CN104844197B - A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate - Google Patents

A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate Download PDF

Info

Publication number
CN104844197B
CN104844197B CN201510231730.7A CN201510231730A CN104844197B CN 104844197 B CN104844197 B CN 104844197B CN 201510231730 A CN201510231730 A CN 201510231730A CN 104844197 B CN104844197 B CN 104844197B
Authority
CN
China
Prior art keywords
solution
film
bismuth
silicon substrate
base film
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201510231730.7A
Other languages
Chinese (zh)
Other versions
CN104844197A (en
Inventor
杨长红
冯超
李姝欣
韩亚洁
胡雪卿
焦芳莹
钱进
杜雄斌
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Jinan
Original Assignee
University of Jinan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Jinan filed Critical University of Jinan
Priority to CN201510231730.7A priority Critical patent/CN104844197B/en
Publication of CN104844197A publication Critical patent/CN104844197A/en
Application granted granted Critical
Publication of CN104844197B publication Critical patent/CN104844197B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention belongs to electronic functional material field, and in particular to a kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate.The chemical general formula of the series thin film is Na0.5Bi0.5Ti1‑yXyO3‑δ, wherein X is doped chemical;Y is the doping of doped chemical;δ is to maintain the number of oxygen atom that charge balance lost.The present invention on a silicon substrate, is prepared for the bismuth-sodium titanate base film with (100) preferred orientation using the chemical solution deposition technology of preparing of optimization.Whole preparation process of the invention is simple, easily-controllable, with low cost, and the film crystalline phase prepared is single, and preferred orientation degree is high.

Description

A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate
Technical field
The invention belongs to electronic functional material and devices field, and in particular to be one kind grow on a silicon substrate (100) method of preferred orientation bismuth titanate sodium base film.
Background technology
It is difficult to sink in the ferro-electric device based on ferroelectricity-semiconductor heterostructure by perovskite structure, on silicon chip The single Perovskite Phase of product.For example, Kumar et al. deposition growing PMN-PT film [bibliography on different substrates:P. Kumar, Sonia, R.K. Patel, C. Prakash, T.C. Goel, Effect of substrates on phase formation in PMN-PT 68/32 thin films by sol-gel process, Mater. Chem. Phys, 2008,110(1):7-10.].The result of research finds that the Perovskite Phase being deposited directly on silicon has only reached 49%.Together Sample, to the bismuth-sodium titanate (Na of unleaded perovskite structure0.5Bi0.5TiO3) for film, due to silicon chip and Na0.5Bi0.5TiO3It is thin The mistake matching degree of film is up to 40% so that pure Perovskite Phase is grown on monocrystalline silicon substrate extremely difficult.Gong et al. has found straight Meet (the Na being grown on silicon0.8K0.2)0.5Bi0.5TiO3Almost without Perovskite Phase, Jiao Lvshi phase [bibliography is all: Y.Q. Gong, R.J. Huang, X.J. Li, X.J. Zheng, Effects of lattice and thermal mismatch induced by different seed layerson (Na0.8K0.2)0.5Bi0.5TiO3 ferroelectric thin film, Appl. Mach. Mater, 2013, 291-294: 2636-2640].Although Kim et al. has grown many Brilliant Perovskite Phase Na0.5Bi0.5TiO3Film, but still there is burnt green stone phase (at 30 ° of peak positions) [bibliography:C.Y. Kim, The synthesis of lead-free ferroelectric Bi1/2Na1/2TiO3 thin film by solution Sol-gel method,J. Sol-Gel. Sci. Tech, 2005, 33, 307-314] .As can be seen here, in monocrystalline silicon substrate It is difficult to the Na for growing pure perovskite phase on piece0.5Bi0.5TiO3Film.
In addition, the miniaturization for realizing device using film, it is necessary to the uniformity of holding structure.Structure it is uneven Property will cause the inhomogeneities of performance, and then directly influence the stability and reliability of device.But the film of mono-crystalline structures High cost is prepared, technique is harsh.And the polycrystal film of preferred orientation has the performance for being similar to monocrystalline.Selected therefore, it is necessary to prepare The film of excellent orientation realizes the optimization of performance.
The present invention grows bismuth-sodium titanate by the chemical solution deposition and Technology for Heating Processing of optimization on monocrystalline silicon substrate Base film, the Na prepared0.5Bi0.5TiO3Base film has pure perovskite phase and with (100) preferred orientation.
The content of the invention
It is an object of the invention to provide a kind of Na of oriented growth0.5Bi0.5TiO3The preparation method of base film, more specifically It is to disclose a kind of growth (100) preferred orientation Na on a silicon substrate0.5Bi0.5TiO3The method of base film.Prepared Na0.5Bi0.5TiO3Base film has (100) preferred orientation, and good crystallinity, consistency are high.
Above-mentioned Na0.5Bi0.5TiO3The chemical general formula of base film is Na0.5Bi0.5Ti1-yXyO3-δ, wherein X is doped chemical;y For the doping of doped chemical;δ is to maintain the number of oxygen atom that charge balance lost.
Above-mentioned Na0.5Bi0.5TiO3Doped chemical X is manganese ion, zirconium ion, zinc ion and iron ion in base film.
Above-mentioned Na0.5Bi0.5TiO3The preparation method of base film includes following steps:
(1) preparation of bismuth-sodium titanate base film precursor solution
1. it is raw material to choose sodium acetate, bismuth nitrate, manganese acetate, zirconium nitrate, zinc acetate, ferric nitrate and tetra-n-butyl titanate. According to Na0.5Bi0.5Ti1-yXyO3-δStoichiometric proportion, accurately weigh raw material.Appropriate polyethylene glycol 20,000 is separately weighed, it is standby Use
2. weigh a certain amount of acetylacetone,2,4-pentanedione the tetra-n-butyl titanate of equivalent is weighed in beaker, then and acetyl is added dropwise In acetone.At room temperature, the chelating for completing titanium for 4-8 hours is stirred on magnetic stirring apparatus.It is defined as solution 1.
3. the dissolving of sodium, bismuth, manganese, zirconium, zinc and iron material can be one kind of following situations:
A is by the sodium acetate weighed, bismuth nitrate and manganese acetate(Or zinc acetate, ferric nitrate)It is dissolved in appropriate acetic acid 40 ~ 60 °C of lower heating stirrings are defined as solution 2 up to being completely dissolved;
The sodium acetate weighed, bismuth nitrate are dissolved in appropriate acetic acid in 40 ~ 60 °C of lower heating stirrings until completely molten by b Solution;The zirconium nitrate weighed is dissolved in 40 ~ 60 °C of lower heating stirrings in ethylene glycol monomethyl ether, does not wait solution cooling to be added dropwise appropriate Acetylacetone,2,4-pentanedione to clarify.Two kinds of solution are mixed and are defined as solution 2.
4. the polyethylene glycol 20,000 weighed is dissolved in ethylene glycol monomethyl ether, in 50 ~ 70 °C of heating stirrings until completely molten Solution, is defined as solution 3.
5. after after the cooling of all solution, solution 2, solution 3 are gradually added in solution 1, and is stirred on magnetic stirring apparatus 8 ~ 14 hours are mixed to being well mixed, the concentration of precursor solution is controlled in 0.2 ~ 0.4mol/L.
(2) cleaning of monocrystalline silicon substrate
1. acetone is cleaned by ultrasonic;2. absolute ethyl alcohol is cleaned by ultrasonic;3. the concentrated sulfuric acid:Hydrogen peroxide=1:1 boils and keeps 15min; 4. 10min is rinsed in the deionized water boiled;5. infrared lamp dry for standby;
(3) preparation of thin-film material:Annealing process layer by layer is combined with spin-coating method and prepares film
1. precursor solution is evenly coated on silicon chip using the method for spin coating, is then placed on electric boiling plate It is upper to be pre-processed, then it is put into progress annealing in RTA stove
2. the film after annealing is repeated into said process, until the thickness of film reaches that 300~500nm thickness will Ask.
In above-mentioned preparation process, heat treatment process is:Pre-processed 2 ~ 3 minutes at 250-300 °C, 120s be incubated at 300 °C, Then 20s is incubated at 450 °C, is finally incubated 600s at 500 ~ 600 °C.
The present invention is prepared for the Na of preferred orientation on a silicon substrate first0.5Bi0.5TiO3Base film.The film of preparation has (100) preferred orientation.
Brief description of the drawings
Fig. 1 is the Na grown on a silicon substrate0.5Bi0.5TiO3The X ray diffracting spectrum of film.Wherein, abscissa is to spread out The θ of firing angle 2, ordinate is diffracted intensity.(100) degree of orientation is 93%.
Fig. 2 is the Na grown on a silicon substrate0.5Bi0.5TiO3The scanning electron microscope (SEM) photograph of film.
Fig. 3 is the Na grown on a silicon substrate0.5Bi0.5Ti0.98Mn0.02O3-δThe X ray diffracting spectrum of film.Wherein, it is horizontal Coordinate is the θ of the angle of diffraction 2, and ordinate is diffracted intensity.(100) degree of orientation is 88%.
Fig. 4 is the Na grown on a silicon substrate0.5Bi0.5Ti0.98Mn0.02O3-δThe scanning electron microscope (SEM) photograph of film.
Fig. 5 is the Na grown on a silicon substrate0.5Bi0.5Ti0.98Zr0.02O3-δThe X ray diffracting spectrum of film.Wherein, it is horizontal Coordinate is the θ of the angle of diffraction 2, and ordinate is diffracted intensity.(100) degree of orientation is 91%.
Fig. 6 is the Na grown on a silicon substrate0.5Bi0.5Ti0.98Zr0.02O3-δThe scanning electron microscope (SEM) photograph of film.
Fig. 7 is the Na grown on a silicon substrate0.5Bi0.5Ti0.99Zn0.01O3-δThe X ray diffracting spectrum of film.Wherein, it is horizontal Coordinate is the θ of the angle of diffraction 2, and ordinate is diffracted intensity.(100) degree of orientation is 94%.
Fig. 8 is the Na grown on a silicon substrate0.5Bi0.5Ti0.99Zn0.01O3-δThe scanning electron microscope (SEM) photograph of film.
Fig. 9 is the Na grown on a silicon substrate0.5Bi0.5Ti0.99Fe0.01O3-δThe X ray diffracting spectrum of film.Wherein, it is horizontal Coordinate is the θ of the angle of diffraction 2, and ordinate is diffracted intensity.(100) degree of orientation is 86%.
Figure 10 is the Na grown on a silicon substrate0.5Bi0.5Ti0.99Fe0.01O3-δThe scanning electron microscope (SEM) photograph of film.
Embodiment
With reference to specific embodiment, the present invention will be further elaborated, it is necessary to illustrate, the description below is only In order to explain the present invention, its content is not limited.
Embodiment 1
(1) according to Na0.5Bi0.5TiO3Stoichiometric proportion, 0.3446g CH is weighed exactly3COONa (excessive 4 %), 2.1167g Bi (NO3)3·5H2O (excessive 8 %) and 0.3g polyethylene glycol 20,000, it is standby.2.78ml second is measured exactly The tetra-n-butyl titanate that acyl acetone measures 2.78ml in beaker, then is added dropwise in acetylacetone,2,4-pentanedione, on magnetic stirring apparatus Stirring completes the chelating of titanium for 4 hours, is defined as solution 1.By load weighted CH3COONa、Bi(NO3)3·5H2O, which is added to, to be filled In the beaker of 15ml glacial acetic acid, in 40 °C of lower heating stirrings, until all dissolvings, are adding 5ml ethylene glycol monomethyl ether, definition For solution 2.Load weighted polyethylene glycol 20,000 is added in the beaker for filling 5ml ethylene glycol monomethyl ethers, it is straight in 50 °C of heating stirrings To whole dissolvings, solution 3 is defined as.After after the cooling of all solution, solution 2 and 3 is respectively added slowly in solution 1.Will be mixed The solution got togather is positioned on magnetic stirring apparatus and stirred 8 hours.Obtain concentration uniform and stable for 0.23mol/L Na0.5Bi0.5TiO3Precursor solution
(2) with sol evenning machine using the method for spin-coating by Na0.5Bi0.5TiO3Precursor solution is deposited on a silicon substrate. The rotating speed of sol evenning machine is 4000r/min, and spin coating time is 30s.Then film is placed on electric boiling plate and pre-processed, pretreatment Temperature is 250 °C, and the time of pretreatment is 2min or so.Finally film is placed in RTA stove and carried out at annealing Reason.The technical process of annealing is:It is incubated under 300 °C under 120s, 450 °C and is incubated 20s, is incubated under certain annealing temperature 600s.First 6 layers of annealing temperature is that 550-570 °C, latter two layers of annealing temperature is 540-550 °C.Above-mentioned technical process is repeated, Until film thickness reaches about 280nm.
Embodiment 2
(1) according to Na0.5Bi0.5Ti0.98Mn0.02O3-δStoichiometric proportion, 0.3446g CH is weighed exactly3COONa (excessive 4 %), 2.1167g Bi (NO3)3·5H2O (excessive 8 %), 0.0396g C4H6MnO4·4H2O and 0.3g poly- second Glycol 20,000, it is standby.The tetra-n-butyl titanate that 2.72ml acetylacetone,2,4-pentanedione measures 2.72ml in beaker, then is measured exactly It is added dropwise in acetylacetone,2,4-pentanedione, the chelating for completing titanium for 6 hours is stirred on magnetic stirring apparatus, solution 1 is defined as.Will be load weighted CH3COONa、Bi(NO3)3·5H2O、C4H6MnO4·4H2O is added in the beaker for the glacial acetic acid for filling 15ml to be heated under 50 °C Stirring, until all dissolvings, are adding 5ml ethylene glycol monomethyl ether, be defined as solution 2.Load weighted polyethylene glycol 20,000 is added Into the beaker for filling 5ml ethylene glycol monomethyl ethers, in 70 °C of heating stirrings until all dissolving, solution 3 is defined as.Treat all solution After cooling, solution 2 and 3 is respectively added slowly in solution 1.The solution mixed is positioned on magnetic stirring apparatus and stirs 10 Hour.It is Na uniform and stable 0.23mol/L to obtain concentration0.5Bi0.5Ti0.98Mn0.02O3-δPrecursor solution
(2) with sol evenning machine using the method for spin-coating by Na0.5Bi0.5Ti0.98Mn0.02O3-δPrecursor solution is deposited on silicon On substrate.The rotating speed of sol evenning machine is 4000r/min, and spin coating time is 30s.Then film is placed on electric boiling plate and pre-processed, The temperature of pretreatment is 300 °C, and the time of pretreatment is 2min or so.Finally film is placed in RTA stove and carried out Annealing.The technical process of annealing is:It is incubated under 300 °C under 120s, 450 °C and is incubated 20s, under certain annealing temperature It is incubated 600s.Annealing temperature is 550 °C.Above-mentioned technical process is repeated, until film thickness reaches about 500nm.
Embodiment 3
(1) according to Na0.5Bi0.5Ti0.98Zr0.02O3Stoichiometric proportion, 0. 3446g CH is weighed exactly3COONa (excessive 4 %), 2.1167g Bi (NO3)3·5H2O (excessive 8 %), 0.0639g Zr (NO3)4·5H2O and 0.3g poly- second Glycol 20,000, it is standby.The tetra-n-butyl titanate that 2.72ml acetylacetone,2,4-pentanedione measures 2.72ml in beaker, then is measured exactly It is added dropwise in acetylacetone,2,4-pentanedione, the chelating for completing titanium for 6 hours is stirred on magnetic stirring apparatus, solution 1 is defined as.Will be load weighted Zr(NO3)4·5H2O adds 5ml ethylene glycol monomethyl ether heating stirring, does not wait solution cooling that 5ml acetylacetone,2,4-pentanedione is added dropwise extremely Clarification.By load weighted CH3COONa、Bi(NO3)3·5H2O is added in the beaker for the glacial acetic acid for filling 15ml to be added under 50 °C Thermal agitation, until all dissolvings.Above two solution is mixed and is defined as solution 2.Load weighted polyethylene glycol 20,000 is added to In the beaker for filling 5ml ethylene glycol monomethyl ethers, in 60 °C of heating stirrings until all dissolving, solution 3 is defined as.Treat that all solution are cold But after, solution 2 and 3 is respectively added slowly in solution 1.The solution mixed is positioned over stirring 12 on magnetic stirring apparatus small When.It is Na uniform and stable 0.23mol/L to obtain concentration0.5Bi0.5Ti0.98Zr0.02O3Precursor solution
(2) with sol evenning machine using the method for spin-coating by Na0.5Bi0.5Ti0.98Zr0.02O3Precursor solution is deposited on silicon On substrate.The rotating speed of sol evenning machine is 4000r/min, and spin coating time is 30s.Then film is placed on electric boiling plate and pre-processed, The temperature of pretreatment is 250 °C, and the time of pretreatment is 2min or so.Finally film is placed in RTA stove and carried out Annealing.The technical process of annealing is:It is incubated under 280 °C under 120s, 450 °C and is incubated 20s, under certain annealing temperature It is incubated 600s.First 9 layers of annealing temperature is that 570-580 °C, latter 5 layers of annealing temperature is 560-570 °C.Repeat above-mentioned technique mistake Journey, until film thickness reaches about 470nm.
Embodiment 4
(1) according to Na0.5Bi0.5Ti0.99Zn0.01O3-δStoichiometric proportion, 0.3446g CH is weighed exactly3COONa (excessive 4 %), 2.1167g Bi (NO3)3·5H2O (excessive 8 %), 0.0177g C4H6ZnO4·4H2O and 0.3g poly- second Glycol 20,000, it is standby.The tetra-n-butyl titanate that 2.75ml acetylacetone,2,4-pentanedione measures 2.75ml in beaker, then is measured exactly It is added dropwise in acetylacetone,2,4-pentanedione, the chelating for completing titanium for 6 hours is stirred on magnetic stirring apparatus, solution 1 is defined as.Will be load weighted CH3COONa、Bi(NO3)3·5H2O、C4H6ZnO4·4H2O is added in the beaker for the glacial acetic acid for filling 15ml to be heated under 40 °C Stirring, until all dissolvings, are adding 5ml ethylene glycol monomethyl ether, be defined as solution 2.Load weighted polyethylene glycol 20,000 is added Into the beaker for filling 5ml ethylene glycol monomethyl ethers, in 50 °C of heating stirrings until all dissolving, solution 3 is defined as.Treat all solution After cooling, solution 2 and 3 is respectively added slowly in solution 1.The solution mixed is positioned on magnetic stirring apparatus and stirs 10 Hour.It is Na uniform and stable 0.23mol/L to obtain concentration0.5Bi0.5Ti0.99Zn0.01O3-δPrecursor solution
(2) with sol evenning machine using the method for spin-coating by Na0.5Bi0.5Ti0.99Zn0.01O3-δPrecursor solution is deposited on silicon On substrate.The rotating speed of sol evenning machine is 4000r/min, and spin coating time is 30s.Then film is placed on electric boiling plate and pre-processed, The temperature of pretreatment is 250 °C, and the time of pretreatment is 3min or so.Finally film is placed in RTA stove and carried out Annealing.The technical process of annealing is:It is incubated under 260 °C under 120s, 450 °C and is incubated 20s, under certain annealing temperature It is incubated 600s.First 7 layers of annealing temperature is that 560 °C, latter 6 layers of annealing temperature is 550 °C.Above-mentioned technical process is repeated, until Film thickness reaches about 440nm.
Embodiment 5
(1) according to Na0.5Bi0.5Ti0.99Fe0.01O3-δStoichiometric proportion, 0.3446g CH is weighed exactly3COONa (excessive 4 %), 2.1167g Bi (NO3)3·5H2O (excessive 8 %), 0.0177g C4H6ZnO4·4H2O and 0.3g poly- second Glycol 20,000, it is standby.The tetra-n-butyl titanate that 2.75ml acetylacetone,2,4-pentanedione measures 2.75ml in beaker, then is measured exactly It is added dropwise in acetylacetone,2,4-pentanedione, the chelating for completing titanium for 4 hours is stirred on magnetic stirring apparatus, solution 1 is defined as.Will be load weighted CH3COONa、Bi(NO3)3·5H2O、C4H6ZnO4·4H2O is added in the beaker for the glacial acetic acid for filling 15ml to be heated under 50 °C Stirring, until all dissolvings, are adding 5ml ethylene glycol monomethyl ether, be defined as solution 2.Load weighted polyethylene glycol 20,000 is added Into the beaker for filling 5ml ethylene glycol monomethyl ethers, in 60 °C of heating stirrings until all dissolving, solution 3 is defined as.Treat all solution After cooling, solution 2 and 3 is respectively added slowly in solution 1.The solution mixed is positioned on magnetic stirring apparatus and stirs 8 Hour.It is Na uniform and stable 0.23mol/L to obtain concentration0.5Bi0.5Ti0.99Fe0.01O3-δPrecursor solution
(2) with sol evenning machine using the method for spin-coating by Na0.5Bi0.5Ti0.99Fe0.01O3-δPrecursor solution is deposited on silicon On substrate.The rotating speed of sol evenning machine is 4000r/min, and spin coating time is 30s.Then film is placed on electric boiling plate and pre-processed, The temperature of pretreatment is 250 °C, and the time of pretreatment is 2min or so.Finally film is placed in RTA stove and carried out Annealing.The technical process of annealing is:It is incubated under 270 °C under 120s, 450 °C and is incubated 20s, under certain annealing temperature It is incubated 600s.First 4 layers of annealing temperature is that 560-570 °C, latter 4 layers of annealing temperature is 540-560 °C.Repeat above-mentioned technique mistake Journey, until film thickness reaches about 300nm.

Claims (3)

1. a kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate;The method of preparation is optimization Chemical solution deposition and Technology for Heating Processing;It is characterized in that:With chemical general formula Na0.5Bi0.5Ti1-yXyO3-δ, wherein X is doping Element;Y is the doping of doped chemical;δ is to maintain the number of oxygen atom that charge balance lost;Wherein, the titanium The preparation technology of sour bismuth sodium base film includes following steps:
(1) preparation of bismuth-sodium titanate base film precursor solution
1) it is raw material to choose sodium acetate, bismuth nitrate, manganese acetate, zirconium nitrate, zinc acetate, ferric nitrate and tetra-n-butyl titanate;According to Na0.5Bi0.5Ti1-yXyO3-δStoichiometric proportion, accurately weigh raw material;Appropriate polyethylene glycol 20,000 is separately weighed, it is standby;
2) weigh a certain amount of acetylacetone,2,4-pentanedione the tetra-n-butyl titanate of equivalent is weighed in beaker, then and acetylacetone,2,4-pentanedione is added dropwise In;At room temperature, the chelating for completing titanium for 4-8 hours is stirred on magnetic stirring apparatus;It is defined as solution 1;
3) dissolving of sodium, bismuth, manganese, zirconium, zinc and iron material can be one kind of following situations:
A weighs any of sodium acetate and bismuth nitrate, and manganese acetate, zinc acetate, ferric nitrate raw material respectively, is dissolved in appropriate In acetic acid, in 40 ~ 60 °C of lower heating stirrings until being completely dissolved, solution 2 is defined as;
The sodium acetate weighed, bismuth nitrate are dissolved in appropriate acetic acid by b, in 40 ~ 60 °C of lower heating stirrings until being completely dissolved; The zirconium nitrate weighed is dissolved in 40 ~ 60 °C of lower heating stirrings in ethylene glycol monomethyl ether, does not wait solution cooling to be added dropwise appropriate Acetylacetone,2,4-pentanedione is extremely clarified;Two kinds of solution are mixed and are defined as solution 2;
4) polyethylene glycol 20,000 weighed is dissolved in ethylene glycol monomethyl ether, it is fixed in 50 ~ 70 °C of heating stirrings until being completely dissolved Justice is solution 3;
5) after all solution cooling after, solution 2, solution 3 are gradually added in solution 1, and on magnetic stirring apparatus stirring 8 ~ To being well mixed, the concentration of precursor solution is controlled in 0.2 ~ 0.4mol/L within 14 hours;
(2) cleaning of monocrystalline silicon substrate
1) acetone is cleaned by ultrasonic;2) absolute ethyl alcohol is cleaned by ultrasonic;3) concentrated sulfuric acid:Hydrogen peroxide=1:1 boils and keeps 15min;4) exist 10min is rinsed in the deionized water boiled;5) infrared lamp dry for standby;
(3) preparation of thin-film material:Annealing process layer by layer is combined with spin-coating method and prepares film
1) precursor solution is evenly coated on silicon chip using the method for spin coating, is then placed on electric boiling plate enterprising Row pretreatment, then be put into RTA stove and made annealing treatment;
2) film after annealing is repeated into said process, until the thickness of film reaches 300 ~ 500nm thickness requirements.
2. one kind grows the method for (100) preferred orientation bismuth titanate sodium base film on a silicon substrate as described in the appended claim 1, its It is characterized in:Doped chemical X is manganese ion, zirconium ion, zinc ion and iron ion.
3. one kind grows the method for (100) preferred orientation bismuth titanate sodium base film on a silicon substrate as described in claim 1, It is characterized in that:Pre-processed 2 ~ 3 minutes at 250-300 °C, 120s is incubated at 300 °C, be then incubated 20s at 450 °C, finally exist 500-600 °C of insulation 600s.
CN201510231730.7A 2015-05-08 2015-05-08 A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate Expired - Fee Related CN104844197B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510231730.7A CN104844197B (en) 2015-05-08 2015-05-08 A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510231730.7A CN104844197B (en) 2015-05-08 2015-05-08 A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate

Publications (2)

Publication Number Publication Date
CN104844197A CN104844197A (en) 2015-08-19
CN104844197B true CN104844197B (en) 2017-07-14

Family

ID=53844244

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510231730.7A Expired - Fee Related CN104844197B (en) 2015-05-08 2015-05-08 A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate

Country Status (1)

Country Link
CN (1) CN104844197B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113970529A (en) * 2021-10-21 2022-01-25 西安微电子技术研究所 Method for testing boron doping amount of bipolar integrated circuit isolation process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072129A (en) * 2014-04-18 2014-10-01 济南大学 B-position equivalent zirconium doped sodium bismuth titanate film
CN104496468A (en) * 2014-11-27 2015-04-08 济南大学 Method for realizing coercive field reduction and pressure resistance improvement of sodium bismuth titanate-based film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072129A (en) * 2014-04-18 2014-10-01 济南大学 B-position equivalent zirconium doped sodium bismuth titanate film
CN104496468A (en) * 2014-11-27 2015-04-08 济南大学 Method for realizing coercive field reduction and pressure resistance improvement of sodium bismuth titanate-based film

Also Published As

Publication number Publication date
CN104844197A (en) 2015-08-19

Similar Documents

Publication Publication Date Title
CN105957970B (en) A kind of preparation method of large size single crystal perovskite thin film
CN100587910C (en) Preparation for ferroelectric material with quartz/lanthanum nickelate/bismuth ferrite-lead titanate three-layer structure
CN109627043B (en) Preparation method of pure-phase bismuth ferrite film with high preferred orientation
CN104193316B (en) Yttrium iron garnet film and preparation method thereof
CN101665915B (en) Method for preparing bismuth ferric film material
CN103073064B (en) Method for preparing Gd and Co codoped high-remanent-polarization BiFeO3 thin film by sol-gel method
CN101183595B (en) P type doping ZnO based rare magnetic semiconductor material and method of producing the same
CN103833416B (en) A kind of chemical solution deposition preparation method of the sour lanthanum conductive film of nickel
CN106410045B (en) Based on CH3NH3PbI3P-type HHMT transistor of material and preparation method thereof
CN106449993B (en) N-type HEMT device and preparation method thereof using perovskite as light absorbing layer
CN101587763B (en) Method for preparing buffer layers of high-temperature superconducting coating conductors
CN104844197B (en) A kind of method for growing (100) preferred orientation bismuth titanate sodium base film on a silicon substrate
CN103074576B (en) Zno-based diluted semi-conductor thin-film and preparation method thereof
CN103060887B (en) Method for preparing high-remanent-polarization BiFeO3 film with preferentially growing (110) crystal face by sol-gel process
CN102534587A (en) Method for preparing BiFeO3 film through sol-gel method
CN103553000A (en) Method for preparing topological insulator Bi2Se3 and perovskite oxide La0.7Sr0.3MnO3 composite structure
CN101211764A (en) Chromium doped titanium dioxide ferromagnetic film room temperature preparation method
CN103073303B (en) Method for preparing highly oriented (100) lead-free piezoelectric thin film
CN110950660B (en) Method for improving dielectric and pyroelectric properties of relaxor ferroelectric film
CN104131333B (en) Method for preparing K0.5Na0.5NbO3 single crystal
CN107034452B (en) The chemical production method of flexible doping type ZnO-based transparent conductive film
CN113774485B (en) Lead indium niobate-lead magnesium niobate-lead titanate ferroelectric film material, preparation and application thereof
CN110172734B (en) Cubic phase doped cerium ferrite magneto-optical material and preparation method and application thereof
CN103011813A (en) Method for preparing high-concentration lithium tantalite thin film by sol-gel method
CN102863019B (en) Preparation method of spinel-structured film type lithium titanate negative electrode material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
EXSB Decision made by sipo to initiate substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170714

Termination date: 20200508

CF01 Termination of patent right due to non-payment of annual fee