CN103820677B - Between the novel compound material containing β-γTiAl metallic Nb-Mn and its preparation method - Google Patents

Between the novel compound material containing β-γTiAl metallic Nb-Mn and its preparation method Download PDF

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CN103820677B
CN103820677B CN 201410090759 CN201410090759A CN103820677B CN 103820677 B CN103820677 B CN 103820677B CN 201410090759 CN201410090759 CN 201410090759 CN 201410090759 A CN201410090759 A CN 201410090759A CN 103820677 B CN103820677 B CN 103820677B
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CN 201410090759
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CN103820677A (en )
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陈子勇
宫子琪
周峰
柴丽华
相志磊
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北京工业大学
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Abstract

一种含Mn高Nb新型β-γTiAl金属间化合物材料及其制备方法,属于金属间化合物材料。 Nb-Mn containing novel β-γTiAl intermetallic compound material and its preparation method, belonging to an intermetallic compound material. 其元素的摩尔百分含量为:43%~45%的Al、5~15%的Nb、不高于1%的Mn和余量的Ti及不可避免的杂质。 Mole percent of its elements is: 43% ~ 45% Al, 5 ~ 15% of Nb, not more than 1% of Ti and unavoidable impurities, and the balance of Mn. 按照组成将原料通过金属压块机进行压块成型,自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层。 The raw material composition according to the briquetting machine by metal clamps, respectively, from bottom to top layers of titanium sponge layer, a high purity aluminum layer, an aluminum alloy layer intermediate niobium, manganese and titanium sponge layer sheet. 将压块放入到水冷铜坩埚真空感应悬浮熔炼炉,抽真空,以20~30kW/min速率将熔炼功率升至160~180kW后停止增加功率,然后在恒定功率下熔炼得熔体,使熔体混合均匀;将熔体浇铸到预热的金属铸型中并将铸型进行离心旋转,并随炉冷却。 The compact water-cooled copper crucible placed in a vacuum induction suspension smelting furnace, evacuated to / min to a rate of 20 ~ 30kW melting power was raised from 160 to 180kW after power stops increasing, and then melted to obtain a melt at a constant power, so that the melt blended uniformly; casting the melt into a preheated metal mold and the mold was centrifuged in rotation, and cooling with the furnace. 本发明得到了组织均匀细小且无明显偏析的高铌TiAl合金。 The present invention has been no segregation and uniform and fine high Nb TiAl Alloy.

Description

一种含Μη高Nb新型β-γΉΑΙ金属间化合物材料及其制备方法 Μη containing β-γΉΑΙ new high-Nb intermetallic compound material and method

技术领域 FIELD

[0001] 本发明涉及一种金属间化合物及其制备工艺,尤其涉及一种含Μη高Nb新型β-Τ TiAl金属间化合物材料及其制备方法,属于金属间化合物材料。 [0001] The present invention relates to an intermetallic compound and its preparation process, in particular new compound material Nb High-β-Τ TiAl metal and its preparation involves containing Μη, belonging to an intermetallic compound material.

背景技术 Background technique

[0002] TiAl金属间化合物具有低密度、良好的高温力学性能和较好的抗高温氧化能力等特点,被认为是二十一世纪最具应用潜力并且有望广泛应用在航空、航天以及汽车等领域的高温结构材料。 [0002] TiAl intermetallic compound has a low density, excellent high temperature mechanical properties and good high temperature oxidation resistance and other characteristics, it is considered the 21st century the most potential applications and is expected to widely used in aviation, aerospace and automotive fields high temperature structural materials. 然而,TiAl金属间化合物室温塑性低和热加工性能差等缺点限制了其广泛应用。 However, the compound TiAl intermetallic low room temperature ductility and the hot workability poor shortcomings have limited its wide application. 数十年来,国内外学者在TiAl金属间化合物的组织与性能方面做了大量的探索与研究。 Exploration and Research on domestic and foreign scholars have done a lot in the microstructure and properties of TiAl intermetallic compound of respect for decades. 结果显示,引入β相是提高TiAl金属间化合物力学性能和热加工性能的重要手段。 The results show that the introduction of a β-phase TiAl intermetallic important means of mechanical properties and hot workability of the compound increases. 而近年来,国内外兴起的高铌TiAl金属间化合物由于其具有良好的综合性能而备受关注。 In recent years, the rise of High-niobium TiAl metal compounds at home and abroad due to its good overall performance and concern. 然而关于含有β相的高铌TiAl金属间化合物材料的制备及Μη在高铌TiAl合金中的物理冶金行为尚未见报道。 However, physical metallurgical behavior of the preparation of compound material disposed between the high metal content of TiAl phase and a β Μη high of TiAl alloy has not been reported.

发明内容 SUMMARY

[0003] 本发明的目的是提供一种通过添加β相稳定元素Μη得到含有β相的组织,进而改善材料性能的含Μη高Nb新型β - γ TiAl金属间化合物材料及制备方法。 [0003] The object of the present invention is to provide a high Μη by adding β Nb-containing element Μη obtain novel β structure containing β-phase, thereby improving the material properties with stable - γ TiAl intermetallic compound between material and preparation method.

[0004] 本发明的一种含Μη高铌新型β - γ TiAl金属间化合物材料,其特征在于,其元素的摩尔百分含量为:43%〜45%的Al、5〜15% (优选8%)的Nb、不高于1%的Μη和余量的Ti及不可避免的杂质。 [0004] the present invention containing niobium high Μη novel β - γ TiAl intermetallic compound between the material, wherein the mole percent of its elements is: 43% ~ 45% of Al, 5~15% (preferably 8 %) of Nb, not more than 1%, and the balance of Μη Ti and inevitable impurities.

[0005] 本发明的含Μη高Nb新型β - γ TiAl金属间化合物的制备方法,通过下述步骤实现的: [0005] the present invention containing high Nb Μη novel β - γ TiAl metal between the preparation of compounds, achieved by the following steps:

[0006] (1)、称取如下原料:海绵钛、高纯铝、铝铌中间合金和电解锰片;其中控制Al、Nb、Μη和Ti元素的摩尔百分含量为43%〜45%的Al、5〜15%的Nb、不高于1%的Μη和余量为Ti及不可避免的杂质; [0006] (1) Weigh the following ingredients: titanium sponge, high-purity aluminum, niobium, aluminum and manganese alloy sheet intermediate; wherein the control Al, Nb, Μη mole percent of Ti and 43% ~ 45% of al, 5~15% of Nb, not more than 1% and a balance Μη Ti and unavoidable impurities;

[0007] (2)、将步骤(1)称得的原料通过金属压块机进行压块成型,压块时自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层; [0007] (2), the step (1), said raw material obtained by briquetting metal briquetting machine, from bottom to top, each layer of titanium sponge layer, a high purity aluminum layer, an aluminum master alloy when compacts niobium layer, manganese and titanium sponge layer sheet;

[0008] (3)将步骤(2)得到的压块放入到可离心浇注的水冷铜坩祸真空感应悬浮熔炼炉中,熔炼前将金属铸型预热至300〜400°C,将水冷铜坩祸真空感应熔炼炉抽真空至1.0〜3.0X10 3mbar,以20〜30kW/min (优选25kW/min)增长速率将水冷铜坩祸真空感应熔炼炉熔炼功率升至160〜180kW后停止增加功率,然后在恒定功率下熔炼200〜250s得熔体,使熔体混合均匀; [0008] (3) The step (2) was put into a compact centrifugal casting may be water-cooled copper crucible vacuum induction disaster suspension smelting furnace before melting the metal mold preheated to 300~400 ° C, water-cooled disaster copper crucible vacuum induction melting furnace was evacuated to 1.0~3.0X10 3mbar, to 20~30kW / min (preferably 25kW / min) water-cooled copper crucible growth rate disaster melting power vacuum induction melting furnace was raised to stop the increase in the power after 160~180kW then melted at a constant power 200~250s obtained melt, the melt mixed;

[0009] (4)将熔体浇铸到预热后的且离心旋转的金属铸型中,离心机转速优选为120r/min,形成含Μη高银TiAl金属间化合物铸锭,并随炉冷却。 [0009] (4) casting the melt into a preheated metal mold and the rotation of the centrifuge, the centrifuge speed is preferably 120r / min, is formed between the high-silver-containing Μη TiAl intermetallic compound ingots, and cooling with the furnace.

[0010] 本发明步骤(1)中海绵钛的质量纯度为99.7%,高纯铝的质量纯度为99.99%,铝铌中间合金的质量纯度为99.8%,电解锰片的质量纯度为99.99% ;各原料为市售产品。 [0010] The present invention Step (1) of titanium sponge mass purity of 99.7% by mass of high purity of 99.99% aluminum, niobium intermediate-purity aluminum alloy mass was 99.8% by mass of a purity of 99.99% manganese sheet; various materials are commercially available products.

[0011] 本发明确定了Μη的最佳加入量范围,在材料凝固过程中,Μη的加入改变了合金的凝固路线,由传统的L — L+β — α —...变为L — L+β — β—...,得到的高铌TiAl金属间化合物材料显微组织非常细小,且无明显偏析出现,形成的β相主要出现在片层晶团晶界处,并呈网状分布。 [0011] The present invention determines the optimum range Μη amount of the material during solidification, the solidification Μη added route change alloy, the conventional L - L + β - α -... becomes L - L + β - β -..., high-niobium TiAl intermetallic compound obtained very fine microstructure of the material, and no segregation occurs, mainly beta] phase formed at the grain boundaries appear colonies sheet, and reticulate . 细小均匀、无明显偏析的组织有利于合金的热加工性,改善合金的 Fine and uniform, without significant segregation tissue facilitate hot workability of the alloy to improve the alloy

生會to Students' Association to

[0012] 本发明得到了均匀细小且无明显偏析的的TiAl合金组织,且采用水冷铜坩祸真空感应悬浮熔炼炉熔炼,工艺过程简单易操作。 [0012] The present invention is to obtain a fine and homogeneous without significant segregation of the TiAl alloy, and the use of water-cooled copper crucible levitation melting furnace disaster vacuum induction melting, the process is easy to operate.

附图说明 BRIEF DESCRIPTION

[0013] 图1实施例1的含Μη高Nb新型β - γ TiAl金属间化合物T1-43Al-8Nb_0.ΙΜη铸态合金光学显微组织图; [0013] FIG 1 of Example 1 containing high Nb Μη novel β - γ TiAl intermetallic compound between T1-43Al-8Nb_0.ΙΜη cast alloy microstructure optical FIG;

[0014] 图2实施例1的含Μη高Nb新型β - γ TiAl金属间化合物T1-43Al-8Nb_0.ΙΜη铸态合金X-射线衍射谱图; [0014] FIG. 2 of Example 1 containing high Nb Μη novel β - γ TiAl intermetallic compound between T1-43Al-8Nb_0.ΙΜη cast alloy X- ray diffraction spectrum;

[0015] 图3实施例1的含Μη高Nb新型β - γ TiAl金属间化合物T1-43Al-8Nb_0.ΙΜη铸态合金扫描电子显微图; [0015] FIG. 3 of Example 1 containing high Nb Μη novel β - γ TiAl intermetallic compound between T1-43Al-8Nb_0.ΙΜη cast alloy scanning electron micrograph;

[0016] 图4实施例2的含Μη高Nb新型β - γ TiAl金属间化合物T1-45Al-8Nb_lMn铸态合金光学显微组织图; [0016] Example 2 FIG. 4 embodiment Μη containing high Nb novel β - γ TiAl intermetallic compound between T1-45Al-8Nb_lMn cast alloy microstructure optical FIG;

[0017] 图5实施例2的含Μη高Nb新型β - γ TiAl金属间化合物T1-45Al-8Nb_lMn铸态合金X-射线衍射谱图; [0017] Example 2 FIG. 5 embodiment Μη containing high Nb novel β - γ TiAl intermetallic compound between T1-45Al-8Nb_lMn cast alloy X- ray diffraction spectrum;

[0018] 图6实施例2的含Μη高Nb新型β - γ TiAl金属间化合物T1-45Al-8Nb_lMn铸态合金扫描电子显微图。 [0018] FIG. 6 of Example 2 containing Nb high Μη novel β - γ TiAl intermetallic compound between T1-45Al-8Nb_lMn cast alloy scanning electron micrograph of FIG.

[0019] 图7实施例3的含Μη高Nb新型β - γ TiAl金属间化合物T1-44Al-8Nb_0.35Mn铸态合金光学显微组织图; [0019] FIG. 7 of Example 3 containing high Nb Μη novel β - γ TiAl intermetallic compound between T1-44Al-8Nb_0.35Mn cast alloy microstructure optical FIG;

[0020] 图8实施例3的含Μη高Nb新型β - γ TiAl金属间化合物T1-44Al-8Nb_0.35Mn铸态合金X-射线衍射谱图; [0020] FIG. 8 of Example 3 containing high Nb Μη novel β - γ TiAl intermetallic compound between T1-44Al-8Nb_0.35Mn cast alloy X- ray diffraction spectrum;

[0021] 图9实施例3的含Μη高Nb新型β - γ TiAl金属间化合物T1-44Al-8Nb_0.35Mn铸态合金扫描电子显微图。 Γ TiAl intermetallic compound between T1-44Al-8Nb_0.35Mn cast alloy scanning electron micrographs - high Nb Μη containing the novel β 3 [0021] Example 9 FIG.

具体实施方式 detailed description

[0022] 下面结合实施例对本发明做进一步说明,但本发明并不限于以下实施例。 [0022] The following embodiments in conjunction with embodiments of the present invention is further illustrated, but the present invention is not limited to the following embodiments.

[0023] 实施例1 [0023] Example 1

[0024] 本实施例的含Μη高Nb新型β _ γ TiAl金属间化合物材料制备通过下述步骤实现:一、称取如下原料:海绵钛、高纯铝、铝铌中间合金和电解锰片,其中Ti48.9at.%、A143at.%、Nb8at.%、Mn0.lat.% ;二、将步骤一称得的原料通过金属压块机进行压块成型,压块时自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层;三、将步骤二得到的压块放入到可离心浇注的水冷铜坩祸真空感应悬浮熔炼炉中,熔炼前将金属铸型预热至320°C,将水冷铜坩祸真空感应熔炼炉抽真空至1.0X10 3mbar ;四、以25kff/min增长速率将水冷铜坩祸真空感应熔炼炉熔炼功率升至180kW后停止增加功率,然后在恒定功率下熔炼200s得熔体,使熔体混合均匀;五、将熔体浇铸到预热后的且离心旋转的金属铸型中,离心机转速优选为120r/min,铸锭尺寸为Φ 50X 180mm,并随炉冷却,得 [0024] The present embodiment Μη containing novel beta] _ of Nb γ TiAl intermetallic compound between the material prepared by the following steps to achieve: a weighed the following materials: titanium sponge, high-purity aluminum, niobium, aluminum and manganese alloy intermediate sheet, which Ti48.9at%, A143at%, Nb8at%, Mn0.lat%;... Second, a step known as a raw material obtained by briquetting metal briquetting machine, from bottom to top, each layer of the compact when titanium sponge layer, a high purity aluminum layer, an aluminum alloy layer intermediate niobium, manganese and titanium sponge layer sheet; III obtained in step two compact centrifugal put into a pourable water-cooled copper crucible vacuum induction disaster suspension smelting furnace in the former, the melting metal mold preheated to 320 ° C, the water-cooled copper crucible disaster vacuum induction melting furnace was evacuated to 1.0X10 3mbar; Fourth, 25kff / min the growth rate of water-cooled copper crucible vacuum induction melting furnace disaster melting power after warming to 180kW power stops increasing, and 200s have a melt melting at constant power, the melt mixed; five, and casting the melt into a metal mold preheated centrifuge rotor, the centrifuge speed is preferably 120r / min, the ingot size Φ 50X 180mm, and furnace cooling to give 到T1-43Al-8Nb-0.ΙΜη化合物铸锭。 To T1-43Al-8Nb-0.ΙΜη compound ingot.

[0025] 米用电火花线切割方法从铸锭上切取15 X 15 X 10mm试样,金相与扫描试样经金相砂纸从180目磨到2000目,再用电解抛光机精抛;X射线衍射试样经水洗砂纸从180目磨到1000目,再用无水乙醇清洗表面;透射样品为0.5mm的薄片,用砂纸磨到40um厚,再采用双喷减薄技术制备。 [0025] The method of rice wire EDM cut from the ingot 15 X 15 X 10mm sample, the scanning metallographic sample metallographic sandpaper from 180 mesh to 2000 mesh grinding, electrolytic polishing machine and then fine polishing; X- ray diffraction sample was washed from the 180 mesh sand paper to 1000 mesh mill, then ethanol washing surface; transmittance of the sample sheet of 0.5mm, grinding with sandpaper to 40um thick, double-jet technique were prepared and then thinned. 利用金相显微镜观察T1-43Al-8Nb-0.ΙΜη的显微组织发现,TiAl合金的组织呈细小的等轴晶组织,见图1 ;利用XRD(X射线衍射仪)进行分析发现,合金中除了%和γ相之外,还有β相出现,见图2;利用扫描电子显微镜和电子探针进行分析发现,白色亮相主要分布在片层晶团晶界处,见图3。 By optical microscope T1-43Al-8Nb-0.ΙΜη microstructure found tissue was TiAl alloy fine equiaxed grains, see Figure 1; the use of XRD (X-ray diffraction) analysis found alloy % and a γ-phase in addition to, β-phase also occurs as shown in Figure 2; use of scanning electron microscopy and electron microprobe analysis found that white appearance mainly at grain boundaries colonies sheet, shown in Figure 3.

[0026] 实施例2 [0026] Example 2

[0027] 本实施方式的含Μη高Nb新型β _ γ TiAl金属间化合物材料制备通过下述步骤实现:一、称取如下原料:海绵钛、高纯铝、铝铌中间合金和电解锰片合金,其中Ti46at.%、A145at.%、Nb8at.%、Mnl.0at.% ;二、将步骤一称得的原料通过金属压块机进行压块成型,压块时自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层;三、将步骤二得到的压块放入到可离心浇注的水冷铜坩祸真空感应悬浮熔炼炉中,熔炼前将金属铸型预热至400°C,将水冷铜坩祸真空感应熔炼炉抽真空至2.8X10 3mbar ;四、以25kff/min增长速率将水冷铜坩祸真空感应熔炼炉熔炼功率升至180kW后停止增加功率,然后在恒定功率下熔炼250s得熔体,使熔体混合均匀;五、将熔体浇铸到预热后的且离心旋转的金属铸型中,离心机转速优选为120r/min,铸锭尺寸为Φ 50X 180mm,并随炉冷 Containing the [0027] embodiment according to the present embodiment of Nb Μη novel beta] _ inter γ TiAl intermetallic compound material prepared by the following steps to achieve: a weighed the following materials: titanium sponge, high-purity aluminum, aluminum alloy and an intermediate niobium, manganese alloy sheet wherein Ti46at%, A145at%, Nb8at%, Mnl.0at%;.... Second, a step known as a raw material obtained by briquetting metal briquetting machine, from bottom to top when the compact layers were titanium sponge layer, a high purity aluminum layer, an aluminum alloy layer intermediate niobium, manganese and titanium sponge layer sheet; Third, the compact obtained in step two can be put into the centrifugal water-cooled copper casting crucible vacuum induction disaster suspension smelting furnace before melting the metal mold preheated to 400 ° C, the water-cooled copper crucible disaster vacuum induction melting furnace was evacuated to 2.8X10 3mbar; Fourth, 25kff / min the growth rate of water-cooled copper crucible vacuum induction melting furnace disaster melting power liters 180kW of power to the rear stops increasing, and 250s have a melt melting at constant power, the melt mixed; five, and casting the melt into a metal mold preheated centrifuge rotor, the centrifuge speed is preferably 120r / min, the ingot size Φ 50X 180mm, and cooling with the furnace ,得到T1-45Al-8Nb-lMn化合物铸锭。 To afford compound T1-45Al-8Nb-lMn ingot.

[0028] 米用电火花线切割方法从铸锭上切取15 X 15 X 10mm试样,金相与扫描试样经金相砂纸从180目磨到2000目,再用电解抛光机精抛;X射线衍射试样经水洗砂纸从140目磨到1000目,再用超声震荡机清洗表面;透射样品为0.5mm的薄片,用砂纸磨到40um厚,再采用双喷减薄技术制备。 [0028] The method of rice wire EDM cut from the ingot 15 X 15 X 10mm sample, the scanning metallographic sample metallographic sandpaper from 180 mesh to 2000 mesh grinding, electrolytic polishing machine and then fine polishing; X- ray diffraction sample was washed with water sandpaper from 140 mesh to 1000 mesh, and then ultrasonic vibration machine cleaning surface; sample transmittance of a sheet 0.5mm, grinding with sandpaper to 40um thick, double-jet technique were prepared and then thinned. 利用金相显微镜观察T1-45Al-8Nb-lMn的显微组织发现,TiAl合金的组织呈细小的等轴晶组织,见图4 ;利用XRD (X射线衍射仪)进行分析发现,合金中除了%和γ相之外,还有β相出现,见图5;利用扫描电子显微镜和电子探针进行分析发现,白色亮相主要分布在片层晶团晶界处并呈网状分布,见图6。 By optical microscope T1-45Al-8Nb-lMn microstructure found tissue was TiAl alloy fine equiaxed grains, see Figure 4; using XRD (X ray diffraction) analysis found,% alloy addition and γ-phase, there are β-phase appears, shown in Figure 5; by scanning electron microscopy and electron microprobe analysis found mainly in white sheet appeared colonies at the grain boundaries and the distribution network was shown in Figure 6.

[0029] 实施例3 [0029] Example 3

[0030] 本实施方式的含Μη高Nb新型β _ γ TiAl金属间化合物材料制备通过下述步骤实现:一、称取如下原料:海绵钛、高纯铝、铝铌中间合金和电解锰片,其中Ti47.65at.%、A144at.%、Nb8at.%、Mn0.35at.% ;二、将步骤一称得的原料通过金属压块机进行压块成型,压块时自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层;三、将步骤二得到的压块放入到可离心浇注的水冷铜坩祸真空感应悬浮熔炼炉中,熔炼前将金属铸型预热至350°C,将水冷铜坩祸真空感应熔炼炉抽真空至1.8X 10 3mbar ;四、以25kff/min增长速率将水冷铜坩祸真空感应熔炼炉熔炼功率升至170kW后停止增加功率,然后在恒定功率下熔炼230s得熔体,使熔体混合均匀;五、将熔体浇铸到预热后的且离心旋转的金属铸型中,离心机转速优选为120r/min,铸锭尺寸为Φ 50X 180mm,并随炉冷却 [0030] The embodiment according to the present embodiment having high Nb Μη novel beta] _ inter γ TiAl intermetallic compound material prepared by the following steps to achieve: a weighed the following materials: titanium sponge, high-purity aluminum, niobium, aluminum and manganese alloy intermediate sheet, which Ti47.65at%, A144at%, Nb8at%, Mn0.35at%;... Second, a step known as a raw material obtained by briquetting metal briquetting machine, from bottom to top, each layer of the compact when titanium sponge layer, a high purity aluminum layer, an aluminum alloy layer intermediate niobium, manganese and titanium sponge layer sheet; III obtained in step two compact centrifugal put into a pourable water-cooled copper crucible vacuum induction disaster suspension smelting furnace in the former, the melting metal mold preheated to 350 ° C, the water-cooled copper crucible disaster vacuum induction melting furnace was evacuated to 1.8X 10 3mbar; Fourth, 25kff / min the growth rate of water-cooled copper crucible vacuum induction melting furnace smelting curse after warming to 170kW power stops increasing power, and 230s have a melt melting at constant power, the melt mixed; five, and casting the melt into a metal mold preheated centrifuge rotor, the centrifuge speed is preferably is 120r / min, the ingot size Φ 50X 180mm, and cooling with the furnace ,得到T1-44Al-8Nb-0.35Mn 化合物铸锭。 To afford compound T1-44Al-8Nb-0.35Mn ingot.

[0031] 采用电火花线切割方法从铸锭上切取15X15X 10mm试样,金相与扫描试样经金相砂纸从180目磨到2000目,再用电解抛光机精抛;X射线衍射试样经水洗砂纸从140目磨到1000目,再用超声震荡机清洗表面;透射样品为0.5mm的薄片,用砂纸磨到40um厚,再采用双喷减薄技术制备。 [0031] The method of using wire EDM cut from the ingot sample 15X15X 10mm, metallographic sample metallographic sandpaper scanning from 180 mesh to 2000 mesh grinding, electrolytic polishing machine and then fine polishing; X-ray diffraction sample washed with water sandpaper from 140 mesh to 1000 mesh, and then ultrasonic vibration machine cleaning surface; sample transmittance of a sheet 0.5mm, grinding with sandpaper to 40um thick, double-jet technique were prepared and then thinned. 利用金相显微镜观察T1-44Al-8Nb-0.35Mn的显微组织发现,TiAl合金的组织呈细小的等轴晶组织,见图7 ;利用XRD(X射线衍射仪)进行分析发现,合金中除了02和γ相之外,还有β相出现,见图8 ;利用扫描电子显微镜和电子探针进行分析发现,白色亮相主要分布在片层晶团晶界处并呈网状分布,见图9。 By optical microscope T1-44Al-8Nb-0.35Mn microstructure found tissue was TiAl alloy fine equiaxed grains, see Figure 7; using XRD (X ray diffraction) analysis found that, in addition to the alloy than 02 and γ-phase, β-phase also occurs as shown in Figure 8; the use of scanning electron microscopy and electron microprobe analysis found mainly in white sheet appeared colonies at the grain boundaries and reticulate, Figure 9 .

[0032] 实施例4 [0032] Example 4

[0033] (1)、称取如下原料:海绵钛、高纯铝、铝铌中间合金和铝钨铌中间合金;其中控制Al、Nb、Mn和Ti元素的摩尔百分含量为43%〜45%的Al、8〜10%的Nb、0.1-1%的Μη和余量的Ti及杂质; [0033] (1), weighed raw materials are as follows: titanium sponge, high-purity aluminum, niobium, aluminum, tungsten, niobium and aluminum master alloy intermediate alloy; wherein the mole percent of control Al, Nb, Mn and Ti elements is 43% ~ 45 % of Al, 8~10% of Nb, Ti and impurities 0.1-1% and the balance Μη;

[0034] (2)、将步骤(1)称得的原料通过金属压块机进行压块成型,压块时自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层; [0034] (2), the step (1), said raw material obtained by briquetting metal briquetting machine, from bottom to top, each layer of titanium sponge layer, a high purity aluminum layer, an aluminum master alloy when compacts niobium layer, manganese and titanium sponge layer sheet;

[0035] (3)将步骤(2)得到的压块放入到可离心浇注的水冷铜坩祸真空感应悬浮熔炼炉中,熔炼前将金属铸型预热至300〜400°C,将水冷铜坩祸真空感应熔炼炉抽真空至1.0〜3.0X10 3mbar,以20〜30kW/min (优选25kW/min)增长速率将水冷铜坩祸真空感应熔炼炉熔炼功率升至160〜180kW后停止增加功率,然后在恒定功率下熔炼200〜250s得熔体,使熔体混合均匀; [0035] (3) The step (2) was put into a compact centrifugal casting may be water-cooled copper crucible vacuum induction disaster suspension smelting furnace before melting the metal mold preheated to 300~400 ° C, water-cooled disaster copper crucible vacuum induction melting furnace was evacuated to 1.0~3.0X10 3mbar, to 20~30kW / min (preferably 25kW / min) water-cooled copper crucible growth rate disaster melting power vacuum induction melting furnace was raised to stop the increase in the power after 160~180kW then melted at a constant power 200~250s obtained melt, the melt mixed;

[0036] (4)将熔体浇铸到预热后的且离心旋转的金属铸型中,离心机转速优选为120r/min,形成含Μη高Nb TiAl金属间化合物铸锭,并随炉冷却。 [0036] (4) casting the melt into a preheated metal mold and the rotation of the centrifuge, the centrifuge speed is preferably 120r / min, is formed between the high Μη containing Nb TiAl ingot metal compound, and cooling with the furnace.

[0037] 采用与实施例1、实施例2和实施例3相同的表征得到的含Μη高铌TiAl金属间化合物材料显微组织细小均匀且无明显偏析,组织中出现了亮白色的β相,主要分布在片层晶团晶界处并呈网状分布。 [0037] as in Example 1, Example 2 and Example 3 containing the same characterization of the obtained niobium Μη High-TiAl intermetallic compound fine and uniform microstructure of the material and no segregation, the tissue appears bright white β-phase embodiment, mainly in the colonies and grain boundaries reticulate sheet.

Claims (7)

  1. 1.一种含Μη高Nb新型β - γ TiAl金属间化合物材料,其特征在于,其元素的摩尔百分含量:43%〜45%的Al、5〜15%的他、不高于1%的Μη和余量的Ti及不可避免的杂质,β相主要出现在片层晶团晶界处,并呈网状分布。 A high-Nb-containing Μη novel β - γ TiAl intermetallic compound between the material, wherein the mole percent of its elements: 43% ~ 45% of Al, 5~15% of He, not more than 1% Μη of Ti and unavoidable impurities and the balance, mainly in beta] phase crystal grain boundaries group sheet, and reticulate.
  2. 2.按照权利要求1的一种含Μη高Nb新型β - γ TiAl金属间化合物材料,其特征在于,Nb的摩尔百分含量8%,Μη的摩尔百分含量不高于1%。 2. A method according to claim 1 containing high Nb Μη novel β - γ TiAl intermetallic compound between the material, wherein the mole percent of Nb 8% Μη mole percent is not more than 1%.
  3. 3.按照权利要求1的一种含Μη高Nb新型β - γ TiAl金属间化合物材料,其特征在于,Nb的摩尔百分含量8%,Μη的摩尔百分含量0.1〜1%。 3. A method according to claim 1 containing high Nb Μη novel β - γ TiAl intermetallic compound between the material, wherein the mole percent of Nb 8%, the mole percent Μη 0.1~1%.
  4. 4.含Μη高Nb新型β - γ TiAl金属间化合物的制备方法,其特征在于,包括下述步骤: (1)、称取如下原料:海绵钛、高纯铝、铝铌中间合金和电解锰片;其中控制Al、Nb、Mn和Ti元素的摩尔百分含量为43 %〜45 %的A1、5〜15 %的Nb、不高于1 %的Μη和余量的Ti及杂质; (2)、将步骤(1)称得的原料通过金属压块机进行压块成型,压块时自下而上各层分别为海绵钛层、高纯铝层、铝铌中间合金层、电解锰片层和海绵钛层; (3)、将步骤(2)得到的压块放入到可离心浇注的水冷铜坩祸真空感应悬浮熔炼炉中,熔炼前将金属铸型预热至300〜400°C,将水冷铜坩祸真空感应熔炼炉抽真空至1.0〜.3.0X10 3mbar,以20〜30kW/min增长速率将水冷铜坩祸真空感应熔炼炉熔炼功率升至.160〜180kW后停止增加功率,然后在恒定功率下熔炼200〜250s得熔体,使熔体混合均匀; (4)、将熔体浇铸到预热后的且离 4. High Nb containing Μη novel β - γ TiAl metal between the preparation of compounds, wherein, comprising the steps of: (1) Weigh the following ingredients: titanium sponge, high-purity aluminum, aluminum alloys and manganese niobium intermediate sheet; wherein the control Al, mole percent of Nb, Mn and Ti elements is 43% ~ 45% of A1,5~15% of Nb, not more than 1% of Ti and impurities and the balance Μη; (2 ), the (1), said material obtained in step by briquetting metal briquetting machine, from bottom to top, each layer of titanium sponge layer, a high purity aluminum layer, an aluminum alloy layer intermediate niobium, manganese sheet when briquetting sponge layer and titanium layer; obtained in (3), the step (2) may be placed in a compact water-cooled copper crucible centrifugal casting vacuum induction disaster suspension smelting furnace before melting the metal mold preheated to 300~400 ° C, the water-cooled copper crucible disaster vacuum induction melting furnace was evacuated to 1.0~.3.0X10 3mbar, to 20~30kW / min the growth rate of water-cooled copper crucible vacuum induction melting furnace disaster melting power was raised to stop the increase in the power after .160~180kW then melting 200~250s constant power obtained melt, the melt is mixed; after (4), and casting the melt into a preheated from 旋转的金属铸型中,形成含Μη高铌TiAl金属间化合物铸锭,并随炉冷却。 Rotation of the metal mold, is formed between the high Μη containing niobium ingots TiAl intermetallic compound, and cooling with the furnace.
  5. 5.按照权利要求4的方法,其特征在于,以25kW/min增长速率将水冷铜坩祸真空感应悬浮熔炼炉熔炼功率升至160〜180kW且进行离心浇注成型。 The method according to claim 4, characterized in that, in order to 25kW / min The growth rate of water-cooled copper crucible disaster vacuum induction melting power raised to a suspension smelting furnace and subjected to centrifugal casting molding 160~180kW.
  6. 6.按照权利要求4的方法,其特征在于,离心机转速优选为120r/min。 6. The method according to claim 4, characterized in that the rotational speed of the centrifuge preferably is 120r / min.
  7. 7.按照权利要求4的方法,其特征在于,(1)中海绵钛的质量纯度为99.7 %,高纯铝的质量纯度为99.99%,铝铌中间合金的质量纯度为99.8%,电解锰片的质量纯度为.99.99%。 7. A method according to claim 4, characterized in that (1) the quality of purity titanium sponge was 99.7% by mass of high purity aluminum of 99.99% by mass of niobium intermediate-purity aluminum alloy is 99.8%, manganese sheet mass .99.99% purity.
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CN101457314A (en) * 2007-12-13 2009-06-17 Gkss-盖斯特哈赫特研究中心有限责任公司 Titanium aluminide alloys
CN103074520A (en) * 2013-01-14 2013-05-01 北京工业大学 Er-containing high-niobium Ti-Al intermetallic compound material and preparation method thereof
CN103409660A (en) * 2013-08-12 2013-11-27 南京理工大学 Novel Beta/Gamma-TiAl alloy with ultra-fine grain

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EP0519849A2 (en) * 1991-06-18 1992-12-23 Howmet Corporation Cr-bearing gamma titanium aluminides and method of making same
CN101457314A (en) * 2007-12-13 2009-06-17 Gkss-盖斯特哈赫特研究中心有限责任公司 Titanium aluminide alloys
CN103074520A (en) * 2013-01-14 2013-05-01 北京工业大学 Er-containing high-niobium Ti-Al intermetallic compound material and preparation method thereof
CN103409660A (en) * 2013-08-12 2013-11-27 南京理工大学 Novel Beta/Gamma-TiAl alloy with ultra-fine grain

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