CN1332058C - Prepn of rod superfine crystal material - Google Patents

Prepn of rod superfine crystal material Download PDF

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CN1332058C
CN1332058C CNB2004100790675A CN200410079067A CN1332058C CN 1332058 C CN1332058 C CN 1332058C CN B2004100790675 A CNB2004100790675 A CN B2004100790675A CN 200410079067 A CN200410079067 A CN 200410079067A CN 1332058 C CN1332058 C CN 1332058C
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rod
shaped metal
bar
deformation
induction coil
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CN1637162A (en
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杜随更
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Northwestern Polytechnical University
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Abstract

本发明公开了一种棒状超细晶材料的制备方法,其特征是:待细化组织的棒状金属材料(1)卡在固定夹具(10)与旋转夹具(3)之间,通过中频电源(6)与感应线圈(7)对棒状金属材料(1)进行局部加热;当温度达到设定值后,由伺服电机(4)带动旋转夹具(3)旋转,在扭转剪切应力作用下,变形区(9)处的金属晶粒破碎细化;使感应线圈(7)逐渐沿材料(1)轴向移动;同时,冷却圈(45)与感应线圈(7)同步移动,冷却变形区(9)后方的区域,保持已细化的细晶组织;当感应线圈(7)移动到棒状金属材料(1)的另一端时,即可得到一段超细晶组织棒材。本发明一次成形,变形程度高,所用设备吨位低,并可降低超细晶材料的成本。

Figure 200410079067

The invention discloses a method for preparing a rod-shaped ultrafine-grained material, which is characterized in that: the rod-shaped metal material (1) to be refined is stuck between a fixing fixture (10) and a rotating fixture (3), and is passed through an intermediate frequency power supply ( 6) and the induction coil (7) to locally heat the rod-shaped metal material (1); when the temperature reaches the set value, the servo motor (4) drives the rotating fixture (3) to rotate, and under the action of torsional shear stress, the deformation The metal grains at the zone (9) are broken and refined; the induction coil (7) is gradually moved along the axial direction of the material (1); at the same time, the cooling ring (45) moves synchronously with the induction coil (7), cooling the deformation zone (9 ) maintains the refined fine-grain structure; when the induction coil (7) moves to the other end of the rod-shaped metal material (1), a section of ultra-fine-grain structure rod can be obtained. The invention has one-time forming, high degree of deformation, low tonnage of equipment used, and can reduce the cost of ultra-fine crystal materials.

Figure 200410079067

Description

棒状超细晶材料的制备方法Preparation method of rod-shaped ultrafine-grained material

技术领域:Technical field:

本发明涉及一种棒状超细晶材料的制备方法。The invention relates to a preparation method of a rod-shaped ultrafine crystal material.

背景技术:Background technique:

制备超细晶材料的一般方法有:惰性气体凝聚法、气相沉淀法、机械法、机械合金化法、强烈塑性变形法等。强烈塑性变形法又分为两种,一种是高压扭转塑性变形法,另一种是S型等径侧向挤压法。The general methods for preparing ultrafine-grained materials include: inert gas condensation method, gas phase precipitation method, mechanical method, mechanical alloying method, strong plastic deformation method, etc. The strong plastic deformation method is divided into two types, one is the high-pressure torsional plastic deformation method, and the other is the S-type equal radial extrusion method.

参见图6,在1999年第四期《材料导报》中,沈辉的“剧烈塑性变形法制备纳米材料Ni和Ni/SiO2”一文中采用高压扭转塑性变形法,对厚度为0.2mm、直径为8mm的圆片状Ni试样进行高压扭转,制备出平均晶粒尺寸约为52nm的超细晶材料。V.R.Gertsman在《scripta metallurgica and mechanical》1994年第229页,“On the structure and strength ofultrafine-grained copper produced by severe plastic deformation”一文中记载了采用高压扭转塑性变形法,对厚度为200μm,直径为3mm的金属圆片状材料进行高压扭转,制备出平均晶粒直径为170nm的超细晶组织。该方法缺陷是,只能对小片材料进行处理,制备不出大面积或块状的超细晶组织材料,不能应用于工业生产。See Figure 6. In the fourth issue of "Materials Herald" in 1999, Shen Hui's article "Preparation of Nanomaterials Ni and Ni/SiO 2 by Severe Plastic Deformation" used high-pressure torsional plastic deformation method, for thickness 0.2mm, diameter An ultra-fine-grained material with an average grain size of about 52nm was prepared by high-pressure torsion for an 8mm disc-shaped Ni sample. VRGertsman recorded in "scripta metallurgica and mechanical" 1994, page 229, "On the structure and strength of ultrafine-grained copper produced by severe plastic deformation" the use of high-pressure torsional plastic deformation method, for the thickness of 200μm, the diameter of 3mm The metal disc material is twisted under high pressure to prepare an ultra-fine grain structure with an average grain diameter of 170nm. The defect of this method is that only small pieces of material can be processed, and no large-area or massive ultra-fine-grained structure material can be prepared, so it cannot be applied to industrial production.

参见图7,Z.Y.Liu在《Materials science and Engineering》1998年A242卷137~140页“The effect of cumulative large plastic strain on the structurc and properties of a Cu-Znalloy”一文中,记载了采用S型等径侧向挤压法,在高温条件下,对含锌38%的铜锌合金棒材进行多次挤压,最后生成平均晶粒直径为0.3~0.4μm的超细晶材料。该方法的缺陷是设备吨位高,变形程度低,需要多次反复进行。See Figure 7, Z.Y.Liu in "Materials science and Engineering" 1998 A242 volume 137-140 pages "The effect of cumulative large plastic strain on the structure and properties of a Cu-Znalloy", recorded the use of S-type equal diameter In the lateral extrusion method, the copper-zinc alloy bar containing 38% zinc is extruded several times under high temperature conditions, and finally an ultra-fine-grained material with an average grain diameter of 0.3-0.4 μm is produced. The disadvantage of this method is that the tonnage of the equipment is high, the degree of deformation is low, and it needs to be repeated many times.

发明内容:Invention content:

本发明目的是提供一种制备棒状超细晶材料的方法。The purpose of the present invention is to provide a method for preparing rod-shaped ultrafine-grained material.

本发明解决其技术问题所采用的技术方案是:一种棒状超细晶材料的制备方法,其特征在于:The technical solution adopted by the present invention to solve the technical problem is: a preparation method of a rod-shaped ultrafine-grained material, characterized in that:

1)待细化组织的棒状金属材料(1)卡在固定夹具(10)与旋转夹具(3)之间,通过中频电源(6)与感应线圈(7)对棒状金属材料(1)进行局部加热,加热温度低于材料的动态再结晶温度;1) The rod-shaped metal material (1) to be refined is clamped between the fixed fixture (10) and the rotating fixture (3), and the rod-shaped metal material (1) is locally processed by the intermediate frequency power supply (6) and the induction coil (7). Heating, the heating temperature is lower than the dynamic recrystallization temperature of the material;

2)当温度达到设定值后,由伺服电机(4)带动旋转夹具(3)旋转,在扭转剪切应力作用下,变形区(9)处的金属晶粒破碎细化;2) When the temperature reaches the set value, the servo motor (4) drives the rotating fixture (3) to rotate, and under the action of torsional shear stress, the metal grains in the deformation zone (9) are broken and refined;

3)通过控制滑台(44)的移动,使感应线圈(7)逐渐沿材料(1)轴向移动,变换加热区域;同时,冷却圈(45)与感应线圈(7)同步移动,冷却棒状金属材料(1)上变形区(9)后方的区域,保持已细化的细晶组织;3) By controlling the movement of the sliding table (44), the induction coil (7) gradually moves along the axial direction of the material (1) to change the heating area; at the same time, the cooling ring (45) moves synchronously with the induction coil (7), cooling the rod-shaped The area behind the deformation zone (9) on the metal material (1) maintains the refined fine-grain structure;

4)当感应线圈(7)从待细化的棒状金属材料(1)的一端移动到另一端时,依次停止加热、冷却及扭转,即可得到一段超细晶组织棒材;4) When the induction coil (7) moves from one end of the rod-shaped metal material (1) to be thinned to the other end, stop heating, cooling and twisting in sequence to obtain a section of ultra-fine-grained rod;

5)对已成型的超细晶组织棒材进行退火处理。5) Perform annealing treatment on the formed rod with ultra-fine grain structure.

本发明相比现有技术的优点在于,由于采用热扭转偏移法,可制备整块的棒状超细晶材料,而且一次成形,变形程度高,所用设备吨位低。降低了超细晶材料的成本。Compared with the prior art, the present invention has the advantages that, due to the thermal torsion offset method, a whole block of rod-shaped ultra-fine-grained material can be prepared, and it can be formed once, with high degree of deformation and low tonnage of the equipment used. The cost of ultrafine-grained materials is reduced.

附图说明:Description of drawings:

图1为热扭转偏移法制备棒状超细晶材料示意图Figure 1 is a schematic diagram of the preparation of rod-shaped ultrafine-grained materials by the thermal torsion migration method

图2为高压扭转塑性变形法制备超细晶材料示意图Figure 2 is a schematic diagram of the preparation of ultrafine-grained materials by high-pressure torsional plastic deformation

图3为S型等径侧向挤压法制备超细晶材料示意图Figure 3 is a schematic diagram of the preparation of ultrafine-grained materials by S-type equal diameter lateral extrusion method

图2和图3为背景技术附图Fig. 2 and Fig. 3 are accompanying drawings of background technology

图中1-材料,2-轴承,3-旋转夹具,-4-伺服电机,5-温度传感器,6-中频电源,7-感应线圈,8-冷却系统,9-变形区10-固定夹具,61-压扭模具,71-压头,72-挤压模具。In the figure 1-material, 2-bearing, 3-rotary fixture, -4-servo motor, 5-temperature sensor, 6-intermediate frequency power supply, 7-induction coil, 8-cooling system, 9-deformation zone, 10-fixing fixture, 61-press torsion die, 71-pressure head, 72-extrusion die.

具体实施方式:Detailed ways:

实施例1:参照图1,本例是利用热扭转偏移法制备棒状超细晶材料,属于变形区转移法制备棒(块)状超细晶材料的一种方法。具体过程如下:待细化组织的棒状金属材料1卡在固定夹具10与旋转夹具3之间。旋转夹具3由伺服电机4驱动,在旋转夹具3与伺服电机4中间安装有扭矩传感器41。感应线圈7与中频电源6可对棒状金属材料1进行局部加热。冷却圈45与冷却系统8可对棒状金属材料1进行局部冷却。由温度传感器5用来测量加热区温度。Embodiment 1: Referring to Fig. 1, this example is to prepare rod-shaped ultra-fine-grained material by thermal torsion migration method, which belongs to a method for preparing rod (block)-shaped ultra-fine-grained material by deformation zone transfer method. The specific process is as follows: the rod-shaped metal material 1 to be refined is stuck between the fixed fixture 10 and the rotating fixture 3 . The rotary clamp 3 is driven by a servo motor 4 , and a torque sensor 41 is installed between the rotary clamp 3 and the servo motor 4 . The induction coil 7 and the intermediate frequency power supply 6 can locally heat the rod-shaped metal material 1 . The cooling ring 45 and the cooling system 8 can locally cool the rod-shaped metal material 1 . The temperature sensor 5 is used to measure the temperature of the heating zone.

通过中频电源6与感应线圈7对棒状金属材料1进行局部加热,加热温度低于材料的动态再结晶温度;The rod-shaped metal material 1 is locally heated by the intermediate frequency power supply 6 and the induction coil 7, and the heating temperature is lower than the dynamic recrystallization temperature of the material;

当温度达到设定值后,由伺服电机4带动旋转夹具3旋转。由于感应加热的区域温度相对其他区域高,变形抗力小,故塑性变形集中在加热变形区9。由于变形集中,变形区9的变形速率高,容易达到大应变程度,在扭转剪切应力作用下,金属晶粒易于破碎,形成细化晶粒。同时由于是局部变形,设备加载能力要求低,变形过程便于控制。When the temperature reaches the set value, the rotary fixture 3 is driven by the servo motor 4 to rotate. Since the temperature of the induction heating area is higher than that of other areas and the deformation resistance is small, the plastic deformation is concentrated in the heating deformation area 9 . Due to the concentration of deformation, the deformation rate of the deformation zone 9 is high, and it is easy to reach a large strain degree. Under the action of torsional shear stress, the metal grains are easily broken to form fine grains. At the same time, due to the local deformation, the requirements for the loading capacity of the equipment are low, and the deformation process is easy to control.

当起始加热变形区9的温度、变形程度达到设定值,使晶粒细化到一定程度后,通过控制滑台44的移动,使感应线圈7逐渐沿材料1轴向移动,变换加热区域。同时,冷却圈45随滑台44的移动与感应线圈7同步移动,启动冷却系统8,冷却棒状金属材料1上变形区9后方的区域,保持已细化的细晶组织。这样,随着滑台44的移动,棒状金属材料1上的加热变形区9跟随感应线圈7一起移动,使新的加热变形区9的晶粒得到细化、保持。随着加热变形区9的不断移动,就会形成连续的棒(块)状细化金属体。When the temperature and degree of deformation of the initial heating deformation zone 9 reach the set value, and the grains are refined to a certain extent, by controlling the movement of the sliding table 44, the induction coil 7 is gradually moved along the axial direction of the material 1, and the heating area is changed. . Simultaneously, the cooling ring 45 moves synchronously with the induction coil 7 with the movement of the sliding table 44, starts the cooling system 8, cools the area behind the deformation zone 9 on the rod-shaped metal material 1, and maintains the refined fine-grain structure. In this way, with the movement of the slide table 44, the heated deformation zone 9 on the rod-shaped metal material 1 moves together with the induction coil 7, so that the crystal grains in the new heated deformation zone 9 are refined and maintained. Along with the continuous movement of the heated deformation zone 9, a continuous rod (block)-shaped refined metal body will be formed.

当感应线圈7从待细化的棒状金属材料1的一端移动到另一端时,依次停止加热、冷却及扭转。从夹具上取下棒状金属材料1,去掉两头过渡段,即可得到一段超细晶组织棒材。When the induction coil 7 moves from one end to the other end of the rod-shaped metal material 1 to be thinned, heating, cooling and twisting are stopped sequentially. The rod-shaped metal material 1 is removed from the fixture, and the transition sections at both ends are removed to obtain a rod with an ultra-fine grain structure.

通过控制加热温度、扭转速度和移动速度,可以调节扭转变形过程的变形程度和动态再结晶程度,以在棒状金属材料1内部得到不同程度的细化晶粒。By controlling the heating temperature, twisting speed and moving speed, the degree of deformation and the degree of dynamic recrystallization in the torsional deformation process can be adjusted to obtain different degrees of refined grains inside the rod-shaped metal material 1 .

最后,将已细化晶粒的棒状金属材料1进行适当的回火热处理,以降低残余应力,稳定组织。Finally, the rod-shaped metal material 1 with refined grains is properly tempered to reduce residual stress and stabilize the structure.

Claims (1)

1, a kind of preparation method of rod superfine crystal material is characterized in that:
1) bar-shaped metal materials (1) for the treatment of thinning microstructure is stuck between stationary fixture (10) and the rolling clamp (3), by intermediate frequency power supply (6) and ruhmkorff coil (7) bar-shaped metal materials (1) is carried out local heating, Heating temperature is lower than the dynamic recrystallization temperature of material;
2) after temperature reaches set(ting)value, by servomotor (4) driven rotary anchor clamps (3) rotation, under the torsional shear stress, the broken refinement of the metal grain that distorted area (9) are located;
3) by controlling moving of slide unit (44), make ruhmkorff coil (7) move axially the conversion heating region gradually along material (1); Simultaneously, cooling ring (45) and the same moved further of ruhmkorff coil (7), cooling bar-shaped metal materials (1) goes up the zone at rear, distorted area (9), keeps the fine grained texture of refinement;
4) when ruhmkorff coil (7) when an end of the bar-shaped metal materials (1) for the treatment of refinement moves to the other end, stop heating successively, cool off and reverse, can obtain one section ultrafine-grained's bar;
5) in type ultrafine-grained (UFG) microstructure bar is carried out anneal.
CNB2004100790675A 2003-01-10 2003-01-10 Prepn of rod superfine crystal material Expired - Fee Related CN1332058C (en)

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US20110224473A1 (en) * 2010-03-09 2011-09-15 Kurion, Inc. Microwave-Enhanced System for Pyrolysis and Vitrification of Radioactive Waste
CN103290183B (en) * 2013-05-29 2015-03-18 中国科学院力学研究所 Method for improving intensity of metal material
CN105543734B (en) * 2016-02-02 2017-06-09 西安建筑科技大学 A kind of low-melting-point metal Electroplastic ring rolles over rub fine method and its device
CN106011417B (en) * 2016-07-29 2018-04-13 北方工业大学 A method for preparing rod-like metal gradient nanostructures
CN111375721A (en) * 2020-03-23 2020-07-07 哈尔滨工业大学(威海) Device and method for preparing ultrafine crystals of material difficult to deform
CN113249664B (en) * 2021-05-14 2022-04-19 安徽力幕新材料科技有限公司 Processing method and processing equipment for light-weight high-strength aluminum alloy
CN115652138A (en) * 2022-10-27 2023-01-31 陕西天成航空材料有限公司 Preparation method of ultrafine-grained titanium alloy bar for aircraft engine rotor

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