CN113802042A - Uniformly dispersed Al2O3Preparation method of/Fe composite material - Google Patents
Uniformly dispersed Al2O3Preparation method of/Fe composite material Download PDFInfo
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- CN113802042A CN113802042A CN202111089362.9A CN202111089362A CN113802042A CN 113802042 A CN113802042 A CN 113802042A CN 202111089362 A CN202111089362 A CN 202111089362A CN 113802042 A CN113802042 A CN 113802042A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0235—Starting from compounds, e.g. oxides
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0026—Matrix based on Ni, Co, Cr or alloys thereof
Abstract
The invention relates to a method for preparing uniformly dispersed Al2O3A production method of a/Fe composite material belongs to the technical field of composite material preparation. The process comprises the following steps: (1) preparing an iron source, glycine, an aluminum source and an additive (ammonium nitrate and the like) into a solution according to a certain proportion; (2) heating and stirring, volatilizing the solution, concentrating and decomposing to obtain precursor powder; (3) and reacting the precursor powder for 1-3 hours at the temperature of 300-600 ℃ under a certain protective atmosphere to obtain the composite powder. (4) Pressing and molding the composite powder, and calcining at 800-1300 ℃ in a certain atmosphereAnd (4) sintering to obtain the alumina/iron composite material. The method has the advantages of cheap and easily-obtained raw materials, simple and quick manufacturing process, low process energy consumption and low cost, can realize large-scale production, and obtains the aluminum oxide/iron composite material with fine and uniformly-distributed oxide particles.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and particularly relates to a production method of a uniformly dispersed aluminum oxide/iron composite material.
Background
The metal material has excellent comprehensive mechanical property and physical and chemical properties, is one of the most important structural materials, and is the most widely used material in the human society at present. With the continuous progress of science and technology, the high-tech field puts higher demands on the research and development and application of new materials, and the preparation means of metal material composite materials are increasingly paid attention, namely, an 'enhancing body/functional body' is added into the metal material, on the basis that the intrinsic performance of the matrix is kept, the matrix and the enhancing body generate the synergistic coupling effect and the interface effect in the modes of uniform dispersion and interface control, the components make up for the deficiencies of a single material, and the comprehensive performance of the composite material is improved. The metal matrix composite material has excellent properties of high specific strength, high specific modulus, high wear resistance, high temperature resistance and the like, and thus becomes one of the most attractive materials in aerospace, automobile industry, mine metallurgy and coal industry. According to different reinforcement types, the reinforcement can be divided into 3 types of particle, whisker and fiber reinforcement. The ceramic particle reinforced metal matrix composite material has become the most extensive research and application due to the advantages of low cost, simple preparation, isotropy and the like, and the common ceramic particle reinforcement is Al2O3、SiC、TiC、B4C and the like. Al (Al)2O3The ceramic is an oxidation-resistant, corrosion-resistant and wear-resistant high-temperature structural ceramic material, has good chemical stability, ensures that the ceramic has good performance at high temperature, is low in price, is most applied to industrial production, and is considered as a good reinforcement of a metal-based composite material. Al (Al)2O3The particles can be uniformly dispersed in the metal matrix and canEffectively pinning dislocation, crystal boundary and subcrystal boundary, hindering the movement of dislocation and storing dislocation, and limiting the growth of crystal grains, thereby strengthening the material and improving the mechanical property of the material. Al (Al)2O3Reinforced iron-based composites generally have high strength, high toughness, high wear resistance, and high temperature resistance. In addition, the iron matrix in the composite material system generally has high conductivity, permeability and saturation magnetization, while Al2O3The electrolyte materials have small magnetic conductivity, and the composite material formed by the electrolyte materials not only has good mechanical property, but also has possible unique electromagnetic property, so that the composite material becomes a novel electromagnetic wave absorbent and shielding material with high electromagnetic wave absorption performance, and can be widely applied to the aspects of magnetic media, wave absorbing materials, dielectric materials, corrosion resistant materials, antioxidant materials and the like.
Currently, nano Al is prepared2O3Methods for reinforcing iron-based composite materials include mechanical methods, thermal decomposition methods, precipitation methods, hydrolysis methods, sol-gel methods, and the like. In publication No. CN110355373B, Li Guangzhi et Al prepared Al with dense, uniform and crack-free film layer by using zirconium hydride, zirconium oxychloride, boehmite, polyethylene, isopropanol as raw materials and through certain technological process including sol-gel synthesis, sintering, coating and the like2O3Toughened ZrO2The method for preparing the/Zr stainless steel composite material is tedious and long, has multiple working procedures, can generate a plurality of hazardous wastes of liquid, and has low practical production and application values. In publication No. CN112430763A, Chengaiyong et Al mechanically alloyed Al is prepared by annealing atomized Cu-Al alloy as copper source and oxidized Cu-Al alloy powder as oxygen source, ball milling and mixing at a certain ratio, reducing, and sintering2O3The method is simple and easy to implement, but needs to carry out annealing, reduction and sintering for a long time, and has high energy consumption and high cost. In publication No. CN109518033A, Wangliden et al first treated aluminum powder, reaction powder, foaming agent, K2TiF4Pretreating, mixing with rare-earth compound, heating, removing surface dross, spraying it into molten aluminium, degassing, extruding and heat treatingTo obtain Al2O3The method is novel, but needs to add rare earth oxide, increases the cost, has long production period and is not suitable for industrial large-scale production.
According to the Orowan theory, at the same volume fraction of reinforcement phase, the strength of the composite material increases as the particle size of the reinforcement decreases. A large number of researches also show that under the condition of the same volume fraction, nano Al is dispersed and distributed2O3Micron-sized Al2O3The reinforcing efficiency of the particles to the composite material is higher, and certain plasticity can be kept while the strength of the composite material is obviously improved. The invention provides a method for preparing nano Al2O3The method for uniformly dispersing the iron-based composite material is characterized in that oxide particles and a matrix are uniformly mixed at an atomic level in a liquid-liquid mixing mode, the reaction time is short, the cost is low, the energy consumption is low, the powder particles of the product are fine and uniform, the sintering activity is high, the densification temperature and time can be reduced, the reaction cost is greatly saved, and a wider application range is provided for the oxide particle reinforced metal-based composite material.
Disclosure of Invention
The invention aims to provide a simple and low-cost production method for preparing uniformly dispersed aluminum oxide/iron composite material.
The method for producing the nano composite material is characterized by comprising the following steps:
a. dissolving an iron source and a fuel in deionized water according to a certain proportion, wherein the proportion of the iron source to the fuel is 1 (1-6) in a molar ratio, and the adding amount of an aluminum source is 0.5-10% of the mass fraction of aluminum oxide in the prepared composite material;
b. heating and stirring the solution formed in the step a to volatilize, concentrate and decompose the solution to obtain precursor powder;
c. b, reacting the precursor powder obtained in the step b for 1-3 hours at the temperature of 300-600 ℃ in a certain protective atmosphere to obtain iron/aluminum oxide composite powder;
d. c, pressing and molding the iron/aluminum oxide composite powder obtained in the step c to obtain an iron/aluminum oxide composite green body;
e. and d, calcining the green body obtained in the step d at the temperature of 800-1300 ℃ under a certain condition to obtain the aluminum oxide/iron composite material.
Further, the iron source added in the step a is soluble iron salt such as ferric nitrate, ferric sulfate, ferric chloride and the like; when the iron source is ferric nitrate, the fuel is an oxidant such as glycine, urea, glucose or citric acid, and the molar ratio of the iron source to the fuel is 1 (1-6); wherein the aluminum source is soluble aluminum salt such as aluminum nitrate, aluminum sulfate and the like. When soluble aluminum salt such as aluminum sulfate and aluminum chloride is used, ammonium nitrate as an additive is required.
Further, the predetermined atmosphere in step c is a reducing atmosphere such as hydrogen or carbon monoxide. The optimal reaction temperature is 400-500 ℃; the optimal reaction time is 1.5 to 2.5 hours.
Furthermore, the compression molding process in the step d uses compression molding and cold isostatic pressing, and the pressure is 150-300 MPa.
Furthermore, the sintering conditions in the step e are protective atmospheres such as vacuum, hydrogen, nitrogen and the like. The sintering time is 1-3 hours.
The key points of the technology of the invention are as follows:
firstly, uniformly mixed oxide precursor powder is prepared by using a solution combustion synthesis method, the prepared powder is loose, is not easy to agglomerate, has high reaction activity, is reduced in a reducing atmosphere according to the difference of reduction activities of iron oxide and aluminum oxide in the precursor to obtain aluminum oxide/iron composite powder, has high sintering activity, can realize densification at a lower sintering temperature to obtain an aluminum oxide/iron composite material, and has fine and uniformly dispersed particles, and the mechanical property of the aluminum oxide/iron composite material is greatly improved.
The preparation method comprises the steps of preparing precursor powder by controlling the adding amounts of an iron source, a fuel and an aluminum source, and reacting at the temperature of 300-600 ℃ in a protective atmosphere to obtain iron/aluminum oxide composite powder; then, the aluminum oxide/iron composite material is obtained through compression and calcination treatment. The prepared composite material alumina particles are fine and uniformly dispersed in an iron matrix, the product performance is excellent, the process is simple, the cost is low, and the large-scale production can be realized.
The method has the following advantages: (1) the reaction is carried out in a liquid phase, so that the uniform mixing of the atomic levels of all components can be realized, and the uniform dispersion distribution of particles in a matrix can be realized; (2) gas generated in the reaction process can play a role in dispersing products, the precursor prepared by agglomeration of powder particles (3) can be effectively prevented from having high reaction activity, the subsequent reaction temperature can be reduced, and the reaction speed is improved; (4) the prepared composite powder has uniform dispersion, fine particles and high activity, and can effectively reduce the subsequent densification temperature; (5) the prepared composite material alumina particles are fine and uniformly dispersed in an iron matrix; (6) the raw materials are cheap and easy to obtain, the preparation process is simple, convenient and quick, the process energy consumption is low, the cost is low, and the large-scale production can be realized.
Drawings
FIG. 1 is a microscopic view of the alumina/iron composite of the present invention.
Detailed Description
The present invention is further illustrated below with reference to examples, which are intended to illustrate the invention and not to limit the scope of the invention. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the teachings herein, and such equivalents may fall within the scope of the invention as defined in the appended claims.
Example 1:
weighing 0.1 mol of ferric nitrate, 0.2 mol of glycine and 0.002 mol of aluminum nitrate, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 2 hours at the temperature of 400 ℃ in a hydrogen atmosphere to obtain the iron/aluminum oxide composite powder. And pressing the composite powder on a hydraulic press to obtain a green body, wherein the pressing pressure is 200MPa, so as to obtain the green body. And (3) putting the green body into a sintering furnace, and sintering for 2h at 900 ℃ in a hydrogen atmosphere to obtain the iron/aluminum oxide composite material.
Example 2:
weighing 0.1 mol of ferric chloride, 0.3 mol of glycine and 0.006 mol of aluminum source, dissolving the raw materials in deionized water to prepare a mixed solution, and placing the mixed solution on a temperature-controllable electric furnace for heating. The solution is subjected to a series of reactions such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder is reacted for 2 hours at 500 ℃ in a hydrogen atmosphere to obtain the iron/aluminum oxide nano composite material. And pressing the composite powder on a hydraulic press to obtain a green body, wherein the pressing pressure is 300MPa to obtain the green body. And (3) putting the green body into a sintering furnace, and sintering for 3h at 800 ℃ in a hydrogen atmosphere to obtain the iron/aluminum oxide composite material.
Example 3:
0.1 mol of ferric sulfate, 0.4 mol of glycine, 0.009 mol of aluminum source and 0.015 mol of ammonium nitrate are weighed, dissolved in distilled water to prepare a solution, and the solution is placed on a temperature-controllable electric furnace for heating. The solution reacts after a series of processes such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder reacts in a furnace for 2.5 hours at the temperature of 400 ℃ in the atmosphere of carbon monoxide to obtain the iron/aluminum oxide nano composite material. And (3) carrying out cold isostatic pressing on the composite powder, and pressing under 150MPa to obtain a green body. And (3) placing the green body into a sintering furnace, and sintering for 2h at 1100 ℃ in a vacuum atmosphere to obtain the iron/aluminum oxide composite material.
Example 4:
0.1 mol of ferric nitrate, 0.4 mol of glycine and 0.01 mol of aluminum nitrate are weighed and dissolved in deionized water to prepare a mixed solution, and the mixed solution is placed on a temperature-controllable electric furnace for heating. The solution reacts after a series of processes such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder reacts in a furnace for 1 hour at the temperature of 600 ℃ in the atmosphere of carbon monoxide to obtain the iron/aluminum oxide nano composite material. And pressing the composite powder on a hydraulic press to obtain a green body, wherein the pressing pressure is 200MPa, so as to obtain the green body. And (3) placing the green body into a sintering furnace, and sintering for 1h at 1300 ℃ in a nitrogen atmosphere to obtain the iron/aluminum oxide composite material.
Example 5:
0.1 mol of ferric nitrate, 0.6 mol of glycine and 0.005 mol of aluminum nitrate are weighed and dissolved in deionized water to prepare a mixed solution, and the mixed solution is placed on a temperature-controllable electric furnace for heating. The solution reacts after a series of processes such as volatilization, concentration, decomposition and the like to obtain precursor powder, and the precursor powder reacts in a furnace for 2.5 hours at the temperature of 400 ℃ in hydrogen atmosphere to obtain the iron/aluminum oxide nano composite material. And pressing the composite powder on a hydraulic press to obtain a green body, wherein the pressing pressure is 200MPa, so as to obtain the green body. And (3) placing the green body into a sintering furnace, and sintering for 2h at 900 ℃ in an argon atmosphere to obtain the iron/aluminum oxide composite powder.
Claims (5)
1. A production method of a uniformly dispersed alumina/iron composite material is characterized by comprising the following steps:
a. dissolving an iron source and a fuel in deionized water according to a certain proportion, wherein the proportion of the iron source to the fuel is 1 (1-6) in a molar ratio, and the adding amount of an aluminum source is 0.5-10% of the mass fraction of aluminum oxide in the prepared composite material;
b. heating and stirring the solution formed in the step a to volatilize, concentrate and decompose the solution to obtain precursor powder;
c. b, reacting the precursor powder obtained in the step b for 1-3 hours at the temperature of 300-600 ℃ in a certain protective atmosphere to obtain iron/aluminum oxide composite powder;
d. c, pressing and molding the iron/aluminum oxide composite powder obtained in the step c to obtain an iron/aluminum oxide composite green body;
e. and d, calcining the green body obtained in the step d at the temperature of 800-1300 ℃ under a certain condition to obtain the aluminum oxide/iron composite material.
2. The method for preparing a uniformly dispersed alumina/iron composite according to claim 1, wherein the iron source added in step a is ferric nitrate, ferric sulfate, ferric chloride soluble ferric salt; wherein when the iron source is ferric nitrate, the fuel is glycine, urea, glucose or citric acid oxidant, and the molar ratio of the iron source to the fuel is 1: (1-6); wherein the aluminum source is aluminum nitrate and aluminum sulfate soluble aluminum salt, when the aluminum sulfate and aluminum chloride soluble aluminum salt are used, an additive ammonium nitrate is required to be added, and the adding amount of the aluminum salt is 0.5-10% of the mass fraction of the aluminum oxide in the prepared composite material.
3. The method for preparing the uniformly dispersed alumina/iron composite material according to claim 1, wherein the atmosphere in step c is a reducing protective atmosphere of hydrogen and carbon monoxide, and the reaction temperature is 300-600 ℃; the reaction time is 1-3 hours.
4. The method as claimed in claim 1, wherein the compression molding process in step d comprises compression molding and cold isostatic pressing at a pressure of 150-300 MPa.
5. The method for preparing a uniformly dispersed alumina/iron composite material according to claim 1, wherein the sintering conditions in the step e are vacuum, hydrogen and nitrogen protective atmospheres, and the sintering temperature is 800-1300 ℃ and the sintering time is 1-3 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5338714A (en) * | 1990-07-24 | 1994-08-16 | Centre National De La Recherche Scientifique (C.N.R.S.) | Composite alumina/metal powders, cermets made from said powders, and processes of production |
| JPH06339630A (en) * | 1993-01-27 | 1994-12-13 | Hanyou Kagaku Kk | Preparation of alumina-iron salt composite body |
| CN1644279A (en) * | 2005-01-19 | 2005-07-27 | 华南理工大学 | Preparation of warm pressed diffusing particle reinforced iron-based powder metallized composite materials |
| CN104525962A (en) * | 2014-12-17 | 2015-04-22 | 北京科技大学 | Method for preparing nanoscale oxide dispersion strengthening iron-based composite powder |
| CN109371308A (en) * | 2018-12-17 | 2019-02-22 | 湘潭大学 | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5338714A (en) * | 1990-07-24 | 1994-08-16 | Centre National De La Recherche Scientifique (C.N.R.S.) | Composite alumina/metal powders, cermets made from said powders, and processes of production |
| JPH06339630A (en) * | 1993-01-27 | 1994-12-13 | Hanyou Kagaku Kk | Preparation of alumina-iron salt composite body |
| CN1644279A (en) * | 2005-01-19 | 2005-07-27 | 华南理工大学 | Preparation of warm pressed diffusing particle reinforced iron-based powder metallized composite materials |
| CN104525962A (en) * | 2014-12-17 | 2015-04-22 | 北京科技大学 | Method for preparing nanoscale oxide dispersion strengthening iron-based composite powder |
| CN109371308A (en) * | 2018-12-17 | 2019-02-22 | 湘潭大学 | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end |
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