KR0157625B1 - The fabrication method of high temperature superconductor thin film by bismuth diffusion - Google Patents
The fabrication method of high temperature superconductor thin film by bismuth diffusionInfo
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- KR0157625B1 KR0157625B1 KR1019900017561A KR900017561A KR0157625B1 KR 0157625 B1 KR0157625 B1 KR 0157625B1 KR 1019900017561 A KR1019900017561 A KR 1019900017561A KR 900017561 A KR900017561 A KR 900017561A KR 0157625 B1 KR0157625 B1 KR 0157625B1
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- H10N60/00—Superconducting devices
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Abstract
본 발명은 Bi확산에 의한 고온 초전도 박막의 제조방법에 관한 것으로, 좀더 구체적으로 Pb를 첨가한 PbxSr2Ca2Cu4Oy기판에 Bi를 진공증착한 후, 적당한 온도에서 열처리하여 100K이상의 임계온도를 갖는 고온 초전도 박막의 제조방법에 관한 것이다.The present invention relates to a method for manufacturing a high temperature superconducting thin film by Bi diffusion, and more specifically, by vacuum deposition of Bi on a Pb x Sr 2 Ca 2 Cu 4 O y substrate with Pb, heat treatment at an appropriate temperature of 100K or more It relates to a method for producing a high temperature superconducting thin film having a critical temperature.
Sr:Ca:Cu=2:2:4 이고 Pb를 첨가한 것으로서 Bi계 초전도체와 결정구조 및 열팽창율이 유사한 PbxSr2Ca2Cu4Oy(0×0.5)화합물 기판에 Bi를 증착하고 800~850℃에서 열처리하여 본 발명의 고온 초전도 박막을 제조한다.Bi was deposited on a Pb x Sr 2 Ca 2 Cu 4 O y (0 × 0.5) compound substrate with Sr: Ca: Cu = 2: 2: 4 and Pb added and similar in crystal structure and thermal expansion rate to the Bi-based superconductor. Heat treatment at 800 ~ 850 ℃ to prepare a high temperature superconducting thin film of the present invention.
Description
제1도는 본 발명에 따른 고온 초전도 박막의 제조공정도를 나타내는 것이다.Figure 1 shows a manufacturing process diagram of the high temperature superconducting thin film according to the present invention.
* 도면의 주요부분에 대한 부호의 설명* Explanation of symbols for main parts of the drawings
1 : PbxSr2Ca2Cu4Oy기판2 : Bi금속층1: Pb x Sr 2 Ca 2 Cu 4 O y substrate 2: Bi metal layer
3 : Bi2-xPbxSr2Ca2Cu3Oy고온초전도 박막3: Bi 2-x Pb x Sr 2 Ca 2 Cu 3 O y high temperature superconducting thin film
본 발명은 Bi확산에 의한 고온 초전도 박막의 제조방법에 관한 것으로, 좀더 구체적으로 Pb를 첨가한 PbxSr2Ca2Cu4Oy기판에 Bi를 진공증착한 후, 적당한 온도에서 열처리하여 100K이상의 임계온도를 갖는 고온 초전도 박막의 제조방법에 관한 것이다.The present invention relates to a method for manufacturing a high temperature superconducting thin film by Bi diffusion, and more specifically, by vacuum deposition of Bi on a Pb x Sr 2 Ca 2 Cu 4 O y substrate with Pb, heat treatment at an appropriate temperature of 100K or more It relates to a method for producing a high temperature superconducting thin film having a critical temperature.
고온 초전도 박막을 제조하기 위한 기판으로서 종래에는 SrTiO3, MgO등과 같은 단결정 기판을 사용하든가 또는 알루미늄 기판을 사용하여 왔으나, 이들 기판들은 값이 비싸거나 고온 초전도 특성을 발현하는데 좋지 못한 결과를 가져왔다.Conventionally, a single crystal substrate such as SrTiO 3 , MgO, or an aluminum substrate has been used as a substrate for manufacturing a high temperature superconducting thin film, but these substrates are expensive or have poor results in expressing high temperature superconducting properties.
또한, 초전도 박막을 제조하는 방법으로는 마그네트론 스퍼터링(Magnetron Sputtering), 레이저 애브래이션(Laser Ablation), 전자 비임 증착(Electron Beam Evaporation) 및 화학적인 증착(Chemical Vapor Deposition)등이 있으나, 이들 방법은 조성 제어가 어렵고 대부분 고가의 설비를 사용해야 하는 단점이 있었다.In addition, a method of manufacturing a superconducting thin film may include magnetron sputtering, laser ablation, electron beam evaporation, and chemical vapor deposition. Composition control was difficult and mostly had the disadvantage of using expensive equipment.
따라서, 본 발명의 목적은 고가의 설비를 필요로하지 않을 뿐만 아니라 값이 싼 기판을 사용하여 고온 초전도 박막을 제조하는 방법을 제공하는데 있다.Accordingly, it is an object of the present invention to provide a method of manufacturing a high temperature superconducting thin film using a cheap substrate as well as not requiring expensive equipment.
본 발명의 목적을 달성하기 위하여 Bi계 고온 초전도체와 격자상수 및 열팽창율이 유사한 Pb를 첨가한 PbxSr2Ca2Cu3Oy(O×0.5)기판에 진공증착한 후, 대기중에서 800~850℃의 온도로 열처리하여 Bi를 기판으로 확산시킴으로서 100k 이상의 임계온도를 갖는 Bi2-xPbxSr2Ca2Cu3Oy고온 초전도 박막을 제조하였다.In order to achieve the object of the present invention, after vacuum deposition on a Pb x Sr 2 Ca 2 Cu 3 O y (O x 0.5) substrate containing a Bi-based high-temperature superconductor Pb similar in lattice constant and thermal expansion rate, 800 ~ in the air By heat treatment at a temperature of 850 ℃ to diffuse Bi into the substrate to prepare a Bi 2-x Pb x Sr 2 Ca 2 Cu 3 O y high temperature superconducting thin film having a critical temperature of 100k or more.
또한, Pb를 증착시 Bi에 혼합하여 증착할 경우, 열처리 과정에서 Pb 또는 PbO가 거의 증발되어 Pb첨가에 따른 효과가 별로 발생되지 않으므로 기판 제조시 Pb를 첨가하여 열처리시에 발생하는 상기 단점을 해결하였다.In addition, when Pb is deposited by mixing with Bi during deposition, Pb or PbO is almost evaporated during the heat treatment process, so that the effect of Pb addition is not generated much. It was.
본 발명을 좀더 구체적으로 설명하면 다음과 같다.The present invention will be described in more detail as follows.
먼저 PbxSr2Ca2Cu4Oy(O×0.5)기판을 종래의 고상반응법으로 제조한다. 즉, Pb:Sr:Ca:Cu=X:2:2:4 (0×0.5) 가 되도록 칭량하여 미분으로 분쇄하여 완전히 섞이도록 한 다음, 공기중에서 900℃로 12시간동안 하소 (calcination)한후, 분쇄하여 분말로 제조하고 압력을 가하여 일정한 형태로 성형한다. 성형체를 공기중에서 950℃로 12시간동안 소결(sintering)하여 냉각시켜 PbxSr2Ca2Cu4Oy기판을 제조하였다.First, a Pb x Sr 2 Ca 2 Cu 4 O y (O x 0.5) substrate is manufactured by a conventional solid phase reaction method. That is, Pb: Sr: Ca: Cu = X: 2: 2: 4 (0 × 0.5) is weighed and pulverized into fine powder to be thoroughly mixed, and then calcined at 900 ° C. in air for 12 hours. It is pulverized, made into a powder, and molded into a constant shape by applying pressure. The molded body was sintered at 950 ° C. in air for 12 hours and cooled to prepare a Pb × Sr 2 Ca 2 Cu 4 O y substrate.
제조된 PbxSr2Ca2Cu4Oy기판상에 Bi를 진공증착기를 사용하여 0.5~1.0μm의 두께로 증착한 후, 대기중에서 800~850℃의 온도로 1시간동안 열처리하여 Bi를 기판으로 확산시켜 Bi:Pb:Sr:Ca:Cu=2-x:x:2:2:3(0x0.5)인 Bi2-xPbxSr2Ca2Cu3Oy고온 초전도 박막을 제조하였다.After depositing Bi on the prepared Pb x Sr 2 Ca 2 Cu 4 O y substrate using a vacuum evaporator to a thickness of 0.5 ~ 1.0μm, and heat treatment at 800 ~ 850 ℃ temperature in the air for 1 hour to substrate Bi Bi -x Pb x Sr 2 Ca 2 Cu 3 O y high-temperature superconducting thin film having Bi: Pb: Sr: Ca: Cu = 2-x: x: 2: 2: 3 (0x0.5) was prepared. .
기판 제조공정중에서 기판의 조성으로 Pb를 첨가함으로서 고온 초전도상의 형성을 촉진시켜 형성되는 초전도 박막의 임계온도(Tc)를 향상시켰을 뿐만 아니라, Bi증착시 Pb를 첨가하는 방법에서 발생되는 Pb(융점:327.3℃)와 PbO(융점=820℃)의 증발을 방지하였으며, 열부석 결과로 부터알수 있는 바와같이 223조성보다 융점이 낮으며 Cu를 과량으로 하는 것이 고온 초전도상 형성에 효과적이므로 기판의 조성을 Sr:Ca:Cu=2:2:4로 함으로서 기판의 융점을 저하시켜 Bi증착후 열처리시 열처리의 온도를 낮추었다.The addition of Pb to the composition of the substrate during the substrate manufacturing process not only improved the critical temperature (Tc) of the superconducting thin film formed by promoting the formation of a high temperature superconducting phase, but also caused the Pb (melting point: 327.3 ℃) and PbO (melting point = 820 ℃) to prevent the evaporation, as can be seen from the heat stone results, the melting point is lower than the 223 composition and the excess Cu is effective in the formation of high temperature superconducting phase, Sr By lowering the melting point of the substrate by setting: Ca: Cu = 2: 2: 4, the temperature of the heat treatment during the heat treatment after Bi deposition was lowered.
본 발명의 초전도 박막은 Bi의 확산에 의해 결정구조가 형성되므로 다른 고온 초전도상에 비해서 안정한 고온 초전도상인 2223상이 자연적으로 형성된다.In the superconducting thin film of the present invention, since the crystal structure is formed by the diffusion of Bi, the 2223 phase, which is a stable high temperature superconducting phase, is naturally formed as compared with other high temperature superconducting phases.
또한, 본 발명의 고온 초전도 박막 제조방법은 기판으로서 Bi계 초전도체와 결정구조 및 열팽창율이 유사한 PbxSr2Ca2Cu4Oy(O×0.5)화합물을 사용함으로서 열처리시 박리되는 문제점을 해결하였다.In addition, the method of manufacturing a high temperature superconducting thin film of the present invention solves the problem of peeling during heat treatment by using a Pb x Sr 2 Ca 2 Cu 4 O y (O x 0.5) compound having similar crystal structure and thermal expansion coefficient as Bi-based superconductor as a substrate. It was.
다음의 실시예는 본 발명에 다른 고온 초전도 박막의 제조방법을 좀더 구체적으로 설명하는 것이지만, 본 발명의 범주를 한정하는 것은 아니다.The following examples further illustrate the method of manufacturing a high temperature superconducting thin film according to the present invention in more detail, but do not limit the scope of the present invention.
[실시예 1]Example 1
Pb:Sr:Ca:Cu=x:2:2:4(0×0.5)의 비율이 되도록 저울로 정확히 측정하여 통상의 분쇄기에서 평균입도가 10μm이하가 되도록 분쇄하고 각각의 성분들이 균일하게 혼합되도록 혼합한다.Pb: Sr: Ca: Cu = x: 2: 2: 4 (0 × 0.5), precisely measured with a balance, pulverized to an average particle size of 10 μm or less in a conventional mill, and uniformly mixed with each component. Mix.
혼합된 조성물을 900℃의 온도에서 12시간동안 가열하여 하소(calcination)한 다음, 다시 분쇄하여 분말로 제조한 후, 3톤의 압력을 가하여 판상으로 성형한다. 성형체를 950℃온도에서 12시간동안 소결함으로서 PbxSr2Ca2Cu4Oy기판을 제조한다.The mixed composition is calcined by heating at a temperature of 900 ° C. for 12 hours, then pulverized to form a powder, and then molded into a plate by applying a pressure of 3 tons. The Pb x Sr 2 Ca 2 Cu 4 O y substrate was prepared by sintering the molded body at a temperature of 950 ° C for 12 hours.
제조된 기판에 진공증착기를 사용하여 Bi를 0.5μm의 두께로 증착한 다음, 850℃에서 1시간동안 열처리를 행하여 기판으로 Bi를 확산시켜 Bi2-xPbxSr2Ca2Cu3Oy초전도 박막을 제조하였다Bi was deposited to a thickness of 0.5 μm using a vacuum evaporator on the substrate, and then heat-treated at 850 ° C. for 1 hour to diffuse Bi into the substrate, thereby obtaining Bi 2-x Pb x Sr 2 Ca 2 Cu 3 O y superconductivity. A thin film was prepared
상술한 바와같이, 본 발명의 초전도 박막은 진공증착기만을 사용하여 제조하므로 종래의 박막 제조를 위한 고가의 설비가 필요 었으며, 공정이 용이하며, Bi계 초전도체와 결정구조 및 열팽창률이 유사한 PbxSr2Ca2Cu4Oy(0×0.5)화합물을 기판으로 사용함으로서 종래의 단결정 기판을 사용한 초전도 박막에 비하여 특성면에서 매우 뛰어나고, 본발명의 초전도 박막은 Bi확산에 의해 결정 구조가 형성되므로 다른 초전도상에 비해서 안정한 2223고온 초전도상이 형성된다.As described above, since the superconducting thin film of the present invention is manufactured using only a vacuum evaporator, an expensive facility for manufacturing a conventional thin film is required, and the process is easy, and Pb x Sr having a crystal structure and thermal expansion coefficient similar to that of the Bi-based superconductor is required. By using 2 Ca 2 Cu 4 O y (0 × 0.5) compound as a substrate, it is very excellent in characteristics compared to the superconducting thin film using a conventional single crystal substrate, and the superconducting thin film of the present invention has a crystal structure formed by Bi diffusion, A stable 2223 high temperature superconducting phase is formed compared to the superconducting phase.
또한, Pb를 기판의 조성으로 첨가함으로서 Bi증착시 Pb를 첨가할 경우에 발생되는 Pb 및 PbO증발을 방지 하였고 Sr:Ca:Cu=2:2:4로 함으로서 기판의 융점을 저하시켜 열처리 온도를 낮추었고,이로 인하여 고온 초전도상의 형성이 효과적이다.In addition, by adding Pb as a substrate composition, Pb and PbO evaporation generated when Pb was added during Bi deposition was prevented. Sr: Ca: Cu = 2: 2: 4 was used to lower the melting point of the substrate to reduce the heat treatment temperature. Lower, which makes the formation of high temperature superconducting phases effective.
한편, 본 발명의 초전도 박막은 소자 패턴(pattern)제작시, 열처리 전에 Bi를 에칭(etching)함으로서 패턴(pattern)제작시 발생되는 화학제제(chemical)에 의한 특성 저하를 방지할 수 있으므로 소자 패턴 제작이 용이하다.On the other hand, the superconducting thin film of the present invention can prevent the deterioration of characteristics due to chemicals generated during the pattern production by etching Bi before heat treatment during the production of the device pattern (pattern), the device pattern production This is easy.
본 발명의 방법으로 제조된 고온 초전도 박막은 센서(sensor), 컴퓨터 메모리셀(computer memory cell), 스위칭 디바이스(switching) 및 방사선 검출기(radiation detector)등에 응용할 수 있다.The high temperature superconducting thin film manufactured by the method of the present invention can be applied to a sensor, a computer memory cell, a switching device, a radiation detector and the like.
Claims (3)
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