TWI391504B - Grain - refined magnesium alloy sheet and its manufacturing method - Google Patents
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本發明係關於一種鎂合金板材及其製造方法，尤其係指一種晶粒細化之鎂合金板材及其製造方法，其係應用於汽車、航太工業或其他需高抗拉強度及快速成形特性之領域。The invention relates to a magnesium alloy sheet and a manufacturing method thereof, in particular to a grain refining magnesium alloy sheet and a manufacturing method thereof, which are applied to automobiles, aerospace industries or other high tensile strength and rapid forming characteristics. The field.
近年來在汽車、航太、家電及辦公家具產業追求輕量化之潮流中，具低密度之鎂合金的應用受到各領域的矚目。然而鎂合金欠缺常溫加工性之製程瓶頸，一直是成形的障礙。為改善鎂合金之成形性及在汽車產業上之應用，已有許多具有耐溫成形性之鎂合金出現，其中以ZK60(Mg－6wt%Zn－0.5wt%Zr)鎂合金最具潛力。然而因成形性及成形速率尚無法達到汽車產業所要求之規格，因此提高ZK60鎂合金之抗拉強度及具備快速成形特性(應變速率>10－2 S－1 ，伸長率>200%)是必要的。In recent years, in the pursuit of lightweight in the automotive, aerospace, home appliance and office furniture industries, the application of low-density magnesium alloys has attracted attention in various fields. However, magnesium alloys lack the process bottleneck of normal temperature processability, which has always been an obstacle to forming. In order to improve the formability of magnesium alloys and their applications in the automotive industry, many magnesium alloys with temperature-resistant formability have emerged, among which ZK60 (Mg-6wt% Zn-0.5wt% Zr) magnesium alloy has the most potential. However, since the formability and the forming rate cannot meet the specifications required by the automotive industry, it is necessary to increase the tensile strength of ZK60 magnesium alloy and to have rapid forming characteristics (strain rate >10 -2 S -1 , elongation >200%). of.
鑑於上述習知技術之缺點，本發明提供一種晶粒細化之鎂合金板材及其製造方法，其能細化ZK60鎂合金板材的晶粒，故能提高ZK60鎂合金板材之抗拉強度，並使ZK60鎂合金板材具備快速成形之優點，以適用於汽車工業。In view of the above disadvantages of the prior art, the present invention provides a grain refining magnesium alloy sheet material and a method of manufacturing the same, which can refine the grain of the ZK60 magnesium alloy sheet, thereby improving the tensile strength of the ZK60 magnesium alloy sheet, and The ZK60 magnesium alloy sheet has the advantages of rapid forming for use in the automotive industry.
本發明之主要目的在於提供一種晶粒細化之鎂合金板材及其製造方法，其能細化ZK60鎂合金板材的晶粒，故能提高ZK60鎂合金板材之抗拉強度，並使ZK60鎂合金板材具備快速成形之優點。The main object of the present invention is to provide a grain refining magnesium alloy sheet material and a manufacturing method thereof, which can refine the grain of the ZK60 magnesium alloy sheet, thereby improving the tensile strength of the ZK60 magnesium alloy sheet and enabling the ZK60 magnesium alloy. The sheet has the advantage of rapid prototyping.
本發明之次要目的在於提供一種晶粒細化之鎂合金板材及其製造方法，其能細化ZK60鎂合金板材的晶粒，以適用於汽車工業。A secondary object of the present invention is to provide a grain refining magnesium alloy sheet material and a method of manufacturing the same that can refine the grain of a ZK60 magnesium alloy sheet to be suitable for use in the automotive industry.
本發明提供一種晶粒細化之鎂合金板材及其製造方法，該晶粒細化之鎂合金板材，包括：複數個ZK 60鎂合金晶粒；及其中該複數個ZK 60鎂 合金晶粒之平均粒徑係小於10μm。該晶粒細化鎂合金板材之製造方法，其步驟包括：將一ZK 60鎂合金以豎型直接激冷式鑄造法製作出一ZK 60鎂合金鑄錠；將該ZK 60鎂合金鑄錠均質化熱處理；將該ZK 60鎂合金鑄錠擠製後，退火以消除應力；及軋延後再結晶退火，形成一晶粒細化之ZK 60鎂合金板材。The present invention provides a grain refining magnesium alloy sheet material and a method of manufacturing the same, the grain refining magnesium alloy sheet material comprising: a plurality of ZK 60 magnesium alloy crystal grains; and the plurality of ZK 60 magnesium The average grain size of the alloy crystal grains is less than 10 μm. The method for manufacturing the grain refining magnesium alloy sheet comprises the steps of: forming a ZK 60 magnesium alloy ingot by a vertical direct chill casting method for a ZK 60 magnesium alloy; and homogenizing the ZK 60 magnesium alloy ingot Heat treatment; after extruding the ZK 60 magnesium alloy ingot, annealing to eliminate stress; and recrystallization annealing after rolling to form a grain refined ZK 60 magnesium alloy sheet.
茲為使 貴審查委員對本發明之特徵及方法步驟有更進一步之瞭解與認識，現將詳細設計之原理及本發明之較佳實施例說明如後。The principles of the detailed design and the preferred embodiments of the present invention are set forth in the following description.
本發明之晶粒細化之鎂合金板材，包括：複數個ZK 60鎂合金晶粒；及其中該複數個ZK 60鎂合金晶粒之平均粒徑係小於10μm，其中該複數個ZK 60鎂合金晶粒較佳之平均粒徑係小於5μm。The grain refining magnesium alloy sheet of the present invention comprises: a plurality of ZK 60 magnesium alloy grains; and wherein the plurality of ZK 60 magnesium alloy grains have an average particle diameter of less than 10 μm, wherein the plurality of ZK 60 magnesium alloys The preferred average grain size of the grains is less than 5 μm.
本發明之晶粒細化鎂合金板材之製造方法，其步驟包括(如第一圖所示)：S11將一ZK 60鎂合金以豎型直接激冷式鑄造法製作出一ZK 60鎂合金鑄錠；S12將該ZK 60鎂合金鑄錠均質化熱處理；S13將該ZK 60鎂合金鑄錠擠製後，退火以消除應力；及S14軋延後退火以消除應力，形成一晶粒細化之ZK 60鎂合金板材。The method for manufacturing the grain refining magnesium alloy sheet of the present invention comprises the following steps (as shown in the first figure): S11 is a ZK 60 magnesium alloy cast by a vertical direct chill casting method. Ingot; S12 homogenizes the ZK 60 magnesium alloy ingot; S13 extrudes the ZK 60 magnesium alloy ingot to eliminate stress; and S14 post-rolls annealing to eliminate stress and form a grain refinement ZK 60 magnesium alloy sheet.
其中步驟S12中，該均質化熱處理之溫度為370~390℃。In the step S12, the temperature of the homogenization heat treatment is 370 to 390 °C.
其中步驟S13中，該擠製製程之擠製比為60~100：1。步驟S13中，更包括一以示差掃描熱卡計測量ZK 60鎂合金相變態溫度，以確認再結晶溫度範圍，再於該溫度範圍退火以消除應力之步驟。以示差掃描熱卡計測量ZK 60鎂合金相變態溫度，以確認ZK 60鎂合金再結晶溫度範圍，再於該溫度範圍退火以消除應力之步驟中，ZK 60鎂合金再結晶溫度範圍為227~265℃。In the step S13, the extrusion process has an extrusion ratio of 60 to 100:1. In step S13, a step of measuring the phase transition temperature of the ZK 60 magnesium alloy by a differential scanning calorimeter to confirm the recrystallization temperature range and annealing at the temperature range to eliminate the stress is further included. ZK 60 magnesium alloy phase metamorphic temperature was measured by differential scanning calorimeter to confirm the recrystallization temperature range of ZK 60 magnesium alloy, and then annealing in the temperature range to eliminate stress, the recrystallization temperature range of ZK 60 magnesium alloy was 227~ 265 ° C.
其中步驟S14中，軋延溫度為300~450℃及軋延率為20~80%；較佳軋 延溫度為350℃及較佳軋延率為80%。步驟S14中，退火溫度為255~275℃及退火時間大於16小時。In step S14, the rolling temperature is 300-450 ° C and the rolling rate is 20-80%; The extension temperature is 350 ° C and the preferred rolling rate is 80%. In step S14, the annealing temperature is 255 to 275 ° C and the annealing time is greater than 16 hours.
鎂合金的細晶強化主要通過控制鎂合金晶粒大小的方法實現，細晶組織材料其晶界是滑移傳遞的有效障礙，晶界前方的應力集中使得更多的滑移系被活化，合金的整體變形更加均勻，使得鎂合金強度和韌性獲得改善。細晶強化對於HCP結構的鎂合金效果更加明顯。合金的降伏強度與晶粒尺寸的關係可用Hall－Petch關係來表示，即σyield ＝σ0 ＋kd－1/2 ，式中σ0 為單晶降伏強度，k為Hall－Petch equation之斜率，d為晶粒大小。常用鎂合金具有相當高的k值，因此當鎂合金晶粒細化後，其強度提昇相當顯著。當晶粒細化至次微米(submicron)時，合金就會表現出超塑性。而獲得細小等軸的晶粒可以改善合金的性能，本發明ZK 60鎂合金的晶粒度可透過熱加工、塑性變形等方法控制，且ZK60鎂合金經動態再結晶之熱機處理可達到<10μm之細晶組織，再經退火處理使晶粒成為等軸晶，於拉伸試驗中藉由增加大量的晶界滑移而達到超塑性之目的。The fine grain strengthening of magnesium alloy is mainly achieved by the method of controlling the grain size of magnesium alloy. The grain boundary of fine grained structure material is an effective obstacle to the slip transfer. The stress concentration in front of the grain boundary makes more slip system activated. The overall deformation is more uniform, resulting in improved strength and toughness of the magnesium alloy. Fine grain strengthening is more effective for the magnesium alloy of the HCP structure. The relationship between the drop strength of the alloy and the grain size can be expressed by the Hall-Petch relationship, ie σ yield = σ 0 + kd - 1/2 , where σ 0 is the single crystal drop strength, k is the slope of the Hall-Petch equation, d It is the grain size. Commonly used magnesium alloys have a relatively high k value, so when the grain of the magnesium alloy is refined, its strength is considerably improved. When the grain is refined to submicron, the alloy exhibits superplasticity. Obtaining fine equiaxed grains can improve the performance of the alloy. The grain size of the ZK 60 magnesium alloy of the present invention can be controlled by thermal processing, plastic deformation, etc., and the ZK60 magnesium alloy can be treated by thermal recrystallization by dynamic recrystallization to reach <10 μm. The fine-grained structure is annealed to make the crystal grains equiaxed, and the superplasticity is achieved by increasing a large amount of grain boundary slip in the tensile test.
本發明先將ZK 60鎂合金(中科院製造ZK60鎂合金：Mg－5.29wt%zn－0.59wt%Zr)以豎型直接激冷式(Vertical Direct Chill Type,簡稱VDC)連鑄機製作出一直徑8吋之圓柱狀ZK 60鎂合金鑄錠。該ZK 60鎂合金鑄錠於380℃下並經過24小時的均質化熱處理後，再使用熱擠壓機，以擠製比60~100：1、約350℃下、擠製速度約為65 sec/m之擠製條件下，將圓柱狀之ZK 60鎂合金鑄錠擠製成厚度6 mm及寬度90 mm之板材。The invention firstly makes a diameter of a ZK 60 magnesium alloy (ZK60 magnesium alloy manufactured by the Chinese Academy of Sciences: Mg-5.29wt% zn-0.59wt% Zr) in a vertical direct chilling type (VDC) continuous casting mechanism. 8 inch cylindrical ZK 60 magnesium alloy ingot. The ZK 60 magnesium alloy ingot is subjected to a homogenization heat treatment at 380 ° C for 24 hours, and then a hot extrusion machine is used to extrude at a ratio of 60 to 100:1, about 350 ° C, and an extrusion speed of about 65 sec. Under the extrusion condition of /m, the cylindrical ZK 60 magnesium alloy ingot was extruded into a plate having a thickness of 6 mm and a width of 90 mm.
ZK 60鎂合金擠製板材先經示差掃描熱卡計(DSC)量測鎂合金相變態溫度，結果如第二圖所示，顯示ZK60鎂合金再結晶溫度(DBTT)的範圍為227~265℃。ZK 60 magnesium alloy extruded sheet was firstly measured by differential scanning calorimeter (DSC) to measure the phase transition temperature of magnesium alloy. The results are shown in the second figure, showing that the recrystallization temperature (DBTT) of ZK60 magnesium alloy ranges from 227 to 265 °C. .
ZK60鎂合金擠製板材(Mg－5.29wt%Zn－0.59wt%zr)於227~265℃溫度範圍退火3小時消除殘留應力後，再於300℃、350℃、400℃及450℃之不同軋延溫度，20%、40%、60%及80%之不同軋延率下，軋延成不同厚度之板材(其中300℃軋延溫度、20%以上軋延率軋延會造成薄板邊緣開 裂，故只作20%軋延率)。再經光學顯微鏡(OM)觀察以確認晶粒細化之最佳製程參數，如第三圖所示，顯示為350℃軋延溫度、80%軋延率軋延，晶粒細化至3μm最佳。此最佳細晶組織再經265℃退火16小時，可得到等軸晶粒，如第四圖所示。ZK60 magnesium alloy extruded sheet (Mg-5.29wt%Zn-0.59wt%zr) is annealed in the temperature range of 227~265°C for 3 hours to eliminate residual stress, and then rolled at 300°C, 350°C, 400°C and 450°C. Extension temperature, 20%, 40%, 60% and 80% of different rolling rates, rolling into different thickness of the sheet (300 °C rolling temperature, more than 20% rolling rate rolling will cause the edge of the sheet to open Crack, so only 20% rolling rate). Observed by optical microscopy (OM) to confirm the optimum process parameters for grain refinement, as shown in the third figure, it shows the calendering temperature of 350 °C, the rolling elongation of 80% rolling, and the grain refinement to 3 μm. good. This optimum fine-grained structure was annealed at 265 ° C for 16 hours to obtain equiaxed grains, as shown in the fourth figure.
ZK60鎂合金擠製材、擠製後於265℃下再結晶退火3小時得到擠製退火材，及以最佳製程參數350℃軋延溫度、80%軋延率軋延後於265℃下退火16小時得到之軋延退火ZK60鎂合金板材，作常溫、高溫拉伸之機械性質比較，其結果如表1和第五圖及第六圖所示。ZK60 magnesium alloy extruded material, after extrusion, recrystallization annealing at 265 ° C for 3 hours to obtain extruded annealed material, and annealing at 265 ° C with the optimum process parameters of 350 ° C rolling temperature, 80% rolling rate rolling and rolling 16 The rolling annealed ZK60 magnesium alloy sheet obtained in an hour is compared for mechanical properties at room temperature and high temperature stretching, and the results are shown in Table 1, Figure 5 and Figure 6.
由表1得知，ZK60鎂合金擠製材室溫抗拉強度為264MPa，延伸率為13.9%，擠製後再於265℃下退火3小時之試片，室溫抗拉強度可達263MPa，延伸率為15.7%，延伸率稍有改善。再於350℃軋延溫度、80%軋延率軋延後，於265℃下退火16小時，室溫抗拉強度和延伸率明顯較擠製材提昇很多，室溫抗拉強度為322MPa，延伸率為19%，在300℃、10－2 S－1 快速拉伸應變速率拉伸，伸長率可達240%。故ZK60鎂合金板材經細化晶 粒的步驟後，其可應用於汽車產業。It can be seen from Table 1 that the tensile strength of ZK60 magnesium alloy extruded material is 264 MPa and the elongation is 13.9%. After extrusion, the test piece is annealed at 265 ° C for 3 hours. The tensile strength at room temperature can reach 263 MPa. The rate was 15.7% and the elongation rate improved slightly. After calendering at 350 °C and rolling at 80% rolling rate, annealing at 265 °C for 16 hours, the tensile strength and elongation at room temperature are significantly improved compared with the extruded material. The tensile strength at room temperature is 322 MPa, elongation. It is 19%, stretched at 300 ° C, 10 -2 S -1 at a rapid tensile strain rate, and the elongation is up to 240%. Therefore, after the step of refining the grain of the ZK60 magnesium alloy sheet, it can be applied to the automobile industry.
惟以上所述者，僅為本發明之較佳實施例而已，並非用來限定本發明實施之範圍，舉凡依本發明申請專利範圍所述之構造、特徵及精神所為之均等變化與修飾，均應包括於本發明之申請專利範圍內。The above is only the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and the equivalents and modifications of the structures, features and spirits described in the claims of the present invention are It should be included in the scope of the patent application of the present invention.
第一圖為本發明之晶粒細化鎂合金板材之製造方法的步驟流程圖。The first figure is a flow chart of the steps of the method for manufacturing the grain refined magnesium alloy sheet of the present invention.
第二圖為ZK60鎂合金擠製材之DSC量測圖。The second figure shows the DSC measurement of ZK60 magnesium alloy extruded material.
第三圖為ZK60鎂合金擠製材之軋延溫度、軋延率與晶粒大小之關係圖。The third figure shows the relationship between rolling temperature, rolling rate and grain size of ZK60 magnesium alloy extruded material.
第四圖為以350℃軋延溫度、80%軋延率製做出之晶粒細化之ZK60鎂合金板材之光學顯微鏡(OM)圖。The fourth figure is an optical microscope (OM) diagram of a grain refinement ZK60 magnesium alloy sheet made by a rolling temperature of 350 ° C and a rolling rate of 80%.
第五圖為本發明晶粒細化之ZK60鎂合金板材於300℃、10－2 S－1 速率拉伸之抗拉強度和伸長率之關係圖。The fifth graph is a graph showing the tensile strength and elongation of the grain-refined ZK60 magnesium alloy sheet at 300 ° C and 10 -2 S -1 rate.
第六圖為本發明晶粒細化之ZK60鎂合金板材於300℃、10－3 S－1 速率拉伸之抗拉強度和伸長率之關係圖。Fig. 6 is a graph showing the relationship between the tensile strength and the elongation of the grain-refined ZK60 magnesium alloy sheet at 300 ° C, 10 -3 S -1 rate.
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| US5078806A (en) * | 1988-05-23 | 1992-01-07 | Allied-Signal, Inc. | Method for superplastic forming of rapidly solidified magnesium base metal alloys |
| TW200304951A (en) * | 2002-03-04 | 2003-10-16 | Sumitomo Sei Steel Wire Corp | Magnesium alloy pipe and method for producing the same |
| TW200500473A (en) * | 2003-05-30 | 2005-01-01 | Sumitomo Sei Steel Wire Corp | The method for producing magnesium alloy molding |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5078806A (en) * | 1988-05-23 | 1992-01-07 | Allied-Signal, Inc. | Method for superplastic forming of rapidly solidified magnesium base metal alloys |
| TW200304951A (en) * | 2002-03-04 | 2003-10-16 | Sumitomo Sei Steel Wire Corp | Magnesium alloy pipe and method for producing the same |
| TW200500473A (en) * | 2003-05-30 | 2005-01-01 | Sumitomo Sei Steel Wire Corp | The method for producing magnesium alloy molding |
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