CN110277493A - A Novel Multilayer Structure with Lower Leakage - Google Patents
A Novel Multilayer Structure with Lower Leakage Download PDFInfo
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- 230000007704 transition Effects 0.000 claims abstract description 33
- 239000010409 thin film Substances 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 230000002929 anti-fatigue Effects 0.000 claims 1
- 239000010408 film Substances 0.000 abstract description 45
- 239000000969 carrier Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 80
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 48
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 48
- 239000002243 precursor Substances 0.000 description 29
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 16
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 16
- 238000010438 heat treatment Methods 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 14
- 238000003756 stirring Methods 0.000 description 13
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 12
- 230000005291 magnetic effect Effects 0.000 description 12
- 229910001220 stainless steel Inorganic materials 0.000 description 12
- 239000010935 stainless steel Substances 0.000 description 12
- 238000000137 annealing Methods 0.000 description 10
- 238000005485 electric heating Methods 0.000 description 9
- 229960000583 acetic acid Drugs 0.000 description 8
- 239000012362 glacial acetic acid Substances 0.000 description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 description 8
- 229910002902 BiFeO3 Inorganic materials 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000005621 ferroelectricity Effects 0.000 description 2
- 230000005307 ferromagnetism Effects 0.000 description 2
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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Abstract
本发明通过构筑多层结构的过渡层来达到降低薄膜漏电流的目的。构筑的多层结构基底层选用Pt片，过渡层材料为Sr2Bi4Ti5O18，薄膜层材料为BiFeO3和Sr2Bi4Ti5O18。一方面Sr2Bi4Ti5O18材料本身具有较小的漏电特性，组成多层结构之后，阻断了载流子在BiFeO3薄膜和Pt电极间的移动，使得比直接沉积在ITO上BiFeO3薄膜的漏电流小；另一方面Sr2Bi4Ti5O18和BiFeO3两相的界面处特殊的接触状态，也抑制了薄膜载流子的运动，使得比直接沉积在ITO上BiFeO3薄膜的漏电流小。The invention achieves the purpose of reducing the thin film leakage current by constructing the transition layer of the multilayer structure. The base layer of the constructed multilayer structure is made of Pt sheet, the material of the transition layer is Sr 2 Bi 4 Ti 5 O 18 , and the material of the thin film layer is BiFeO 3 and Sr 2 Bi 4 Ti 5 O 18 . On the one hand, the Sr 2 Bi 4 Ti 5 O 18 material itself has small leakage characteristics. After forming a multilayer structure, it blocks the movement of carriers between the BiFeO 3 film and the Pt electrode, making it easier to deposit BiFeO on ITO than directly deposited on ITO. 3 The leakage current of the thin film is small; on the other hand, the special contact state at the interface between Sr 2 Bi 4 Ti 5 O 18 and BiFeO 3 also inhibits the movement of carriers in the thin film, making BiFeO 3 directly deposited on ITO Thin film leakage current is small.
Description
技术领域technical field
本发明属于电子陶瓷技术领域，具体涉及一种用于铁电存储器件的新型具有较低漏电流的多层结构及其制备方法。The invention belongs to the technical field of electronic ceramics, and in particular relates to a novel multilayer structure with lower leakage current for ferroelectric storage devices and a preparation method thereof.
背景技术Background technique
BiFeO3是一种集铁电性和铁磁性于一体的单相多铁材料，室温下具有铁电有序和反铁磁有序，且铁电性和铁磁性之间存在耦合效应。BiFeO3的理论剩余极化强度很高，而结晶温度较低，这些使得BiFeO3在高温信息存储、传感器和微机电系统等多功能器件中有巨大的应用价值。BiFeO 3 is a single-phase multiferroic material integrating ferroelectricity and ferromagnetism. It has ferroelectric order and antiferromagnetic order at room temperature, and there is a coupling effect between ferroelectricity and ferromagnetism. The theoretical remnant polarization of BiFeO 3 is very high, and the crystallization temperature is low, which makes BiFeO 3 have great application value in multifunctional devices such as high-temperature information storage, sensors and micro-electromechanical systems.
纯相BiFeO3薄膜的制备温度范围很窄，烧结过程中不可避免的出现Bi2O3、Bi2Fe4O9等杂相，同时高温下的Bi元素容易挥发和Fe3+容易变价成为Fe2+，这都会导致大量氧空位使BiFeO3样品的漏电流密度很大。由于漏电流严重，施加在BiFeO3 薄膜上的有效电场就会很小，导致铁电畴无法翻转，甚至在很低的电压下材料就被击穿，无法显示其优良的铁电性能。The preparation temperature range of the pure phase BiFeO 3 thin film is very narrow, and impurity phases such as Bi 2 O 3 and Bi 2 Fe 4 O 9 inevitably appear during the sintering process. At the same time, the Bi element is easy to volatilize and Fe 3+ is easy to change into Fe at high temperature. 2+ , which will lead to a large number of oxygen vacancies and make the leakage current density of BiFeO 3 samples very large. Due to the serious leakage current, the effective electric field applied to the BiFeO3 thin film will be very small, resulting in the failure of the ferroelectric domain to flip, and the material will be broken down even at a very low voltage, failing to show its excellent ferroelectric properties.
目前改善BiFeO3薄膜性能的方法主要有控制薄膜取向、元素掺杂，构筑多层结构等。现有的构筑多层结构的研究中所选用的过渡层与所制备的薄膜样品的失配度很小，构筑多层结构时过渡层的厚度较大，这将降低施加在BiFeO3基薄膜上的有效电场强度。因此，需要寻找一种有效降低薄膜漏电流，构筑多层结构的过渡层材料。而Sr2Bi4Ti5O18材料具有较低的漏电流，与BiFeO3的失配度较小。At present, the methods to improve the properties of BiFeO 3 films mainly include controlling the film orientation, element doping, and building multilayer structures. The mismatch between the transition layer selected in the existing research on building a multilayer structure and the prepared film sample is very small, and the thickness of the transition layer is relatively large when building a multilayer structure, which will reduce the thickness of the transition layer applied on the BiFeO 3 -based film. effective electric field strength. Therefore, it is necessary to find a transition layer material that can effectively reduce the leakage current of the film and build a multilayer structure. The Sr 2 Bi 4 Ti 5 O 18 material has a lower leakage current and a smaller mismatch with BiFeO 3 .
发明内容Contents of the invention
本发明的目的在于提供一种与BiFeO3失配度较小，厚度较小，能够有效降低BiFeO3薄膜漏电性能的过渡层材料，构筑多层结构。The purpose of the present invention is to provide a transition layer material with a small mismatch with BiFeO 3 and a small thickness, which can effectively reduce the leakage performance of the BiFeO 3 film, and build a multi-layer structure.
本发明的技术方案为：一种新型的具有较低漏电流的多层结构，它包括由下至上依次设置基底层、过渡层、BiFeO3层和Sr2Bi4Ti5O18层，基底层选用Pt片，过渡层材料为Sr2Bi4Ti5O18，薄膜层材料为BiFeO3和Sr2Bi4Ti5O18。The technical solution of the present invention is: a novel multi-layer structure with lower leakage current, which includes a base layer, a transition layer, a BiFeO 3 layer and a Sr 2 Bi 4 Ti 5 O 18 layer arranged sequentially from bottom to top, and the base layer A Pt sheet is selected, the material of the transition layer is Sr 2 Bi 4 Ti 5 O 18 , and the material of the thin film layer is BiFeO 3 and Sr 2 Bi 4 Ti 5 O 18 .
本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中Sr2Bi4Ti5O18过渡层和薄膜层前驱体溶液的制备工艺，以硝酸铋，乙酸锶，乙二醇，乙酰丙酮，钛酸四丁酯为原料，采用溶胶-凝胶法合成，具体步骤如下：The preparation process of Sr 2 Bi 4 Ti 5 O 18 transition layer and thin film layer precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, with bismuth nitrate, strontium acetate , ethylene glycol, acetylacetone, tetrabutyl titanate as raw materials, using sol-gel synthesis, the specific steps are as follows:
（1）以钛酸四丁酯和乙酰丙酮按照体积比为1:1的比例配制A溶液：钛酸四丁酯乙酰丙酮缓缓滴入乙酰丙酮溶液中，将混合好的溶液继续搅拌24小时，得到澄清黄褐色透明的A溶液；(1) Prepare solution A with tetrabutyl titanate and acetylacetone at a volume ratio of 1:1: slowly drop tetrabutyl titanate acetylacetone into the acetylacetone solution, and continue to stir the mixed solution for 24 hours , to obtain a clear yellow-brown transparent A solution;
（2）称量1.2g乙酸锶、5.9g硝酸铋、18.8ml乙二醇，将三者充分混合，放置在多头磁力搅拌器上搅拌24小时，得到透明的B溶液；(2) Weigh 1.2g of strontium acetate, 5.9g of bismuth nitrate, and 18.8ml of ethylene glycol, mix the three thoroughly, place them on a multi-head magnetic stirrer and stir for 24 hours to obtain a transparent B solution;
（3）将B溶液缓缓加入到A溶液中，将混合后的溶液充分搅拌24小时，得到淡黄色的溶液C；(3) Slowly add solution B to solution A, and stir the mixed solution thoroughly for 24 hours to obtain light yellow solution C;
（4）将C溶液静置24小时，得到Sr2Bi4Ti5O18前驱体溶液。(4) Let the C solution stand for 24 hours to obtain the Sr 2 Bi 4 Ti 5 O 18 precursor solution.
本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中BiFeO3层前驱体溶液的制备工艺，以硝酸铋，硝酸铁，冰乙酸，乙酰丙酮，乙二醇为原料，采用溶胶-凝胶法合成，具体步骤如下：The preparation process of BiFeO 3 -layer precursor solution in the novel multi-layer structure with lower leakage current for ferroelectric memory devices described in the present invention, with bismuth nitrate, iron nitrate, glacial acetic acid, acetylacetone, ethylene glycol As a raw material, it is synthesized by a sol-gel method, and the specific steps are as follows:
（1）首先称量9.2g硝酸铋，量取5ml乙二醇、15ml冰乙酸作为溶剂充分混合，放置在多头磁力搅拌器上充分搅拌8小时，得到透明溶液；(1) First weigh 9.2g of bismuth nitrate, measure 5ml of ethylene glycol and 15ml of glacial acetic acid as solvents and mix them thoroughly, place them on a multi-head magnetic stirrer and stir for 8 hours to obtain a transparent solution;
（2）量取40ml乙酰丙酮加入到（1）中得到的透明溶液中，称量7.4g硝酸铁也加入到（1）中得到的透明溶液中。在多头磁力搅拌器上搅拌24小时得到暗红色半透明BiFeO3前驱体溶液；(2) Measure 40ml of acetylacetone and add it to the transparent solution obtained in (1), and weigh 7.4g of ferric nitrate and add it to the transparent solution obtained in (1). Stirred on multi-head magnetic stirrer for 24 hours to obtain dark red translucent BiFeO 3 precursor solution;
（3）将前驱体溶液常温下静置24小时。(3) Let the precursor solution stand at room temperature for 24 hours.
本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构的制备工艺，具体步骤如下：The preparation process of the novel multi-layer structure with lower leakage current for ferroelectric memory devices described in the present invention, the specific steps are as follows:
（1）将过渡层Sr2Bi4Ti5O18前驱体溶液均匀的旋涂在Pt/Ti/SiO2/Si（100）衬底上，继而放到200℃不锈钢电热板上烘干2-3min；(1) Evenly spin-coat the transition layer Sr 2 Bi 4 Ti 5 O 18 precursor solution on the Pt/Ti/SiO 2 /Si (100) substrate, and then put it on a stainless steel electric heating plate at 200 ° C for 2- 3min;
（2）将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s；(2) Place the preliminarily dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s;
（3）重复上述步骤（1）-（2）多次，直到得到一定厚度的过渡层；(3) Repeat the above steps (1)-(2) multiple times until a transition layer of a certain thickness is obtained;
（4）将BiFeO3前驱体溶液均匀的旋涂在过渡层上，继而放到200℃不锈钢电热板上烘干2-3min；(4) Evenly spin-coat the BiFeO 3 precursor solution on the transition layer, and then put it on a 200°C stainless steel electric heating plate to dry for 2-3min;
（5）将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到500℃保温300s；(5) Place the pre-dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 500°C for 300s;
（6）重复上述步骤（3）-（4）多次，直到得到一定厚度的BiFeO3薄膜层；(6) Repeat the above steps (3)-(4) multiple times until a certain thickness of BiFeO 3 film layer is obtained;
（7）将Sr2Bi4Ti5O18前驱体溶液均匀的旋涂在BFO薄膜层上，继而放到200℃不锈钢电热板上烘干2-3min；(7) Spin-coat the Sr 2 Bi 4 Ti 5 O 18 precursor solution evenly on the BFO film layer, and then put it on a stainless steel heating plate at 200°C for 2-3 minutes to dry;
（8）将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s；(8) Put the pre-dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s;
（9）重复上述步骤（7）-（8）多次，直到得到一定厚度的Sr2Bi4Ti5O18薄膜层。(9) Repeat the above steps (7)-(8) for several times until a certain thickness of Sr 2 Bi 4 Ti 5 O 18 film layer is obtained.
本发明用于铁电存储器件的新型具有较低漏电流的多层结构，较现有的结构具有以下的优点：The novel multi-layer structure with lower leakage current used in the ferroelectric storage device of the present invention has the following advantages compared with the existing structure:
1、过渡层选用的Sr2Bi4Ti5O18材料本身具有较小的漏电特性，组成多层结构之后，阻断了载流子在BiFeO3薄膜和Pt电极间的移动，使得比直接沉积在ITO上BiFeO3薄膜的漏电流小；1. The Sr 2 Bi 4 Ti 5 O 18 material used for the transition layer itself has small leakage characteristics. After forming a multi-layer structure, it blocks the movement of carriers between the BiFeO 3 film and the Pt electrode, making it easier to deposit than direct deposition The leakage current of BiFeO 3 film on ITO is small;
2、Sr2Bi4Ti5O18和BiFeO3两相的界面处特殊的接触状态，也抑制了薄膜载流子的运动，使得比直接沉积在ITO上BiFeO3薄膜的漏电流小。2. The special contact state at the interface of Sr 2 Bi 4 Ti 5 O 18 and BiFeO 3 phases also inhibits the movement of carriers in the film, making the leakage current smaller than that of BiFeO 3 films deposited directly on ITO.
附图说明Description of drawings
附图1为本发明中沉积到130nm厚Sr2Bi4Ti5O18过渡层的BiFeO3-Sr2Bi4Ti5O18薄膜和直接沉积到ITO上BiFeO3薄膜漏电流密度曲线图。Accompanying drawing 1 is the leakage current density curve of the BiFeO 3 -Sr 2 Bi 4 Ti 5 O 18 film deposited to the 130nm thick Sr 2 Bi 4 Ti 5 O 18 transition layer and the BiFeO 3 film directly deposited on ITO in the present invention.
附图2为本发明中沉积到260nm厚Sr2Bi4Ti5O18过渡层的BiFeO3-Sr2Bi4Ti5O18薄膜和直接沉积到ITO上BiFeO3薄膜漏电流密度曲线图。Accompanying drawing 2 is the leakage current density curve of the BiFeO 3 -Sr 2 Bi 4 Ti 5 O 18 film deposited to the 260nm thick Sr 2 Bi 4 Ti 5 O 18 transition layer and the BiFeO 3 film directly deposited on ITO in the present invention.
附图3为本发明中沉积到390nm厚Sr2Bi4Ti5O18过渡层的BiFeO3-Sr2Bi4Ti5O18薄膜和直接沉积到ITO上BiFeO3薄膜漏电流密度曲线图。Accompanying drawing 3 is the leakage current density curve of the BiFeO 3 -Sr 2 Bi 4 Ti 5 O 18 thin film deposited to a 390nm thick Sr 2 Bi 4 Ti 5 O 18 transition layer and the BiFeO 3 thin film directly deposited on ITO in the present invention.
具体实施方式Detailed ways
实施案例1Implementation Case 1
（1）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中Sr2Bi4Ti5O18过渡层和薄膜层前驱体溶液的制备工艺，以硝酸铋，乙酸锶，乙二醇，乙酰丙酮，钛酸四丁酯为原料，采用溶胶-凝胶法合成，具体步骤如下：以钛酸四丁酯和乙酰丙酮按照体积比为1:1的比例配制A溶液：钛酸四丁酯乙酰丙酮缓缓滴入乙酰丙酮溶液中，将混合好的溶液继续搅拌24小时，得到澄清黄褐色透明的A溶液；称量1.2g乙酸锶、5.9g硝酸铋、18.8ml乙二醇，将三者充分混合，放置在多头磁力搅拌器上搅拌24小时，得到透明的B溶液；将B溶液缓缓加入到A溶液中，将混合后的溶液充分搅拌24小时，得到淡黄色的溶液C；将C溶液静置24小时，得到Sr2Bi4Ti5O18前驱体溶液。(1) The preparation process of the Sr 2 Bi 4 Ti 5 O 18 transition layer and thin film layer precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, using bismuth nitrate , strontium acetate, ethylene glycol, acetylacetone, and tetrabutyl titanate are used as raw materials, and are synthesized by sol-gel method. The specific steps are as follows: prepare tetrabutyl titanate and acetylacetone at a volume ratio of 1:1 Solution A: Slowly drop tetrabutyl titanate acetylacetone into the acetylacetone solution, and continue to stir the mixed solution for 24 hours to obtain a clear, yellow-brown and transparent A solution; weigh 1.2g of strontium acetate, 5.9g of bismuth nitrate, 18.8ml of ethylene glycol, fully mixed the three, placed on a multi-head magnetic stirrer and stirred for 24 hours to obtain a transparent B solution; slowly added the B solution to the A solution, and fully stirred the mixed solution for 24 hours, A light yellow solution C was obtained; the solution C was left to stand for 24 hours to obtain a Sr 2 Bi 4 Ti 5 O 18 precursor solution.
（2）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中薄膜层BiFeO3前驱体溶液的制备工艺，以硝酸铋，硝酸铁，冰乙酸，乙酰丙酮，乙二醇为原料，采用溶胶-凝胶法合成，具体步骤如下：首先称量9.2g硝酸铋，量取5ml乙二醇、15ml冰乙酸作为溶剂充分混合，放置在多头磁力搅拌器上充分搅拌8小时，得到透明溶液；量取40ml乙酰丙酮加入到上文中得到的透明溶液中，称量7.4g硝酸铁也加入上文中得到的透明溶液中。在多头磁力搅拌器上搅拌24小时得到暗红色半透明BiFeO3溶液；将溶液常温下静置24小时得到BiFeO3的前驱体溶液。( 2 ) The preparation process of the thin film layer BiFeO3 precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, with bismuth nitrate, iron nitrate, glacial acetic acid, acetylacetone , ethylene glycol as raw material, using sol-gel synthesis, the specific steps are as follows: first weigh 9.2g of bismuth nitrate, measure 5ml of ethylene glycol, 15ml of glacial acetic acid as a solvent and mix them fully, place them on a multi-head magnetic stirrer to fully Stir for 8 hours to obtain a transparent solution; measure 40ml of acetylacetone and add to the above obtained transparent solution, weigh 7.4g of ferric nitrate and add to the above obtained transparent solution. Stir on a multi-head magnetic stirrer for 24 hours to obtain a dark red translucent BiFeO 3 solution; leave the solution at room temperature for 24 hours to obtain a BiFeO 3 precursor solution.
（3）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构的制备工艺，具体步骤如下：将Sr2Bi4Ti5O18过渡层前驱体溶液均匀的旋涂在Pt片基底上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s，重复上述步骤得到130nm厚的过渡层；将BiFeO3前驱体溶液均匀的旋涂在过渡层上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到500℃保温300s；重复上述步骤得到直到得到一定厚度的BiFeO3薄膜层；将Sr2Bi4Ti5O18薄膜层前驱体溶液均匀的旋涂在BiFeO3薄膜层上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s，重复上述步骤得到1000nm厚的BiFeO3-Sr2Bi4Ti5O18薄膜层。(3) The preparation process of the new multi-layer structure with lower leakage current for ferroelectric memory devices described in the present invention, the specific steps are as follows: uniformly mix the Sr 2 Bi 4 Ti 5 O 18 transition layer precursor solution Spin-coat on the Pt sheet substrate, and then place it on a 200°C stainless steel electric heating plate to dry for 2-3min; place the preliminarily dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s, repeat The above steps obtained a transition layer with a thickness of 130nm; evenly spin-coat the BiFeO 3 precursor solution on the transition layer, and then put it on a 200°C stainless steel electric heating plate to dry for 2-3min; Heat at 350°C for 180s in the furnace, then continue heating to 500°C for 300s; repeat the above steps until a certain thickness of BiFeO 3 film layer is obtained; evenly spin-coat the precursor solution of Sr 2 Bi 4 Ti 5 O 18 film layer on BiFeO 3 On the film layer, put it on a 200°C stainless steel heating plate and dry it for 2-3min; place the preliminarily dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s, repeat the above steps to get 1000nm thick BiFeO 3 -Sr 2 Bi 4 Ti 5 O 18 film layer.
实施案例2Implementation Case 2
（1）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中Sr2Bi4Ti5O18过渡层和薄膜层前驱体溶液的制备工艺，以硝酸铋，乙酸锶，乙二醇，乙酰丙酮，钛酸四丁酯为原料，采用溶胶-凝胶法合成，具体步骤如下：以钛酸四丁酯和乙酰丙酮按照体积比为1:1的比例配制A溶液：钛酸四丁酯乙酰丙酮缓缓滴入乙酰丙酮溶液中，将混合好的溶液继续搅拌24小时，得到澄清黄褐色透明的A溶液；称量1.2g乙酸锶、5.9g硝酸铋、18.8ml乙二醇，将三者充分混合，放置在多头磁力搅拌器上搅拌24小时，得到透明的B溶液；将B溶液缓缓加入到A溶液中，将混合后的溶液充分搅拌24小时，得到淡黄色的溶液C；将C溶液静置24小时，得到Sr2Bi4Ti5O18前驱体溶液。(1) The preparation process of the Sr 2 Bi 4 Ti 5 O 18 transition layer and thin film layer precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, using bismuth nitrate , strontium acetate, ethylene glycol, acetylacetone, and tetrabutyl titanate are used as raw materials, and are synthesized by sol-gel method. The specific steps are as follows: prepare tetrabutyl titanate and acetylacetone at a volume ratio of 1:1 Solution A: Slowly drop tetrabutyl titanate acetylacetone into the acetylacetone solution, and continue to stir the mixed solution for 24 hours to obtain a clear, yellow-brown and transparent A solution; weigh 1.2g of strontium acetate, 5.9g of bismuth nitrate, 18.8ml of ethylene glycol, fully mixed the three, placed on a multi-head magnetic stirrer and stirred for 24 hours to obtain a transparent B solution; slowly added the B solution to the A solution, and fully stirred the mixed solution for 24 hours, A light yellow solution C was obtained; the solution C was left to stand for 24 hours to obtain a Sr 2 Bi 4 Ti 5 O 18 precursor solution.
（2）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中BiFeO3薄膜层前驱体溶液的制备工艺，以硝酸铋，硝酸铁，冰乙酸，乙酰丙酮，乙二醇为原料，采用溶胶-凝胶法合成，具体步骤如下：首先称量9.2g硝酸铋，量取5ml乙二醇、15ml冰乙酸作为溶剂充分混合，放置在多头磁力搅拌器上充分搅拌8小时，得到透明溶液；量取40ml乙酰丙酮加入到上文中得到的透明溶液中，称量7.4g硝酸铁也加入上文中得到的透明溶液中。在多头磁力搅拌器上搅拌24小时得到暗红色半透明BiFeO3溶液；将溶液常温下静置24小时得到BiFeO3的前驱体溶液。( 2 ) The preparation process of BiFeO3 thin film layer precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, with bismuth nitrate, iron nitrate, glacial acetic acid, acetylacetone , ethylene glycol as raw material, using sol-gel synthesis, the specific steps are as follows: first weigh 9.2g of bismuth nitrate, measure 5ml of ethylene glycol, 15ml of glacial acetic acid as a solvent and mix them fully, place them on a multi-head magnetic stirrer to fully Stir for 8 hours to obtain a transparent solution; measure 40ml of acetylacetone and add to the above obtained transparent solution, weigh 7.4g of ferric nitrate and add to the above obtained transparent solution. Stir on a multi-head magnetic stirrer for 24 hours to obtain a dark red translucent BiFeO 3 solution; leave the solution at room temperature for 24 hours to obtain a BiFeO 3 precursor solution.
（3）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构的制备工艺，具体步骤如下：将Sr2Bi4Ti5O18过渡层前驱体溶液均匀的旋涂在Pt片基底上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s，重复上述步骤得到260nm厚的过渡层；将BiFeO3前驱体溶液均匀的旋涂在过渡层上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到500℃保温300s；重复上述步骤得到直到得到一定厚度的BiFeO3薄膜层；将Sr2Bi4Ti5O18薄膜层前驱体溶液均匀的旋涂在BiFeO3薄膜层上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s，重复上述步骤得到1000nm厚的BiFeO3-Sr2Bi4Ti5O18薄膜层。(3) The preparation process of the new multi-layer structure with lower leakage current for ferroelectric memory devices described in the present invention, the specific steps are as follows: uniformly mix the Sr 2 Bi 4 Ti 5 O 18 transition layer precursor solution Spin-coat on the Pt sheet substrate, and then place it on a 200°C stainless steel electric heating plate to dry for 2-3min; place the preliminarily dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s, repeat The above steps obtained a transition layer with a thickness of 260nm; evenly spin-coat the BiFeO 3 precursor solution on the transition layer, and then put it on a 200°C stainless steel electric heating plate to dry for 2-3min; Heat at 350°C for 180s in the furnace, then continue heating to 500°C for 300s; repeat the above steps until a certain thickness of BiFeO 3 film layer is obtained; evenly spin-coat the precursor solution of Sr 2 Bi 4 Ti 5 O 18 film layer on BiFeO 3 On the film layer, put it on a 200°C stainless steel heating plate and dry it for 2-3min; place the preliminarily dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s, repeat the above steps to get 1000nm thick BiFeO 3 -Sr 2 Bi 4 Ti 5 O 18 film layer.
实施案例3Implementation Case 3
（1）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中Sr2Bi4Ti5O18过渡层和薄膜层前驱体溶液的制备工艺，以硝酸铋，乙酸锶，乙二醇，乙酰丙酮，钛酸四丁酯为原料，采用溶胶-凝胶法合成，具体步骤如下：以钛酸四丁酯和乙酰丙酮按照体积比为1:1的比例配制A溶液：钛酸四丁酯乙酰丙酮缓缓滴入乙酰丙酮溶液中，将混合好的溶液继续搅拌24小时，得到澄清黄褐色透明的A溶液；称量1.2g乙酸锶、5.9g硝酸铋、18.8ml乙二醇，将三者充分混合，放置在多头磁力搅拌器上搅拌24小时，得到透明的B溶液；将B溶液缓缓加入到A溶液中，将混合后的溶液充分搅拌24小时，得到淡黄色的溶液C；将C溶液静置24小时，得到Sr2Bi4Ti5O18前驱体溶液。(1) The preparation process of the Sr 2 Bi 4 Ti 5 O 18 transition layer and thin film layer precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, using bismuth nitrate , strontium acetate, ethylene glycol, acetylacetone, and tetrabutyl titanate are used as raw materials, and are synthesized by sol-gel method. The specific steps are as follows: prepare tetrabutyl titanate and acetylacetone at a volume ratio of 1:1 Solution A: Slowly drop tetrabutyl titanate acetylacetone into the acetylacetone solution, and continue to stir the mixed solution for 24 hours to obtain a clear, yellow-brown and transparent A solution; weigh 1.2g of strontium acetate, 5.9g of bismuth nitrate, 18.8ml of ethylene glycol, fully mixed the three, placed on a multi-head magnetic stirrer and stirred for 24 hours to obtain a transparent B solution; slowly added the B solution to the A solution, and fully stirred the mixed solution for 24 hours, A light yellow solution C was obtained; the solution C was left to stand for 24 hours to obtain a Sr 2 Bi 4 Ti 5 O 18 precursor solution.
（2）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构中薄膜层BiFeO3前驱体溶液的制备工艺，以硝酸铋，硝酸铁，冰乙酸，乙酰丙酮，乙二醇为原料，采用溶胶-凝胶法合成，具体步骤如下：首先称量9.2g硝酸铋，量取5ml乙二醇、15ml冰乙酸作为溶剂充分混合，放置在多头磁力搅拌器上充分搅拌8小时，得到透明溶液；量取40ml乙酰丙酮加入到上文中得到的透明溶液中，称量7.4g硝酸铁也加入上文中得到的透明溶液中。在多头磁力搅拌器上搅拌24小时得到暗红色半透明BiFeO3溶液；将溶液常温下静置24小时得到BiFeO3的前驱体溶液。( 2 ) The preparation process of the thin film layer BiFeO3 precursor solution in the novel multilayer structure with lower leakage current for ferroelectric memory devices described in the present invention, with bismuth nitrate, iron nitrate, glacial acetic acid, acetylacetone , ethylene glycol as raw material, using sol-gel synthesis, the specific steps are as follows: first weigh 9.2g of bismuth nitrate, measure 5ml of ethylene glycol, 15ml of glacial acetic acid as a solvent and mix them fully, place them on a multi-head magnetic stirrer to fully Stir for 8 hours to obtain a transparent solution; measure 40ml of acetylacetone and add to the above obtained transparent solution, weigh 7.4g of ferric nitrate and add to the above obtained transparent solution. Stir on a multi-head magnetic stirrer for 24 hours to obtain a dark red translucent BiFeO 3 solution; leave the solution at room temperature for 24 hours to obtain a BiFeO 3 precursor solution.
（3）本发明中所述的用于铁电存储器件的新型具有较低漏电流的多层结构的制备工艺，具体步骤如下：将Sr2Bi4Ti5O18过渡层前驱体溶液均匀的旋涂在Pt片基底上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s，重复上述步骤得到390nm厚的过渡层；将BiFeO3薄膜层前驱体溶液均匀的旋涂在过渡层上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到500℃保温300s；重复上述步骤得到直到得到一定厚度的BiFeO3薄膜层；将Sr2Bi4Ti5O18薄膜层前驱体溶液均匀的旋涂在BiFeO3薄膜层上，继而放到200℃不锈钢电热板上烘干2-3min；将初步烘干的薄膜样品放在快速退火炉中350℃保温180s后继续加热到700℃保温300s，重复上述步骤得到1000nm厚的BiFeO3-Sr2Bi4Ti5O18薄膜层。(3) The preparation process of the new multi-layer structure with lower leakage current for ferroelectric memory devices described in the present invention, the specific steps are as follows: uniformly mix the Sr 2 Bi 4 Ti 5 O 18 transition layer precursor solution Spin-coat on the Pt sheet substrate, and then place it on a 200°C stainless steel electric heating plate to dry for 2-3min; place the preliminarily dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s, repeat The above steps obtain a transition layer with a thickness of 390nm; evenly spin-coat the BiFeO 3 film layer precursor solution on the transition layer, and then put it on a 200°C stainless steel electric heating plate to dry for 2-3min; put the pre-dried film sample on Heat at 350°C for 180s in a rapid annealing furnace, then continue heating to 500°C for 300s; repeat the above steps until a certain thickness of BiFeO 3 film layer is obtained; spin-coat the precursor solution of Sr 2 Bi 4 Ti 5 O 18 film layer evenly on the On the BiFeO 3 film layer, put it on a stainless steel electric heating plate at 200°C and dry it for 2-3min; place the pre-dried film sample in a rapid annealing furnace at 350°C for 180s, then continue heating to 700°C for 300s, repeat the above steps A 1000 nm thick BiFeO 3 -Sr 2 Bi 4 Ti 5 O 18 film layer was obtained.
由于采用了上述结构方案，本发明用于铁电存储器件的新型具有较低漏电流的多层结构，相较现有的结构具有以下的优点：Due to the adoption of the above structural scheme, the novel multilayer structure with lower leakage current used in ferroelectric memory devices of the present invention has the following advantages compared with the existing structures:
1、过渡层选用的Sr2Bi4Ti5O18材料本身具有较小的漏电特性，组成多层结构之后，阻断了载流子在BiFeO3薄膜和Pt电极间的移动，使得比直接沉积在ITO上BiFeO3薄膜的漏电流小；1. The Sr 2 Bi 4 Ti 5 O 18 material used for the transition layer itself has small leakage characteristics. After forming a multi-layer structure, it blocks the movement of carriers between the BiFeO 3 film and the Pt electrode, making it easier to deposit than direct deposition The leakage current of BiFeO 3 film on ITO is small;
2、Sr2Bi4Ti5O18和BiFeO3两相的界面处特殊的接触状态，也抑制了薄膜载流子的运动，使得比直接沉积在ITO上BiFeO3薄膜的漏电流小。2. The special contact state at the interface of Sr 2 Bi 4 Ti 5 O 18 and BiFeO 3 phases also inhibits the movement of carriers in the film, making the leakage current smaller than that of BiFeO 3 films deposited directly on ITO.
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