumina sol for continuously adding step 3) preparation using scattered xerogel as initial powder, 50 are heated to
~60 DEG C, while mechanical stirring is used, and keep the temperature 2~4h, obtain two-step gelation；Put it to the drying that temperature is 40~50 DEG C
Dry 20~36h, obtains xerogel in case, continues through mode that glass bar is slightly ground in the process for gel dispersion simultaneously
Sieving；
7) it repeats the above steps 6) until 6~8 gel process of progress, place into vacuum sintering furnace after drying, be warming up to
800~1200 DEG C of 2~6h of heat preservation, then cool to room temperature with the furnace, obtain alumina-coated crome metal powder.
2. a kind of alumina-coated crome metal raw powder's production technology according to claim 1, which is characterized in that its feature
It is, in step 1), the volume ratio of silane coupling agent and ethyl alcohol is 1:(50~150).
3. a kind of alumina-coated crome metal raw powder's production technology according to claim 1, which is characterized in that its feature
It is, in step 1), silane coupling agent KH550, crome metal powder diameter is 3~100 μm.
4. a kind of alumina-coated crome metal raw powder's production technology according to claim 1, which is characterized in that its feature
It is, in step 1), revolving speed when mechanical constant speed stirs is 200~300rpm.
5. a kind of alumina-coated crome metal raw powder's production technology according to claim 1, which is characterized in that its feature
It is, in step 2), it is 60~80 DEG C that the mixed liquor sealing that step 1) obtains, which is placed on whipping temp on magnetic stirring apparatus, is turned
Speed is that 150~250rpm cleans obtained solid formation 2~4 times with ethyl alcohol, then under conditions of temperature is 110~130 DEG C
Dry 2~6h.
6. a kind of alumina-coated crome metal raw powder's production technology according to claim 1, which is characterized in that its feature
It is, in step 5), the revolving speed of mechanical agitator constant speed stirring is 200~300rpm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111790916A (en) * | 2019-04-01 | 2020-10-20 | 通用电气公司 | Preparation of chromium metal mixtures in the form of core-shell nanoparticles |
| RU2760847C1 (en) * | 2021-03-16 | 2021-11-30 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кубанский государственный технологический университет" (ФГБОУ ВО "КубГТУ") | Cladding method for powder magnetic material |
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Application publication date: 20181207 |