镁基块体非晶的制备及其碳纳米管复合材料的增韧研究
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摘要
镁基非晶态合金因具有轻质、高强度、高弹性极限、低价格等优点而受到关注,拥有广阔的发展潜力和应用前景。其中,Mg-Ni基非晶态合金相比于其它镁基非晶材料更是具有优异的力学性能、高储氢量和高耐蚀性能等优点。目前Mg-Ni基块体非晶有两个主要缺点阻碍了其发展和应用:①Mg-Ni基合金系非晶形成能力较低,目前研究发现的最大非晶尺寸仅为直径3mm;②塑韧性差,断裂形式表现为显著的脆性断裂,一般压缩实验中的形变位移最大为1%左右。本工作以Mg-Ni-Gd三元合金系为基础,通过改变合金成分配比,在合金系中添加新组元等方式得到一系列非晶形成能力良好的合金成分;另一方面,以碳纳米管作为外加第二相,以期提高韧性,改善Mg-Ni非晶基体的断裂性能。考虑到碳纳米管的添加对非晶形成能力可能造成的负面影响,制备得到非晶形成能力良好的合金成分是研究碳纳米管增韧机制的基础。实验得到的主要结果如下:
(1)Gd元素含量在Mg-Ni-Gd三元合金系中对于非晶形成能力有显著的影响,Gd原子个数含量取_(10)at.%对于合金系的非晶形成能力有最佳优化作用;通过改变原子个数配比,发现Mg-Ni-Gd合金系中具最佳非晶形成能力的成分点Mg_(75)Ni_(15)Gd_(10),非晶临界尺寸3mm。通过晶态峰识别发现对Mg-Ni-Gd三元系非晶形成能力影响较大的强势晶态相GdNi_3。
(2)Ag部分替代Mg_(75)Ni_(15)Gd_(10)合金中Mg元素对非晶形成能力有显著的影响,替代得到的四元合金成分Mg_(69)Ni_(15)Gd_(10)Ag_6,临界非晶尺寸为直径6mm。用伪三元相图成分定位的方法得到一批非晶形成能力优良的成分点,其中有五个成分点可达临界尺寸6mm,分别为Mg_(70)Ni_(14.3)Gd_(10)Ag_(5.7)、Mg_(69)Ni_(15)Gd_(10)Ag_6、Mg_(68)Ni_(15.7)Gd_(10)Ag_(6.3)、Mg_(64)Ni_(18.6)Gd_(10)Ag_(7.4)和Mg_(63)Ni_(19.3)Gd_(10)Ag_(7.7)。通过稀土元素掺杂法,得到了具有优良非晶形成能力的五元成分Mg_(69)Ni_(15)Ag_6Gd_7Pr_3,临界非晶形成尺寸为直径8mm,为目前所知最大尺寸的Mg-Ni基非晶合金。
(3)球磨工艺可以改善碳纳米管的团聚问题,但部分碳纳米管会在球磨处理过程中被打断而变短。CNTs-Mg_(69)Ni_(15)Ag_6Gd_7Pr_3块体非晶复合材料的压缩应力和形变位移随碳纳米管体积含量的增大而提高,当含量为2vt.%时均达到最高值,分别为925MPa和2.26%,比之不添加碳纳米管时分别提高198MPa和0.74%,观察断口形貌,发现复合材料基体中出现一定规模的表征非晶韧性的脉络状花纹。
Mg-based amorphous alloy with the vast development potential and prospects for the advantages of a lightweight, high strength, high elastic limit and low price. Compared to other Mg-based amorphous material, Mg-Ni based amorphous alloy have excellent mechanical properties, high hydrogen storage capacity and high corrosion resistance and so on. Presently, Mg-Ni-based bulk metallic glass has two major drawbacks which hinder their development and application:①Mg-Ni based alloy have lower GFA, the current study found that the largest diameter of the amorphous size is only 3mm.②Poor toughness. The fracture is a significant form of brittle fracture,the general displacement of compression experiment in a maximum of 1%. The work is based on the Mg-Ni-Gd ternary alloy system, hope that get a group of good GFA of alloy composition by changing the alloy composition ratio. On the other hand, take carbon nanotubes as a second phase to improving the toughness and the the Mg-Ni amorphous matrix fracture properties. Taking into account the addition of carbon nanotubes have the possible negative effects on the glass forming ability, good glass forming ability of the alloy composition is the basis of toughening mechanisms of carbon nanotubes. The main results obtained from the experiment are as follows:
(1)Gd content have significant impact on the Mg-Ni-Gd ternary alloys glass forming ability, _(10)at.% of Gd in the formation of amorphous alloys have the best ability to optimize the GFA; by changing the ratio of atomic number,we could found that the Mg-Ni-Gd alloy system have the best glass forming ability in the composition of point Mg_(75)Ni_(15)Gd_(10), whose amorphous critical size of 3mm. The other way, the strong crystalline phase GdNi_3 have a significant effect on the GFA of Mg-Ni-Gd ternary system.
(2)Ag partial substitution Mg in the Mg_(75)Ni_(15)Gd_(10) alloy have a significant impact on the glass forming ability, the best alternative to alloy composition is Mg_(69)Ni_(15)Gd_(10)Ag_6, with the critical diameter of the amorphous size 6mm. By positioning components in the Pseudo ternary phase diagram, have obtained an excellent group of glass forming ability components. Five component points have the critical size of diameter 6mm, respectively Mg_(70)Ni_(14.3)Gd_(10)Ag_(5.7), Mg_(69)Ni_(15)Gd_(10)Ag_6, Mg_(68)Ni_(15.7)Gd_(10)Ag_(6.3), Mg_(64)Ni_(18.6)G-d_(10)Ag_(7.4), and Mg_(63)Ni_(19.3)Gd_(10)Ag_(7.7)。By the rare earth doped method, have obtained the five-component Mg_(69)Ni_(15)Ag_6Gd_7Pr_3, which with excellent glass forming ability of critical diameter of glass forming size 8mm. It’s the maximum size of the amorphous Mg-Ni based alloys as far as we know.
(3)Milling process can release the agglomeration of carbon nanotubes, in the milling progress, part of carbon nanotubes will be interrupted and short. The compressive stress and strain displacement of CNTs-Mg_(69)Ni_(15)Ag_6Gd_7Pr_3 bulk amorphous composites will improve with the increase of volume content of carbon.The volume fraction of 2% reached the highest value of respectively 925MPa and 2.26%. It’s 198MPa and 0.74% increased than haven't add Carbon nanotubes. The pattern of the context increased significantly in the amorphous matrix which is the characterization of toughness in the composite materials by observation of fracture morphology.
(1)Gd元素含量在Mg-Ni-Gd三元合金系中对于非晶形成能力有显著的影响,Gd原子个数含量取_(10)at.%对于合金系的非晶形成能力有最佳优化作用;通过改变原子个数配比,发现Mg-Ni-Gd合金系中具最佳非晶形成能力的成分点Mg_(75)Ni_(15)Gd_(10),非晶临界尺寸3mm。通过晶态峰识别发现对Mg-Ni-Gd三元系非晶形成能力影响较大的强势晶态相GdNi_3。
(2)Ag部分替代Mg_(75)Ni_(15)Gd_(10)合金中Mg元素对非晶形成能力有显著的影响,替代得到的四元合金成分Mg_(69)Ni_(15)Gd_(10)Ag_6,临界非晶尺寸为直径6mm。用伪三元相图成分定位的方法得到一批非晶形成能力优良的成分点,其中有五个成分点可达临界尺寸6mm,分别为Mg_(70)Ni_(14.3)Gd_(10)Ag_(5.7)、Mg_(69)Ni_(15)Gd_(10)Ag_6、Mg_(68)Ni_(15.7)Gd_(10)Ag_(6.3)、Mg_(64)Ni_(18.6)Gd_(10)Ag_(7.4)和Mg_(63)Ni_(19.3)Gd_(10)Ag_(7.7)。通过稀土元素掺杂法,得到了具有优良非晶形成能力的五元成分Mg_(69)Ni_(15)Ag_6Gd_7Pr_3,临界非晶形成尺寸为直径8mm,为目前所知最大尺寸的Mg-Ni基非晶合金。
(3)球磨工艺可以改善碳纳米管的团聚问题,但部分碳纳米管会在球磨处理过程中被打断而变短。CNTs-Mg_(69)Ni_(15)Ag_6Gd_7Pr_3块体非晶复合材料的压缩应力和形变位移随碳纳米管体积含量的增大而提高,当含量为2vt.%时均达到最高值,分别为925MPa和2.26%,比之不添加碳纳米管时分别提高198MPa和0.74%,观察断口形貌,发现复合材料基体中出现一定规模的表征非晶韧性的脉络状花纹。
Mg-based amorphous alloy with the vast development potential and prospects for the advantages of a lightweight, high strength, high elastic limit and low price. Compared to other Mg-based amorphous material, Mg-Ni based amorphous alloy have excellent mechanical properties, high hydrogen storage capacity and high corrosion resistance and so on. Presently, Mg-Ni-based bulk metallic glass has two major drawbacks which hinder their development and application:①Mg-Ni based alloy have lower GFA, the current study found that the largest diameter of the amorphous size is only 3mm.②Poor toughness. The fracture is a significant form of brittle fracture,the general displacement of compression experiment in a maximum of 1%. The work is based on the Mg-Ni-Gd ternary alloy system, hope that get a group of good GFA of alloy composition by changing the alloy composition ratio. On the other hand, take carbon nanotubes as a second phase to improving the toughness and the the Mg-Ni amorphous matrix fracture properties. Taking into account the addition of carbon nanotubes have the possible negative effects on the glass forming ability, good glass forming ability of the alloy composition is the basis of toughening mechanisms of carbon nanotubes. The main results obtained from the experiment are as follows:
(1)Gd content have significant impact on the Mg-Ni-Gd ternary alloys glass forming ability, _(10)at.% of Gd in the formation of amorphous alloys have the best ability to optimize the GFA; by changing the ratio of atomic number,we could found that the Mg-Ni-Gd alloy system have the best glass forming ability in the composition of point Mg_(75)Ni_(15)Gd_(10), whose amorphous critical size of 3mm. The other way, the strong crystalline phase GdNi_3 have a significant effect on the GFA of Mg-Ni-Gd ternary system.
(2)Ag partial substitution Mg in the Mg_(75)Ni_(15)Gd_(10) alloy have a significant impact on the glass forming ability, the best alternative to alloy composition is Mg_(69)Ni_(15)Gd_(10)Ag_6, with the critical diameter of the amorphous size 6mm. By positioning components in the Pseudo ternary phase diagram, have obtained an excellent group of glass forming ability components. Five component points have the critical size of diameter 6mm, respectively Mg_(70)Ni_(14.3)Gd_(10)Ag_(5.7), Mg_(69)Ni_(15)Gd_(10)Ag_6, Mg_(68)Ni_(15.7)Gd_(10)Ag_(6.3), Mg_(64)Ni_(18.6)G-d_(10)Ag_(7.4), and Mg_(63)Ni_(19.3)Gd_(10)Ag_(7.7)。By the rare earth doped method, have obtained the five-component Mg_(69)Ni_(15)Ag_6Gd_7Pr_3, which with excellent glass forming ability of critical diameter of glass forming size 8mm. It’s the maximum size of the amorphous Mg-Ni based alloys as far as we know.
(3)Milling process can release the agglomeration of carbon nanotubes, in the milling progress, part of carbon nanotubes will be interrupted and short. The compressive stress and strain displacement of CNTs-Mg_(69)Ni_(15)Ag_6Gd_7Pr_3 bulk amorphous composites will improve with the increase of volume content of carbon.The volume fraction of 2% reached the highest value of respectively 925MPa and 2.26%. It’s 198MPa and 0.74% increased than haven't add Carbon nanotubes. The pattern of the context increased significantly in the amorphous matrix which is the characterization of toughness in the composite materials by observation of fracture morphology.
引文
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[2] Brenner A, Couch D E. Deposition of nickel and cobalt by chemical reduction[J]. J. Res. Nat. Bur. Stand., 1947, 37: 385-395
[3] Brenner A, Couch D E. Electrodeposition of alloys of phosphorus with nickel or cobalt[J]. J. Res. Nat. Bur. Stand., 1950, 44: 109-119
[4] Turnbull D. Kinetics of solidification of supercooled liquid mercury droplets[J]. J. Chem. Phys., 1952, 20: 411-424
[5] Klements W, Willens R H, Duwez P. Non-crystalline structure in solidified gold-silicon alloys[J]. Nature, 1960, 187: 869-870
[6]卢博斯基F E.非晶态金属合金[M].(柯成,唐于堪,罗阳,译者).北京:冶金工业出版社,1989
[7]王一禾,杨膺善.非晶态合金[M],北京:冶金工业出版社,1985
[8] Inoue A, Zhang T, Masumoto T. Al-La-Ni amorphous alloys with a wide supercooled liquid region[J]. Materials Transactions JIM, 1989, 30(12): 965-972
[9] Inoue A, Kita K, Zhang T. An amorphous La_(55)Al_(25)Ni_(20) alloy prepared by water quenching[J]. Tran. JIM, 1989, 30(9): 722-972
[10] Inoue A, Yamaguchi H, Zhang T. Al-La-Cu amorphous alloys with a wide supercooled lisuid region[J]. Mater. Trans. JIM, 1990, 31(2): 104-109
[11] Inoue A, Kohinata M, Masumoto T, et al. Mg-Ni-La amorphous alloys with a wide supercooled liquid region[J]. Materials Transactions JIM, 1989, 30(5): 378-381.
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