技术领域technical field
本发明涉及一种涂层导体用高强度立方织构镍基合金基带及其制备方法，属于高温超导涂层导体金属基带技术领域。The invention relates to a high-strength cubic-textured nickel-based alloy substrate for coated conductors and a preparation method thereof, belonging to the technical field of high-temperature superconducting coated conductor metal substrates.
背景技术Background technique
在采用轧制辅助双轴织构技术(RABiTS)制备二代高温超导涂层YBa2Cu3O7-x(YBCO)导线工艺中，作为超导涂层载体的金属基带对超导涂层的质量和最终获得的超导线的导电性能有显著的影响。金属基带的织构会影响外延生长的涂层的晶粒取向，导致超导层临界电流密度的变化；而金属基带的力学性能，尤其是屈服强度，会影响涂层制备工艺选择以及由此造成的涂层与基带结合强度的变化。因此，探索和开发既具有集中的立方织构、又具有合适屈服强度的金属基带，一直是RABiTS技术中的重要内容之一。In the process of preparing second-generation high-temperature superconducting coated YBa2 Cu3 O7-x (YBCO) wires using rolling-assisted biaxial texturing technology (RABiTS), the metal substrate as the carrier of the superconducting coating is opposed to the superconducting coating have a significant impact on the quality of the superconducting wire and the conductivity of the resulting superconducting wire. The texture of the metal substrate will affect the grain orientation of the epitaxially grown coating, resulting in a change in the critical current density of the superconducting layer; while the mechanical properties of the metal substrate, especially the yield strength, will affect the choice of coating preparation process and the resulting Changes in the bonding strength of the coating to the substrate. Therefore, exploring and developing metal substrates with both concentrated cubic texture and suitable yield strength has always been one of the important contents in RABiTS technology.
纯镍是最早应用RABiTS技术制备二代高温超导涂层导线的基带材料。其经过轧制和再结晶退火后很容易形成集中的立方织构，能够较好的匹配YBCO晶格，且具有较好的抗氧化性，但也存在不可忽视的本征缺陷，如力学性能较差(屈服强度59MPa)，常温下呈现铁磁性，在沉积过渡层和超导层的工艺温度下理化性质不稳定等。为了弥补纯镍的这种缺陷，合金化技术被广泛的应用。在纯镍中添加合金元素后一方面可以降低居里温度，另一方面通过固溶强化，大大提高了合金的强度，但合金元素的添加也会降低合金的层错能，致使塑性变形机制由原来的交滑移转变为剪切带变形或孪生变形，最终影响立方织构的生成。Pure nickel is the baseband material for the first application of RABiTS technology to prepare second-generation high-temperature superconducting coated wires. After rolling and recrystallization annealing, it is easy to form a concentrated cubic texture, which can better match the YBCO lattice and has good oxidation resistance, but there are also intrinsic defects that cannot be ignored, such as poor mechanical properties. Poor (yield strength 59MPa), exhibits ferromagnetism at room temperature, unstable physical and chemical properties at the process temperature of depositing transition layer and superconducting layer, etc. In order to make up for this defect of pure nickel, alloying technology is widely used. Adding alloying elements to pure nickel can lower the Curie temperature on the one hand, and on the other hand greatly improve the strength of the alloy through solid solution strengthening, but the addition of alloying elements will also reduce the stacking fault energy of the alloy, resulting in the plastic deformation mechanism by The original cross-slip transforms into shear band deformation or twin deformation, which finally affects the generation of cubic texture.
目前研究最多、应用最广泛的是镍钨合金基带，其中Ni-5at.％W基带已经进入商业化生产。研究表明，分别添加2，3，5，7，9at.％W后其屈服强度由127MPa增加至270MPa，然而添加7～9.5at.％W降低了合金的层错能，致使退火后的合金基带的立方织构份额仅45％左右(取向差≤15°)，难以达到98％以上。除此之外，研究人员对添加Cr、Mo、V等能够显著降低磁性能的合金元素也进行了大量的研究。研究发现，在纯镍中添加13at.％Cr或9at.％V同样可以在液氮温区得到无磁性的立方织构基带，然而，合金中高含量的铬和钒在沉积缓冲层的温度下极易氧化，会影响后续过渡层和超导层的外延生长和立方织构的形成。添加5at.％Mo在退火后更容易得到旋转立方取向，大大降低了立方取向的集中度。对三元合金如Ni-Cr-W和Ni-Cr-V的研究结果也表明，在纯镍中加入合金元素后抗氧化性和立方织构的集中度都不同程度下降。因此，制备高强度，高立方织构且低磁或无磁的合金基带仍是目前超导领域亟需解决的问题。At present, the most researched and most widely used is the nickel-tungsten alloy baseband, and the Ni-5at.%W baseband has entered commercial production. Studies have shown that the yield strength of the alloy increases from 127MPa to 270MPa after adding 2, 3, 5, 7, and 9 at.% W respectively, but the addition of 7-9.5 at.% W reduces the stacking fault energy of the alloy, resulting in the alloy matrix after annealing The proportion of cubic texture in the glass is only about 45% (orientation difference ≤ 15°), and it is difficult to reach more than 98%. In addition, researchers have also conducted a lot of research on the addition of Cr, Mo, V and other alloying elements that can significantly reduce the magnetic properties. The study found that adding 13at.%Cr or 9at.%V to pure nickel can also obtain a non-magnetic cubic texture baseband in the liquid nitrogen temperature zone. It is easy to oxidize, which will affect the epitaxial growth and cubic texture formation of the subsequent transition layer and superconducting layer. Adding 5 at.% Mo makes it easier to obtain spin-cubic orientation after annealing, which greatly reduces the concentration of cubic orientation. The research results on ternary alloys such as Ni-Cr-W and Ni-Cr-V also show that the oxidation resistance and the concentration of cubic texture are reduced to varying degrees after adding alloying elements to pure nickel. Therefore, the preparation of high-strength, high-cubic-textured and low-magnetic or non-magnetic alloy substrates is still an urgent problem in the field of superconductivity.
本发明在纯镍中添加多种合金元素，晶粒得到细化，在保证织构集中度的前提下，大大提高了合金基带的屈服强度，同时一定程度上降低了合金的磁性能。The invention adds various alloy elements to pure nickel to refine the crystal grains, greatly improves the yield strength of the alloy base band and reduces the magnetic properties of the alloy to a certain extent under the premise of ensuring the concentration of the texture.
发明内容Contents of the invention
针对现有技术存在的缺陷，本发明的目的是提出一种涂层导体用高强度立方织构镍基合金基带及其制备方法。通过添加多种合金元素、冶炼、以及形变与再结晶，获得了具有高屈服强度、高立方织构且抗氧化性良好的合金基带。In view of the defects existing in the prior art, the object of the present invention is to provide a high-strength cubic texture nickel-based alloy substrate for coated conductors and a preparation method thereof. Through adding various alloying elements, smelting, deformation and recrystallization, an alloy substrate with high yield strength, high cubic texture and good oxidation resistance is obtained.
为达到上述目的，本发明采用如下技术方案：To achieve the above object, the present invention adopts the following technical solutions:
一种涂层导体用高强度立方织构镍基合金基带，其组分及质量百分比为：Ni 73.9～85.4wt.％，Cr 7.8～12.5wt.％，Co 0.2～1wt.％，Mo 2～8wt.％，Fe 3wt.％，Cu1.6wt.％。A high-strength cubic-textured nickel-based alloy substrate for a coated conductor, the components and mass percentages of which are: Ni 73.9-85.4wt.%, Cr 7.8-12.5wt.%, Co 0.2-1wt.%, Mo 2- 8wt.%, Fe 3wt.%, Cu1.6wt.%.
一种涂层导体用高强度立方织构镍基合金基带的制备方法，具有以下的工艺过程和步骤：A method for preparing a high-strength cubic-textured nickel-based alloy substrate for a coated conductor has the following process and steps:
(a)合金冶炼和锻造(a) Alloy smelting and forging
将纯度均为99.95％以上的Ni、Cr、Co、Mo、Fe和Cu按照上述成分配比进行称重配料，将六种原材料置于真空感应熔炼炉中冶炼，获得镍基合金初始坯锭；将坯锭在1050℃下均匀化处理20h，然后热锻成(40～45)mm×(10～20)mm×(10～20)mm的锻件；Ni, Cr, Co, Mo, Fe and Cu with a purity of more than 99.95% are weighed and batched according to the above composition ratio, and the six raw materials are smelted in a vacuum induction melting furnace to obtain an initial nickel-based alloy ingot; Homogenize the ingot at 1050°C for 20 hours, and then hot forge it into a forging of (40-45)mm×(10-20)mm×(10-20)mm;
(b)锻件热轧和冷轧(b) Hot rolling and cold rolling of forgings
将锻件随炉升温至1100℃并保温30min后热轧，道次压下量为3～10％，总压下量为30～50％；热轧板经过1050℃中间退火和酸洗处理后，进行道次压下量不大于10％、总压下量98％以上的冷轧，最终获得厚度为80μm的合金基带；The forging is heated up to 1100°C with the furnace and held for 30 minutes, and then hot-rolled. The pass reduction is 3-10%, and the total reduction is 30-50%. Carry out cold rolling with a reduction of no more than 10% in each pass and a total reduction of more than 98%, and finally obtain an alloy base strip with a thickness of 80 μm;
(c)冷轧基带的再结晶退火(c) Recrystallization annealing of cold-rolled base strip
在真空条件下，以5～15℃/min的升温速率将冷轧基带升温至950～1050℃，保温120min；或以5～15℃/min的升温速率升温至750℃时保温30min，然后再以相同的升温速率升温至950～1050℃并保温120min。Under vacuum conditions, raise the temperature of the cold-rolled base strip to 950-1050°C at a heating rate of 5-15°C/min, and keep it for 120 minutes; Raise the temperature to 950-1050°C at the same heating rate and keep it warm for 120min.
与现有技术相比，本发明具有如下突出的实质性特点和显著的进步：Compared with the prior art, the present invention has the following outstanding substantive features and remarkable progress:
本发明在纯镍中添加多种合金元素，在保证织构质量的前提下降低了磁性能，同时大大提高了合金的力学性能；与纯镍及二元和三元镍基合金相比，本发明的六元镍基合金基带通过固溶强化作用不仅提高了合金的力学性能，细化了晶粒，并且易于得到集中的立方织构。通过本发明得到的镍基合金基带更能满足制备高温超导涂层导体的实际需要。The invention adds various alloying elements to pure nickel, reduces the magnetic properties under the premise of ensuring the texture quality, and at the same time greatly improves the mechanical properties of the alloy; compared with pure nickel and binary and ternary nickel-based alloys, the present invention The inventive six-element nickel-based alloy base strip not only improves the mechanical properties of the alloy through solid solution strengthening, but also refines the grains, and is easy to obtain a concentrated cubic texture. The nickel-based alloy base strip obtained by the invention can better meet the actual needs of preparing high-temperature superconducting coated conductors.
附图说明Description of drawings
图1为实施例1中不同升温速率下的X射线衍射图。Fig. 1 is the X-ray diffraction diagram under different heating rates in Example 1.
图2为实施例1中合金基带退火后(111)极图。FIG. 2 is the (111) pole figure of the alloy substrate in Example 1 after annealing.
图3为实施例2中合金基带退火后(111)极图。Fig. 3 is the (111) pole figure of the alloy substrate in Example 2 after annealing.
图4为实施例3中合金基带退火后(111)极图。Figure 4 is the (111) pole figure of the alloy substrate in Example 3 after annealing.
图5为实施例1，2，3中合金基带在1050℃退火后的得到的应力应变曲线。Fig. 5 is the stress-strain curve obtained after annealing at 1050° C. for the alloy base strips in Examples 1, 2, and 3.
具体实施方式detailed description
实施例1Example 1
将纯度均为99.95％以上的Ni、Cr、Co、Mo、Fe、Cu按照73.9％、12.5％、1％、8％、3％及1.6％的重量百分比进行配料，配料经过真空感应熔炼炉充分冶炼后，获得初始坯锭；将坯锭在1050℃下均匀化处理20h，使合金化学成分更加均匀，然后将坯锭热锻成尺寸为45×15×13mm的锻件；将锻件随炉升温至1100℃保温30min后进行热轧，道次压下量约为10％，最后得到厚度为4.88mm的热轧板。将热轧板在1050℃退火处理和酸洗后，进行道次压下量为3～10％、总压下量为98.4％的冷轧，获得厚度为80μm的合金基带。将冷轧基带用丙酮超声清洗除油后在真空环境下进行退火，退火工艺为以15℃/min的升温速率升至1050℃保温120min，最终得到立方织构基带。该合金基带的X射线衍射分析结果见图1，该合金基带的(111)极图示于图2，立方织构集中度：面外和面内FWHM分别为Dω＝6.0°和体积分数为82％，该合金的应力应变曲线如图5所示，屈服强度为92MPa。说明此合金可以获得较高强度和高集中度的立方织构。Ni, Cr, Co, Mo, Fe, Cu with a purity of more than 99.95% are batched according to the weight percentage of 73.9%, 12.5%, 1%, 8%, 3% and 1.6%. After smelting, the initial ingot is obtained; the ingot is homogenized at 1050°C for 20 hours to make the chemical composition of the alloy more uniform, and then the ingot is hot forged into a forging with a size of 45×15×13mm; the forging is heated up with the furnace to After heat preservation at 1100°C for 30 minutes, hot rolling is carried out, and the reduction in each pass is about 10%, and finally a hot-rolled sheet with a thickness of 4.88mm is obtained. After the hot-rolled sheet is annealed and pickled at 1050°C, it is cold-rolled with a pass reduction of 3-10% and a total reduction of 98.4%, to obtain an alloy base strip with a thickness of 80 μm. The cold-rolled base strip was cleaned and degreased by ultrasonic cleaning with acetone, and then annealed in a vacuum environment. The annealing process was to increase the temperature at a rate of 15 °C/min to 1050 °C for 120 min, and finally obtain a cubic texture base band. The X-ray diffraction analysis results of the alloy baseband are shown in Figure 1, and the (111) pole diagram of the alloy baseband is shown in Figure 2. The cubic texture concentration: out-of-plane and in-plane FWHM are Dω=6.0° and The volume fraction is 82%, the stress-strain curve of the alloy is shown in Figure 5, and the yield strength is 92MPa. It shows that this alloy can obtain high strength and high concentration of cubic texture.
实施例2Example 2
将纯度均为99.95％以上的Ni、Cr、Co、Mo、Fe、Cu按照79.9％、11％、0.5％、4％、3％及1.6％的重量百分比进行配料，配料经过真空感应熔炼炉充分冶炼后，获得初始坯锭；将坯锭在1050℃下均匀化处理20h，使合金化学成分更加均匀，然后将坯锭热锻成尺寸为43×16×14mm的锻件；将锻件随炉升温至1100℃保温30min后进行热轧，道次压下量约为10％，最后得到厚度为4.82mm的热轧板。将热轧板在1050℃退火处理和酸洗后，进行道次压下量为3～10％、总压下量为98.3％的冷轧，获得厚度为80μm的合金基带。将冷轧基带用丙酮超声清洗除油后在真空环境下进行退火，退火工艺为10℃/min的升温速率升至750℃保温30min然后再以10℃/min的升温速率升至1000℃保温120min，最终得到立方织构基带。该合金基带的(111)极图示于图3，立方织构集中度：面外和面内FWHM分别为Dω＝6.2°和体积分数为98％，该合金的应力应变曲线如图5所示，屈服强度为140MPa。说明此合金可以获得高强度高集中度的立方织构。Ni, Cr, Co, Mo, Fe, Cu with a purity of more than 99.95% are batched according to the weight percentage of 79.9%, 11%, 0.5%, 4%, 3% and 1.6%, and the batching is fully processed through the vacuum induction melting furnace After smelting, the initial ingot is obtained; the ingot is homogenized at 1050°C for 20 hours to make the chemical composition of the alloy more uniform, and then the ingot is hot forged into a forging with a size of 43×16×14mm; the forging is heated up with the furnace to After heat preservation at 1100°C for 30 minutes, hot rolling is carried out, and the reduction in each pass is about 10%, and finally a hot-rolled sheet with a thickness of 4.82mm is obtained. After the hot-rolled sheet is annealed and pickled at 1050°C, it is cold-rolled with a reduction of 3-10% in each pass and a total reduction of 98.3%, to obtain an alloy base strip with a thickness of 80 μm. The cold-rolled base strip is ultrasonically cleaned with acetone to remove oil, and then annealed in a vacuum environment. The annealing process is to raise the heating rate of 10°C/min to 750°C for 30 minutes, and then increase the heating rate of 10°C/min to 1000°C for 120 minutes. , and finally get the cubic textured baseband. The (111) polar diagram of the alloy baseband is shown in Fig. 3. The cubic texture concentration: out-of-plane and in-plane FWHM are Dω=6.2° and The volume fraction is 98%, the stress-strain curve of the alloy is shown in Figure 5, and the yield strength is 140MPa. It shows that this alloy can obtain high-strength and high-concentration cubic texture.
实施例3Example 3
将纯度均为99.95％以上的Ni、Cr、Co、Mo、Fe、Cu按照85.4％、7.8％、0.2％、2％、3％及1.6％的重量百分比进行配料，配料经过真空感应熔炼炉充分冶炼后，获得初始坯锭；将坯锭在1050℃下均匀化处理20h，使合金化学成分更加均匀，然后将坯锭热锻成尺寸为41×19×12mm的锻件；将锻件随炉升温至1100℃保温30min后进行热轧，道次压下量约为10％，最后得到厚度为4.92mm的热轧板。将热轧板在1050℃退火处理和酸洗后，进行道次压下量为3～10％、总压下量为98.4％的冷轧，获得厚度为80μm的合金基带。将冷轧基带用丙酮超声清洗除油后在真空环境下进行退火，退火工艺为10℃/min的升温速率升至950℃保温120min，最终得到立方织构基带。该合金基带的(111)极图示于图4，立方织构集中度：面外和面内FWHM分别为Dω＝5.1°和体积分数为96％，该合金的应力应变曲线如图5所示，屈服强度为148MPa。说明此合金可以获得高强度高集中度的立方织构。Ni, Cr, Co, Mo, Fe, Cu with a purity of more than 99.95% are batched according to the weight percentage of 85.4%, 7.8%, 0.2%, 2%, 3% and 1.6%. After smelting, the initial ingot is obtained; the ingot is homogenized at 1050°C for 20 hours to make the chemical composition of the alloy more uniform, and then the ingot is hot forged into a forging with a size of 41×19×12mm; the forging is heated up with the furnace to After heat preservation at 1100°C for 30 minutes, hot rolling is carried out, and the reduction in each pass is about 10%, and finally a hot-rolled sheet with a thickness of 4.92 mm is obtained. After the hot-rolled sheet is annealed and pickled at 1050°C, it is cold-rolled with a pass reduction of 3-10% and a total reduction of 98.4%, to obtain an alloy base strip with a thickness of 80 μm. The cold-rolled base strip was cleaned and degreased by ultrasonic cleaning with acetone, and then annealed in a vacuum environment. The annealing process was to increase the temperature from 10 °C/min to 950 °C for 120 min, and finally obtain a cubic texture base band. The (111) pole diagram of the alloy baseband is shown in Fig. 4. The cubic texture concentration: out-of-plane and in-plane FWHM are Dω=5.1° and The volume fraction is 96%, the stress-strain curve of the alloy is shown in Figure 5, and the yield strength is 148MPa. It shows that this alloy can obtain high-strength and high-concentration cubic texture.
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