CN101781728B - A kind of magnesium tin base alloy and preparation method thereof - Google Patents
A kind of magnesium tin base alloy and preparation method thereof Download PDFInfo
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Abstract
Description
技术领域technical field
本发明属于金属结构材料及制备技术领域，特别是一种不含稀土的新型镁锡基合金及其冶炼和热处理工艺。The invention belongs to the technical field of metal structural materials and preparation, in particular to a novel rare earth-free magnesium-tin-based alloy and its smelting and heat treatment processes.
背景技术Background technique
镁合金是一种新型的轻合金，与铝合金和钛合金相比它具有密度更低，阻尼性能更好，铸造性能更优越等优点。高性能镁合金的研制是近年来各国金属材料领域的热点。镁铝系是最常用的镁合金系，但是已有的镁铝合金的使用温度一般低于150℃，不能满足许多构件的要求。目前能够改善高温强度和蠕变性能的商业镁合金主要都是以稀土元素为主要合金元素，且大多数镁稀土基合金中稀土元素的用量≥7％，但是组织稳定性问题仍然是限制这些合金使用温度的重要因素，价格则制约了这些合金在民用产品上的普及。在不含稀土元素的高温高强镁合金组分设计中，已有的工作主要分为三个方向：1，在已获得广泛应用的镁铝系合金中添加微量元素；2，以钙、硅等为主要合金元素；3，以锡为主要合金元素。镁铝基系合金可以随微量元素的不同而获得不同程度的性能改变，但是相对实际应用所需要的指标，没有本质的改善；镁钙基系和镁硅基系合金依靠晶界上稳定的共晶相起到强化作用，但是这些晶界共晶往往比较粗大，而且基体内部得不到细小弥散的强化相。目前主要的镁锡基合金多为三元合金，其中性能较好且具有商用潜力的是Mg-Sn-Zn三元镁锡基合金。该系列镁锡基合金具有一定的时效强化效果，但是达时效峰值的时间较长。合金在200-250℃时效，时效峰值在70～75HV之间，到达时效峰值所需的时间在70h～100h之间，这不利于工业生产。因此，改善镁锡基合金的工作是很有必要的。Magnesium alloy is a new type of light alloy. Compared with aluminum alloy and titanium alloy, it has the advantages of lower density, better damping performance and superior casting performance. The development of high-performance magnesium alloys has become a hot spot in the field of metal materials in various countries in recent years. Magnesium-aluminum series is the most commonly used magnesium alloy series, but the service temperature of existing magnesium-aluminum alloys is generally lower than 150°C, which cannot meet the requirements of many components. At present, commercial magnesium alloys that can improve high-temperature strength and creep properties mainly use rare earth elements as the main alloying elements, and the amount of rare earth elements in most magnesium rare earth-based alloys is ≥ 7%, but the problem of structural stability is still a limitation for these alloys. The important factor of use temperature, the price restricts the popularity of these alloys in civilian products. In the composition design of high-temperature and high-strength magnesium alloys that do not contain rare earth elements, the existing work is mainly divided into three directions: 1, adding trace elements to magnesium-aluminum alloys that have been widely used; 2, adding calcium, silicon, etc. 3. Tin is the main alloying element. Magnesium-aluminum-based alloys can obtain different degrees of performance changes with different trace elements, but compared with the indicators required for practical applications, there is no essential improvement; magnesium-calcium-based alloys and magnesium-silicon-based alloys rely on stable co- The crystal phase plays a strengthening role, but these grain boundary eutectics are often relatively coarse, and there is no fine and dispersed strengthening phase inside the matrix. At present, the main magnesium-tin-based alloys are mostly ternary alloys, among which the Mg-Sn-Zn ternary magnesium-tin-based alloy has better performance and commercial potential. This series of magnesium-tin-based alloys has a certain aging strengthening effect, but the time to reach the aging peak value is relatively long. The alloy is aged at 200-250°C, the aging peak is between 70-75HV, and the time required to reach the aging peak is between 70h-100h, which is not conducive to industrial production. Therefore, it is necessary to improve the work of magnesium-tin-based alloys.
发明内容Contents of the invention
本发明的目的是为克服已有技术的不足之处，提供一种新型的镁锡基合金及其制备方法，通过改良组分及热处理工艺，使其具有时效强化效果明显，时效峰值出现较快，过时效缓慢，组织稳定性较好的特点，以增加镁合金的合金体系，优化其性能。The purpose of the present invention is to overcome the deficiencies of the prior art, provide a new type of magnesium-tin-based alloy and its preparation method, through the improvement of components and heat treatment process, it has obvious aging strengthening effect, and the aging peak appears faster , slow over-aging, and good structural stability to increase the alloy system of magnesium alloys and optimize their performance.
本发明提供的一种镁锡基合金，其特征在于，该镁锡基合金的组分由镁、锡、锌、锰和银五种元素组成；各组分含量的质量百分比为：A magnesium-tin-based alloy provided by the present invention is characterized in that the components of the magnesium-tin-based alloy are composed of five elements: magnesium, tin, zinc, manganese and silver; the mass percentage of each component content is:
锡(Sn)：6～8％Tin (Sn): 6-8%
锌(Zn)：2～3％Zinc (Zn): 2 to 3%
锰(Mn)：0.2～0.5％Manganese (Mn): 0.2～0.5%
银(Ag)：0.1～0.5％Silver (Ag): 0.1～0.5%
其余为镁(Mg)。The remainder is magnesium (Mg).
本发明提供的上述镁锡基合金的制备方法，包括冶炼，均匀化热处理，时效热处理；其特征在于，包括以下步骤：The preparation method of the above-mentioned magnesium-tin-based alloy provided by the present invention includes smelting, homogenization heat treatment, and aging heat treatment; it is characterized in that it includes the following steps:
步骤一：制备镁锡基合金坯料Step 1: Prepare magnesium-tin-based alloy billet
按下列组分及质量百分比含量配料：6～8％锡，2～3％锌，0.2～0.5％锰，0.1～0.5％银，其余为镁；原料中各组分的纯度均超过99.99％，在坩埚中依次放入镁，锡，锌，锰，银，加热至700～720℃，搅拌8-10分钟，静置6-10分钟成合金液体，将合金液体浇注到铸造用冷模具中形成镁锡基合金坯料；The ingredients are formulated according to the following components and mass percentages: 6-8% tin, 2-3% zinc, 0.2-0.5% manganese, 0.1-0.5% silver, and the rest is magnesium; the purity of each component in the raw materials exceeds 99.99%. Put magnesium, tin, zinc, manganese, and silver in the crucible in turn, heat to 700-720°C, stir for 8-10 minutes, let it stand for 6-10 minutes to form an alloy liquid, and pour the alloy liquid into a cold mold for casting to form Magnesium-tin-based alloy billets;
步骤二：均匀化热处理Step 2: Homogenization heat treatment
将镁锡基合金坯料放入常规电阻炉，在空气气氛下进行加热，加热温度为440-450℃，保温时间为27-30小时，冷水淬火得到均匀化的镁锡基合金；Put the magnesium-tin-based alloy billet into a conventional resistance furnace, heat it in an air atmosphere, the heating temperature is 440-450°C, the holding time is 27-30 hours, and quench in cold water to obtain a homogenized magnesium-tin-based alloy;
步骤三：时效热处理Step 3: aging heat treatment
将均匀化的镁锡基合金在常规电阻炉中空气气氛下进行时效热处理，加热温度为200-220℃，保温时间为25～30小时，冷水淬火得到时效强化的镁锡基合金。The homogenized magnesium-tin-based alloy is subjected to aging heat treatment in an air atmosphere in a conventional resistance furnace, the heating temperature is 200-220° C., the holding time is 25-30 hours, and the aging-strengthened magnesium-tin-based alloy is obtained by quenching in cold water.
本发明与现有技术相比，具有如下优点：Compared with the prior art, the present invention has the following advantages:
1、本发明提出的这种镁合金的特征在于综合考察了Mg-Sn、Mg-Zn、Mg-Mn等相图，以及可能的金属间化合物，采用廉价的主合金元素，不含稀土元素，只需要添加微量的银元素，其余主要合金元素均为较便宜的非稀土元素，材料的成本在可接受的范围。1. This magnesium alloy proposed by the present invention is characterized in that phase diagrams such as Mg-Sn, Mg-Zn, Mg-Mn, and possible intermetallic compounds have been comprehensively investigated, and cheap main alloying elements are used without rare earth elements. Only a small amount of silver element needs to be added, and the rest of the main alloying elements are relatively cheap non-rare earth elements, and the cost of the material is within an acceptable range.
2、本发明的镁锡基合金具备高温高强应用的潜力，时效峰值超过80HV，高于其他系列的镁锡基合金。2. The magnesium-tin-based alloy of the present invention has the potential for high-temperature and high-strength applications, and the aging peak value exceeds 80HV, which is higher than other series of magnesium-tin-based alloys.
3、本发明所制备的镁锡基合金，时效峰值到达的时间为25-30小时，远低于其他系列的镁锡基合金，很大程度上节省了热处理所需要的时间和热处理需要的能耗。3. For the magnesium-tin-based alloy prepared by the present invention, the aging peak arrival time is 25-30 hours, which is far lower than other series of magnesium-tin-based alloys, which greatly saves the time required for heat treatment and the energy required for heat treatment. consumption.
4、本发明所制备的镁锡基合金在200℃以上时效，合金显微硬度值在55小时之后稳定保持在70HV左右，材料组织的高温稳定性能很好。4. The magnesium-tin-based alloy prepared by the present invention is aged above 200°C, and the microhardness value of the alloy remains stable at about 70HV after 55 hours, and the high-temperature stability of the material structure is very good.
5、本发明设计的镁锡基合金可以通过常规电阻炉进行热处理，热处理过程中无需氩气等气体保护，无需额外增加特殊设备，在企业应用时可节约设备成本。5. The magnesium-tin-based alloy designed in the present invention can be heat-treated by a conventional resistance furnace, without gas protection such as argon gas during the heat treatment process, and without additional special equipment, which can save equipment costs in enterprise applications.
具体实施方式Detailed ways
本发明的目的是提供一种高温性能稳定且时效反应较快的镁锡基合金。The purpose of the present invention is to provide a magnesium-tin-based alloy with stable performance at high temperature and fast aging response.
通过如下实施例对本发明做进一步说明：The present invention will be further described by following examples:
实施例1：Example 1:
步骤一：制备镁锡基合金坯料Step 1: Prepare magnesium-tin-based alloy billet
(1)按下列组分及质量百分比含量配料：6％锡，2％锌，0.2％锰，0.1％银，其余为镁；原料的纯度均为99.999％，坩埚和铸造用模具采用低碳钢材质。坩埚目标温度定为700℃；然后将所述各种配料放在烘箱中预热至160℃，同时将占所制备镁锡基合金总重量2wt％的RJ-2覆盖剂放入烘箱中烘烤；将浇铸用模具在另外的箱式炉中预热至300℃；(1) Ingredients are prepared according to the following components and mass percentages: 6% tin, 2% zinc, 0.2% manganese, 0.1% silver, and the rest are magnesium; the purity of the raw materials is 99.999%, and the crucible and casting molds are made of low carbon steel material. The target temperature of the crucible is set at 700°C; then the various ingredients are preheated to 160°C in an oven, and at the same time, the RJ-2 covering agent that accounts for 2wt% of the total weight of the prepared magnesium-tin-based alloy is put into the oven and baked ;Preheat the casting mold to 300°C in another box furnace;
(2)当坩埚升温至300℃时，通入CO2气体至坩埚内进行气体置换，然后在坩埚底部加入1/2左右的已烘烤的覆盖剂，再后将预热好的纯镁配料放入坩埚内；(2) When the temperature of the crucible rises to 300°C, CO 2 gas is introduced into the crucible for gas replacement, and then about 1/2 of the baked covering agent is added to the bottom of the crucible, and then the preheated pure magnesium ingredients are added into the crucible;
(3)镁配料熔化并且等坩埚温度稳定在700℃后，根据熔点由高到低依次加入预热的其它各种配料，然后熔体进行搅拌约8分钟；此过程中，酌情加入剩余的已烘烤的覆盖剂，以表面不燃为准；(3) After the magnesium ingredients are melted and the temperature of the crucible is stabilized at 700°C, add other preheated ingredients according to the melting point from high to low, and then stir the melt for about 8 minutes; during this process, add the remaining preheated ingredients as appropriate. For baked coverings, the non-combustible surface shall prevail;
(4)坩埚温度稳定在700℃后，熔体静置6分钟，按体积百分比，在99.5％空气(或CO2)+1％SF6混合气体保护下掏渣；(4) After the temperature of the crucible is stabilized at 700 ° C, the melt is left to stand for 6 minutes, and the slag is removed under the protection of 99.5% air (or CO 2 ) + 1% SF 6 mixed gas according to the volume percentage;
(5)掏渣完毕后，维持坩埚温度稳定在700℃，按体积百分比，在99.5％空气(或CO2)+1％SF6混合气体保护下浇铸成镁锡基合金坯料；(5) After the slagging is completed, keep the crucible temperature stable at 700°C, and cast it into a magnesium-tin-based alloy billet under the protection of 99.5% air (or CO 2 )+1% SF 6 mixed gas according to the volume percentage;
步骤二：均匀化热处理Step 2: Homogenization heat treatment
将镁锡基合金坯料放入常规电阻炉，在空气气氛下进行加热，加热温度为440℃，保温时间为27小时，冷水淬火得到均匀化的镁锡基合金；Put the magnesium-tin-based alloy billet into a conventional resistance furnace, heat it in an air atmosphere, the heating temperature is 440°C, the holding time is 27 hours, and quench in cold water to obtain a homogenized magnesium-tin-based alloy;
步骤三：时效热处理Step 3: aging heat treatment
将均匀化的镁锡基合金在常规电阻炉中空气气氛下进行时效热处理，时效过程中使用的温度为200℃，保温时间为30小时，冷水淬火得到时效强化的镁锡基合金。The homogenized magnesium-tin-based alloy is subjected to aging heat treatment in an air atmosphere in a conventional resistance furnace. The temperature used in the aging process is 200°C, the holding time is 30 hours, and the aging-strengthened magnesium-tin-based alloy is obtained by quenching in cold water.
实施例2：Example 2:
步骤一：制备镁锡基合金坯料Step 1: Prepare magnesium-tin-based alloy billet
(1)按下列组分及质量百分比含量配料：7％锡，2.5％锌，0.3％锰，0.3％银，其余为镁。原料的纯度均为99.999％，坩埚和铸造用模具采用低碳钢材质。定坩埚目标温度为710℃，然后将所述各种配料放在烘箱中预热至160℃，同时将占所制备镁锡基合金总重量2wt％的RJ-2覆盖剂放入烘箱中烘烤；将浇铸用模具在另外的箱式炉中预热至300℃；(1) Dosing according to the following components and mass percentage content: 7% tin, 2.5% zinc, 0.3% manganese, 0.3% silver, and the rest is magnesium. The purity of the raw materials is 99.999%, and the crucible and casting molds are made of low carbon steel. Set the target temperature of the crucible to 710°C, then preheat the various ingredients in an oven to 160°C, and simultaneously put the RJ-2 covering agent that accounts for 2wt% of the total weight of the prepared magnesium-tin-based alloy into the oven for baking ;Preheat the casting mold to 300°C in another box furnace;
(2)当坩埚升温至300℃时，通入CO2气体至坩埚内进行气体置换，然后在坩埚底部加入1/2左右的已烘烤的覆盖剂，再后将预热好的纯镁配料放入坩埚内；(2) When the temperature of the crucible rises to 300°C, CO 2 gas is introduced into the crucible for gas replacement, and then about 1/2 of the baked covering agent is added to the bottom of the crucible, and then the preheated pure magnesium ingredients are added into the crucible;
(3)镁配料熔化并且等坩埚温度稳定在710℃后，根据熔点由高到低依次加入预热的其它各种配料，然后熔体进行搅拌约9分钟；此过程中，酌情加入剩余的已烘烤的覆盖剂，以表面不燃为准。(3) After the magnesium ingredients are melted and the temperature of the crucible is stabilized at 710°C, add other preheated ingredients according to the melting point from high to low, and then stir the melt for about 9 minutes; during this process, add the remaining preheated ingredients as appropriate. For baked coverings, the non-combustible surface shall prevail.
(4)坩埚温度稳定在710℃后，熔体静置8分钟，按体积百分比，在99.5％空气(或CO2)+1％SF6混合气体保护下掏渣；(4) After the temperature of the crucible is stabilized at 710°C, the melt is left to stand for 8 minutes, and the slag is removed under the protection of 99.5% air (or CO 2 )+1% SF 6 mixed gas according to the volume percentage;
(5)掏渣完毕后，维持坩埚温度稳定在710℃，按体积百分比，在99.5％空气(或CO2)+1％SF6混合气体保护下浇铸成镁锡基合金坯料。(5) After slag removal, keep the temperature of the crucible at 710°C, and cast magnesium-tin-based alloy blanks under the protection of 99.5% air (or CO 2 ) + 1% SF 6 mixed gas according to volume percentage.
步骤二：均匀化热处理Step 2: Homogenization heat treatment
将镁锡基合金坯料放入常规电阻炉，在空气气氛下进行加热，加热温度为445℃，保温时间为28小时，冷水淬火得到均匀化的镁锡基合金。Put the magnesium-tin-based alloy billet into a conventional electric resistance furnace, heat it in an air atmosphere, the heating temperature is 445°C, the holding time is 28 hours, and quench in cold water to obtain a homogenized magnesium-tin-based alloy.
步骤三：时效热处理Step 3: aging heat treatment
将均匀化的镁锡基合金在常规电阻炉中空气气氛下进行时效热处理，时效过程中使用的温度为210℃，保温时间为27小时，冷水淬火得到时效强化的镁锡基合金。The homogenized magnesium-tin-based alloy is subjected to aging heat treatment in an air atmosphere in a conventional resistance furnace. The temperature used in the aging process is 210°C, the holding time is 27 hours, and the aging-strengthened magnesium-tin-based alloy is obtained by cold water quenching.
实施例3：Example 3:
步骤一：制备镁锡基合金坯料Step 1: Prepare magnesium-tin-based alloy billet
(1)按下列组分及质量百分比含量配料：8％锡，3％锌，0.5％锰，0.5％银，其余为镁。原料的纯度均为99.999％，坩埚和铸造用模具采用低碳钢材质。定坩埚目标温度为720℃，开始加热。然后将各种配料放在烘箱中预热至160℃，同时将占所制备镁锡基合金总重量2wt％的RJ-2覆盖剂放入烘箱中烘烤；将浇铸用模具在另外的箱式炉中预热至300℃。(1) Dosing according to the following components and mass percentage content: 8% tin, 3% zinc, 0.5% manganese, 0.5% silver, and the rest is magnesium. The purity of the raw materials is 99.999%, and the crucible and casting molds are made of low carbon steel. Set the target temperature of the crucible to 720°C and start heating. Then various ingredients are placed in the oven and preheated to 160 ° C, and the RJ-2 covering agent that accounts for 2wt% of the total weight of the prepared magnesium-tin-based alloy is put into the oven and baked; the casting mold is placed in another box Preheat the furnace to 300°C.
(2)当坩埚升温至300℃时，通入CO2气体至坩埚内进行气体置换，然后在坩埚底部加入1/2左右的已烘烤的覆盖剂，再后将预热好的纯镁配料放入坩埚内。(2) When the temperature of the crucible rises to 300°C, CO 2 gas is introduced into the crucible for gas replacement, and then about 1/2 of the baked covering agent is added to the bottom of the crucible, and then the preheated pure magnesium ingredients are added Put it in the crucible.
(3)镁配料熔化并且等坩埚温度稳定在720℃后，根据熔点由高到低依次加入预热的各种配料，然后熔体进行搅拌约10分钟；此过程中，酌情加入剩余的已烘烤的覆盖剂，以表面不燃为准。(3) After the magnesium ingredients are melted and the temperature of the crucible is stabilized at 720°C, add the preheated ingredients in order according to the melting point from high to low, and then stir the melt for about 10 minutes; during this process, add the remaining baked For baked coverings, the non-combustible surface shall prevail.
(4)坩埚温度稳定在720℃后，熔体静置10分钟，按体积百分比，在99.5％空气(或CO2)+1％SF6混合气体保护下掏渣；(4) After the temperature of the crucible is stabilized at 720°C, the melt is left to stand for 10 minutes, and the slag is removed under the protection of 99.5% air (or CO 2 )+1% SF 6 mixed gas according to the volume percentage;
(5)掏渣完毕后，维持坩埚温度稳定在720℃，按体积百分比，在99.5％空气(或CO2)+1％SF6混合气体保护下浇铸成镁锡基合金坯料。(5) After slag removal, keep the temperature of the crucible at 720°C, and cast magnesium-tin-based alloy blanks under the protection of 99.5% air (or CO 2 ) + 1% SF 6 mixed gas according to volume percentage.
步骤二：均匀化热处理Step 2: Homogenization heat treatment
将镁锡基合金坯料放入常规电阻炉，在空气气氛下进行加热，加热温度为450℃，保温时间为30小时，冷水淬火得到均匀化的镁锡基合金。Put the magnesium-tin-based alloy billet into a conventional electric resistance furnace, heat it in an air atmosphere, the heating temperature is 450°C, the holding time is 30 hours, and quench in cold water to obtain a homogenized magnesium-tin-based alloy.
步骤三：时效热处理Step 3: aging heat treatment
将均匀化的镁锡基合金在常规电阻炉中空气气氛下进行时效热处理，时效过程中使用的温度为220℃，保温时间为25小时，冷水淬火得到时效强化的镁锡基合金。The homogenized magnesium-tin-based alloy is subjected to aging heat treatment in an air atmosphere in a conventional resistance furnace. The temperature used in the aging process is 220°C, the holding time is 25 hours, and the aging-strengthened magnesium-tin-based alloy is obtained by quenching in cold water.
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