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CN101333583A - A kind of preparation method of fine-grained superplastic material with short process - Google Patents

A kind of preparation method of fine-grained superplastic material with short process Download PDF

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CN101333583A
CN101333583A CNA2007100118874A CN200710011887A CN101333583A CN 101333583 A CN101333583 A CN 101333583A CN A2007100118874 A CNA2007100118874 A CN A2007100118874A CN 200710011887 A CN200710011887 A CN 200710011887A CN 101333583 A CN101333583 A CN 101333583A
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马宗义
刘峰超
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Institute of Metal Research of CAS
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Abstract

Disclosed is a process for preparing short process fine crystalline superplasticity materials, which is characterized in that: cast alloy is used as a starting material for carrying out the agitation and friction processing after the homogenization heat treatment, and a bulky, loose and uneven cast structure is changed into an even and compact fine crystalline superplasticity structure.

Description

一种短流程细晶超塑性材料制备方法 A kind of preparation method of fine-grained superplastic material with short process

技术领域: Technical field:

本发明涉及金属材料,特别提供了一种短流程细晶超塑性材料制备方法,适用于加工铝合金、镁合金、锌合金、铜合金。The invention relates to metal materials, and in particular provides a preparation method of a short-flow fine-grained superplastic material, which is suitable for processing aluminum alloys, magnesium alloys, zinc alloys, and copper alloys.

背景技术: Background technique:

超塑性已逐步发展成为一种成熟的整体工业部件成型工艺,在汽车、航空等工业领域得到广泛应用。传统上,细晶超塑性铝合金的制备采用热机械加工手段,涉及过时效处理、多道次温轧、再结晶处理等工序,工序繁杂、制备成本高。Superplasticity has gradually developed into a mature overall industrial component forming process, which is widely used in automotive, aviation and other industrial fields. Traditionally, the preparation of fine-grain superplastic aluminum alloys adopts thermomechanical processing methods, involving overaging treatment, multi-pass warm rolling, recrystallization treatment and other processes, which are complicated and costly.

搅拌摩擦加工是在搅拌摩擦焊基本原理基础上发展起来的一种新的金属材料塑性加工技术。与其它塑性加工技术相比,搅拌摩擦加工工序简单,一步加工即可实现微观结构的细化,采用该技术已在几种商业铝合金中获得了细晶超塑性结构,取得良好的超塑性性能。Friction stir processing is a new plastic processing technology for metal materials developed on the basis of the basic principles of friction stir welding. Compared with other plastic processing techniques, the friction stir processing process is simple, and the microstructure can be refined in one step. Using this technology, fine-grained superplastic structures have been obtained in several commercial aluminum alloys, and good superplastic properties have been obtained. .

早期研究工作均是以轧制板或挤压板作为搅拌摩擦加工的起始材料(ActaMaterialia,vol.50,No.17(2002)p.4419-4430),工序繁杂,成本较高。为简化加工工序,研究者尝试直接使用铸态合金作为起始材料,通过搅拌摩擦加工把粗大的铸造组织直接转变成细晶超塑性结构,并取得了较好的超塑性性能(ScriptaMaterialia,vol.50,No.7(2004)p.931-935)。然而,需要指出的是,由于合金铸件存在明显的成分偏析和组织不均匀性,不仅合金的加工性能差,而且一步搅拌摩擦加工不易实现成分和组织的完全均匀化。In the early research work, the rolling plate or extruded plate was used as the starting material of friction stir processing (ActaMaterialia, vol.50, No.17(2002) p.4419-4430), and the process was complicated and the cost was high. In order to simplify the processing procedure, the researchers tried to directly use the cast alloy as the starting material, and directly transformed the coarse cast structure into a fine-grained superplastic structure through friction stir processing, and achieved good superplastic properties (ScriptaMaterialia, vol. 50, No.7 (2004) p.931-935). However, it should be pointed out that due to the obvious composition segregation and microstructure inhomogeneity in alloy castings, not only the processing performance of the alloy is poor, but also it is difficult to achieve complete homogenization of composition and microstructure in one-step friction stir processing.

发明内容:Invention content:

本发明的目的在于提供一种短流程细晶超塑性材料制备方法,适用于加工铝合金、镁合金、锌合金、铜合金。The purpose of the present invention is to provide a short-flow process fine-grained superplastic material preparation method, which is suitable for processing aluminum alloys, magnesium alloys, zinc alloys, and copper alloys.

本发明提供了一种短流程细晶超塑性材料制备方法,其特征在于:使用铸态合金作为起始材料,经均匀化热处理后,再进行搅拌摩擦加工,把粗大、疏松、不均匀的铸造组织转变成均匀、致密的细晶超塑性结构。The invention provides a method for preparing a short-flow fine-grained superplastic material, which is characterized in that: the as-cast alloy is used as the starting material, and after homogenization heat treatment, friction stir processing is carried out, and the coarse, loose and uneven casting The organization transforms into a uniform, dense fine-grained superplastic structure.

本发明短流程细晶超塑性材料制备方法中,合金铸造成型后,在(0.7-0.85)Tm的温度下均匀化热处理10-24小时后再进行搅拌摩擦加工,加工工具转速400-1500转/分钟、行进速度50-400毫米/分钟。In the method for preparing the short-flow fine-grained superplastic material of the present invention, after the alloy is cast and formed, the friction stir processing is performed after homogenizing heat treatment at a temperature of (0.7-0.85) T m for 10-24 hours, and the processing tool speed is 400-1500 rpm /min, travel speed 50-400mm/min.

本发明提出了一个新的短流程细晶超塑性材料制备方法,使用铸态合金作为起始材料,首先进行均匀化热处理以改善铸件成分偏析和组织不均匀性,然后再进行搅拌摩擦加工,把粗大的铸造组织转变成细晶超塑性结构,建立铸造+均匀化热处理+搅拌摩擦加工新方法。与轧制(挤压)+搅拌摩擦加工方法相比,本发明工艺明显缩短细晶超塑性材料的制备工艺流程、降低制造成本;与铸造+搅拌摩擦加工方法相比,本发明方法可制备出更均匀的细晶超塑性材料,明显提高材料的超塑性性能。因此,有理由相信这种新的细晶超塑性材料制备工艺在高强度合金超塑成型方面将有着广阔的工业应用前景。The present invention proposes a new short-flow fine-grained superplastic material preparation method, using as-cast alloy as the starting material, firstly performing homogenization heat treatment to improve the composition segregation and structure inhomogeneity of the casting, and then performing friction stir processing. The coarse casting structure is transformed into a fine-grained superplastic structure, and a new method of casting + homogenization heat treatment + friction stir processing is established. Compared with the rolling (extrusion)+friction stir processing method, the process of the present invention significantly shortens the preparation process of fine-grained superplastic materials and reduces manufacturing costs; compared with the casting+friction stir processing method, the inventive method can prepare A more uniform fine-grained superplastic material significantly improves the superplastic properties of the material. Therefore, there is reason to believe that this new fine-grained superplastic material preparation process will have broad industrial application prospects in the superplastic forming of high-strength alloys.

具体实施方式: Detailed ways:

实施例1Example 1

使用8毫米厚的7075铝合金铸态板材,在460℃进行24小时均匀化退火处理后再进行搅拌摩擦加工,在工具转速1200转/分钟、行进速度100毫米/分钟的加工参数下,获得晶粒尺寸3微米的均匀细晶结构。超塑性拉伸试验显示,在350-470℃的温度区间内均获得良好的超塑性性能,在470℃没有异常晶粒长大,仍可得到700%的超塑性。最大超塑性为1050%,在450℃和1×10-2s-1的高应变速率下取得。Using an 8 mm thick 7075 aluminum alloy as-cast plate, after homogenization annealing at 460 ° C for 24 hours, then friction stir processing, under the processing parameters of tool speed 1200 rpm and travel speed 100 mm / min, the obtained grain Uniform fine-grained structure with a grain size of 3 microns. The superplastic tensile test shows that good superplastic properties are obtained in the temperature range of 350-470°C, and there is no abnormal grain growth at 470°C, and 700% superplasticity can still be obtained. The maximum superplasticity is 1050%, achieved at 450°C and a high strain rate of 1× 10-2 s -1 .

比较例1Comparative example 1

使用8毫米厚的7075铝合金铸态板材直接进行搅拌摩擦加工,在工具转速1200转/分钟、行进速度100毫米/分钟的参数下获得平均晶粒尺寸3-5微米的细晶结构,但晶粒尺寸和第二相粒子分布不是非常均匀。超塑性拉伸试验表明,加工后的7075铝合金在400-450℃的温度范围内均获得超塑性,高于450℃由于组织不均匀造成异常晶粒长大,超塑性消失。最大超塑性为600%,在450℃和1×10-2s-1的高应变速率下取得。Using 8 mm thick 7075 aluminum alloy as-cast plate for direct friction stir processing, under the parameters of tool speed 1200 rpm and travel speed 100 mm/min, a fine-grained structure with an average grain size of 3-5 microns was obtained, but the The particle size and second phase particle distribution are not very uniform. The superplastic tensile test shows that the processed 7075 aluminum alloy obtains superplasticity in the temperature range of 400-450°C, and the superplasticity disappears due to abnormal grain growth due to uneven structure above 450°C. The maximum superplasticity is 600%, achieved at 450°C and a high strain rate of 1× 10-2 s -1 .

实施例2Example 2

使用6毫米厚的2024铝合金铸态板材,在490℃进行12小时均匀化退火处理后再进行搅拌摩擦加工,在工具转速500转/分钟、行进速度100毫米/分钟的参数下获得晶粒尺寸4.5微米的均匀细晶结构。取得的最大超塑性为450%,在430℃和3×10-3s-1的应变速率下取得。Using a 6 mm thick 2024 aluminum alloy as-cast plate, perform homogenization annealing at 490°C for 12 hours and then perform friction stir processing. The grain size is obtained under the parameters of tool speed 500 rpm and travel speed 100 mm/min Uniform fine-grained structure of 4.5 microns. The maximum superplasticity achieved is 450%, achieved at 430 °C and a strain rate of 3 × 10-3 s -1 .

比较例2Comparative example 2

使用6毫米厚的2024铝合金铸态板材,在工具转速500转/分钟、行进速度100毫米/分钟的参数下进行搅拌摩擦加工,加工后晶粒尺寸和第二相粒子分布不是非常均匀,平均晶粒尺寸大约为5-7微米。取得的最大超塑性为300%,在430℃和3×10-3s-1的应变速率下取得。Using a 6mm thick 2024 aluminum alloy as-cast plate, friction stir processing was carried out under the parameters of the tool speed of 500 rpm and the travel speed of 100 mm/min. After processing, the grain size and the distribution of the second phase particles were not very uniform. The grain size is approximately 5-7 microns. The maximum superplasticity achieved is 300%, achieved at 430 °C and a strain rate of 3 × 10-3 s -1 .

实施例3Example 3

使用6毫米厚的Mg-Zn-Y-Zr铸态板材,在420℃进行10小时均匀化退火处理后再进行搅拌摩擦加工,在工具转速600转/分钟、行进速度100毫米/分钟的参数下获得晶粒尺寸5微米的均匀细晶结构。取得的最大超塑性为550%,在450℃和3×10-3s-1的应变速率下取得。Use a 6 mm thick Mg-Zn-Y-Zr as-cast plate, perform homogenization annealing at 420°C for 10 hours, and then perform friction stir processing, under the parameters of tool speed 600 rpm and travel speed 100 mm/min A uniform fine-grained structure with a grain size of 5 microns was obtained. The maximum superplasticity achieved is 550%, achieved at 450 °C and a strain rate of 3 × 10-3 s -1 .

比较例3Comparative example 3

使用6毫米厚的Mg-Zn-Y-Zr铸态板材,在工具转速600转/分钟、行进速度100毫米/分钟的参数下进行搅拌摩擦加工,加工后晶粒尺寸和第二相粒子分布不是非常均匀,平均晶粒尺寸大约为5-7微米。取得的最大超塑性为400%,在450℃和3×10-3s-1的应变速率下取得。Using a 6 mm thick Mg-Zn-Y-Zr as-cast plate, friction stir processing was performed under the parameters of tool speed 600 rpm and travel speed 100 mm/min, the grain size and second phase particle distribution after processing were not Very uniform, with an average grain size of approximately 5-7 microns. The maximum superplasticity achieved is 400%, achieved at 450 °C and a strain rate of 3 × 10-3 s -1 .

实施例4Example 4

使用5毫米厚的Zn-22Al铸态板材,在200℃进行8小时均匀化退火处理后再进行搅拌摩擦加工,在工具转速500转/分钟、行进速度100毫米/分钟的参数下获得晶粒尺寸3微米的均匀细晶结构。在160℃和1×10-3s-1的应变速率下取得350%的超塑性。Using a 5 mm thick Zn-22Al as-cast plate, conduct a homogenization annealing treatment at 200°C for 8 hours and then perform friction stir processing. The grain size is obtained under the parameters of tool speed 500 rpm and travel speed 100 mm/min Uniform fine-grained structure of 3 microns. A superplasticity of 350% was achieved at 160 °C and a strain rate of 1×10 -3 s -1 .

比较例4Comparative example 4

使用5毫米厚的Zn-22Al铸态板材,在工具转速500转/分钟、行进速度100毫米/分钟的参数下进行搅拌摩擦加工,加工后晶粒尺寸分布不是非常均匀,平均晶粒尺寸大约为3-5微米。在160℃和1×10-3s-1的应变速率下取得240%的超塑性。Using a 5 mm thick Zn-22Al as-cast plate, friction stir processing was performed under the parameters of tool speed 500 rpm and travel speed 100 mm/min. After processing, the grain size distribution was not very uniform, and the average grain size was about 3-5 microns. A superplasticity of 240% was achieved at 160 °C and a strain rate of 1×10 -3 s -1 .

Claims (3)

1、一种短流程细晶超塑性材料制备方法,其特征在于过程如下:合金铸造成型后进行均匀化热处理,以改善成分偏析和组织不均匀性,均匀化热处理温度为(0.7-0.85)Tm,其中Tm是材料以开尔文表示的熔点温度,时间是10-24小时;然后进行搅拌摩擦加工。1. A method for preparing a short-flow fine-grained superplastic material, characterized in that the process is as follows: after the alloy is cast and formed, homogenization heat treatment is carried out to improve component segregation and structural inhomogeneity, and the homogenization heat treatment temperature is (0.7-0.85) T m , where T m is the melting temperature of the material in Kelvin, for 10-24 hours; then friction stir processing. 2、按照权利要求1所述短流程细晶超塑性材料制备方法,其特征在于搅拌摩擦加工工艺参数为,加工工具转速400-1500转/分钟、行进速度50-400毫米/分钟。2. According to claim 1, the preparation method of the short-flow fine-grained superplastic material is characterized in that the friction stir processing parameters are as follows: the speed of the processing tool is 400-1500 rpm, and the travel speed is 50-400 mm/min. 3、按照权利要求1所述短流程细晶超塑性材料制备方法,其特征在于所述合金包括铝合金、镁合金、锌合金、铜合金。3. The short-process fine-grained superplastic material preparation method according to claim 1, characterized in that said alloys include aluminum alloys, magnesium alloys, zinc alloys, and copper alloys.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102560040A (en) * 2010-12-24 2012-07-11 中国科学院金属研究所 Short-flow plastic processing method for prolonging service life of gear/rack
CN102672276A (en) * 2011-03-17 2012-09-19 中国科学院金属研究所 Short-process plastic processing method for prolonging service life of saw blade
CN104985393A (en) * 2015-06-10 2015-10-21 东北大学 Manufacturing method capable of improving mechanical performance of thick 7050-T7451 aluminum alloy plate
CN109773327A (en) * 2019-02-02 2019-05-21 中铝材料应用研究院有限公司 A method of improving high-strength aluminium room temperature forming
CN109940259A (en) * 2019-02-02 2019-06-28 中铝材料应用研究院有限公司 A method of improving aluminum alloy plate materials bending and forming
CN115927980A (en) * 2022-12-16 2023-04-07 中国科学院金属研究所 A method to improve the superplasticity of high-entropy alloys
CN116083822A (en) * 2022-10-28 2023-05-09 西安诺博尔稀贵金属材料股份有限公司 A kind of preparation method of niobium alloy material with fine grain/ultrafine grain structure

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CN1968783A (en) * 2004-03-24 2007-05-23 Sii米加钻石公司 Solid state processing of materials through friction stir processing and friction stir mixing

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102560040A (en) * 2010-12-24 2012-07-11 中国科学院金属研究所 Short-flow plastic processing method for prolonging service life of gear/rack
CN102560040B (en) * 2010-12-24 2014-03-26 中国科学院金属研究所 Short-flow plastic processing method for prolonging service life of gear/rack
CN102672276A (en) * 2011-03-17 2012-09-19 中国科学院金属研究所 Short-process plastic processing method for prolonging service life of saw blade
CN102672276B (en) * 2011-03-17 2014-10-22 中国科学院金属研究所 Short-process plastic processing method for prolonging service life of saw blade
CN104985393A (en) * 2015-06-10 2015-10-21 东北大学 Manufacturing method capable of improving mechanical performance of thick 7050-T7451 aluminum alloy plate
CN109773327A (en) * 2019-02-02 2019-05-21 中铝材料应用研究院有限公司 A method of improving high-strength aluminium room temperature forming
CN109940259A (en) * 2019-02-02 2019-06-28 中铝材料应用研究院有限公司 A method of improving aluminum alloy plate materials bending and forming
CN116083822A (en) * 2022-10-28 2023-05-09 西安诺博尔稀贵金属材料股份有限公司 A kind of preparation method of niobium alloy material with fine grain/ultrafine grain structure
CN116083822B (en) * 2022-10-28 2024-12-10 西安诺博尔稀贵金属材料股份有限公司 A method for preparing fine-grained/ultra-fine-grained niobium alloy material
CN115927980A (en) * 2022-12-16 2023-04-07 中国科学院金属研究所 A method to improve the superplasticity of high-entropy alloys

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