CN111961899A - Method for removing impurity iron in magnesium alloy by using Al-Zr master alloy - Google Patents
Method for removing impurity iron in magnesium alloy by using Al-Zr master alloy Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 61
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 56
- 239000000956 alloy Substances 0.000 title claims abstract description 56
- 239000012535 impurity Substances 0.000 title claims abstract description 43
- 229910018580 Al—Zr Inorganic materials 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 23
- 239000000155 melt Substances 0.000 claims abstract description 16
- 239000000919 ceramic Substances 0.000 claims abstract description 7
- 238000003723 Smelting Methods 0.000 claims abstract description 6
- 238000005266 casting Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims 2
- 150000001875 compounds Chemical class 0.000 abstract description 9
- 238000001556 precipitation Methods 0.000 abstract description 5
- 239000002344 surface layer Substances 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 2
- 238000007670 refining Methods 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 6
- 229910052749 magnesium Inorganic materials 0.000 description 6
- 239000011777 magnesium Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000004927 clay Substances 0.000 description 3
- 238000004512 die casting Methods 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- 229910003023 Mg-Al Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 235000021190 leftovers Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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- Casting Support Devices, Ladles, And Melt Control Thereby (AREA)
Abstract
本发明提供了一种使用Al‑Zr中间合金除去镁合金中杂质铁的方法，在镁合金熔炼过程中加入Al‑Zr中间合金，熔体浇注时使用陶瓷过滤片对熔体进行过滤。所述Al‑Zr中间合金中Zr元素含量为3~20wt%，单个杂质元素含量≤0.5%，杂质元素总和≤1.0%，余量为Al。本发明Al‑Zr中间合金中的除铁有效组分是粗大的针状及骨骼状Al3Zr相。这些Al3Zr相在镁合金熔体中，随着表层Zr、Al元素的溶解，依附于表层形成含Zr、Fe的化合物。这些化合物连同Al3Zr相尺寸粗大，很容易通过过滤网进行阻挡，因此不需要进行静置使之沉淀而实现除铁。
The invention provides a method for removing impurity iron in magnesium alloy by using Al-Zr master alloy. The Al-Zr master alloy is added in the magnesium alloy smelting process, and a ceramic filter is used to filter the melt when the melt is poured. The content of Zr element in the Al-Zr master alloy is 3-20wt%, the content of a single impurity element is ≤0.5%, the sum of the impurity elements is ≤1.0%, and the balance is Al. The effective components for iron removal in the Al-Zr master alloy of the present invention are coarse needle-like and bone-like Al 3 Zr phases. In the magnesium alloy melt, these Al 3 Zr phases adhere to the surface layers to form compounds containing Zr and Fe along with the dissolution of Zr and Al elements in the surface layers. These compounds, together with the Al 3 Zr phase, are large in size and can be easily blocked by a filter screen, so it is not necessary to stand for precipitation to achieve iron removal.
Description
技术领域technical field
本发明涉及镁合金的熔炼净化，提高镁合金产品耐蚀性的技术领域，具体涉及一种使用Al-Zr中间合金除去镁合金中杂质铁的方法。The invention relates to the technical field of smelting and purification of magnesium alloys and improving the corrosion resistance of magnesium alloy products, in particular to a method for removing impurity iron in magnesium alloys by using Al-Zr master alloy.
背景技术Background technique
镁合金中的Fe杂质会严重影响合金的耐蚀性，因此镁合金中Fe杂质的含量受到严格限制。特别是镁合金生产中的回炉料、边角料以镁合金产品的回收再利用，必须有效地除去其中的Fe杂质。Fe impurities in magnesium alloys will seriously affect the corrosion resistance of the alloys, so the content of Fe impurities in magnesium alloys is strictly limited. In particular, in the production of magnesium alloys, the recycled materials and scraps are recycled and reused as magnesium alloy products, and the Fe impurities in them must be effectively removed.
现有的镁合金熔炼除Fe方法，都是一种沉淀法，即通过添加某种元素与镁合金熔体中的Fe结合成稳定的密度高于镁的化合物，经过静置使之沉于熔体底部。沉淀除Fe工艺，镁合金熔体在浇铸前必须充分静置。这一方面会增加镁合金熔体的吸气倾向，另一方面也容易使熔体中的某些合金元素产生偏析或使熔体中细化镁合金晶粒的异质晶核数量减少。此外，镁合金熔体在浇铸时常常难以准确控制以避免已沉淀于熔体底部的杂质Fe化合物进入铸件。The existing methods for removing Fe by smelting magnesium alloys are all precipitation methods, that is, by adding a certain element and combining with Fe in the magnesium alloy melt to form a stable compound with a density higher than that of magnesium, which is allowed to settle in the molten metal after standing. body bottom. In the precipitation and Fe removal process, the magnesium alloy melt must be sufficiently left to stand before casting. On the one hand, it will increase the inhalation tendency of the magnesium alloy melt, and on the other hand, it is easy to segregate some alloy elements in the melt or reduce the number of heterogeneous nuclei that refine the magnesium alloy grains in the melt. In addition, magnesium alloy melts are often difficult to accurately control during casting to avoid impurity Fe compounds that have precipitated at the bottom of the melt from entering the casting.
发明内容SUMMARY OF THE INVENTION
本发明提出了一种使用Al-Zr中间合金除去镁合金（Mg-Al系）中杂质铁的方法，目的在于克服现有镁合金熔炼过程中沉淀除Fe工艺存在的不足。The present invention proposes a method for removing impurity iron in magnesium alloys (Mg-Al series) by using Al-Zr master alloy, aiming at overcoming the deficiencies in the existing process of precipitation and removing Fe in the smelting process of magnesium alloys.
实现本发明的技术方案是：The technical scheme that realizes the present invention is:
使用Al-Zr中间合金除去镁合金中杂质铁的方法，在镁合金熔炼过程中加入Al-Zr中间合金，熔体浇注时对熔体进行过滤。In the method of removing impurity iron in magnesium alloy by using Al-Zr master alloy, the Al-Zr master alloy is added during the smelting process of magnesium alloy, and the melt is filtered when the melt is poured.
所述的使用Al-Zr中间合金除去镁合金中杂质铁的方法，具体步骤如下：Described use Al-Zr master alloy to remove the method for impurity iron in magnesium alloy, concrete steps are as follows:
（1）将镁合金熔化并使熔体温度达到680~780℃；(1) Melt the magnesium alloy and make the melt temperature reach 680~780℃;
（2）向步骤（1）熔体中加入Al-Zr中间合金，由中间合金向熔体中提供除铁有效元素Zr，搅拌熔化；(2) adding an Al-Zr master alloy to the melt in step (1), providing Zr, an effective iron-removing element, into the melt from the master alloy, and stirring and melting;
（3）待Al-Zr中间合金在熔体中熔化均匀后，在680~780℃温度范围内对镁合金进行精炼和除气，然后使熔体通过陶瓷过滤片进行浇铸。(3) After the Al-Zr master alloy is uniformly melted in the melt, the magnesium alloy is refined and degassed in the temperature range of 680~780°C, and then the melt is cast through a ceramic filter.
以Al-Zr中间合金中Zr元素质量、镁合金和Al-Zr中间合金中含有的全部Fe元素质量计，步骤（2）Al-Zr中间合金中Zr元素质量和全部Fe元素质量之比为（5~10）：1。Based on the mass of Zr element in the Al-Zr master alloy, the mass of all Fe elements contained in the magnesium alloy and the Al-Zr master alloy, the ratio of the mass of Zr element to the mass of all Fe elements in the Al-Zr master alloy in step (2) is ( 5~10): 1.
所述步骤（3）中浇铸温度为650-800℃，陶瓷过滤片的孔隙率为15-50ppi，陶瓷过滤片的材质为SiC或MgO。In the step (3), the casting temperature is 650-800° C., the porosity of the ceramic filter is 15-50 ppi, and the material of the ceramic filter is SiC or MgO.
所述Al-Zr中间合金中Zr元素含量为3~20wt%，单个杂质元素含量≤0.5%，杂质元素总和≤1.0%，余量为Al。The content of Zr element in the Al-Zr master alloy is 3-20wt%, the content of a single impurity element is ≤0.5%, the sum of the impurity elements is ≤1.0%, and the balance is Al.
本发明的有益效果是：使用Al-Zr中间合金除去杂质铁的方法适用于Mg-Al系镁合金的熔铸除铁，且除Fe效果稳定，适用于工业规模。现有的镁合金熔铸除铁方法，是通过形成密度高于镁合金熔体的含Fe化合物，这些化合物尺寸很细小，在10-5微米以下，浇注时通过过滤网难以阻挡，使用孔隙率过高的过滤网又会滤掉合金熔体中的有效组分，如晶粒细化剂。在本发明中，Al-Zr中间合金中的除铁有效组分是粗大的针状及骨骼状Al3Zr相，见附图1。这些Al3Zr相在镁合金熔体中，随着表层Zr、Al元素的溶解，依附于表层形成含Zr、Fe的化合物，见附图2。这些化合物连同Al3Zr相尺寸粗大，很容易通过过滤网进行阻挡，因此不需要进行静置使之沉淀而实现除铁。The beneficial effects of the present invention are that the method for removing impurity iron by using the Al-Zr intermediate alloy is suitable for iron removal by melting and casting of Mg-Al magnesium alloys, and the Fe removal effect is stable, which is suitable for industrial scale. The existing magnesium alloy melting and casting iron removal method is to form Fe-containing compounds with a density higher than that of the magnesium alloy melt. The size of these compounds is very small, below 10-5 microns. The high filter screen will filter out the effective components in the alloy melt, such as grain refiners. In the present invention, the effective components for iron removal in the Al-Zr master alloy are coarse acicular and skeletal Al 3 Zr phases, as shown in FIG. 1 . In the magnesium alloy melt, these Al 3 Zr phases adhere to the surface layers to form compounds containing Zr and Fe along with the dissolution of Zr and Al elements in the surface layers, as shown in FIG. 2 . These compounds, together with the Al 3 Zr phase, are large in size and can be easily blocked by a filter screen, so it is not necessary to stand for precipitation to achieve iron removal.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the following briefly introduces the accompanying drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained according to these drawings without creative efforts.
图1为所使用的Al-Zr中间合金中的针状和骨骼状Al3Zr相（扫描电子显微镜照片）。Figure 1 shows the needle-like and bone-like Al 3 Zr phases in the Al-Zr master alloy used (scanning electron micrograph).
图2为除铁过程中在镁合金熔体的Al3Zr相表面形成的含Zr、Fe的化合物（扫描电子显微镜照片）。Fig. 2 shows the compounds containing Zr and Fe formed on the surface of the Al 3 Zr phase of the magnesium alloy melt during the iron removal process (scanning electron microscope photo).
具体实施方式Detailed ways
下面将结合本发明实施例，对本发明的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有付出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
实施例1Example 1
原牌号为AZ91D的镁合金压铸件边角料和回炉料共3.2kg，合金中杂质Fe的平均含量为0.015%（质量分数，以下相同）。Al-5Zr中间合金，其Zr元素含量5.2%，杂质Fe含量0.05%。The original grade of AZ91D magnesium alloy die-casting scrap and return material totals 3.2kg, and the average content of impurity Fe in the alloy is 0.015% (mass fraction, the same below). The Al-5Zr master alloy has a Zr element content of 5.2% and an impurity Fe content of 0.05%.
将上述镁合金置于石墨粘土坩埚中并在电阻坩埚炉中加热熔化。The above magnesium alloy was placed in a graphite clay crucible and heated and melted in a resistance crucible furnace.
镁合金熔体温度740℃，按Zr元素6倍于杂质Fe含量加入Al-5Zr中间合金58g。中间合金熔化后通入氩气进行精炼，精炼完成后750℃合金熔体通过预热750℃的20ppi SiC过滤片浇入石墨模中。The magnesium alloy melt temperature is 740℃, and 58g of Al-5Zr master alloy is added according to the content of Zr element 6 times that of impurity Fe. After the master alloy is melted, argon gas is introduced for refining. After refining, the alloy melt at 750°C is poured into a graphite mold through a 20ppi SiC filter preheated at 750°C.
化学成分分析经除Fe后的镁合金，其杂质Fe含量0.0031%，残余Zr含量小于0.001%。Chemical composition analysis After removing Fe, the magnesium alloy has an impurity Fe content of 0.0031% and a residual Zr content of less than 0.001%.
除Fe后的镁合金中杂质Fe含量达到国家标准GB/T5153-2016《变形镁及镁合金牌号和化学成分》对AZ91D镁合金中杂质Fe含量的要求，其中Zr元素含量小于该牌号规定的其他单个元素的限量。The impurity Fe content in the magnesium alloy after Fe removal meets the requirements of the national standard GB/T5153-2016 "Wrought Magnesium and Magnesium Alloy Grades and Chemical Composition" for the impurity Fe content in AZ91D magnesium alloy, and the Zr element content is less than the other specified by the grade. The limit of a single element.
实施例2Example 2
原牌号为AZ31的镁合金压铸件边角料和回炉料共2kg，合金中杂质Fe的平均含量为0.011%。Al-3Zr中间合金，其Zr元素含量3.1%，杂质Fe含量0.01%。The original grade is AZ31 of magnesium alloy die-casting scraps and return material totaling 2kg, and the average content of impurity Fe in the alloy is 0.011%. The Al-3Zr master alloy has a Zr element content of 3.1% and an impurity Fe content of 0.01%.
将上述镁合金置于石墨粘土坩埚中并在电阻坩埚炉中加热熔化。The above magnesium alloy was placed in a graphite clay crucible and heated and melted in a resistance crucible furnace.
镁合金熔体温度680℃，按Zr元素5倍于杂质Fe含量加入Al-3Zr中间合金36g。中间合金熔化后通入氩气进行精炼，精炼完成后650℃合金熔体通过预热760℃的15ppi SiC过滤片浇入石墨模中。The temperature of magnesium alloy melt is 680℃, and 36g of Al-3Zr master alloy is added according to the content of Zr element 5 times that of impurity Fe. After the master alloy is melted, argon gas is introduced for refining. After refining, the alloy melt at 650°C is poured into a graphite mold through a 15ppi SiC filter preheated at 760°C.
化学成分分析经除Fe后的镁合金，其杂质Fe含量0.002%。Chemical composition analysis After removing Fe, the magnesium alloy has an impurity Fe content of 0.002%.
实施例3Example 3
原牌号为AZ91的镁合金压铸件边角料和回炉料共2.2kg，合金中杂质Fe的平均含量为0.021%。Al-20Zr中间合金，其Zr元素含量19.8%，杂质Fe含量0.02%。The original grade of AZ91 magnesium alloy die-casting scrap and return material totals 2.2kg, and the average content of impurity Fe in the alloy is 0.021%. The Al-20Zr master alloy has a Zr element content of 19.8% and an impurity Fe content of 0.02%.
将上述镁合金置于中频感应加热炉的镁砂坩埚中加热熔化。The above magnesium alloy is heated and melted in a magnesia crucible of an intermediate frequency induction heating furnace.
镁合金熔体温度780℃，按Zr元素10倍于杂质Fe含量加入Al-3Zr中间合金24g。中间合金熔化后通入氩气进行精炼，精炼完成后800℃合金熔体通过50ppi SiC过滤片浇入石墨模中。The temperature of magnesium alloy melt is 780℃, and 24g of Al-3Zr master alloy is added according to the content of
化学成分分析经除Fe后的镁合金，其杂质Fe含量0.0033%，残余Zr含量小于0.001%。Chemical composition analysis After removing Fe, the magnesium alloy has an impurity Fe content of 0.0033% and a residual Zr content of less than 0.001%.
实施例4Example 4
AZ31镁合金挤压件料头及边角料3.5kg，其中杂质Fe含量0.025%。Al-20Zr中间合金，其Zr元素含量20.2%，杂质Fe含量0.03%。AZ31 magnesium alloy extrusion head and leftovers are 3.5kg, of which the impurity Fe content is 0.025%. The Al-20Zr master alloy has a Zr element content of 20.2% and an impurity Fe content of 0.03%.
将镁合金于石墨粘土坩埚中并在电阻坩埚炉中加热熔化。The magnesium alloy was melted in a graphite clay crucible and heated in a resistance crucible furnace.
镁熔体温度750℃，按Zr元素7倍于杂质Fe含量加入Al-20Zr中间合金32g。中间合金熔化后，加入精炼剂并通入氩气进行精炼3分钟，精炼完成后760℃合金熔体通过预热780℃的20ppi 的MgO过滤片浇入石墨模中。The temperature of magnesium melt is 750℃, and 32g of Al-20Zr master alloy is added according to the content of Zr element 7 times that of impurity Fe. After the master alloy was melted, a refining agent was added and argon gas was introduced for refining for 3 minutes. After refining, the alloy melt at 760°C was poured into a graphite mold through a 20ppi MgO filter preheated at 780°C.
化学成分分析经除Fe后的镁合金，其杂质Fe含量0.0023%，残余Zr含量小于0.001%.除Fe后的镁合金中杂质Fe含量达到国家标准GB/T5153-2016《变形镁及镁及镁合金牌号和化学成分》对镁合金AZ31B中杂质Fe含量的要求，其中Zr元素含量小于该牌号规定的其他单个元素的限量。Chemical composition analysis of the magnesium alloy after Fe removal, the impurity Fe content is 0.0023%, and the residual Zr content is less than 0.001%. The impurity Fe content in the magnesium alloy after Fe removal reaches the national standard GB/T5153-2016 "Deformed Magnesium and Magnesium and Magnesium" "Alloy Grade and Chemical Composition" requirements for the content of impurity Fe in magnesium alloy AZ31B, wherein the content of Zr element is less than the limit of other single elements specified by the grade.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the scope of the present invention. within the scope of protection.
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| CN114438357A (en) * | 2022-02-11 | 2022-05-06 | 中原工学院 | Method for Eliminating Segregation of Titanium and Zirconium Elements by Melting and Casting of Aluminum Alloy Welding Wire Ingot |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102517458A (en) * | 2011-12-30 | 2012-06-27 | 中原工学院 | Method for removing Fe impurity in magnesium or magnesium alloys by adopting Mg-Zr intermediate alloy |
| WO2018177168A1 (en) * | 2017-04-01 | 2018-10-04 | 比亚迪股份有限公司 | Magnesium alloy, preparation and moulding methods thereof, and magnesium alloy member |
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| CN102517458A (en) * | 2011-12-30 | 2012-06-27 | 中原工学院 | Method for removing Fe impurity in magnesium or magnesium alloys by adopting Mg-Zr intermediate alloy |
| WO2018177168A1 (en) * | 2017-04-01 | 2018-10-04 | 比亚迪股份有限公司 | Magnesium alloy, preparation and moulding methods thereof, and magnesium alloy member |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114438357A (en) * | 2022-02-11 | 2022-05-06 | 中原工学院 | Method for Eliminating Segregation of Titanium and Zirconium Elements by Melting and Casting of Aluminum Alloy Welding Wire Ingot |
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