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CN1290795C - Lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof - Google Patents

Lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof Download PDF

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CN1290795C
CN1290795C CN 200510011664 CN200510011664A CN1290795C CN 1290795 C CN1290795 C CN 1290795C CN 200510011664 CN200510011664 CN 200510011664 CN 200510011664 A CN200510011664 A CN 200510011664A CN 1290795 C CN1290795 C CN 1290795C
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film
nickel oxide
lithium titanium
ceramic film
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CN1699273A (en
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张波萍
董燕
张雅如
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University of Science and Technology Beijing USTB
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Abstract

The present invention provides a lithium titanium codoped nickel oxide base ceramic film and a preparation method thereof, which belongs to the technical field of oxide ceramic film materials. The lithium titanium codoped nickel oxide base ceramic film is suitable for dielectric film materials. The chemical formula of the ceramic film of the present invention is LixTiyNi (1-x-y) O, wherein x is from 0.05 to 0.5, and y is from 0.02 to 0.2. The lithium titanium codoped nickel oxide base ceramic film adopts a sol-gel method to prepare precursor solutions, and uses a glue homogenizer to prepare films, so the price of the film is low. The lithium titanium codoped nickel oxide base ceramic film material is a new dielectric medium film material without lead, and the properties of the dielectric medium film material are stable. The lithium titanium codoped nickel oxide base ceramic film materials have high dielectric constant, the frequency is 1000Hz, and epsilon is larger than 100; the lithium titanium codoped nickel oxide base ceramic film materials can meet the requirements of various film devices of high dielectric constant. The film can be used for manufacturing film capacitors and dynamic random access memories DRAM in the field of dielectric media.

Description

A kind of lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof
Technical field
The invention belongs to oxide ceramic film material technology field, a kind of lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof particularly is provided, be applicable to dielectric film material.
Background technology
The nickel oxide-base film not only has good chemical stability, is a kind of lead-free, and optics, electricity, magnetism characteristic are preferably arranged, and purposes is very extensive.It is used as [the Y.M.Lu such as electrode materials of antiferromagnetic substance, electrochromic material, p type transparent conductor material and chemical-sensitive material (as gas sensitive) and battery, W.S.Hwang et al.:Surface and Coatings Technology, 155 (2002) 231-235].The adulterated nickel oxide-base thin-film material of research has Li at present xNiO y, LiNi 1-xCo xO 2, LiNi 1-xMn xO 2, LiNi 0.5Co 0.5VO 2Deng, but these researchs mainly concentrate on the electrode materials of electrochromic property and battery.[P.Lunkenheimer, A.Loidl et al.:Phys.Rev.B 44 (11) (1991) 5927-5930; A.Urbano, S.C.deCastro et al.:Journal of Power Sources 97-98 (2001) 328-331; E.Endo, T.Yasuda et al.:Journal ofPower Sources 93 (2001) 87-92; Wu Yonggang, Wu Guangming etc.: Tongji University's journal, 26 (2) (1998) 207-300; K.-S.Han, S.-W Song et al, Solid State Ionics 151 (2002) 11-18; H.-K Kim, T.-Y.Seong et al.:Journal of Power Sources 109 (2002) 178-183; M.Mohamedi, M.Makinoet al, Electrochemical Acta 48 (2002) 79-84.]
The dielectric substance of high-dielectric coefficient commonly used can be divided into following a few class substantially at present.What one class was that Tao Li etc. mentions in its article [Materials Letters 44 (2000) 1-5] is the high dielectric oxide of representative or the composite oxides of perovskite structure with titanium, niobium.It is hundreds of that its dielectric constant values can reach, and is porcelain and titanium magnesium group of the lanthanides porcelain etc. as rutile porcelain, calcium titanate ceramics, magnesium titanate porcelain, titanium zirconium.Another kind of what be that Sun Rizhen mentions in the book of " Dielectric Physics basis " [press of South China Science ﹠ Engineering University, 2000] is sulfide, selenide, the telluride of representative with copper, silver, mercury, thallium etc., and its dielectric coefficient is about tens.Also having a class material is ferroelectric ceramic(s).Lee marks and mentions barium titanate based ceramic and leaded ferroelectric system (as PMN, PZN, PFW, PFN, PNN etc.) in Rong Dengzai " inorganic dielectric " [press of HUST, the 1995] book, and its dielectric coefficient is up to 10 3～10 4But all there is significant disadvantages in above material: the specific inductivity of (1) preceding two class materials is less than normal, all less than 1000; (2) and the specific inductivity instability of ferroelectric material, along with temperature generation considerable change; (3) ferroelectric material that specific inductivity is bigger generally all contains lead (as PZN, PFW, PFN, PNN etc.), and is seriously polluted in preparation and use, is unfavorable for environmental requirement.Low-loss, the novel lead-free high dielectric material of good temperature, frequency stability is the focus of studying in the world always.Report a kind of no lead oxides CaCu in the recent period 3Ti 4O 12(CCTO) bulk and film at room temperature have very high static dielectric (ε ≈ 10 5), the frequency of specific inductivity and temperature stability are good under 100K～380K.[C.C.Homes?et?al.，Science?293(2001)673；M.A.Subramanian?et?al.，J.Solid?State?Chem.151，(2000)323；A.P.Ramirez?et?al.，Solid?State?Commun.115(2000)217；Liang?Fang，Mingrong?Shen，Thin?Solid?Films?440(2003)60-65；Y.Lin，Y.B.Chen，T.Garret?et?al.，Appl.Phys.Lett.，Vol.81，No.4，(2002)631；W.Si，E.M.Cruz，P.Johnsonet?al.，Appl.Phys.Lett.，Vol.81，No.11，(2002)2056；A.F.L.Almeida，R.S.de?Oliveira?etal.，Materials?Science?and?Engineering?B96(2002)275-283]。The Nan Cewen of Tsing-Hua University in 2002 etc. has carried out detailed research to the nickel oxide-base block body ceramic material, finds the lithium titanium Ni-based ceramic block material of oxygen-dopedization altogether, and mol ratio one timing when lithium and titanium has high low-frequency dielectric constant (ε a≈ 10 4～10 5) and good specific inductivity temperature and frequency stability, can compare favourably with the CCTO of report.[Nan Cewen, Wu Junbo, the Southern Army, Deng Yuan, patent publication No.: CN 1384079A; J.Wu, C.-W.Nan, Y.Lin and Y.Deng, PHYSYCAL REVIEW LETTERS 89 (21) (2002) 217601; Z.-M.Dang, J.-B.Wu, L.-Z.Fan, C.-W.Nan, Chemical Physics Letters 376 (2003) 389-394; Y.Deng, J.Wu et al., Journal of Physics and Chemistry of Solids 64 (2003) 607-610; J.Wu, J.Nan, C.-W.Nan et al., Phys.Stat.Sol. (a) 193, (2002) 78-85; J.B.Wu, J.Nan, C.-W.Nan et al., Materials Science and Engineering B99 (2003) 294-297; J.-F.Wang, Y.-H.Lin et al., Key Engineering materials Vols.280-283 (2005) 115-118; Wu Junbo, the Southern Army etc.: Rare Metals Materials and engineering 31, (2002) 335-339].But, about the application in the dielectric substance field yet there are no report to the adulterated ceramic membrane of nickel oxide.
Summary of the invention
The objective of the invention is to: a kind of lithium titanium co-doped nickel oxide base ceramic film and preparation method thereof is provided, utilizes sol-gel method to carry out the preparation of lithium titanium co-doped nickel oxide base ceramic film.Sol-gel method has that operational path is simple, and required equipment is uncomplicated, does not need vacuum condition, does not also need special reaction cabin, and is easy to operate, and can accurately control the advantages such as stoichiometric ratio of film, is fit to the preparation nano thin-film.The prepared film material, can in dynamic RAM (DRAM), be used as the capacitor dielectric of information storage, also can be used as the transistor gate dielectric medium in CMOS (CMOS) field-effect transistor (FET) logical device, be applied to the semiconductor microactuator electronics industry.
Technical scheme of the present invention is as follows:
Li and Ti doped nickel oxide-base chest porcelain film of the present invention has following chemical formula: Li xTi yNi 1-x-yO, wherein: x is 0.05～0.5, y is 0.02～0.2.Above-mentioned lithium titanium co-doped nickel oxide base ceramic film.
Lithium titanium co-doped nickel oxide base ceramic film of the present invention is prepared as follows:
1, weighing is 0.93～0.3,0.05～0.5,0.02～0.2 (C in molar ratio respectively 2H 5O 2) 2Ni4H 2O, Li (C 2H 3O 2) 22H2 OAnd Ti (O (CH 2) 2CH 3) 4
2, preparation precursor solution: at first with (C 2H 3O 2) 2Ni4H 2O and Li (C 2H 3O 2) 22H 2O is dissolved in CH 3OCH 2CH 2In the OH solvent, solution is heated to 100 ℃～150 ℃, and constantly stirs, carry out 2～10 hours dehydration reaction, add Ti (O (CH after solution is cooled to 60 ℃～90 ℃ 2) 2CH 3) 4, solution was heated to 100 ℃～150 ℃ stirring and refluxing 2～10 hours once more, use CH then 3OCH 2CH 2OH adjusts strength of solution, and adds stablizer Glacial acetic acid 1～5 person of outstanding talent's liter, makes the Li-Ti-Ni-O precursor solution;
3, preparation Li-Ti-Ni-O film: carry out film preparation with sol evenning machine, substrate is platinum electrode substrate [Pt/Ti/SiO 2/ Si]; Before the even film, with precursor solution by after considering membrane filtration, with sol evenning machine it is deposited on the substrate, after 200～1000 rev/mins of running several 3～500 seconds, 1000～5000 rev/mins of 5～2000 seconds of running again, whenever even glue carries out thermal decomposition process one time after once, behind the even glue 1～50 time, sample put in the heat treatment furnace anneal, make its crystallization, repeat to make the Li-Ti-Ni-O film after even glue-thermolysis-annealing operation 1～50 time.Heat decomposition temperature is 200 ℃～600 ℃, and the time was 5～3000 seconds; Annealing temperature is 300 ℃～900 ℃, and annealing time is 1～100 minute.
The invention has the advantages that: prepare precursor solution by sol-gel method, adopt sol evenning machine to prepare film, cheap, temperature of reaction (300 ℃-900 ℃) is lower than conventional sintering method, thin film composition is controlled easily, and preparation cycle is short, saves the energy.The lithium titanium co-doped nickel oxide base ceramic film material is a kind of novel unleaded thin dielectric mould material, the demand that adapts to the unleaded environment compatibility ceramic membrane material of exploitation, the stable performance of this thin-film material, structure different and perovskite structure and ferroelectric material, the doping that changes lithium and titanium can obviously change the dielectric characteristics of film.Li and Ti doped nickel oxide ceramic membrane material of the present invention has high specific inductivity, and (frequency is 1000Hz, ε＞100), application aspect electronic product is very extensive, be fit to the requirement of various high dielectric constant film devices, in the dielectric medium field, can be used for making film capacitor and dynamic easy assess memorizer (DRAM).
Description of drawings
Fig. 1: XRD figure spectrum (a) Li of different lithium and titanium doped content sample 0.05Ti 02Ni 0.75O (b) Li 0.5Ti 0.02Ni 0.48O (c) Li 0.05Ti 0.02Ni 0.93O (d) Li 0.5Ti 0.2Ni 0.3O.
Fig. 2: the surface scan Electronic Speculum figure of typical Li-Ti-Ni-O sample.
Fig. 3: the cross section sem photograph of typical Li-Ti-Ni-O sample.
Fig. 4: Li 0.05Ti 0.2Ni 0.75The optical photograph figure of O sample.
Fig. 5: Li 0.5Ti 0.02Ni 0.48The optical photograph figure of O sample.
Fig. 6: Li 0.05Ti 0.02Ni 0.93The optical photograph figure of O sample.
Fig. 7: Li 0.5Ti 0.2Ni 0.3The optical photograph figure of O sample.
Fig. 8: under the room temperature, relative permittivity is with variation (a) Li of frequency 0.05Ti 0.02Ni 0.93O,
(b)Li 0.5Ti 0.02Ni 0.48O，(c)Li 0.05Ti 0.2Ni 0.75O，(d)Li 0.5Ti 0.2Ni 0.3O。
Embodiment
All pharmaceutical chemicalss are commercially available analytical pure without being further purified.
Embodiment 1
With load weighted 0.05205g (0.0005mol) Li (C 2H 3O 2) 22H 2O and 1.90454g (0.0075mol) (C 2H 3O 2) 2Ni4H 2O is dissolved in 40mlCH 3OCH 2CH 2In the OH solvent, solution is heated to 100 ℃, and constantly stirs, carry out 10 hours dehydration reaction, add 0.58012g (0.002mol) Ti (O (CH after solution is cooled to 70 ℃ 2) 2CH 3) 4, solution was heated to 100 ℃ of stirring and refluxing 10 hours once more, use CH then 3OCH 2CH 2OH adjusts strength of solution, and adds stablizer Glacial acetic acid 1 person of outstanding talent's liter, makes the Li-Ti-Ni-O precursor solution; Carry out film preparation with sol evenning machine, substrate is platinum electrode substrate [Pt/Ti/SiO 2/ Si].Before the even film, precursor solution by after considering membrane filtration, is deposited on it on substrate with sol evenning machine, after 200 rev/mins of 500 seconds of turning round, 5000 rev/mins turned round for 5 seconds again.Whenever even glue once 200 ℃ of 3000 seconds of thermal decomposition process, behind the even glue 5 times, is put film to handle in the stove with sample and was carried out anneal 1 minute at 900 ℃, repeat even glue-thermolysis-annealing operation 1 time after, obtain Li 0.05Ti 0.2Ni 0.75O ceramic membrane material.
Embodiment 2
With load weighted 0.05205g (0.0005mol) Li (C 2H 3O 2) 22H 2O and 2.36163g (0.0093mol) (C 2H 3O 2) 2Ni4H 2O is dissolved in 40mlCH 3OCH 2CH 2In the OH solvent, solution is heated to 150 ℃, and constantly stirs, carry out 2 hours dehydration reaction, add O.05801g (0.002mol) Ti (O (CH after solution is cooled to 90 ℃ 2) 2CH 3) 4, solution was heated to 150 ℃ of stirring and refluxing 2 hours once more, use CH then 3OCH 2CH 2OH adjusts strength of solution, and adds stablizer Glacial acetic acid 5 person of outstanding talent's liters, makes the Li-Ti-Ni-O precursor solution; Carry out film preparation with sol evenning machine, substrate is platinum electrode substrate [Pt/Ti/SiO 2/ Si].Before the even film, precursor solution by after considering membrane filtration, is deposited on it on substrate with sol evenning machine, after 1000 rev/mins of 500 seconds of turning round, 4000 rev/mins turned round for 100 seconds again.Whenever even glue once 600 ℃ of 5 seconds of thermal decomposition process, behind the even glue 30 times, is put film to handle in the stove with sample and was carried out anneal 100 minutes at 300 ℃, repeat even glue-thermolysis-annealing operation 30 times after, obtain Li 0.05Ti 0..02Ni 0.93O ceramic membrane material.
Embodiment 3
With load weighted 0.52051g (0.005mol) Li (C 2H 3O 2) 22H 2O and 0.76182g (0.003mol) (C 2H 3O 2) 2Ni4H 2O is dissolved in 40mlCH 3OCH 2CH 2In the OH solvent, solution is heated to 130 ℃, and constantly stirs, carry out 4 hours dehydration reaction, add O.58012g (0.002mol) Ti (O (CH after solution is cooled to 90 ℃ 2) 2CH 3) 4,, use CH then 130 ℃ of following stirring and refluxing 4 hours 3OCH 2CH 2OH adjusts strength of solution, and adds stablizer Glacial acetic acid 3 person of outstanding talent's liters, makes the Li-Ti-Ni-O precursor solution; Carry out film preparation with sol evenning machine, substrate is platinum electrode substrate [Pt/Ti/SiO 2/ Si].Before the even film, precursor solution by after considering membrane filtration, is deposited on it on substrate with sol evenning machine, after 800 rev/mins of 30 seconds of turning round, 3000 rev/mins turned round for 30 seconds again.Whenever even glue once 600 ℃ of 5 seconds of thermal decomposition process, behind the even glue 50 times, is put film to handle in the stove with sample and was carried out anneal 80 minutes at 800 ℃, repeat even glue-thermolysis-annealing operation 10 times after, obtain Li 0.5Ti 0.2Ni 0.3O ceramic membrane material.
Embodiment 4
With load weighted 0.52051g (0.005mol) Li (C 2H 3O 2) 22H 2O and 1.21891g (0.0048mol) (C 2H 3O 2) 2Ni4H 2O is dissolved in 40mlCH 3OCH 2CH 2In the OH solvent, solution is heated to 120 ℃, and constantly stirs, carry out 7 hours dehydration reaction, add 0.05801g (0.002mol) Ti (O (CH after solution is cooled to 60 ℃ 2) 2CH 3) 4,, use CH then 130 ℃ of following stirring and refluxing 4 hours 3OCH 2CH 2OH adjusts strength of solution, and adds stablizer Glacial acetic acid 2 person of outstanding talent's liters, makes the Li-Ti-Ni-O precursor solution; Carry out film preparation with sol evenning machine, substrate is platinum electrode substrate [Pt/Ti/SiO 2/ Si].Before the even film, precursor solution by after considering membrane filtration, is deposited on it on substrate with sol evenning machine, after 600 rev/mins of 200 seconds of turning round, 2000 rev/mins turned round for 2000 seconds again.Whenever even glue once 500 ℃ of 100 seconds of thermal decomposition process, behind the even glue 20 times, is put film speed with sample and is handled in the stove and carried out anneal 100 minutes at 800 ℃, repeat even glue-thermolysis-annealing operation 50 times after, obtain Li 0.5Ti 0.02Ni 0.48O ceramic membrane material.

Claims (2)

1、一种锂钛共掺杂氧化镍基陶瓷薄膜的制备方法，其特征在于：具体制备步骤为：1. A method for preparing a lithium-titanium co-doped nickel oxide-based ceramic film, characterized in that: the specific preparation steps are: a、分别称量按摩尔比为0.93～0.3、0.05～0.5、0.02～0.2的(C2H5O2)2Ni·4H2O、Li(C2H3O2)2·2H2O和Ti(O·(CH2)2·CH3)4；a. Weigh (C 2 H 5 O 2 ) 2 Ni·4H 2 O, Li(C 2 H 3 O 2 ) 2 ·2H 2 O with a molar ratio of 0.93～0.3, 0.05～0.5, 0.02～0.2 respectively and Ti(O·(CH 2 ) 2 ·CH 3 ) 4 ; b、制备前驱体溶液：首先将(C2H3O2)2Ni·4H2O和Li(C2H3O2)2·2H2O溶于CH3OCH2CH2OH溶剂中，将溶液加热至100℃～150℃，并不断搅拌，进行2～10小时的脱水反应，将溶液冷却至60℃～90℃后加入Ti(O·(CH2)2·CH3)4，将溶液加热再次加热至100℃～150℃搅拌回流2～10小时，然后用CH3OCH2CH2OH调整溶液浓度，并加入稳定剂冰醋酸1～10豪升，制得Li-Ti-Ni-O前驱体溶液；b. Preparation of precursor solution: first dissolve (C 2 H 3 O 2 ) 2 Ni·4H 2 O and Li(C 2 H 3 O 2 ) 2 ·2H 2 O in CH 3 OCH 2 CH 2 OH solvent, Heat the solution to 100°C-150°C and keep stirring for 2-10 hours of dehydration reaction, cool the solution to 60°C-90°C and add Ti(O·(CH 2 ) 2 ·CH 3 ) 4 , the Heating the solution again to 100°C to 150°C, stirring and refluxing for 2 to 10 hours, then using CH 3 OCH 2 CH 2 OH to adjust the concentration of the solution, and adding 1 to 10 milliliters of glacial acetic acid as a stabilizer to obtain Li-Ti-Ni- O precursor solution; c、制备Li-Ti-Ni-O薄膜：用匀胶机进行薄膜制备，基板为铂电极基板[Pt/Ti/SiO2/Si]；匀膜之前，将前驱体溶液通过虑膜片过滤后，用匀胶机将其沉积在基板上，以200～1000转/分运转数3～8钟后，再1000～5000转/分运转5～200秒钟，每匀胶一次后进行一次热分解处理，匀胶1～30次后，将试样置热处理炉中退火，使其结晶化，重复匀胶-热分解-退火工序以控制膜厚。c. Preparation of Li-Ti-Ni-O thin film: film preparation with a homogenizer, the substrate is a platinum electrode substrate [Pt/Ti/SiO 2 /Si]; before the homogenization, the precursor solution is filtered through a filter , use a homogenizer to deposit it on the substrate, run it at 200-1000 rpm for 3-8 minutes, then run it at 1000-5000 rpm for 5-200 seconds, and perform a thermal decomposition after each homogenization After 1-30 times of homogenization, the sample is annealed in a heat treatment furnace to make it crystallized, and the homogenization-thermal decomposition-annealing process is repeated to control the film thickness. 2、按照权利要求1所述的方法，其特征在于：热分解温度为200℃～600℃，时间为5～3000秒钟；退火温度为300℃～900℃，退火时间为1～100分钟。2. The method according to claim 1, characterized in that: the thermal decomposition temperature is 200°C-600°C, and the time is 5-3000 seconds; the annealing temperature is 300°C-900°C, and the annealing time is 1-100 minutes.
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EP2734601B1 (en) 2011-07-21 2019-09-04 Sage Electrochromics, Inc. Electrochromic nickel oxide simultaneously doped with lithium and a metal dopant
CN102557589B (en) * 2011-12-16 2014-04-16 桂林理工大学 Li-Co co-doped nickel oxide-based ceramic material and preparation method thereof based on sol-gel method
CN102653863A (en) * 2012-05-10 2012-09-05 东北大学 Preparation method of Ru-Li codoped nickel oxide film
CN103904216B (en) * 2014-03-21 2017-07-28 西安理工大学 A kind of preparation method of titanium doped nickel oxide Memister film
CN104803664A (en) * 2015-04-20 2015-07-29 河南师范大学 Preparation method of lithium molybdenum-codoped nickel oxide base dielectric ceramic material
CN108018541A (en) * 2017-11-30 2018-05-11 齐鲁工业大学 A kind of low temperature fast performance liquid method for preparing nickel oxide film
CN110148632A (en) * 2019-05-17 2019-08-20 华南理工大学 A Giant Dielectric Thin Film Transistor

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