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CN113430646B - A method for the growth of REBCO superconducting bulk materials induced by single-seed bridge structure - Google Patents

A method for the growth of REBCO superconducting bulk materials induced by single-seed bridge structure Download PDF

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CN113430646B
CN113430646B CN202110711199.9A CN202110711199A CN113430646B CN 113430646 B CN113430646 B CN 113430646B CN 202110711199 A CN202110711199 A CN 202110711199A CN 113430646 B CN113430646 B CN 113430646B
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姚忻
朱彦涵
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Abstract

本发明提供一种利用单籽晶桥式结构诱导生长REBCO超导块材的方法,包括以下步骤:配制RE123和RE211纯相粉末,按照RE123+30mol%RE211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料;根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个;将籽晶、籽晶桥、缓冲层、前驱体从上至下依次放置;所述籽晶、所述籽晶桥、所述缓冲层构成单籽晶桥式结构;其中,所述籽晶放置在所述籽晶桥的上表面中心,所述籽晶桥搭设在所述缓冲层上方,所述缓冲层沿所述籽晶[110]晶向排列成一列;将所述放置好的前驱体连同和所述单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长,以实现(110)∥(110)取向诱导生长REBCO超导块材。

Figure 202110711199

The invention provides a method for inducing the growth of REBCO superconducting bulk materials by utilizing a single seed crystal bridge structure, comprising the following steps: preparing RE123 and RE211 pure phase powders, preparing according to the components of RE123+30mol% RE211+1wt% CeO2, fully Milling and mixing uniformly to obtain precursor powder; according to the diameter of the mold, the powder is weighed to an appropriate quality, put into the mold, and pressed into a cylindrical seed crystal bridge, 2 to 3 buffer layers and a precursor 1 place the seed crystal, the seed crystal bridge, the buffer layer, and the precursor in sequence from top to bottom; the seed crystal, the seed crystal bridge, and the buffer layer form a single-seed crystal bridge structure; wherein, the seed crystal The crystal is placed in the center of the upper surface of the seed crystal bridge, the seed crystal bridge is erected above the buffer layer, and the buffer layer is arranged in a row along the [110] crystal direction of the seed crystal; The precursor together with the single-seed bridge structure is placed in a growth furnace for top seed melt texture growth, so as to achieve (110)∥(110) orientation induced growth of REBCO superconducting bulk.

Figure 202110711199

Description

利用单籽晶桥式结构诱导生长REBCO超导块材的方法A method for the growth of REBCO superconducting bulk materials induced by single-seed bridge structure

技术领域technical field

本发明属于超导材料生长方法技术领域,具体涉及一种利用薄膜籽晶,结合桥式结构,实现(110)∥(110)取向诱导生长REBCO超导块材的方法。The invention belongs to the technical field of superconducting material growth methods, and in particular relates to a method for realizing (110)∥(110) orientation induced growth of REBCO superconducting bulk materials by utilizing thin film seed crystals combined with a bridge structure.

背景技术Background technique

自REBa2Cu3O7-δ(简称REBCO、RE123、稀土钡铜氧,其中RE选自Y、Gd、Sm、Nd等)高温超导体被发现以来,因其完全抗磁性,高临界电流密度和高冻结磁场等性质所带来的巨大商业潜能,如飞轮储能,永磁体,磁悬浮力元件等,引起了人们广泛的关注。作为应用的必然前提,具有大尺寸和高性能的REBCO块材的制备是必须要解决的问题。目前为止,顶部籽晶熔融织构生长法(Top-Seeded Melt Textured Growth,简称TSMTG)被普遍认为是一种极具潜力的REBCO高温超导块材制备方法。在生长过程中,单个籽晶被放置在REBCO前驱体的上表面中心,作为唯一的形核点诱导REBCO块体按照籽晶取向定向凝固生长,最终形成单一c轴取向的单畴超导块材。但是,由于RE123较低的生长速率,得到大尺寸的超导块材需花费较长时间;而过长的生长时间会导致自发形核,高温相RE211晶粒粗化等问题。因此,对大尺寸样品而言,缩短制备时间显得尤为重要。Since REBa 2 Cu 3 O 7-δ (referred to as REBCO, RE123, rare earth barium copper oxide, where RE is selected from Y, Gd, Sm, Nd, etc.) high-temperature superconductor was discovered, because of its complete diamagnetism, high critical current density and The huge commercial potential brought by properties such as high freezing magnetic fields, such as flywheel energy storage, permanent magnets, magnetic levitation force elements, etc., has attracted widespread attention. As an inevitable prerequisite for application, the preparation of REBCO blocks with large size and high performance is a problem that must be solved. So far, Top-Seeded Melt Textured Growth (TSMTG) is generally considered to be a promising method for preparing REBCO high-temperature superconducting bulk materials. During the growth process, a single seed crystal is placed in the center of the upper surface of the REBCO precursor, as the only nucleation point to induce the REBCO bulk to solidify and grow according to the seed crystal orientation, and finally form a single c-axis oriented single-domain superconducting bulk material . However, due to the low growth rate of RE123, it takes a long time to obtain large-sized superconducting bulk materials; and excessive growth time will lead to problems such as spontaneous nucleation and grain coarsening of high-temperature phase RE211. Therefore, it is particularly important to shorten the preparation time for large-sized samples.

多籽晶熔融织构法是解决超导块材过长生长时间的一种极为有效的方法,即在样品上表面按一定取向放置多个籽晶。由于多个籽晶同时诱导生长,整个制备流程所需的时间大为缩短。但研究发现,由于传统的多籽晶法一般为(100)∥(100)放置,样品在晶界处会大量残留非超导相,阻碍超导电流环通过晶界,最终导致样品内部存在多个小的超导电流环而不是一整个大的超导电流环,整体性能大大下降。同时,在传统多籽晶等距放置诱导块材制备过程中,随着使用籽晶数目的增加会进一步降低块材内部晶界的弱连接,从而降低块材的超导性能。The multi-seed melt texture method is an extremely effective method to solve the excessive growth time of superconducting bulk materials, that is, placing multiple seed crystals in a certain orientation on the upper surface of the sample. Since multiple seed crystals induce growth at the same time, the time required for the entire preparation process is greatly shortened. However, the study found that because the traditional multi-seed method is generally placed at (100)∥(100), a large number of non-superconducting phases will remain at the grain boundary of the sample, which hinders the superconducting current loop from passing through the grain boundary, and eventually leads to the existence of multiple non-superconducting phases inside the sample. A small superconducting current loop instead of a whole large superconducting current loop, the overall performance is greatly reduced. At the same time, in the process of traditional multi-seed equidistant placement to induce bulk preparation, with the increase of the number of seeds used, the weak connection of grain boundaries inside the bulk will be further reduced, thereby reducing the superconducting properties of the bulk.

发明内容SUMMARY OF THE INVENTION

鉴于以上所述现有技术的缺点,本发明的目的在于提供一种利用薄膜籽晶,结合桥式结构,实现(110)∥(110)取向诱导生长REBCO超导块材的方法,用于更经济有效地推广REBCO超导块材应用。In view of the above-mentioned shortcomings of the prior art, the purpose of the present invention is to provide a method for realizing (110)∥(110) orientation induced growth of REBCO superconducting bulk materials by utilizing thin film seed crystals and combining bridge structures, which is used for more Cost-effectively promote the application of REBCO superconducting bulk materials.

本发明提供一种单籽晶桥式结构实现(110)∥(110)取向诱导生长REBCO超导块材的方法,包括以下步骤:The present invention provides a method for realizing (110)∥(110) orientation induced growth of REBCO superconducting bulk material with a single seed crystal bridge structure, comprising the following steps:

步骤一,按照RE:Ba:Cu=1:2:3和RE:Ba:Cu=2:1:1的比例将RE2O3,BaCO3和CuO粉末配制成RE123和RE211的原始粉末。Step 1, according to the ratio of RE:Ba:Cu=1:2:3 and RE:Ba:Cu=2:1:1, RE 2 O 3 , BaCO 3 and CuO powders are formulated into the original powders of RE123 and RE211.

步骤二,将所述原始粉料充分混合均匀,在空气环境下900℃烧结48小时。为保证最终获得组分均匀单一的RE123和RE211相,将烧结后的粉末再次研磨、烧结,相同工艺共重复三次。In step 2, the original powder is fully mixed and sintered at 900° C. for 48 hours in an air environment. In order to ensure that RE123 and RE211 phases with uniform and single composition are finally obtained, the sintered powders are ground and sintered again, and the same process is repeated three times in total.

步骤三,将步骤二获得的RE123和RE211纯相粉末按照RE123+30mol%RE211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料。In step 3, the pure phase powders of RE123 and RE211 obtained in step 2 are prepared according to the components of RE123+30mol% RE211+1wt% CeO2, fully milled and mixed uniformly to obtain precursor powder.

步骤四,根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个。Step 4: According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, two to three buffer layers and one precursor.

步骤五,将籽晶、籽晶桥、缓冲层、前驱体从上至下依次放置;所述籽晶、所述籽晶桥、所述缓冲层构成单籽晶桥式结构;其中,所述籽晶放置在所述籽晶桥的上表面中心,所述籽晶桥搭设在所述缓冲层上方,所述缓冲层沿所述籽晶[110]晶向排列成一列(即处于籽晶[110]晶向的延长线上)。Step 5, place the seed crystal, the seed crystal bridge, the buffer layer, and the precursor in sequence from top to bottom; the seed crystal, the seed crystal bridge, and the buffer layer form a single-seed crystal bridge structure; wherein, the The seed crystal is placed in the center of the upper surface of the seed crystal bridge, the seed crystal bridge is erected above the buffer layer, and the buffer layer is arranged in a row along the [110] crystal direction of the seed crystal (that is, in the seed crystal [110] crystal direction. 110] on the extension of the crystal orientation).

步骤六,将所述前驱体连同单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长。Step 6, placing the precursor together with the single-seed bridge structure in a growth furnace to perform top seed melting texture growth.

进一步地,所述顶部籽晶熔融织构生长工艺包括以下步骤:Further, the top seed melt texture growth process includes the following steps:

使所述生长炉内的温度在第一时间内升至第一温度,保温1~3小时;raising the temperature in the growth furnace to the first temperature within the first time, and keeping the temperature for 1-3 hours;

使所述生长炉内的温度在第二时间内升至第二温度,保温1~3小时;raising the temperature in the growth furnace to a second temperature within a second time, and keeping the temperature for 1 to 3 hours;

使所述生长炉内的温度在第三时间内降至第三温度;lowering the temperature in the growth furnace to a third temperature within a third time;

使所述生长炉内的温度在第四时间内降至第四温度;reducing the temperature in the growth furnace to a fourth temperature within a fourth time;

最后淬火,获得REBCO超导块材。Finally, quenched to obtain REBCO superconducting bulk.

进一步地,所述第一时间为3~5小时,所述第一温度为850~950℃;所述第二时间为1~2小时,所述第二温度高于所述REBCO超导材料的包晶反应温度40~80℃;所述第三时间为0.5~1小时,所述第三温度为所述REBCO材料的包晶反应温度;所述第四时间为10~80小时,所述第四温度低于所述包晶反应温度5~40℃。Further, the first time is 3-5 hours, the first temperature is 850-950° C.; the second time is 1-2 hours, and the second temperature is higher than the REBCO superconducting material. The peritectic reaction temperature is 40 to 80°C; the third time is 0.5 to 1 hour, and the third temperature is the peritectic reaction temperature of the REBCO material; the fourth time is 10 to 80 hours, and the third temperature is 10 to 80 hours. The temperature is 5-40°C lower than the peritectic reaction temperature.

可选地,缓冲层数量为2~3个,根据实际需要生长的块材尺寸进行选择。Optionally, the number of buffer layers is 2-3, which is selected according to the size of the block material that needs to be grown.

优选地,所述籽晶为NdBCO/YBCO/MgO薄膜籽晶。Preferably, the seed crystal is an NdBCO/YBCO/MgO thin film seed crystal.

优选地,所述籽晶的尺寸为2mm×2mm。Preferably, the size of the seed crystal is 2mm×2mm.

进一步地,前驱体中还可掺杂氧化铈、铂等,以抑制熔体流失。Further, the precursor can also be doped with cerium oxide, platinum, etc. to suppress the melt loss.

进一步地,籽晶桥的直径为10mm,一般需称量0.6g压制;缓冲层的直径为5mm,一般需称量0.15~0.2g压制;前驱体的直径大于等于30mm。Further, the diameter of the seed bridge is 10mm, and generally needs to be weighed 0.6g to be pressed; the diameter of the buffer layer is 5mm, and generally needs to be weighed 0.15-0.2g to be pressed; the diameter of the precursor is greater than or equal to 30mm.

进一步地,REBCO超导材料中RE为Y、Gd、Sm或Nd。Further, RE in the REBCO superconducting material is Y, Gd, Sm or Nd.

本发明提供一种利用单籽晶桥式结构实现(110)∥(110)取向诱导生长REBCO超导块材的方法,具有以下有益效果:The present invention provides a method for realizing (110)∥(110) orientation induced growth of REBCO superconducting bulk material by utilizing a single seed crystal bridge structure, which has the following beneficial effects:

1、本发明采用(110)∥(110)的多籽晶排布方式,有效避免了不同籽晶间(100)/(100)晶界的产生,可以有效排出晶界处的残余熔体,有利于REBCO块材的性能提高。1. The present invention adopts the multi-seed arrangement of (110)∥(110), which effectively avoids the generation of (100)/(100) grain boundaries between different seed crystals, and can effectively discharge the residual melt at the grain boundaries. It is beneficial to improve the performance of REBCO block.

2、本发明通过籽晶桥结合缓冲层的结构实现多籽晶诱导的效果,不仅可以有效缩短生长块材的时间,而且保障了多个“籽晶”(实际为各缓冲层)间取向的一致。方法简单、易于操作、重复可控。2. The present invention realizes the effect of multi-seed induction through the structure of the seed crystal bridge combined with the buffer layer, which can not only effectively shorten the time for growing the bulk material, but also ensure the orientation between multiple "seed crystals" (actually each buffer layer). Consistent. The method is simple, easy to operate, and repeatable and controllable.

3、本发明的只需一个籽晶即可实现目标,使用材料少,能有效降低REBCO超导块材制备的时间成本和经济成本,并对节约资源、提高资源使用率产生积极作用,对生态环境保护产生积极影响。3. The present invention only needs one seed crystal to achieve the goal, uses less material, can effectively reduce the time cost and economic cost of REBCO superconducting block material preparation, and has a positive effect on saving resources and improving resource utilization rate, and has a positive effect on ecological Environmental protection has a positive impact.

4、本发明由于采用具有高热稳定性的薄膜籽晶,对具有高包晶反应温度的REBCO(如GdBCO、SmBCO、NdBCO等)块材的取向诱导生长同样适用。4. Since the present invention adopts the thin film seed crystal with high thermal stability, it is also applicable to the orientation-induced growth of REBCO (such as GdBCO, SmBCO, NdBCO, etc.) bulk materials with high peritectic reaction temperature.

附图说明Description of drawings

下面结合附图对本发明进一步说明。The present invention will be further described below with reference to the accompanying drawings.

图1示意传统多籽晶0°放置时(100)/(100)晶界的形成与生长过程;箭头表示生长前沿前移的方向。Figure 1 illustrates the formation and growth process of the (100)/(100) grain boundary when the traditional polyseed crystal is placed at 0°; the arrows indicate the direction of the growth front.

图2示意多籽晶45°放置时(110)/(110)晶界的形成与生长过程;箭头表示生长前沿前移的方向。Figure 2 illustrates the formation and growth process of the (110)/(110) grain boundary when the multi-seed crystal is placed at 45°; the arrows indicate the direction in which the growth front moves forward.

图3示意使用四籽晶45°放置方式生长的GdBCO块材样品;箭头表示照片左侧晶粒的生长线。Figure 3 illustrates a GdBCO bulk sample grown using a four-seed 45° placement; the arrows indicate the growth lines of the grains on the left side of the photo.

图4示意使用四籽晶45°放置方式生长GdBCO块材样品时两种生长方式对应的种子位置和生长过程示意图。FIG. 4 is a schematic diagram of the seed positions and the growth process corresponding to the two growth methods when the GdBCO bulk sample is grown using the four-seed 45° placement method.

图5示意单籽晶桥式结构实现(110)∥(110)取向诱导的样品俯视图;(a)-(d)展示了使用2个缓冲层时晶体生长随时间的变化。Figure 5 shows the top view of the sample with single-seed bridge structure to achieve (110)∥(110) orientation induction; (a)-(d) show the change of crystal growth with time when two buffer layers are used.

图6展示了单籽晶桥式结构使用3个缓冲层时晶体的生长情况。Figure 6 shows the growth of the crystal when three buffer layers are used in the single-seed bridge structure.

图7示意单籽晶桥式结构使用2个缓冲层实现(110)∥(110)取向诱导的样品剖面图。FIG. 7 illustrates a cross-sectional view of a sample in which the single-seed bridge structure uses two buffer layers to achieve (110)∥(110) orientation induction.

图8示意单籽晶桥式结构使用3个缓冲层实现(110)∥(110)取向诱导的样品剖面图。FIG. 8 illustrates the cross-sectional view of the sample in which the single-seed bridge structure uses three buffer layers to achieve (110)∥(110) orientation induction.

图9示意单籽晶桥式结构使用4个缓冲层时的晶体诱导生长情况(样品俯视图)。FIG. 9 illustrates the crystal-induced growth of the single-seed bridge structure using 4 buffer layers (top view of the sample).

具体实施方式Detailed ways

以下通过特定的具体实例说明本发明的实施方式,本领域技术人员可由本说明书所揭露的内容轻易地了解本发明的其他优点与功效。The embodiments of the present invention are described below through specific specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification.

本发明的发明构思如下:The inventive concept of the present invention is as follows:

在传统多籽晶熔融织构法中,籽晶的排列方式大多采用(100)∥(100)的取向(以下简称0°排列)。随着生长前沿的推进,块材中的高温相和杂质相也相应被推出。以2个籽晶为例,如图1所示,由于0°排列时(100)晶面以一整个平面的形式接触生成晶界,所以生长前沿的非超导相就没有机会排除而被捕获在晶界附近。这种富集非超导相的晶界被称为“受污染”的晶界,会阻碍超导电流环的通过,使得块材的性能大大降低。In the traditional multi-seed melt texturing method, most of the seed crystals are arranged in the (100)∥(100) orientation (hereinafter referred to as 0° arrangement). As the growth front advances, the high temperature and impurity phases in the bulk material are pushed out accordingly. Taking 2 seed crystals as an example, as shown in Figure 1, since the (100) crystal plane contacts in the form of a whole plane to generate grain boundaries, the non-superconducting phase at the growth front has no chance to be excluded and captured. near grain boundaries. Such grain boundaries enriched in non-superconducting phases, known as "contaminated" grain boundaries, impede the passage of superconducting current loops and greatly degrade the performance of the bulk material.

不同的是,如果多个籽晶以(110)∥(110)的取向排列(以下简称45°排列),就不会出现“受污染”的晶界。还是以2个籽晶为例,如图2所示,由于45°排列时(110)晶面以一个点的形式接触生成晶界,所以此时生长前沿的非超导相就不会被捕获入晶界。更进一步,这些非超导相还会随着生长的继续被推向样品的边缘,保证了整个样品中的“干净”。因此,(110)/(110)晶界就不会阻碍超导电流环的通过,从而提高多籽晶诱导生长的块材的性能。另一方面,众所周知,对REBCO体系超导材料来说,(110)晶面是一个非平衡生长面,因此也是一个快速生长面。当采用多籽晶45°排列时,这种快速生长的优势有助于在多个籽晶同时生长的基础上进一步缩短样品制备的时间,尤为适合大尺寸样品,符合工业化的需求。The difference is that if multiple seed crystals are arranged in the orientation of (110)∥(110) (hereinafter referred to as 45° arrangement), there will be no "contaminated" grain boundaries. Taking 2 seed crystals as an example, as shown in Figure 2, since the (110) crystal plane contacts in the form of a point to generate grain boundaries when arranged at 45°, the non-superconducting phase at the growth front will not be captured at this time. into the grain boundary. Furthermore, these non-superconducting phases are also pushed towards the edge of the sample as the growth continues, ensuring "cleanness" throughout the sample. Therefore, the (110)/(110) grain boundary will not hinder the passage of the superconducting current loop, thereby improving the performance of the multi-seed-induced growth bulk material. On the other hand, it is well known that for REBCO system superconducting materials, the (110) crystal face is a non-equilibrium growth face, so it is also a fast growth face. When multi-seed crystals are arranged at 45°, this advantage of rapid growth helps to further shorten the sample preparation time on the basis of simultaneous growth of multiple seed crystals, which is especially suitable for large-sized samples and meets the needs of industrialization.

不足的是,首先,45°的排列方式并没有改变籽晶的使用数量,对产业化的应用需求来说,这样的生长方式无疑具有远比单籽晶法还要高昂的成本。其次,对籽晶的45°排列放置在理论上是容易实现的,但实际上由于人工的操作、或者高温熔融状态下出现籽晶漂移,很容易出现个别籽晶与其他籽晶没有完全呈现45°排列。如图3所示用四籽晶生长的GdBCO块材,左侧两个籽晶在放置时没有完全达成(110)∥(110),导致诱导生长出的晶界不具有(110)/(110)晶界的快速生长特性,且更有可能在生长过程中一定程度上捕获非超导相。相比之下,右侧两个籽晶则是标准的45°排列。图4展示了两种生长模式对应的籽晶位置和生长过程。The disadvantage is that, first of all, the 45° arrangement does not change the number of seeds used. For industrial application requirements, such a growth method undoubtedly has a much higher cost than the single-seed method. Secondly, the 45° arrangement of seed crystals is theoretically easy to achieve, but in fact, due to manual operation or seed crystal drift under high temperature melting state, it is easy to appear that individual seed crystals and other seed crystals do not fully display 45 ° Arrange. For the GdBCO bulk grown with four seed crystals as shown in Figure 3, the two seed crystals on the left did not fully achieve (110)∥(110) when placed, resulting in the induced grain boundary without (110)/(110 ) fast growth characteristics of grain boundaries, and more likely to trap the non-superconducting phase to some extent during the growth process. In contrast, the two seeds on the right are in a standard 45° arrangement. Figure 4 shows the seed positions and growth processes corresponding to the two growth modes.

基于以上多籽晶45°排列方式的优缺点,本发明在保留其优点的前提下消除了其缺点,同时减少了籽晶的使用数量,大大降低了成本。具体来说,通过籽晶桥的使用,使得单个籽晶具备了同时诱导多个缓冲层的能力,而缓冲层在生长完全后又会起到二级籽晶的作用继续诱导前驱体。此时,前驱体同时受到多个缓冲层的诱导,就实现了多籽晶的效果。另一方面,正因为缓冲层都是由同一个籽晶通过生长诱导出来的,这些缓冲层之间就会有固定的、一致的(110)∥(110)的取向,从而避免了45°排列方式中影响最大的人工操作导致的缺陷。由此,45°排列放置最重要的快速生长能力和“干净”的晶界两点优势也都得以保证。图5至图8分别展示了单籽晶桥式结构实现(110)∥(110)取向诱导的样品俯视图和剖面图。图5-6中,501和601表示所示状态下晶畴倾向的平衡形状,502和602表示使用本发明所述方法得到的干净的(110)/(110)晶界,箭头503和603表示生长前沿前移的方向。图7-8中,701和801代表薄膜籽晶,702和802代表籽晶桥,703和803代表缓冲层。使用2个和3个缓冲层的区别也在图上得以体现,明显地,在相同生长时间下,使用3个缓冲层得到的平衡晶面形状更大,也有利于更大尺寸块材的制备。值得一提的是,如图9所示,单籽晶桥式结构在使用4个缓冲层时并不能实现本发明的目的,因为此时由于中心对称的排布方式,最终多个缓冲层间还是会形成(100)/(100)晶界,而不是(110)/(110)晶界。Based on the advantages and disadvantages of the above 45° arrangement of multi-seed crystals, the present invention eliminates its disadvantages on the premise of retaining its advantages, and at the same time reduces the number of seeds used and greatly reduces the cost. Specifically, through the use of seed bridges, a single seed crystal has the ability to induce multiple buffer layers at the same time, and the buffer layers will play the role of secondary seed crystals and continue to induce precursors after the growth is complete. At this time, the precursor is induced by multiple buffer layers at the same time, and the effect of multiple seeds is realized. On the other hand, because the buffer layers are all induced by the same seed crystal through growth, there will be a fixed and consistent (110)∥(110) orientation between these buffer layers, thus avoiding the 45° alignment Defects caused by the most influential manual operations in the method. As a result, the two most important advantages of fast growth capability and "clean" grain boundaries of 45° arrangement are also guaranteed. Figures 5 to 8 show the top view and cross-sectional view of the sample in which the single-seed bridge structure realizes (110)∥(110) orientation induction, respectively. In Figures 5-6, 501 and 601 denote the equilibrium shape of the crystallographic domain tendencies in the states shown, 502 and 602 denote clean (110)/(110) grain boundaries obtained using the method described in the present invention, and arrows 503 and 603 denote The direction in which the growth front moves forward. In FIGS. 7-8, 701 and 801 represent thin film seeds, 702 and 802 represent seed bridges, and 703 and 803 represent buffer layers. The difference between using 2 and 3 buffer layers is also reflected in the figure. Obviously, under the same growth time, the equilibrium crystal plane shape obtained by using 3 buffer layers is larger, which is also conducive to the preparation of larger size bulk materials. . It is worth mentioning that, as shown in FIG. 9 , the single-seed bridge structure cannot achieve the purpose of the present invention when four buffer layers are used, because at this time, due to the center-symmetrical arrangement, the buffer layers are finally arranged between multiple buffer layers. Still (100)/(100) grain boundaries are formed, not (110)/(110) grain boundaries.

基于上述构思,本发明提供一种单籽晶桥式结构实现(110)∥(110)取向诱导生长REBCO超导块材的方法,包括以下步骤:Based on the above concept, the present invention provides a method for realizing (110)∥(110) orientation-induced growth of REBCO superconducting bulk material with a single-seed bridge structure, comprising the following steps:

步骤一,按照RE:Ba:Cu=1:2:3和RE:Ba:Cu=2:1:1的比例将RE2O3,BaCO3和CuO粉末配制成RE123和RE211的原始粉末;Step 1, according to the ratio of RE:Ba:Cu=1:2:3 and RE:Ba:Cu=2:1:1, RE 2 O 3 , BaCO 3 and CuO powders are prepared into original powders of RE123 and RE211;

步骤二,将所述原始粉料充分混合均匀,在空气环境下900℃烧结48小时。为保证最终获得组分均匀单一的RE123和RE211相,将烧结后的粉末再次研磨、烧结,相同工艺共重复三次。In step 2, the original powder is fully mixed and sintered at 900° C. for 48 hours in an air environment. In order to ensure that RE123 and RE211 phases with uniform and single composition are finally obtained, the sintered powders are ground and sintered again, and the same process is repeated three times in total.

步骤三,将获得的纯相粉末按照RE123+30mol%RE211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料。In step 3, the obtained pure phase powder is prepared according to the components of RE123 + 30mol% RE211+1wt% CeO2, fully milled and mixed uniformly to obtain a precursor powder.

步骤四,根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个。Step 4: According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, two to three buffer layers and one precursor.

步骤五,将籽晶、籽晶桥、缓冲层、前驱体按照所述层次从上至下依次放置。In step 5, the seed crystal, the seed crystal bridge, the buffer layer and the precursor are placed in order from top to bottom according to the described layers.

步骤六,将所述放置好的前驱体连同单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长。Step 6, placing the placed precursor together with the single-seed bridge structure in a growth furnace to perform top seed melting texture growth.

本发明还可以通过另外不同的具体实施方式加以实施或应用,本说明书中的各项细节也可以基于不同观点与应用,在没有背离本发明的精神下进行各种修饰或改变。以下实施例不构成对本发明的限定。The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. The following examples do not constitute a limitation of the present invention.

实施例一Example 1

本实施例的一种单籽晶桥式结构实现(110)∥(110)取向诱导生长YBCO超导块材的方法,包括如下工序:A method for realizing (110)∥(110) orientation-induced growth of a YBCO superconducting bulk material with a single-seed bridge structure in this embodiment includes the following steps:

1、按照Y:Ba:Cu=1:2:3和Y:Ba:Cu=2:1:1的比例将Y2O3,BaCO3和CuO粉末配制成Y123和Y211的原始粉末;1. According to the ratio of Y:Ba:Cu=1:2:3 and Y:Ba:Cu=2:1:1, Y 2 O 3 , BaCO 3 and CuO powders were prepared into the original powders of Y123 and Y211;

2、将原始粉料充分混合均匀,在空气环境下900℃烧结48小时。为保证最终获得组分均匀单一的Y123和Y211相,将烧结后的粉末再次研磨、烧结,相同工艺共重复三次。2. Mix the original powder evenly and sinter at 900℃ for 48 hours in an air environment. In order to ensure that the Y123 and Y211 phases with uniform and single composition are finally obtained, the sintered powder is ground and sintered again, and the same process is repeated three times in total.

3、将获得的纯相粉末按照Y123+30mol%Y211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料。3. The obtained pure phase powder is prepared according to the components of Y123 + 30mol% Y211+1wt% CeO2, fully milled and mixed uniformly to obtain precursor powder.

4、根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个。籽晶桥的直径为10mm,一般需称量0.6g压制;缓冲层的直径为5mm,一般需称量0.15~0.2g压制;前驱体的直径为30mm,需称量30g。4. According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, two to three buffer layers and one precursor. The diameter of the seed crystal bridge is 10mm, and it generally needs to be weighed 0.6g for pressing; the diameter of the buffer layer is 5mm, and it generally needs to be weighed 0.15-0.2g for pressing; the diameter of the precursor is 30mm, and it needs to be weighed 30g.

5、将籽晶、籽晶桥、缓冲层、前驱体按照所述层次从上至下依次放置。具体说来,将c轴取向的2mm×2mm大小的NdBCO/YBCO/MgO薄膜籽晶放置在籽晶桥的上表面中心,将缓冲层沿所述籽晶[110]晶向排列成一列(即处于籽晶[110]晶向的延长线上)。5. The seed crystal, the seed crystal bridge, the buffer layer and the precursor are placed in order from top to bottom according to the described layers. Specifically, a NdBCO/YBCO/MgO thin film seed crystal with a size of 2mm×2mm oriented along the c-axis was placed in the center of the upper surface of the seed bridge, and the buffer layer was arranged in a row along the [110] crystal direction of the seed crystal (ie On the extension line of the seed crystal [110] orientation).

6、将放置好的前驱体连同单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长。生长炉的具体温度程序为:6. Place the placed precursor together with the single-seed bridge structure in a growth furnace for melting texture growth of the top seed crystal. The specific temperature program of the growth furnace is:

a、从室温开始经过4h升温至900℃,保温4h。a. The temperature is raised from room temperature to 900°C for 4 hours, and the temperature is kept for 4 hours.

b、继续加热1h,升温至1065℃,保温1h。b. Continue to heat for 1 hour, raise the temperature to 1065°C, and keep the temperature for 1 hour.

c、在30min内,快速降温至1005℃。c. Within 30min, rapidly cool down to 1005℃.

d、以0.3℃/h的冷速缓慢降温生长100h。d. Slowly cool down and grow at a cooling rate of 0.3°C/h for 100h.

e、在4h内随炉快速冷却,制得(110)∥(110)取向诱导的YBCO高温超导块材。e. Rapidly cooling with the furnace within 4h to obtain the (110)∥(110) orientation-induced YBCO high temperature superconducting bulk material.

实施例二Embodiment 2

本实施例的一种单籽晶桥式结构实现(110)∥(110)取向诱导生长GdBCO超导块材的方法,包括如下工序:A method for realizing (110)∥(110) orientation-induced growth of a GdBCO superconducting bulk material with a single-seed bridge structure in this embodiment includes the following steps:

1、按照Gd:Ba:Cu=1:2:3和Gd:Ba:Cu=2:1:1的比例将Gd2O3,BaCO3和CuO粉末配制成Gd123和Gd211的原始粉末;1. According to the ratio of Gd:Ba:Cu=1:2:3 and Gd:Ba:Cu=2:1:1, Gd 2 O 3 , BaCO 3 and CuO powders were prepared into original powders of Gd123 and Gd211;

2、将原始粉料充分混合均匀,在空气环境下900℃烧结48小时。为保证最终获得组分均匀单一的Gd123和Gd211相,将烧结后的粉末再次研磨、烧结,相同工艺共重复三次。2. Mix the original powder evenly and sinter at 900℃ for 48 hours in an air environment. In order to ensure that the Gd123 and Gd211 phases with uniform and single composition are finally obtained, the sintered powder is ground and sintered again, and the same process is repeated three times in total.

3、将获得的纯相粉末按照Gd123+30mol%Gd211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料。3. The obtained pure phase powder is prepared according to the components of Gd123 + 30mol% Gd211+1wt% CeO2, fully milled and mixed uniformly to obtain precursor powder.

4、根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个。籽晶桥的直径为10mm,一般需称量0.6g压制;缓冲层的直径为5mm,一般需称量0.15~0.2g压制;前驱体的直径为30mm,需称量30g。4. According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, two to three buffer layers and one precursor. The diameter of the seed crystal bridge is 10mm, and it generally needs to be weighed 0.6g for pressing; the diameter of the buffer layer is 5mm, and it generally needs to be weighed 0.15-0.2g for pressing; the diameter of the precursor is 30mm, and it needs to be weighed 30g.

5、将籽晶、籽晶桥、缓冲层、前驱体按照所述层次从上至下依次放置。具体说来,将c轴取向的2mm×2mm大小的NdBCO/YBCO/MgO薄膜籽晶放置在籽晶桥的上表面中心,将缓冲层沿所述籽晶[110]晶向排列成一列(即处于籽晶[110]晶向的延长线上)。5. The seed crystal, the seed crystal bridge, the buffer layer and the precursor are placed in order from top to bottom according to the described layers. Specifically, a NdBCO/YBCO/MgO thin film seed crystal with a size of 2mm×2mm oriented along the c-axis was placed in the center of the upper surface of the seed bridge, and the buffer layer was arranged in a row along the [110] crystal direction of the seed crystal (ie On the extension line of the seed crystal [110] orientation).

6、将放置好的前驱体连同单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长。生长炉的具体温度程序为:6. Place the placed precursor together with the single-seed bridge structure in a growth furnace for melting texture growth of the top seed crystal. The specific temperature program of the growth furnace is:

a、从室温开始经过4h升温至900℃,保温4h。a. The temperature is raised from room temperature to 900°C for 4 hours, and the temperature is kept for 4 hours.

b、继续加热1h,升温至1095℃,保温1h。b. Continue to heat for 1 hour, raise the temperature to 1095°C, and keep the temperature for 1 hour.

c、在30min内,快速降温至1045℃。c. Within 30min, rapidly cool down to 1045℃.

d、以0.3℃/h的冷速缓慢降温生长100h。d. Slowly cool down and grow at a cooling rate of 0.3°C/h for 100h.

e、在4h内随炉快速冷却,制得(110)∥(110)取向诱导的GdBCO高温超导块材。e. Rapid cooling with the furnace within 4h to obtain (110)∥(110) orientation-induced GdBCO high-temperature superconducting bulk.

实施例三Embodiment 3

本实施例的一种单籽晶桥式结构实现(110)∥(110)取向诱导生长SmBCO超导块材的方法,包括如下工序:A method for realizing (110)∥(110) orientation-induced growth of a SmBCO superconducting bulk material with a single-seed bridge structure in this embodiment includes the following steps:

1、按照Sm:Ba:Cu=1:2:3和Sm:Ba:Cu=2:1:1的比例将Sm2O3,BaCO3和CuO粉末配制成Sm123和Sm211的原始粉末;1. According to the ratio of Sm:Ba:Cu=1:2:3 and Sm:Ba:Cu=2:1:1, Sm 2 O 3 , BaCO 3 and CuO powders are prepared into the original powders of Sm123 and Sm211;

2、将原始粉料充分混合均匀,在空气环境下900℃烧结48小时。为保证最终获得组分均匀单一的Sm123和Sm211相,将烧结后的粉末再次研磨、烧结,相同工艺共重复三次。2. Mix the original powder evenly and sinter at 900℃ for 48 hours in an air environment. In order to ensure that the Sm123 and Sm211 phases with uniform and single composition are finally obtained, the sintered powder is ground and sintered again, and the same process is repeated three times in total.

3、将获得的纯相粉末按照Sm123+30mol%Sm211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料。3. The obtained pure phase powder is prepared according to the components of Sm123+30mol% Sm211 + 1wt% CeO2, fully milled and mixed uniformly to obtain the precursor powder.

4、根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个。籽晶桥的直径为10mm,一般需称量0.6g压制;缓冲层的直径为5mm,一般需称量0.15~0.2g压制;前驱体的直径为30mm,需称量30g。4. According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, two to three buffer layers and one precursor. The diameter of the seed crystal bridge is 10mm, and it generally needs to be weighed 0.6g for pressing; the diameter of the buffer layer is 5mm, and it generally needs to be weighed 0.15-0.2g for pressing; the diameter of the precursor is 30mm, and it needs to be weighed 30g.

5、将籽晶、籽晶桥、缓冲层、前驱体按照所述层次从上至下依次放置。具体说来,将c轴取向的2mm×2mm大小的NdBCO/YBCO/MgO薄膜籽晶放置在籽晶桥的上表面中心,将缓冲层沿所述籽晶[110]晶向排列成一列(即处于籽晶[110]晶向的延长线上)。5. The seed crystal, the seed crystal bridge, the buffer layer and the precursor are placed in order from top to bottom according to the described layers. Specifically, a NdBCO/YBCO/MgO thin film seed crystal with a size of 2mm×2mm oriented along the c-axis was placed in the center of the upper surface of the seed bridge, and the buffer layer was arranged in a row along the [110] crystal direction of the seed crystal (ie On the extension line of the seed crystal [110] orientation).

6、将放置好的前驱体连同单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长。生长炉的具体温度程序为:6. Place the placed precursor together with the single-seed bridge structure in a growth furnace for melting texture growth of the top seed crystal. The specific temperature program of the growth furnace is:

a、从室温开始经过4h升温至900℃,保温4h。a. The temperature is raised from room temperature to 900°C for 4 hours, and the temperature is kept for 4 hours.

b、继续加热1h,升温至1100℃,保温1h。b. Continue to heat for 1 hour, raise the temperature to 1100°C, and keep the temperature for 1 hour.

c、在30min内,快速降温至1065℃。c. Within 30min, rapidly cool down to 1065℃.

d、以0.3℃/h的冷速缓慢降温生长100h。d. Slowly cool down and grow at a cooling rate of 0.3°C/h for 100h.

e、在4h内随炉快速冷却,制得(110)∥(110)取向诱导的SmBCO高温超导块材。e. Rapid cooling with the furnace within 4h to obtain (110)∥(110) orientation-induced SmBCO high temperature superconducting bulk material.

实施例四Embodiment 4

本实施例的一种单籽晶桥式结构实现(110)∥(110)取向诱导生长NdBCO超导块材的方法,包括如下工序:A method for realizing (110)∥(110) orientation-induced growth of NdBCO superconducting bulk material with a single-seed bridge structure in this embodiment includes the following steps:

1、按照Nd:Ba:Cu=1:2:3和Nd:Ba:Cu=4:2:2的比例将Nd2O3,BaCO3和CuO粉末配制成Nd123和Nd211的原始粉末;1. According to the ratio of Nd:Ba:Cu=1:2:3 and Nd:Ba:Cu=4:2:2, Nd 2 O 3 , BaCO 3 and CuO powders were prepared into original powders of Nd123 and Nd211;

2、将原始粉料充分混合均匀,在空气环境下900℃烧结48小时。为保证最终获得组分均匀单一的Nd123和Nd211相,将烧结后的粉末再次研磨、烧结,相同工艺共重复三次。2. Mix the original powder evenly and sinter at 900℃ for 48 hours in an air environment. In order to ensure that the Nd123 and Nd211 phases with uniform and single composition are finally obtained, the sintered powder is ground and sintered again, and the same process is repeated three times in total.

3、将获得的纯相粉末按照Nd123+30mol%Nd211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料。3. The obtained pure phase powder is prepared according to the components of Nd123 + 30mol% Nd211+1wt% CeO2, fully milled and mixed uniformly to obtain the precursor powder.

4、根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个。籽晶桥的直径为10mm,一般需称量0.6g压制;缓冲层的直径为5mm,一般需称量0.15~0.2g压制;前驱体的直径为30mm,需称量30g。4. According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, two to three buffer layers and one precursor. The diameter of the seed crystal bridge is 10mm, and it generally needs to be weighed 0.6g for pressing; the diameter of the buffer layer is 5mm, and it generally needs to be weighed 0.15-0.2g for pressing; the diameter of the precursor is 30mm, and it needs to be weighed 30g.

5、将籽晶、籽晶桥、缓冲层、前驱体按照所述层次从上至下依次放置。具体说来,将c轴取向的2mm×2mm大小的NdBCO/YBCO/MgO薄膜籽晶放置在籽晶桥的上表面中心,将缓冲层沿所述籽晶[110]晶向排列成一列(即处于籽晶[110]晶向的延长线上)。5. The seed crystal, the seed crystal bridge, the buffer layer and the precursor are placed in order from top to bottom according to the described layers. Specifically, a NdBCO/YBCO/MgO thin film seed crystal with a size of 2mm×2mm oriented along the c-axis was placed in the center of the upper surface of the seed bridge, and the buffer layer was arranged in a row along the [110] crystal direction of the seed crystal (ie On the extension line of the seed crystal [110] orientation).

6、将放置好的前驱体连同单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长。生长炉的具体温度程序为:6. Place the placed precursor together with the single-seed bridge structure in a growth furnace for melting texture growth of the top seed crystal. The specific temperature program of the growth furnace is:

a、从室温开始经过4h升温至900℃,保温4h。a. The temperature is raised from room temperature to 900°C for 4 hours, and the temperature is kept for 4 hours.

b、继续加热1h,升温至1120℃,保温1h。b. Continue to heat for 1 hour, raise the temperature to 1120°C, and keep the temperature for 1 hour.

c、在30min内,快速降温至1090℃。c. Within 30min, rapidly cool down to 1090℃.

d、以0.3℃/h的冷速缓慢降温生长100h。d. Slowly cool down and grow at a cooling rate of 0.3°C/h for 100h.

e、在4h内随炉快速冷却,制得(110)∥(110)取向诱导的NdBCO高温超导块材。e. Rapid cooling with the furnace within 4 hours to obtain (110)∥(110) orientation-induced NdBCO high temperature superconducting bulk materials.

本发明提供一种利用薄膜籽晶结合桥式结构,实现(110)∥(110)取向诱导生长REBCO高温超导块材的方法。本发明利用籽晶桥和缓冲层形成桥式籽晶结构,通过使用单个籽晶即实现了多籽晶的作用,达到了加快生长的效果。同时下层缓冲层通过采用特定的沿[110]晶向的排列方式,实现缓冲层对块材的(110)∥(110)取向诱导生长。由于(110)晶面是快速生长面,此结构可在多籽晶的基础上进一步加速块材的生长,缩短大尺寸超导块材的制备时间。因为(110)/(110)晶界不易积聚高温相或杂质,可以消除样品(100)/(100)晶界处残留非超导相对超导性能的影响,提高块材的性能。The invention provides a method for realizing (110)∥(110) orientation induced growth of REBCO high temperature superconducting bulk material by utilizing thin film seed crystal combined with bridge structure. The present invention utilizes a seed crystal bridge and a buffer layer to form a bridge-type seed crystal structure, realizes the effect of multiple seed crystals by using a single seed crystal, and achieves the effect of accelerating growth. At the same time, by adopting a specific arrangement along the [110] crystal direction, the lower buffer layer realizes the (110)∥(110) orientation induced growth of the buffer layer to the bulk material. Since the (110) crystal plane is a fast growth plane, this structure can further accelerate the growth of bulk materials on the basis of multi-seed crystals, and shorten the preparation time of large-sized superconducting bulk materials. Because the (110)/(110) grain boundary is not easy to accumulate high temperature phase or impurities, the influence of the residual non-superconducting relative superconducting properties at the (100)/(100) grain boundary of the sample can be eliminated, and the performance of the bulk material can be improved.

以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术人员无需创造性劳动就可以根据本发明的构思做出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。The preferred embodiments of the present invention have been described in detail above. It should be understood that those skilled in the art can make numerous modifications and changes according to the concept of the present invention without creative efforts. Therefore, any technical solutions that can be obtained by those skilled in the art through logical analysis, reasoning or limited experiments on the basis of the prior art according to the concept of the present invention shall fall within the protection scope determined by the claims.

Claims (6)

1.一种利用单籽晶桥式结构诱导生长REBCO超导块材的方法,其特征在于,所述方法包括以下步骤:1. a method utilizing single seed crystal bridge structure to induce growth of REBCO superconducting bulk material, is characterized in that, described method comprises the following steps: 步骤一,按照RE:Ba:Cu=1:2:3和RE:Ba:Cu=2:1:1的比例将RE2O3,BaCO3和CuO粉末配制成RE123和RE211的原始粉末;Step 1, according to the ratio of RE:Ba:Cu=1:2:3 and RE:Ba:Cu=2:1:1, RE 2 O 3 , BaCO 3 and CuO powders are prepared into original powders of RE123 and RE211; 步骤二,将所述原始粉料充分混合均匀,在空气环境下900℃烧结48小时;将烧结后的粉末再次研磨、烧结,相同工艺共重复三次;In step 2, the original powder is fully mixed and sintered at 900° C. for 48 hours in an air environment; the sintered powder is ground and sintered again, and the same process is repeated three times in total; 步骤三,将步骤二获得的RE123粉末和RE211粉末按照RE123+30mol%RE211+1wt%CeO2的组分配料,充分碾磨混合均匀,得到前驱粉料;In step 3, the RE123 powder and RE211 powder obtained in step 2 are prepared according to the components of RE123+30mol% RE211+1wt% CeO 2 , fully milled and mixed uniformly to obtain precursor powder; 步骤四,根据模具直径不同,将所述粉料称取合适质量,放入模具,压制成圆柱形状的籽晶桥1个、缓冲层2~3个和前驱体1个;所述籽晶桥的直径为10mm,称量0.6g压制;所述缓冲层的直径为5mm,称量0.15~0.2g压制;所述前驱体的直径大于等于30mm;Step 4: According to the different diameters of the molds, the powder is weighed into a suitable mass, put into the mold, and pressed into one cylindrical seed bridge, 2 to 3 buffer layers and one precursor; the seed bridge The diameter of the buffer layer is 10mm, weighing 0.6g for pressing; the diameter of the buffer layer is 5mm, weighing 0.15-0.2g for pressing; the diameter of the precursor is greater than or equal to 30mm; 步骤五,将籽晶、籽晶桥、缓冲层、前驱体从上至下依次放置;所述籽晶、所述籽晶桥、所述缓冲层构成单籽晶桥式结构;其中,所述籽晶放置在所述籽晶桥的上表面中心,所述籽晶桥搭设在所述缓冲层上方,所述缓冲层沿所述籽晶[110]晶向排列成一列;Step 5, place the seed crystal, the seed crystal bridge, the buffer layer, and the precursor in sequence from top to bottom; the seed crystal, the seed crystal bridge, and the buffer layer form a single-seed crystal bridge structure; wherein, the The seed crystal is placed in the center of the upper surface of the seed crystal bridge, the seed crystal bridge is erected above the buffer layer, and the buffer layer is arranged in a row along the [110] crystal direction of the seed crystal; 步骤六,将所述前驱体和所述单籽晶桥式结构置于生长炉中进行顶部籽晶熔融织构生长,以实现(110)∥(110)取向诱导生长REBCO超导块材。In step 6, the precursor and the single-seed bridge structure are placed in a growth furnace for melting and texture growth of the top seed crystal, so as to achieve (110)∥(110) orientation induced growth of REBCO superconducting bulk material. 2.根据权利要求1所述的方法,其特征在于:所述顶部籽晶熔融织构生长工艺包括以下步骤:2. The method according to claim 1, wherein the top seed melt texture growth process comprises the following steps: 使所述生长炉内的温度在第一时间内升至第一温度,保温1~3小时;raising the temperature in the growth furnace to the first temperature within the first time, and keeping the temperature for 1-3 hours; 使所述生长炉内的温度在第二时间内升至第二温度,保温1~3小时;raising the temperature in the growth furnace to a second temperature within a second time, and keeping the temperature for 1 to 3 hours; 使所述生长炉内的温度在第三时间内降至第三温度;lowering the temperature in the growth furnace to a third temperature within a third time; 使所述生长炉内的温度在第四时间内降至第四温度;reducing the temperature in the growth furnace to a fourth temperature within a fourth time; 最后淬火,获得REBCO超导块材。Finally, quenched to obtain REBCO superconducting bulk. 3.根据权利要求2所述的方法,其特征在于:所述第一时间为3~5小时,所述第一温度为850~950℃;所述第二时间为1~2小时,所述第二温度高于所述REBCO超导材料的包晶反应温度40~80℃;所述第三时间为0.5~1小时,所述第三温度为所述REBCO材料的包晶反应温度;所述第四时间为10~80小时,所述第四温度低于所述包晶反应温度5~40℃。3 . The method according to claim 2 , wherein: the first time is 3-5 hours, the first temperature is 850-950° C.; the second time is 1-2 hours, the The second temperature is 40-80°C higher than the peritectic reaction temperature of the REBCO superconducting material; the third time is 0.5-1 hour, and the third temperature is the peritectic reaction temperature of the REBCO material; the The fourth time is 10-80 hours, and the fourth temperature is 5-40° C. lower than the peritectic reaction temperature. 4.根据权利要求1所述的方法,其特征在于:所述籽晶为c轴取向,所述籽晶为NdBCO/MgO或NdBCO/YBCO/MgO薄膜籽晶。4 . The method according to claim 1 , wherein the seed crystal is c-axis oriented, and the seed crystal is an NdBCO/MgO or NdBCO/YBCO/MgO thin film seed crystal. 5 . 5.根据权利要求1所述的方法,其特征在于:所述籽晶的尺寸为2mm×2mm。5 . The method according to claim 1 , wherein the size of the seed crystal is 2 mm×2 mm. 6 . 6.根据权利要求1所述的方法,其特征在于:所述RE为Y、Gd、Sm或Nd。6. The method according to claim 1, wherein the RE is Y, Gd, Sm or Nd.
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