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CN1958816A - Technique for preparing composite material of aluminum based surface enhanced by inner generated grains through powered supresonic method - Google Patents

Technique for preparing composite material of aluminum based surface enhanced by inner generated grains through powered supresonic method Download PDF

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CN1958816A
CN1958816A CN 200610131677 CN200610131677A CN1958816A CN 1958816 A CN1958816 A CN 1958816A CN 200610131677 CN200610131677 CN 200610131677 CN 200610131677 A CN200610131677 A CN 200610131677A CN 1958816 A CN1958816 A CN 1958816A
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aluminum
melt
based surface
particle
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于思荣
冯海阔
刘耀辉
李英龙
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Jilin University
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Abstract

本发明涉及的是一种表面复合材料制备工艺,特别是涉及一种功率超声法制备内生颗粒增强铝基表面复合材料工艺。该工艺利用功率超声制备内生颗粒增强(TiAl3相)铝基表面复合材料,首先根据变幅坩埚体积及所要得到表面层厚度的大小,在一定加入量的K2TiF6盐和纯铝的重量比例下,熔融后发生反应得到含有TiAl3颗粒的熔体,将装有熔体的变幅坩埚置于超声处理装置中,在改变实验参数的工艺条件下,在功率超声的作用下,TiAl3颗粒向表面移动,获得不同表面层厚度的颗粒增强铝基表面复合材料。本发明解决了具有工艺稳定,操作简便,增强相在基体的表层分布均匀,界面结合好等问题。

Figure 200610131677

The invention relates to a preparation process of a surface composite material, in particular to a process for preparing an internal particle-reinforced aluminum-based surface composite material by a power ultrasonic method. This process utilizes power ultrasound to prepare endogenous particle-reinforced (TiAl 3 phase) aluminum-based surface composite materials. First, according to the volume of the luffing crucible and the thickness of the surface layer to be obtained, a certain amount of K 2 TiF 6 salt and pure aluminum are added. Under the weight ratio, a melt containing TiAl 3 particles is obtained by reaction after melting, and the luffing crucible containing the melt is placed in an ultrasonic treatment device. Under the process conditions of changing the experimental parameters, under the action of power ultrasound, TiAl 3 Particles move toward the surface to obtain particle-reinforced aluminum-based surface composites with different surface layer thicknesses. The invention solves the problems of stable process, simple operation, uniform distribution of the reinforcing phase on the surface of the matrix, good interface bonding and the like.

Figure 200610131677

Description

Process for preparing endogenetic particle reinforced aluminum-based surface composite material by power ultrasonic method
Technical Field
The invention relates to a preparation process of a surface composite material, in particular to a process for preparing an endogenous particle reinforced aluminum-based surface composite material by a power ultrasonic method.
Background
Ultrasonic waves have many applications in the field of metallurgy and metal materials, such as ultrasonic flaw detection, solidification structure refinement, removal of gas and solid inclusions in molten metal, reduction of macro and micro segregation and the like. In addition, ultrasonic waves can also be used for manufacturing metal matrix composites. Most of metal liquid does not wet the ceramic reinforcing phase, which is a difficult problem in the preparation process of the metal matrix composite material and often causes the problems of unstable preparation process, uneven tissue distribution, poor interface bonding strength and the like of the composite material. Under the action of ultrasonic wave, the wetting performance between the ceramic reinforcing phase and the molten metal is improved, and the reinforcing phase can be easily dispersed into the molten metal, so that the metal matrix composite with uniformly distributed tissues is prepared.
The metal-based surface composite material is prepared by compounding ceramic particles or fibers with high hardness, high melting point, high elastic modulus, wear resistance and corrosion resistance in a surface layer of a metal material by a certain process to form a reinforcing layer on the surface of the metal material. The preparation method mainly comprises the following steps: powder metallurgy, squeeze casting, cast infiltration, negative pressure casting, centrifugal casting, and the like. The powder metallurgy method has the characteristics of stable process and good performance, and has the disadvantages of high cost and limited shape and size of materials. The extrusion casting method has the outstanding advantages of stable process, high production efficiency, compact structure and excellent performance, and has the disadvantages that the reinforcing phase is easy to damage when the process parameter is not properly controlled, the specification and the shape of the produced member are also limited, and the method is only suitable for metal matrixes with low melting points. The cast-infiltration method adopts the adhesive and the flux, so the outstanding defects are that the surface composite layer is easy to generate air holes and inclusions (slag), and the process stability is poor, thereby limiting the development and the application of the cast-infiltration method to a certain extent. The negative pressure casting method features no use of adhesive and flux, less defects of air holes and slag inclusion, thicker composite layer, need of special equipment and moulding technique, complex process and low productivity. The centrifugal casting method is characterized by simple equipment, but the shape of the casting is limited to a revolving body. In addition, electromagnetic stirring methods, in-situ reaction generation methods, and the like can also be used for preparing the surface composite material.
Another field of application of ultrasound is the ultrasonic separation of solid and liquid phases. Theprinciple of ultrasonic separation is that standing waves are generated when ultrasonic sound waves are transmitted in liquid, and due to the fact that particles have different acoustic characteristics and the action of sound radiation force, sound pressure nodes and sound abdominal nodes in an ultrasonic standing wave field can be gathered, so that solid particles and the liquid are separated. The separation and purification technology is widely applied to the fields of chemical industry, food, metallurgy and medical treatment, and aims to remove solid particles suspended in liquid. But at present, the ultrasonic treatment technology is not applied to the preparation of the particle reinforced surface composite material.
Disclosure of Invention
The invention aims to provide a process for preparing an endogenous particle reinforced aluminum-based surface composite material by using a power ultrasonic method, wherein the ultrasonic wave has different acoustic effects on a melt and particles in the melt, so that the particles are deviated to one side of the melt and are solidified.
The above object of the present invention is achieved as follows with reference to the accompanying drawings:
the invention uses power ultrasonic to prepare endogenetic particle reinforced (TiAl) with the vibration head of the amplitude-variable crucible upward3Phase) aluminum-based surface composite material, firstly adding K with a certain amount according to the volume of the amplitude-variable crucible and the thickness of the surface layer to be obtained2TiF6The TiAl-containing material is obtained by the reaction after melting under the weight ratio of the salt to the pure aluminum3Placing the amplitude-variable crucible filled with the melt in an ultrasonic treatment device, and under the action of power ultrasound, TiAl under the process condition of changing experimental parameters3The particles move to the surface to obtain the particle reinforced aluminum-based surface composite material with different surface layer thicknesses.
The specific technical scheme is as follows:
a process for preparing an endogenetic particle reinforced aluminum-based surface composite material by a power ultrasonic method comprises the following steps:
firstly, according to the thickness of the particle reinforced layer on the surface of the aluminum base, the endogenetic particle reinforced TiAl to be added is determined3Content of phase according to same mol of TiAl3Requiring the same molar amount of K2TiF6The adding amount of the salt is determined according to the using amount of the salt, and a proper amount of pure aluminum cast ingots are selected according to the size of a crucible for smelting pure aluminum;
secondly, putting the pure aluminum cast ingot into a heating furnace for heating and melting, and then preserving heat to balance the melt;
thirdly, weighing the dried K2TiF6Adding salt into the balanced aluminum melt, stirring at a constant speed, fully reacting, and then carrying out early melt purification and slag removal treatment on the melt after reaction;
the fourth step, the TiAl-containing material obtained by the reaction3Uniformly stirring the melt, injecting a small amount of the melt into a variable amplitude crucible which is kept at 650-700 ℃, carrying out ultrasonic treatment with the ultrasonic power of 45-60W and the treatment time of 5-10 min, then moving out of a heat preservation system, stopping ultrasonic treatment, carrying out rapid water cooling to obtain particle reinforcement (TiAl)3Phase) aluminum-based surface composites.
The amount of said salt used in the first step is according to the formula: and (4) determining.
The selection of the appropriate amount of pure aluminum ingot in the first step is close to the end of the crucible in consideration of the shrinkage of the melt solidification.
The heating furnace in the second step adopts a digital resistance heating furnace with the set temperature of 680-780 ℃, and the temperature is kept for 20-30 min after melting.
Dried K as described in the third step2TiF6And adding the salt into the balanced aluminum melt for 2-3 times within 20-30 min.
The method for preparing the surface composite material has stable process and simple and convenient operation, and the reinforced phase is very uniformly distributed on the surface layer of the matrix because of the particlesReinforced TiAl3The phase is generated by endogenous reaction and is well combined with the interface of the matrix. The thickness of the particle reinforced aluminum-based surface composite layer can be obtained under the action of corresponding power ultrasonic treatment parameters according to the reaction amount of the added salt and the pure aluminum which react with each other. The method leads the endogenous particles in the melt to be partially gathered at one side of the melt, and after solidification, the endogenous particle reinforced aluminum-based surface composite material is prepared.
Compared with the traditional method for preparing the particle reinforced aluminum matrix surface composite material, such as a powder metallurgy method, an extrusion casting method, a cast-infiltration method, a negative pressure casting method,a centrifugal casting method and the like, the method has the advantages of lower cost, simple and complex operation, good process stability, good bonding property of an endogenous reinforcing phase and an aluminum matrix interface and the like.
Drawings
FIG. 1(a) is a graph of particle-reinforced (TiAl) produced3Phase) metallograph of the surface composite material layer connected with the matrix can show that the endogenous reinforced particles are distributed in the surface layer of the matrix very uniformly under the action of ultrasound, the interface between the surface layer and the matrix is smooth,the bonding was good.
FIG. 1(b) is the particle reinforcement (TiAl) of FIG. 2(a)3Phase) surface composite material layer, and the endogenous reinforced particles are uniformly distributed.
FIG. 2(a) is particle enhancement (TiAl) under optical microscope3Phase) metallography of the reinforcing phase in the surface composite layer, TiAl3The phases are all around 20 μm in size.
FIG. 2(b) is the particle reinforcement (TiAl) of FIG. 2(a)3Phase) electron micrograph in the surface composite layer.
Detailed Description
1. If a particle enhancement layer with a surface layer of 5-6 mm is to be obtained, TiAl is enhanced according to endogenous particles to be added3The phase contents were tested under the corresponding process parameters.
2. K used2TiF6The salt is commercialCommercial aluminum was used as the salt, pure aluminum.
3. Selecting a proper amount of pure aluminum ingots of 320-350 g according to the size of a crucible for smelting pure aluminum,
4. obtaining TiAl of 8-10%3Endogenous reinforcing phase, so 32-35 g of TiAl needs to be obtained3And (4) phase(s).
5. According to the formula: same mole of TiAl3Requiring the same molar amount of K2TiF6Salt, thus about 55-65 g of K is required2TiF6And (3) salt.
6. Putting the pure aluminum cast ingot into a digital resistance heating furnace with the set temperature of 680-780 ℃ for heating, and preserving heat for 20-30 min after melting so as to balance the melt.
7. Weighing dried K2TiF6And adding the salt into the balanced aluminum melt for 2-3 times within 20-30 min, and stirring at a constant speed to fully react.
8. Deslagging the reacted melt, and purifying the melt in advance.
9. The TiAl-containing material obtained by the reaction3After the melt is uniformly stirred, a small amount of the melt is injected into a variable amplitude crucible which is kept at the temperature of 650-700 ℃.
10. The melt poured into the crucible, close to the end of the crucible, has a volume of about 6.37X 10, taking into account the shrinkage of the solidification of the melt-5(m3)。
11. The ultrasonic power is 45-60W, and the ultrasonic treatment time is 5-10 min.
12. Then moving out of the heat preservation system, stopping ultrasonic treatment, and carrying out rapid water cooling to obtain particle reinforced (TiAl)3Phase) aluminum-based surface composites.
13. The volume of the prepared cast ingot sample is about 3.5-4.5 multiplied by 10-5(m3) And the obtained endogenous surface composite layer is 4-6 mm.

Claims (5)

1、一种功率超声法制备内生颗粒增强铝基表面复合材料工艺,其特征在于按以下步骤进行:1. A process for preparing endogenous particle-reinforced aluminum-based surface composites by a power ultrasonic method, characterized in that it proceeds in the following steps: 第一步,根据需要制备铝基表面颗粒增强层的厚度,确定所要加入的内生颗粒增强TiAl3相的含量,按相同摩尔的TiAl3相需要相同摩尔的K2TiF6盐的用量确定盐的加入量,按所要熔炼纯铝的坩埚的大小选择适量的纯铝铸锭;The first step is to prepare the thickness of the aluminum-based surface particle-reinforced layer according to the needs, determine the content of the internal particle-reinforced TiAl 3 phase to be added, and determine the amount of K 2 TiF 6 salt according to the same mole of TiAl 3 phase. According to the size of the crucible to smelt pure aluminum, select an appropriate amount of pure aluminum ingot; 第二步,把纯铝铸锭放入加热炉中加热熔化后保温,使熔体达到平衡;The second step is to put the pure aluminum ingot into the heating furnace to heat and melt it and then keep it warm to make the melt reach equilibrium; 第三步,将已称量好的干燥的K2TiF6盐加入到已经平衡的铝熔体中,匀速搅拌,充分反应,然后对反应后的熔体进行先期熔体的净化,除渣处理;The third step is to add the weighed dry K 2 TiF 6 salt into the balanced aluminum melt, stir at a constant speed, and fully react, and then perform the preliminary melt purification and slag removal treatment on the reacted melt ; 第四步,把反应制得的含有TiAl3的熔体均匀搅拌之后,取少量注入已保温在650~700℃“变幅坩埚”内,进行超声处理,超声功率为45~60W,处理时间为5~10min,然后移出保温系统,停止超声处理,进行快速水冷,获得颗粒增强(TiAl3相)铝基表面复合材料。The fourth step is to uniformly stir the melt containing TiAl 3 prepared by the reaction, then take a small amount and pour it into the "amplitude crucible" that has been kept at 650-700°C, and perform ultrasonic treatment. The ultrasonic power is 45-60W, and the processing time is 5 to 10 minutes, then remove the insulation system, stop the ultrasonic treatment, and perform rapid water cooling to obtain particle-reinforced (TiAl 3 phase) aluminum-based surface composite materials. 2、根据权利要求1所述的功率超声法制备内生颗粒增强铝基表面复合材料工艺,其特征在于第一步中所说的盐的用量根据公式:2. The process for preparing endogenous particle-reinforced aluminum-based surface composites by power ultrasonic method according to claim 1, characterized in that the amount of salt in the first step is according to the formula: 确定。 Sure. 3、根据权利要求1所述的功率超声法制备内生颗粒增强铝基表面复合材料工艺,其特征在于第一步中所说的选择适量的纯铝铸锭应考虑到熔体凝固的收缩性,接近于坩埚的端口。3. The process for preparing endogenous particle-reinforced aluminum-based surface composites by power ultrasonic method according to claim 1, characterized in that in the first step, the selection of an appropriate amount of pure aluminum ingots should take into account the shrinkage of the solidification of the melt , close to the port of the crucible. 4、根据权利要求1所述的功率超声法制备内生颗粒增强铝基表面复合材料工艺,其特征在于第二步中所说的加热炉采用设定温度为680~780℃数字电阻加热炉,熔化后保温20~30min。4. The process for preparing endogenous particle-reinforced aluminum-based surface composites by power ultrasonic method according to claim 1, characterized in that the heating furnace in the second step adopts a digital resistance heating furnace with a set temperature of 680-780°C, Keep warm for 20-30 minutes after melting. 5、根据权利要求1所述的功率超声法制备内生颗粒增强铝基表面复合材料工艺,其特征在于第三步中所说的干燥的K2TiF6盐,可在20~30min内,分2~3次加入到已经平衡的铝熔体中。5. The process for preparing endogenous particle-reinforced aluminum-based surface composites by power ultrasonic method according to claim 1, characterized in that the dry K 2 TiF 6 salt mentioned in the third step can be divided within 20 to 30 minutes. Add 2 to 3 times to the already balanced aluminum melt.
CN 200610131677 2006-11-29 2006-11-29 Technique for preparing composite material of aluminum based surface enhanced by inner generated grains through powered supresonic method Pending CN1958816A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880783A (en) * 2010-06-03 2010-11-10 南昌大学 A kind of preparation method of TiAl3 reinforced aluminum matrix composite material
CN102121075A (en) * 2011-02-15 2011-07-13 江苏大学 Method for synthesizing particle reinforced aluminum-based composite under high-intensity ultrasonic field and pulsed electric field
CN102134667A (en) * 2011-02-28 2011-07-27 江苏中欧材料研究院有限公司 Preparation method of submicron particle-reinforced aluminum-based composite material
WO2012159590A1 (en) * 2012-05-23 2012-11-29 深圳市新星轻合金材料股份有限公司 Electrolyte supplement system in aluminum electrolytic process and manufacturing method therefor
CN110747361A (en) * 2019-11-20 2020-02-04 中南大学 Preparation method of titanium boride reinforced aluminum-based composite material based on ultrasonic and mechanical stirring

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101880783A (en) * 2010-06-03 2010-11-10 南昌大学 A kind of preparation method of TiAl3 reinforced aluminum matrix composite material
CN101880783B (en) * 2010-06-03 2012-02-08 南昌大学 Preparation method of TiAl3 enhanced aluminum-based composite material
CN102121075A (en) * 2011-02-15 2011-07-13 江苏大学 Method for synthesizing particle reinforced aluminum-based composite under high-intensity ultrasonic field and pulsed electric field
CN102121075B (en) * 2011-02-15 2013-03-13 江苏大学 Method for synthesizing particle reinforced aluminum-based composite under high-intensity ultrasonic field and pulsed electric field
CN102134667A (en) * 2011-02-28 2011-07-27 江苏中欧材料研究院有限公司 Preparation method of submicron particle-reinforced aluminum-based composite material
WO2012159590A1 (en) * 2012-05-23 2012-11-29 深圳市新星轻合金材料股份有限公司 Electrolyte supplement system in aluminum electrolytic process and manufacturing method therefor
GB2502392A (en) * 2012-05-23 2013-11-27 Shenzhen Sunxing Light Alloys Materials Co Ltd Electrolyte supplement system in aluminium electrolytic process and manufacturing method therefor
GB2502392B (en) * 2012-05-23 2017-11-15 Shenzhen Sunxing Light Alloys Mat Co Ltd Method for preparing an electrolyte supplement system in aluminium electrolysis
CN110747361A (en) * 2019-11-20 2020-02-04 中南大学 Preparation method of titanium boride reinforced aluminum-based composite material based on ultrasonic and mechanical stirring

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