CN103360107A - Gold-lanthanum nickelate composite conductive thin-film material and preparation method for same - Google Patents

Gold-lanthanum nickelate composite conductive thin-film material and preparation method for same Download PDF

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CN103360107A
CN103360107A CN2012100887603A CN201210088760A CN103360107A CN 103360107 A CN103360107 A CN 103360107A CN 2012100887603 A CN2012100887603 A CN 2012100887603A CN 201210088760 A CN201210088760 A CN 201210088760A CN 103360107 A CN103360107 A CN 103360107A
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王占杰
王海玲
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Institute of Metal Research of CAS
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Abstract

The invention provides a gold-lanthanum nickelate composite conductive thin-film material and a preparation method for the gold-lanthanum nickelate composite conductive thin-film material. From composition, the material comprise 2.21-4.32 at% of Au, 19.11-19.56 at% of La, 19.11-19.56 at% of Ni, and the balance of O, wherein the material has the room-temperature resistivity of 350-500 muOhm.cm, and (110) crystal orientation. The preparation method for the material comprises the following steps of: weighing lanthanum nitrate, nickel acetate and chloroauric acid in a molar ratio of 1: 1: (0.113 to 0.226) of La: Ni: Au; taking ethylene glycol monomethyl ether and acetic acid as solvents, and adequately stirring to obtain yellow-green transparent solution; then spinning the obtained solution on a substrate material to form a film; drying for 10 minutes at 120 DEG C, then annealing in an electric furnace for 10-30 minutes at 600-700 DEG C; and repeating the process aforementioned for a plurality of times, so as to obtain the gold-lanthanum nickelate composite conductive thin-film material with a needed thickness. The composite conductive thin film is wide in application prospect in the fields of ferroelectric memories, thin-film capacitors, micro-electromechanical systems and the like as an electrode material.

Description

A kind of gold-nickel acid lanthanum composite conductive thin film material and preparation method thereof
Technical field
The invention belongs to electronic material, functional materials and intelligent material field, be specifically related to a kind of gold-nickel acid lanthanum composite conductive thin film material and preparation method thereof.
Background technology
With Pb-based lanthanumdoped zirconate titanates (Pb (Zr xTi 1-x) O 3) film is that the ferroelectric ceramic thin film of representative has the performances such as good ferroelectric, piezoelectricity, photoelectricity and dielectric, use widely in fields such as ferroelectric memory, film capacitor and MEMS (micro electro mechanical system).In above-mentioned the Research of Integrated Ferroelectric Devices, the normal operation Pt metal is as the bottom electrode material of ferroelectric membranc.Yet, in the ferroelectric membranc that the Pt electrode prepares, exist obvious polarization fatigue phenomenon, for this reason, people use conducting metal oxide (as: LaNiO 3, La 0.5Sr 0.5CoO 3, LaSrMnO 3, YBa 2Cu 3O 7Deng) replace Pt metal as electrode materials to improve ferroelectric membranc polarization fatigue characteristic.Studies show that, use metal oxide electrode can prevent the block room in the accumulation of ferroelectric membranc/electrode interface, effectively improve the anti-polarization fatigue characteristic of ferroelectric membranc.In conductive metal oxide, the nickel of Perovskite Phase structure acid lanthanum (LaNiO 3) film not only has metallic conductivity, and its lattice parameter and Pb (Zr xTi 1-x) O 3Lattice parameter Deng ferroelectric membranc is very approaching, can be used as kind of a crystal layer, with the crystal preferred orientation of control ferroelectric membranc, reaches the microstructure of optimization ferroelectric membranc and the purpose of electric property, becomes first-selected metal oxide electrode material.At present, existing several different methods is for the preparation of LaNiO 3Film comprises the physical methods such as magnetron sputtering and pulsed laser deposition, the chemical processes such as chemical vapour deposition and chemical solution deposition.Because preparation method, substrate material and annealing conditions etc. are different, LaNiO 3The conductivity of film is different, the LaNiO that generally prepares at the Si substrate with chemical solution deposition 3The resistivity of film is 750-5000 μ Ω cm, than Pt film (13 a μ Ω cm) high 1-2 order of magnitude.The LaNiO of high resistivity 3Film can cause multi-layer film structure to have larger dielectric loss, thereby must increase the operating voltage of device.At LaNiO 3Mixing metal in the film is the effective ways that improve its electroconductibility.Such as disclosed " a kind of combination electrode material of platinum adulterated by nickel acid lanthanum and preparation method thereof " of Chinese invention patent specification sheets CN100433415C of authorizing on November 12nd, 2008.The method adopts rf magnetron sputtering codeposition technique to prepare metal platinum and the LaNiO of low-resistivity and high crystalline orientation metal platinum and the combination of nickel acid lanthanum 3Compound conductive film.But, adopt physical method to prepare thin-film material, apparatus expensive, complex process, high in cost of production shortcoming are arranged in general, but and adopt chemical solution deposition prepare thin-film material have technique simple, with low cost, form evenly the advantage such as Large-Area-Uniform film forming.
Summary of the invention
The purpose of this invention is to provide a kind of gold-nickel acid lanthanum composite conductive thin film material and preparation method thereof, have the advantages such as technique is simple, with low cost, the even Large-Area-Uniform film forming of composition but the present invention adopts chemical solution deposition to prepare thin-film material.
The invention provides a kind of gold-nickel acid lanthanum composite conductive thin film material, the moiety of described thin-film material consists of and the atomic percentage conc of each composition satisfies following requirement: Au:2.21～4.32at%, La:19.11～19.56at%, Ni:19.11～19.56at%, all the other are O.
Gold provided by the invention-nickel acid lanthanum composite conductive thin film material, the room temperature resistivity of described thin-film material is 350-500 μ Ω cm, described thin-film material has (110) crystalline orientation.
The present invention also provides gold-nickel acid lanthanum composite conductive thin film material preparation method, and concrete steps are as follows: (1) is with ethylene glycol monomethyl ether (2-MOE) and acetic acid (CH 3COOH) be solvent, lanthanum nitrate (La (NO 3) 36H 2O), nickel acetate (Ni (CH 3COO) 24H 2O) and hydrochloro-auric acid (HAuCl 43.5H 2O) be solute, be 1: 1 according to the mol ratio of La: Ni: Au: 0.113-0.226 takes by weighing lanthanum nitrate (La (NO 3) 36H 2O), nickel acetate (Ni (CH 3COO) 24H 2O) and hydrochloro-auric acid (HAuCl 43.5H 2O), add respectively ethylene glycol monomethyl ether and acetic acid with the concentration standard of 0.13-0.3M, then at room temperature stir, be stirred to lanthanum nitrate, nickel acetate and hydrochloro-auric acid all till the dissolving, obtain the yellow-green colour clear solution; (2) solution that step (1) is prepared drips to spin coating on the substrate, and rotating speed is 1000-3000 rev/min, and the time is 5-30 second, and next heightening rotating speed is 3000-6000 rev/min, and the time is 50-80 second, obtains the raw material film; (3) with the raw material film at 100-150 ℃ of dry 5-20 minute, then in electric furnace 600-700 ℃ annealing 10-30 minute; (4) repeat (2)-(3) step process for several times, make the gold conductive film material compound with the sour lanthanum of nickel of desired thickness.
Gold provided by the invention-nickel acid lanthanum composite conductive thin film material preparation method, described step (2) is preferably the solution that step (1) is prepared and drips to spin coating on the substrate, rotating speed is 1500 rev/mins, time is 10 seconds, next heightening rotating speed is 4000 rev/mins, time is 60 seconds, obtains the raw material film.
Gold provided by the invention-nickel acid lanthanum composite conductive thin film material preparation method, described step (3) are preferably the raw material film 120 ℃ of dryings 10 minutes, then 700 ℃ of annealing 10 minutes in electric furnace.
Advantage of the present invention: the present invention adopts chemical solution deposition to prepare gold-nickel acid lanthanum composite conductive thin film material, and technique is simple, with low cost, the even Large-Area-Uniform film forming of composition but have.And the room temperature resistivity of the gold that makes-nickel acid lanthanum laminated film is lower approximately one times than lanthanum nickelate thin film, has a wide range of applications in fields such as ferroelectric memory, film capacitor and MEMS (micro electro mechanical system).
Description of drawings
Fig. 1 is that the resistivity of the gold that makes of the present invention-nickel acid lanthanum laminated film is with the variation diagram of gold content;
Fig. 2 is that the resistivity of the gold that makes of the present invention-nickel acid lanthanum laminated film is with the variation diagram (annealing temperature is 700 ℃) of annealing time;
Fig. 3 is the X-ray diffractogram (b) of the gold that makes of lanthanum nickelate thin film (a) and the present invention-nickel acid lanthanum laminated film.
Embodiment
Following examples will be further described the present invention, but not thereby limiting the invention.
Embodiment 1
Step 1: obtain solution
Spent glycol methyl ether (2-MOE) and acetic acid (CH 3COOH) be solvent.With nickel acetate (Ni (CH 3COO) 24H 2O), lanthanum nitrate (La (NO 3) 36H 2O) and hydrochloro-auric acid (HAuCl 43.5H 2O) being solute, is 1: 1 weighing lanthanum nitrate and nickel acetate according to the mol ratio of La: Ni, is 0.113: 1 weighing hydrochloro-auric acid according to the mol ratio of Au: La.Concentration standard with 0.13M adds respectively ethylene glycol monomethyl ether and acetic acid, then at room temperature stirs, and is stirred to till the whole dissolvings of lanthanum nitrate, nickel acetate and hydrochloro-auric acid, obtains the yellow-green colour clear solution.
Step 2: preparation thin-film material
(1) uses SiO 2/ Si (100) substrate.The solution that step 1 is configured drips to spin coating on the substrate, and rotating speed is 1500 rev/mins, and the time is 10 seconds, and next heightening rotating speed is 4000 rev/mins, and the time is 60 seconds, obtains the raw material film;
(2) with the raw material film 120 ℃ of dryings 10 minutes, 700 ℃ of annealing is 30 minutes in electric furnace;
(3) repeat above process 5 times, make the compound conductive film material of gold that thickness is 140nm and nickel acid lanthanum.This material has (110) crystalline orientation, and room temperature resistivity is 414.0 μ Ω cm (seeing Fig. 1).
Embodiment 2
Step 1: obtain solution
Spent glycol methyl ether (2-MOE) and acetic acid (CH 3COOH) be solvent.With nickel acetate (Ni (CH 3COO) 24H 2O), lanthanum nitrate (La (NO 3) 36H 2O) and hydrochloro-auric acid (HAuCl 43.5H 2O) being solute, is 1: 1 weighing lanthanum nitrate and nickel acetate according to the mol ratio of La: Ni, is 0.226: 1 weighing hydrochloro-auric acid according to the mol ratio of Au: La.Concentration standard with 0.13M adds respectively ethylene glycol monomethyl ether and acetic acid, then at room temperature stirs, and is stirred to till the whole dissolvings of lanthanum nitrate, nickel acetate and hydrochloro-auric acid, obtains the yellow-green colour clear solution.
Step 2: preparation thin-film material
(1) uses SiO 2/ Si (100) substrate.The solution that step 1 is configured drips to respectively spin coating on five pieces of substrates, and rotating speed is 1500 rev/mins, and the time is 10 seconds, and next heightening rotating speed is 4000 rev/mins, and the time is 60 seconds, obtains the raw material film;
(2) with five pieces of raw material films 120 ℃ of dryings 10 minutes, 700 ℃ of annealing in electric furnace, annealing time was respectively 5,10,20,30,60 minutes;
(3) repeat above process 5 times, make the compound conductive film material of gold that thickness is 140nm and nickel acid lanthanum.The room temperature resistivity of the gold of different annealing times-nickel acid lanthanum composite conductive thin film material is respectively 448.0 μ Ω cm, 352.9 μ Ω cm, 353.5 μ Ω cm, 352.9 μ Ω cm, 410.3 μ Ω cm (seeing Fig. 2).
Comparative Examples 1
Step 1: obtain solution
Spent glycol methyl ether (2-MOE) and acetic acid (CH 3COOH) be solvent.With nickel acetate (Ni (CH 3COO) 24H 2O), lanthanum nitrate (La (NO 3) 36H 2O) being solute, is 1: 1 weighing lanthanum nitrate and nickel acetate according to the mol ratio of La: Ni.Concentration standard with 0.15M adds respectively ethylene glycol monomethyl ether and acetic acid, then at room temperature stirs, and is stirred to till lanthanum nitrate, the whole dissolvings of nickel acetate, obtains the nickel acid lanthanum solution of green transparent.
Spent glycol methyl ether (2-MOE) and acetic acid (CH 3COOH) be solvent.With nickel acetate (Ni (CH 3COO) 24H 2O), lanthanum nitrate (La (NO 3) 36H 2O) and hydrochloro-auric acid (HAuCl 43.5H 2O) being solute, is 1: 1 weighing lanthanum nitrate and nickel acetate according to the mol ratio of La: Ni, is 0.226: 1 weighing hydrochloro-auric acid according to the mol ratio of Au: La.Concentration standard with 0.13M adds respectively ethylene glycol monomethyl ether and acetic acid, then at room temperature stirs, and is stirred to till the whole dissolvings of lanthanum nitrate, nickel acetate and hydrochloro-auric acid, obtains the transparent gold of yellow-green colour-nickel acid lanthanum solution.
Step 2: preparation thin-film material
(1) uses SiO 2/ Si (100) substrate.Nickel acid lanthanum solution and gold-nickel acid lanthanum solution that step 1 is configured drip to respectively spin coating on the substrate, and rotating speed is 1500 rev/mins, and the time is 10 seconds, and next heightening rotating speed is 4000 rev/mins, and the time is 60 seconds, obtains the raw material film of nickel acid lanthanum and gold-nickel acid lanthanum;
(2) with the raw material film of nickel acid lanthanum and gold-nickel acid lanthanum respectively 120 ℃ of dryings 10 minutes, 700 ℃ of annealing is 30 minutes in electric furnace;
(3) repeat above process 5 times, make lanthanum nickel oxide thin-film material and gold-nickel acid lanthanum composite film material that thickness is 140nm.Lanthanum nickel oxide thin-film material has (100) crystalline orientation (seeing Fig. 3 (a)), and room temperature resistivity is 1164.0 μ Ω cm.Gold-nickel acid lanthanum composite film material has (110) crystalline orientation (seeing Fig. 3 (b)), and its room temperature resistivity is 352.9 μ Ω cm, only is 30% of lanthanum nickel oxide thin-film material.The gold of low-resistivity-nickel acid lanthanum composite film material can reduce dielectric loss as the electrode materials of ferroelectric membranc, reduces the operating voltage of the Research of Integrated Ferroelectric Devices, and the fields such as ferroelectric memory, film capacitor and MEMS (micro electro mechanical system) that are expected at have a wide range of applications.

Claims (7)

1. a gold-nickel acid lanthanum composite conductive thin film material, it is characterized in that: the moiety of described thin-film material consists of and the atomic percentage conc of each composition satisfies following requirement:
Au:2.21～4.32at%, La:19.11～19.56at%, Ni:19.11～19.56at%, all the other are O.
2. according to gold claimed in claim 1-nickel acid lanthanum composite conductive thin film material, it is characterized in that: the room temperature resistivity of described thin-film material is 350-500 μ Ω cm.
3. according to gold claimed in claim 1-nickel acid lanthanum composite conductive thin film material, it is characterized in that: described thin-film material has 110 high preferred orientations.
4. gold claimed in claim 1-nickel acid lanthanum composite conductive thin film material preparation method, it is characterized in that: concrete steps are as follows:
(1) take ethylene glycol monomethyl ether and acetic acid as solvent, lanthanum nitrate, nickel acetate and hydrochloro-auric acid are solute, mol ratio according to La: Ni: Au is 1: 1: 0.113-0.226, take by weighing lanthanum nitrate, nickel acetate and hydrochloro-auric acid, concentration standard with 0.13-0.3M adds respectively ethylene glycol monomethyl ether and acetic acid, then at room temperature stir, be stirred to till the whole dissolvings of lanthanum nitrate, nickel acetate and hydrochloro-auric acid, obtain the yellow-green colour clear solution;
(2) solution that step (1) is prepared drips to spin coating on the substrate, and rotating speed is 1000-3000 rev/min, and the time is 5-30 second, and next heightening rotating speed is 3000-6000 rev/min, and the time is 50-80 second, obtains the raw material film;
(3) with the raw material film at 100-150 ℃ of dry 5-20 minute, then in electric furnace 600-700 ℃ annealing 10-30 minute;
(4) repeat (2)-(3) step process for several times, make the gold conductive film material compound with the sour lanthanum of nickel of desired thickness.
5. according to gold claimed in claim 4-nickel acid lanthanum composite conductive thin film material preparation method, it is characterized in that: described step (2) drips to spin coating on the substrate for the solution that step (1) is prepared, rotating speed is 1500 rev/mins, time is 10 seconds, next heightening rotating speed is 4000 rev/mins, time is 60 seconds, obtains the raw material film.
6. according to gold claimed in claim 4-nickel acid lanthanum composite conductive thin film material preparation method, it is characterized in that: described step (3) for the raw material film 120 ℃ of dryings 10 minutes.
7. according to gold claimed in claim 4-nickel acid lanthanum composite conductive thin film material preparation method, it is characterized in that: described step (3) is 700 ℃ of annealing in electric furnace 10 minutes.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103833416A (en) * 2014-01-17 2014-06-04 高俊萍 Preparation method of lanthanum nickelate conductive film by chemical solution deposition
CN106145898A (en) * 2015-04-20 2016-11-23 河南师范大学 A kind of preparation method of silver-nickel acid lanthanum composite conductive thin film material
CN106702327A (en) * 2017-01-10 2017-05-24 河北大学 Optimizing method of electrical transport property of ultrathin lanthanum nickelate film
CN106783810A (en) * 2016-11-30 2017-05-31 中国科学院金属研究所 A kind of nano combined ferroelectric thin-flim materials of golden lead zirconate titanate and preparation method thereof
CN107400880A (en) * 2017-08-11 2017-11-28 苏州南尔材料科技有限公司 A kind of preparation method of metatitanic acid lanthanum film
CN108928856A (en) * 2018-09-12 2018-12-04 北京科技大学 A kind of antivacuum synthetic method of thermodynamics metastable state rare-earth Ni-base oxide material
CN112670087A (en) * 2020-12-09 2021-04-16 南京邮电大学 Ferroelectric film capacitor applied to ferroelectric memory

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CN100433415C (en) * 2006-09-20 2008-11-12 北京航空航天大学 Composite electrode having platinum adulterated by nickel acid lanthanum and its preparing method
CN101343729A (en) * 2008-08-28 2009-01-14 上海交通大学 Method for preparing lanthanum nickelate conductive metallic oxide nano-film
CN101815579A (en) * 2007-08-13 2010-08-25 旭化成化学株式会社 Catalyst for production of carboxylic acid ester, method for producing same, and method for producing carboxylic acid ester

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100433415C (en) * 2006-09-20 2008-11-12 北京航空航天大学 Composite electrode having platinum adulterated by nickel acid lanthanum and its preparing method
CN101815579A (en) * 2007-08-13 2010-08-25 旭化成化学株式会社 Catalyst for production of carboxylic acid ester, method for producing same, and method for producing carboxylic acid ester
CN101343729A (en) * 2008-08-28 2009-01-14 上海交通大学 Method for preparing lanthanum nickelate conductive metallic oxide nano-film

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103833416A (en) * 2014-01-17 2014-06-04 高俊萍 Preparation method of lanthanum nickelate conductive film by chemical solution deposition
CN103833416B (en) * 2014-01-17 2017-08-25 高俊萍 A kind of chemical solution deposition preparation method of the sour lanthanum conductive film of nickel
CN106145898A (en) * 2015-04-20 2016-11-23 河南师范大学 A kind of preparation method of silver-nickel acid lanthanum composite conductive thin film material
CN106145898B (en) * 2015-04-20 2019-02-19 河南师范大学 A kind of preparation method of silver-nickel acid lanthanum composite conductive thin film material
CN106783810A (en) * 2016-11-30 2017-05-31 中国科学院金属研究所 A kind of nano combined ferroelectric thin-flim materials of golden lead zirconate titanate and preparation method thereof
CN106702327A (en) * 2017-01-10 2017-05-24 河北大学 Optimizing method of electrical transport property of ultrathin lanthanum nickelate film
CN106702327B (en) * 2017-01-10 2019-10-11 河北大学 A kind of optimization method of ultra-thin lanthanum nickelate thin film electronic transport performance
CN107400880A (en) * 2017-08-11 2017-11-28 苏州南尔材料科技有限公司 A kind of preparation method of metatitanic acid lanthanum film
CN108928856A (en) * 2018-09-12 2018-12-04 北京科技大学 A kind of antivacuum synthetic method of thermodynamics metastable state rare-earth Ni-base oxide material
CN108928856B (en) * 2018-09-12 2020-06-26 北京科技大学 Non-vacuum synthesis method of thermodynamic metastable state rare earth nickel-based oxide material
CN112670087A (en) * 2020-12-09 2021-04-16 南京邮电大学 Ferroelectric film capacitor applied to ferroelectric memory

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