CN1182063A - Preparation of ceramic grain reinforced aluminium-based composite material - Google Patents
Preparation of ceramic grain reinforced aluminium-based composite material Download PDFInfo
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- CN1182063A CN1182063A CN 97121945 CN97121945A CN1182063A CN 1182063 A CN1182063 A CN 1182063A CN 97121945 CN97121945 CN 97121945 CN 97121945 A CN97121945 A CN 97121945A CN 1182063 A CN1182063 A CN 1182063A
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Abstract
Ceramic grains are treated with fluorate as dipping assistant, specifically, they soaked with 5-15% water solution of K2ZrF6 or K2TiF6 at 80-95 deg. c or mixed with fluorate before stoving. After ceramic grains thus treated are placed at the bottom of molten aluminium and the temperature is maintained for a certain period, molten aluminium stirred is poured into mould. The present invention can improve the wetting property of molten aluminium to the surface of ceramic grains, and through smooth stirring it is possible to prepare required composite material in atmospheric environment.
Description
The invention relates to a preparation method of a ceramic particle reinforced aluminum alloy matrix composite material.
The ceramic reinforced aluminum-based composite material consists of an aluminum alloy matrix and ceramic particles (oxides, carbides and nitrides). Wherein, the ceramic particles are artificially added according to a certain content and are uniformly distributed in the aluminum alloy matrix. The particle reinforced aluminum matrix composite has the characteristics of good wear resistance, high specific strength and rigidity, good high-temperature performance, good dimensional stability and the like, and is a structural and functional material with deep potential. At present, there are many processes for preparing particle-reinforced aluminum matrix composites, such as powder metallurgy, preform infiltration, stirring, spray deposition, etc., and the stirring method is the simplest and most economical, and is to add and disperse particles into an aluminum alloy melt while mechanically stirring the aluminum alloy melt. In the method, because pollutants such as oxide, adsorbed gas, moisture and the like exist on the surface of the particles, and an oxide film exists on the surface of the aluminum alloy melt, the particles are prevented from really contacting with the melt, and the aluminum alloy is preparedThe poor wetting between the particles and the melt at the preparation temperature makes the particles difficult to incorporate and disperse. To improve the wettability of the two, methods are generally used: coating Ni, Cu and other metals on the surface of the particles; adding surface active elements such as Li, Mg and the like into the melt; the surface of the particles is cleaned by organic solvent, baked at high temperature, bombarded by vacuum plasma and the like to purify the surface. For example, Chinese patent application CN1030445A discloses a "metal matrix composite" in which Mg is added to aid in leaching and N is introduced2The gas to form AlN improves the wettability of the ceramic particles. Meanwhile, in the prior art, a special device is needed to be used for preparing the particle reinforced aluminum-based composite material by a stirring method under the protection of vacuum or inert gas, for example, U.S. Pat. No. 4,4786467 discloses a preparation method of a non-metal particle reinforced metal-based composite material, which is to stir in a shearing mode under vacuum to enable particles and metal liquid to mutually shear so as to improve wetting.
The invention aims to improve the prior art according to the problems in the prior art to obtain a preparation method of a ceramic particle reinforced aluminum matrix composite, which is completed in an atmospheric environment, does not need special equipment and vacuum protection, and has a simple manufacturing process.
In order to achieve the purpose, the technical solution provided by the invention is as follows:
a process for preparing the aluminium-base composite material reinforced by ceramic particles includes such steps as stirring the ceramic particles in aluminium liquid, treating the ceramic particles with fluoric acid salt as immersing aid, putting them in the bottom of aluminium liquid, holding temp for a certain time, stirring for a certain time, and pouring the aluminium liquid in mould.
Placing the ceramic particles treated with the fluoride salt leaching aid at the bottom of a crucible heated to an aluminum alloy melting temperature, pouring molten and refined degassed aluminum liquid from above, or placing an aluminum block of a required weight and holding for a period of time.
The leaching aid fluoride salt is K2ZrF6、K2TiF6、Na3AlF6、NaF、CaF2。
The method for treating the ceramic particles by using the fluoride salt leaching aid comprises the following steps: with fluoride salts such as K in the desired concentration2ZrF6、K2TiF6And (3) drying after soaking in the aqueous solution, or drying after mixing the ceramic particles with the fluosilicate.
By K2ZrF6、K2TiF6The method for soaking the ceramic particles by the aqueous solution comprises the following steps: soaking the substrate in a solution with the concentration of 5-15% for 5-15 minutes at the temperature of 80-95 ℃.
The proportion of the leaching aid fluoride salt powder to the ceramic particles is 1: 5-1: 1.
The present invention will be described in further detail with reference to examples.
The invention uses fluosilicate as an auxiliary leaching agent, and the fluosilicate is a solvent commonly used in aluminum alloy smelting and can remove Al on the contact surface of particles and aluminum melt2O3The film promotes the wetting of the aluminum liquid and the ceramic particles, and plays a role in assisting the wetting.
The pretreatment process will be described below by taking SiC particles as an example, the green SiC particles used are obtained by crushing and sieving bulk SiC, and the other ceramic particles are similar to SiC particles.
The auxiliary leaching agent adopted by the invention is fluoric acid salt with K2ZrF6、K2TiF6、Na3AlF6、NaF、CaF2In which K is2ZrF6、K2TiF6The character of (A) is slightly soluble in cold water and soluble in hot water. To coat a thin layer K on the surface of the SiC particles2ZrF6、K2TiF6Crystals of, K2ZrF6、K2TiF6The water solution must reach a certain concentration, so the solution must be prepared at 80-95 ℃, the concentration range is 5-15%, SiC particles are put into the prepared solution which is kept warm, and after soaking for 5-15 minutes, SiC is filtered out and dried. The drying is to prevent the following reaction between the moisture and the aluminum liquid: when water content is small, hydrogen is dissolved into the molten aluminum and is precipitated after solidification to form a needlePores, detrimental to performance; when the moisture content is large, explosion may be caused. For preventing evaporation of water during drying process2ZrF6、K2TiF6Is brought to the outer particle to give K2ZrF6、K2TiF6The distribution is not uniform, and the drying can adopt low temperature and high temperature firstly, or continuously turn over the particles in the drying process. Another pre-treatment method is to mix the particles in the following mass ratios of ceramic particles: the leaching aid (by weight) is 5: 1-1: 1, and the leaching aid fluoric acid salt comprises: k2ZrF6、K2TiF6、Na3AlF6、NaF、CaF2In which Na3AlF6Slightly soluble in water, CaF2Is insoluble in water; NaF is not easy to handle due to strong corrosivity of the aqueous solution, so Na3AlF6、NaF、CaF2Only mixed treatment is possible. The fluoric acid salt powder and the ceramic particles are mixed and dried, and the method is simpler and more convenient to operate and is easy to control the dosage.
The process for preparing the composite material comprises the following steps: placing a crucible in a resistance furnace, heating to the aluminum alloy melting temperature, and then placing ceramic particles. If the ceramic particles and the crucible are heated simultaneously, the temperature is raisedWhen the aluminum is melted, because the high temperature is too long, SiC particles are easy to sinter and agglomerate, and the uniform dispersion of SiC is influenced later. And (3) placing the treated thermal SiC particles at the bottom of the crucible, leveling the loose particles, and pouring aluminum alloy liquid into the crucible. Because the affinity of the aluminum and the oxygen is very large, the aluminum is very easy to oxidize, and continuous Al is formed on the surface of the aluminum liquid even under the low vacuum condition with small oxygen partial pressure2O3If ceramic particles are added into the thin film from the top, stirring is needed to be carried out, so that the particles enter the aluminum liquid, when the particles are added into the aluminum liquid, the oxide film on the surface of the aluminum liquid is inevitably damaged, part of the oxide film on the surface is brought in, the exposed fresh surface is immediately oxidized, and the oxide film stirred in finally forms oxide inclusions in the composite material, so that the performance of the composite material is deteriorated. According to the invention, ceramic particles are added from the bottom, and because the gas quantity among the particles is limited, a large amount of oxidation of the aluminum liquid can be avoided, and meanwhile, the hydrostatic pressure of the aluminum liquid is also beneficial to the aluminum liquid to infiltrate into the gaps among the ceramic particles. The treated ceramic particles can be pressed into blocks, aluminum alloy liquid is pressed in by a smelting bell jar, and aluminum liquid infiltrates gaps among SiC particles under the action of gravity and an infiltration assisting agent, so that the operation is convenient, and the particle pressing blocks are isolated from the outside after the aluminum liquid is pressed in, and the aluminum liquid can be prevented from being oxidized in a large amount. And then preserving heat for 1-30 minutes, putting the stirrer into the aluminum liquid, starting a motor to stir for 15-30 minutes, and preventing the aluminum liquid from rolling and generating vortex during stirring to cause the oxidation of the aluminum liquid because the preparation is carried out in the atmospheric environment. And after stirring is finished, taking out the crucible,and pouring molten aluminum into the casting mold to obtain a SiC particle reinforced aluminum matrix composite casting blank or casting with uniformly distributed particles and compact structure, wherein the volume white fraction of SiC particles is 5-20%.
In addition, the treated particles can be placed at the bottom of a crucible which is heated, an aluminum block is placed on the crucible, the temperature is kept for a period of time after the aluminum block is melted, aluminum liquid is infiltrated into gaps among SiC particles under the action of gravity and an infiltration assisting agent, the temperature is kept for 1-30 minutes, then a stirrer is placed into the aluminum liquid, and the stirring is carried out stably for 15-30 minutes.
Embodiments of the present invention are described below.
Example 1 a 10 volume% SiC particle reinforced ZL109 alloy composite was prepared by the bottom-mount method, the main chemical composition of the ZL109 alloy being (in weight%): si 11.0-13.0, Cu 0.5-1.5, Mg 0.8-1.5, and the balance of Al.
In a water bath at 90 ℃, according to 20 g of K2ZrF6+180 ml of water, 10% K2ZrF6Adding 100 g of 150-mesh SiC particles into the aqueous solution, soaking for 15 min, filtering out SiC, spreading on a watch glass, placing into an infrared drier, opening the drier every 15 min, turning over the particles to prevent K2ZrF6Uneven distribution, after drying, the agglomerated SiC particles are ground by a mortar and put into a 200 ℃ oven for later use.
Raising the temperature of a flat-bottom corundum crucible to 750 ℃ in a resistance furnace, placing the treated particles at the bottom of the crucible, leveling, pouring 900 g of ZL109 alloy liquid at 750 ℃, keeping the temperature for 20 minutes, stirring by using a disc type stirrer, wherein a stirring blade of the disc type stirrer is a disc vertically arranged with a stirring shaft, the rotating speed is 800 revolutions per minute, gradually descending the stirring blade in the stirring process, returning to the middle part of aluminum liquid after reaching the bottom of the crucible, stopping stirring after 15 minutes, taking out the crucible, pouring the composite material into a cylindrical cast iron cavity preheated at 200 ℃ for solidification and cooling, and observing the metallographic structure of the composite material shows that the particles are uniformly distributed and the structure is compact.
Example 2 preparation of 10 vol% SiC particle reinforced ZL109 alloy composite by pressing
100 g of 150 mesh SiC particles are mixed with 50 g of K2ZrF6Powder (SiC particles with K)2ZrF6The mass ratio of the powders is 2: 1), grinding and mixing the powders in a mortar, pressing the mixture into a round cake shape in a mould, placing the round cake into a 250 ℃ oven for baking, melting ZL109 alloy, pressing the round cake into aluminum alloy liquid, and keeping the temperature for 1 minute, wherein the other steps are the same as those of the embodiment 1.
Compared with the prior art, the method has the advantages that the fluoric acid salt is used as the leaching aid, so that the wettability of the aluminum liquid on the surfaces of the ceramic particles can be improved, the ceramic particles can be added from the lower part of the aluminum liquid during operation, the required composite material can be prepared in an atmospheric environment by performing stable stirring, special equipment is not needed, vacuum or inert gas protection is not needed, the process is simple, and the manufacturing cost is low.
Claims (6)
1. A preparation method of ceramic particle reinforced aluminum matrix composite is to put ceramic particles into molten aluminum for stirring, and is characterized in that: after ceramic particles are treated by fluoride salt leaching aid, the ceramic particles are placed at the bottom of aluminum liquid, the temperature is kept for a period of time, and then the aluminum liquid is poured into a casting mould after being stirred stably for a period of time.
2. The method for producing a ceramic particle-reinforced aluminum-based composite material according to claim 1, characterized in that: placing the ceramic particles treated with the fluoride salt leaching aid at the bottom of a crucible heated to an aluminum alloy melting temperature, pouring molten and refined degassed aluminum liquid from above, or placing an aluminum block of a required weight and holding for a period of time.
3. The method for producing a ceramic particle-reinforced aluminum-based composite material according to claim 1, characterized in that: the leaching aid fluoride salt is K2ZrF6、K2TiF6、Na3AlF6、NaF、CaF2。
4. The method for producing a ceramic particle-reinforced aluminum-based composite material as claimed in claim 1, wherein: the method for treating the ceramic particles by using the fluoride salt leaching aid comprises the following steps: with fluoride salts such as K in the desired concentration2ZrF6、K2TiF6And (3) drying after soaking in the aqueous solution, or drying after mixing the ceramic particles with the fluosilicate.
5. The method for producing a ceramic particle-reinforced aluminum-based composite material according to claim 4, characterized in that: said using K2ZrF6、K2TiF6The method for soaking the ceramic particles by the aqueous solution comprises the following steps: soaking the substrate in a solution with the concentration of 5-15% for 5-15 minutes at the temperature of 80-95 ℃.
6. The method for producing a ceramic particle-reinforced aluminum-based composite material according to claim 4, characterized in that: the proportion of the leaching aid fluoride salt powder to the ceramic particles is 1: 5-1: 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN97121945A CN1059710C (en) | 1997-11-27 | 1997-11-27 | Preparation of ceramic grain reinforced aluminium-based composite material |
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| CN97121945A CN1059710C (en) | 1997-11-27 | 1997-11-27 | Preparation of ceramic grain reinforced aluminium-based composite material |
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| CN1182063A true CN1182063A (en) | 1998-05-20 |
| CN1059710C CN1059710C (en) | 2000-12-20 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060979C (en) * | 1998-09-02 | 2001-01-24 | 华中理工大学 | Pressureless penetration casting method for aluminium-base composite material |
| CN103484707A (en) * | 2013-09-23 | 2014-01-01 | 同济大学 | Preparation method for SiC particle reinforced aluminum-based composite material |
| CN106583654A (en) * | 2016-11-30 | 2017-04-26 | 北京天宜上佳新材料股份有限公司 | Aluminum alloy brake disc molten metal and technology for casting brake disc through aluminum alloy brake disc molten metal |
| CN109576520A (en) * | 2018-11-30 | 2019-04-05 | 安徽工业大学 | A method of Alsimin containing nano particle is prepared using nanometer molten salt |
| CN110066937A (en) * | 2019-05-30 | 2019-07-30 | 西安创正新材料有限公司 | A kind of high intensity, the preparation method of high-modulus, high-ductility ceramic particle aluminum matrix composite |
| CN110629106A (en) * | 2019-11-08 | 2019-12-31 | 沈阳工业大学 | Method for reinforcing nodular cast iron material by using nano SiO2 particles |
| CN111172434A (en) * | 2020-01-16 | 2020-05-19 | 西北工业大学 | Method for reducing content of aluminum oxide in aluminum-based composite material by coating potassium fluozirconate on surface of silicon-plated graphite |
| CN111302834A (en) * | 2020-04-15 | 2020-06-19 | 湖南省美程陶瓷科技有限公司 | Microwave magnetron insulating ceramic ring |
| CN111499417A (en) * | 2020-04-24 | 2020-08-07 | 湖南省美程陶瓷科技有限公司 | Insulating ring for microwave magnetron and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2259309A (en) * | 1991-09-09 | 1993-03-10 | London Scandinavian Metall | Ceramic particles |
| CN1145412A (en) * | 1995-09-15 | 1997-03-19 | 卞津良 | A, Sr, Ti, B medium alloy and its prodn. method |
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1997
- 1997-11-27 CN CN97121945A patent/CN1059710C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1060979C (en) * | 1998-09-02 | 2001-01-24 | 华中理工大学 | Pressureless penetration casting method for aluminium-base composite material |
| CN103484707A (en) * | 2013-09-23 | 2014-01-01 | 同济大学 | Preparation method for SiC particle reinforced aluminum-based composite material |
| CN106583654A (en) * | 2016-11-30 | 2017-04-26 | 北京天宜上佳新材料股份有限公司 | Aluminum alloy brake disc molten metal and technology for casting brake disc through aluminum alloy brake disc molten metal |
| CN109576520A (en) * | 2018-11-30 | 2019-04-05 | 安徽工业大学 | A method of Alsimin containing nano particle is prepared using nanometer molten salt |
| CN110066937A (en) * | 2019-05-30 | 2019-07-30 | 西安创正新材料有限公司 | A kind of high intensity, the preparation method of high-modulus, high-ductility ceramic particle aluminum matrix composite |
| CN110629106A (en) * | 2019-11-08 | 2019-12-31 | 沈阳工业大学 | Method for reinforcing nodular cast iron material by using nano SiO2 particles |
| CN110629106B (en) * | 2019-11-08 | 2020-07-24 | 沈阳工业大学 | Method for reinforcing nodular cast iron material by using nano SiO2 particles |
| CN111172434A (en) * | 2020-01-16 | 2020-05-19 | 西北工业大学 | Method for reducing content of aluminum oxide in aluminum-based composite material by coating potassium fluozirconate on surface of silicon-plated graphite |
| CN111302834A (en) * | 2020-04-15 | 2020-06-19 | 湖南省美程陶瓷科技有限公司 | Microwave magnetron insulating ceramic ring |
| CN111302834B (en) * | 2020-04-15 | 2020-10-23 | 湖南省美程陶瓷科技有限公司 | Microwave magnetron insulating ceramic ring |
| CN111499417A (en) * | 2020-04-24 | 2020-08-07 | 湖南省美程陶瓷科技有限公司 | Insulating ring for microwave magnetron and preparation method thereof |
| CN111499417B (en) * | 2020-04-24 | 2020-12-08 | 湖南省美程陶瓷科技有限公司 | Insulating ring for microwave magnetron and preparation method thereof |
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| CN1059710C (en) | 2000-12-20 |
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Owner name: BAOSHAN IRON & STEEL CO., LTD. Free format text: FORMER NAME OR ADDRESS: SHANGHAI BAO STEEL GROUP IRON AND STEEL CO LTD Owner name: SHANGHAI BAO STEEL GROUP IRON AND STEEL CO LTD Free format text: FORMER NAME OR ADDRESS: BAOSHAN STEEL GROUP IRON AND STEEL CO LTD |
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