CN1438200A - Preparation of SrBi2Ta2O9 ferroelectric ceramic film by inorganic salt rawmaterial liquid-phase chemical method - Google Patents

Preparation of SrBi2Ta2O9 ferroelectric ceramic film by inorganic salt rawmaterial liquid-phase chemical method Download PDF

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CN1438200A
CN1438200A CN 03100039 CN03100039A CN1438200A CN 1438200 A CN1438200 A CN 1438200A CN 03100039 CN03100039 CN 03100039 CN 03100039 A CN03100039 A CN 03100039A CN 1438200 A CN1438200 A CN 1438200A
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film
srbi
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CN1223548C (en
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季惠明
徐廷献
徐明霞
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Tianjin University
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Tianjin University
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Abstract

The method of preparing SrBi2Ta2O9 ferroelectric ceramic film by using inorganic salt as raw material and adopting liquid-phase chemical method includes: preparation of soluble inorganic salt raw material, preparation of SrBi2Ta2O9 solution, preparation of SrBi2Ta2O9 sol and preparation of SrBi2Ta2O9 film. Said invention uses inorganics as raw material firstly, and adopts complexing agent chelation technique and utilizes the inorganic salt solution liquid phase chemical method to successfully prepare out SrBi2Ta2O9 ferroelectric ceramic film.

Description

The inorganic salt raw material liquid chemical method prepares SrBi 2Ta 2O 9Ferroelectric ceramic thin film
Technical field
The invention belongs to the electronic material engineering, particularly be that the inorganic salt raw material liquid chemical method prepares SrBi 2Ta 2O 9Ferroelectric ceramic thin film.
Background technology
SrBi 2Ta 2O 9(SBT) ferroelectric ceramic thin film is mainly used in non-volatility ferroelectric random access memory (NVFRAM).Along with the development of information technology, the integrated storage element of this in recent years ferroelectric thin-flim materials and silicon is greatly paid close attention to.
SrBi 2Ta 2O 9Various means, the method for ferroelectric thin-flim materials preparation emerge in an endless stream.Situation from present research report roughly has following kind:
(1) pulsed laser deposition and magnetron sputtering etc. in the physics method.
(2) sol-gel method, chemical Vapor deposition process, metal-organic decomposition method, superpolymer precursor process and metal-organic chemical vapor deposition equipment method etc. in the chemical method.
Sinter target material into after at first various burning raw materials will being mixed in the physics legal system film, and then bombard or sputter system film with laser pulse, this method raw material is easy to get but the membrane equipment complex and expensive, and multi-component material is wayward; No matter in the chemical method be vapor phase process or liquid phase method, the raw material that uses all is the metal organic salt compounds at present.Domestic this raw material lacks very much, and a dependence on import is even price is also very expensive abroad.China is at SrBi 2Ta 2O 9The research of ferroelectric ceramic thin film aspect is subjected to the restriction of factors such as equipment and price, and its developing water Pingyuan County lags behind developed countries such as America and Europe.
Summary of the invention
The objective of the invention is to use homemade common inorganics class to be raw material, utilize liquid chemical method to prepare SrBi 2Ta 2O 9Ferroelectric ceramic thin film.
Technology of the present invention is achieved in that
(1) preparation of soluble inorganic salt raw material
(1) the Bi salt brine solution of preparation 0.35-0.5mol/l; Wherein the salts solution of Bi is mainly inorganic salt such as nitrate, chlorate.
(2) the preparation 0.5-0.6mol/l fluorotantalic acid aqueous solution;
(3) the Sr salt brine solution of preparation 0.4-0.6mol/l, wherein the salts solution of Sr is mainly inorganic salt such as nitrate, chlorate.
(2) SrBi 2Ta 2O 9The preparation of solution and colloidal sol
The about 6-10% of the aqueous citric acid solution of 0.2-0.3mol/l concentration (solution accounts for volume of a container per-cent, below roughly the same) is put into container, add the solution 10-17% of (1) in above-mentioned () then, stir and form uniform citric acid-based Bi solution; Splash into (3) solution among the 3-7% above-mentioned (), the same stirring forms uniform citric acid-based Bi+Sr mixing solutions; Splash into (2) 6-10% in above-mentioned () more gradually, stir more than 30 minutes, form the mixing solutions of Bi+Sr+Ta.Notice stoichiometric ratio and the SrBi of mixing solutions adding at this moment Bi, Sr, Ta 2Ta 2O 9And inequality, the excessive about 20-50% of Bi wherein, this be because Bi in the thin-film material of high surface area, through high-temperature heat treatment, its high saturation vapour pressure can cause the part volatilization of Bi.Therefore excessive one of Bi is to be used to compensate volatilization loss, the 2nd, and the excessive improvement that helps this material ferroelectric properties of suitable Bi.
Splashing into concentration in above mixing solutions is the ethylene glycol solution 3-7% of 0.2-0.3mol/l, and is heated to 50-60 ℃, forms polyreaction, stirs 2-3 hour.Add the ethylenediamine tetraacetic acid (EDTA) that 3-7% concentration is 0.2-0.3mol/l (EDTA) ammonia soln behind the cool to room temperature again, be used to regulate acid-basicity to pH≤3 and polyreaction is further carried out, stirred 2-3 hour, and place more than 3 days, form last complexing stable contain SrBi 2Ta 2O 9Concentration is that the 0.04-0.08mol/lBi+Sr+Ta mixed sols is stand-by.
For SrBi 2Ta 2O 9The preparation of film can be adopted usual method.
The present invention adopts following method:
(1) adopt dip-coating method film forming or rotation to apply film forming;
(2) drying process: the sol pellicle for preparing was toasted about 15-20 minute under 100 ℃ of-150 ℃ of temperature, to remove wherein moisture content and part organic solvent.
(3) thermal treatment: the film after will drying is warming up to 300 ℃-400 ℃ with the speed of 3-5 ℃/min, is incubated 20-40 minute, removes wherein organic complex group and other volatile matter.
(4) sintering: the film of above-mentioned preparation is warmed up to 700 ℃-850 ℃ temperature with the speed of 5-8 ℃/min, and under mobile oxygen condition, carries out sintering, insulation 20-40 minute, form film with certain crystalline state phase composite and even compact.
(5) repetitive operation: the operating process of repetition above (1) to (4) 5-8 time, form film until obtaining the thick SBT of 400-600nm.Method in the preparation of above-mentioned (one) soluble inorganic salt raw material can adopt following method:
(1) system Bi salt brine solution: because the nitrate of Bi and chlorate very little and facile hydrolysis under the solubleness normal temperature in water, so need the following process for preparation of employing: with nitrate is example, takes by weighing Bi (NO 3) 35H 2O raw material 20-30 gram, the salpeter solution of the 30%-40% of adding 20-30ml is heated to 40-50 ℃, stirs 20-30 minute to the solution clarification, adds water 100-120ml and is diluted to 0.35-0.5mol/l concentration, and the cooling back is stand-by.
(2) the preparation fluorotantalic acid aqueous solution: accurately take by weighing Ta powder 5-6 gram, join in about 40% hydrofluoric acid solution of 5ml, at room temperature dissolved 1-2 days, treat that it all after the dissolving, adds water 50-60ml and be diluted to 0.5-0.6mol/l concentration.
(3) preparation Sr salt brine solution: with nitrate is example, accurately weighing Sr (NO 3) 2Raw material 20-25 gram is dissolved in it in 200-250ml water, forms 0.4-0.6mol/l concentration solution.
Above-mentioned SrBi 2Ta 2O 9Rotation coating film is in (1) of the preparation of film: rotation applies film process as shown in Figure 2.With cleaned Si/SiO 2/ Ti/Pt substrate 3 adheres to the center of equal glue machine support pallet 4, after splashing into the SBT colloidal sol 1 for preparing previously on the substrate, under the drive of turning axle 5, apply 20-30 second with the about 2000-4000 of rotating speed rev/min speed rotation, thereby form certain thickness dissolved glue film 2.
Above-mentioned SrBi 2Ta 2O 9The dip-coating method film-forming technology process is in (1) of the preparation of film: clamp substrate through cleaning with the pulling machine dop, slowly immerse among the colloidal sol, static 5-10 is after second, and 0.4-0.6m/min lifts out from colloidal sol with average rate.
Drying process can be carried out the sol pellicle for preparing under heating plate or infrared lamp radiation situation.Heat treatment process can
Putting into electric furnace with the film after will drying carries out.
By the theoretical and experimental study more than 3 years, we are adopting said method successfully, has prepared SrBi 2Ta 2O 9Ferroelectric ceramic thin film reaches and use the metallorganics salt to be the close electrical property result of raw material system film abroad, and its dielectric and ferroelectric properties result are: specific inductivity (10kHz) is 200-238, and dielectric loss (10kHz) is 0.04-0.05, residual polarization 2P r(under the 3.5V) is 8.8-9.8 μ C/cm 2, coercive electric field 2E c(under the 3.5V) is 66-80KV/cm.
SrBi 2Ta 2O 9Ferroelectric ceramic thin film is because its lower read-write voltage, read or write speed faster, advantage such as fatigue resistance preferably, be the ideal material replacer of ferroelectric non-volatile message memory of future generation, it also has tempting application prospect aspect electron devices such as pyroelectric infrared detector, photoswitch, indicating meter simultaneously.
SrBi 2Ta 2O 9The raw material that the preparation of ferroelectric ceramic thin film is adopted aspect liquid chemical method at present both at home and abroad all is the metal organic salt compounds.The present invention is raw material first with the inorganics, adopts the complexing agent chelating technology, utilizes inorganic salt solution-sol-gel (ISG) liquid chemical method successfully to prepare SrBi 2Ta 2O 9Ferroelectric ceramic thin film.This method prepares SrBi to utilizing the china natural resources advantage 2Ta 2O 9Film, the Information of Development industrial technology has important realistic meaning.
Description of drawings Fig. 1: preparation SrBi 2Ta 2O 9The schema of colloidal sol; Fig. 2: dissolved glue film spin coating process synoptic diagram.
Embodiment
Embodiment 1:
1. the preparation of soluble inorganic salt raw material
(1) preparation Bi salts solution: take by weighing Bi (NO 3) 35H 2O raw material 29.1 gram adds 36% the salpeter solution of 20ml, is heated to 50 ℃, stirs 30 minutes to the solution clarification, adds water 100ml and is diluted to 0.5mol/l concentration, and is stand-by after the cooling.
(2) preparation fluorotantalic acid solution: accurately take by weighing Ta powder 6 grams, add in the 5ml hydrofluoric acid and at room temperature dissolved 2 days, treat that it all after the dissolving, adds water 55ml and be diluted to 0.55mol/l concentration.
(3) preparation Sr salts solution: accurate weighing Sr (NO 3) 2Raw material 21.2 grams are dissolved in it in 200ml water, form 0.5mol/l concentration solution.
2.SrBi 2Ta 2O 9The preparation of colloidal sol
The preparation of SBT colloidal sol is shown in the schema of Fig. 1.At first the about 10ml of the aqueous citric acid solution of 0.25mol/l concentration is contained in a 150ml beaker, add the Bi (NO of the 0.5mol/l for preparing then 3) 3Solution 20ml stirs and forms uniform citric acid-based Bi solution.Splash into the Sr (NO of 0.5mol/l 3) 2Solution 8ml, the same stirring forms uniform citric acid-based Bi+Sr mixing solutions.Splash into 0.55mol/l fluorotantalic acid solution 14.5ml more gradually, stir more than 30 minutes, form the mixed solution of Bi+Sr+Ta, wherein Bi is excessive about 25%, the ferroelectric properties that is used to compensate volatilization loss He improves material.
To splash into the ethylene glycol solution 6ml that concentration is 0.25mol/l in the above mixing solutions, and be heated to 50 ℃, form polyreaction, stirred 3 hours.Add the ethylenediamine tetraacetic acid (EDTA) that 6ml concentration is 0.25mol/l (EDTA) ammonia soln behind the cool to room temperature again, be used to regulate acid-basicity and polyreaction is further carried out, stirred 3 hours, and place more than 3 days, form the stable SrBi that contains at last 2Ta 2O 9Concentration is that the Bi+Sr+Ta mixed sols of 0.062mol/l is stand-by.
3.SrBi 2Ta 2O 9The preparation of film
(1) rotation applies: rotation applies film process as shown in Figure 2.With Si/SiO 2/ Ti/Pt substrate 3 usefulness deionized waters and alcohol are cleaned under ultrasonic wave, adhere to the center of equal glue machine support pallet 4, after splashing into the colloidal sol 1 for preparing previously on the substrate, under the drive of turning axle 5, the speed rotation about 3000 rev/mins with rotating speed applied 30 seconds, thereby formed certain thickness dissolved glue film 2.
(2) drying process: the sol pellicle for preparing was toasted about 20 minutes down for 120 ℃ at infrared lamp, to remove wherein moisture content and part organic solvent.
(3) thermal treatment: the film after will drying is put into electric furnace, is warming up to 400 ℃ with the speed of 5 ℃/min, is incubated 30 minutes, removes wherein each other volatile matter of organic complex group.
(4) sintering: the film of above-mentioned preparation with the speed of the 7 ℃/min temperature at 750 ℃, is carried out sintering under the mobile oxygen atmosphere, be incubated 30 minutes, form film with certain phase composite and even compact.
(5) repetitive operation: repeat above operating process 6 times, obtain the thick SBT film of about 450nm.
Embodiment 2:
Step of preparation process is identical with embodiment 1, and different is in the preparation process of film, adopts the dip-coating method film forming to replace rotation to apply film forming.The dip-coating method film-forming technology process is, the about 30ml of colloidal sol of preparation is contained among beaker, clamps substrate through cleaning with the pulling machine dop, slowly immerse among the colloidal sol, after static 5 seconds, 0.5m/min lifts out from colloidal sol with average rate, carries out drying treatment then.Other step is with embodiment 1.Obtain the thick SBT film of about 450nm.
Embodiment 3:
Step of preparation process is identical with embodiment 1, and different is sintering processes temperature difference last in the preparation process of film.This example changes sintering temperature into 800 ℃ by 750 ℃.Obtain the thick SBT film of about 450nm.Embodiment 4:
Step of preparation process is identical with embodiment 1, and different is in the preparation of raw material, and Bi salt and Sr salt adopt BiCl respectively 3And SrCl 2Replace Bi (NO 3) 3And Sr (NO 3) 3The process for preparation of these two kinds of raw materials is as follows in the experiment: take by weighing BiCl 3H 2O raw material 25.0 grams are dissolved in the 150ml hydrochloric acid acidic solution of pH＜2, are heated to 40 ℃, stir more than 40 minutes and clarify to solution, form the solution for later use of 0.5mol/l concentration; Accurate weighing SrCl 36H 2O raw material 26.6 grams are dissolved in it in 200ml water, form 0.5mol/l concentration solution.Other technology is with example 1.Obtain the thick SBT film of about 450nm.
Table 1SrBi 2Ta 2O 9Ferroelectric membranc electrical property table
All methods and technology of preparing that the present invention discloses and proposes, those skilled in the art can be by using for reference this paper content, links such as appropriate change raw material and operational path realize, although method of the present invention and technology of preparing are described by preferred embodiment, person skilled obviously can change or reconfigure method as herein described and technological line in not break away from content of the present invention, spirit and scope, realizes final film technique.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.

Claims (5)

1. an inorganic salt raw material liquid chemical method prepares SrBi 2Ta 2O 9Ferroelectric ceramic thin film, concrete technology may further comprise the steps:
(1) preparation of soluble inorganic salt raw material
(1) the Bi salt brine solution of preparation 0.35-0.5mol/l; Wherein the salts solution of Bi is mainly nitrate, chlorate
In inorganic salt;
(2) the preparation 0.5-0.6mol/l fluorotantalic acid aqueous solution;
(3) the Sr salt brine solution of preparation 0.4-0.6mol/l, wherein the salts solution of Sr is mainly nitrate, chlorate
In inorganic salt;
(2) SrBi 2Ta 2O 9The preparation of solution and colloidal sol
The about 6-10% of the aqueous citric acid solution of 0.2-0.3mol/l concentration (solution accounts for volume of a container per-cent, below roughly the same) is put into container, add the solution 10-17% of above-mentioned (1) then, stir and form uniform citric acid-based Bi solution; Splash into 3-7% above-mentioned (3) solution, the same stirring forms uniform citric acid-based Bi+Sr mixing solutions; Splash into above-mentioned (2) 6-10% more gradually, stir more than 30 minutes, form the mixed solution of Bi+Sr+Ta;
Splashing into concentration in above mixing solutions is the aqueous glycol solution 3-7% of 0.2-0.3mol/l, and is heated to 50-60 ℃, forms polyreaction, stirs 2-3 hour; Add the ethylenediamine tetraacetic acid (EDTA) that 3-7% concentration is 0.2-0.3mol/l (EDTA) ammonia soln behind the cool to room temperature again, be used to regulate acid-basicity (pH≤3) and polyreaction is further carried out, stirred 2-3 hour, and place more than 3 days, form last complexing stable contain SrBi 2Ta 2O 9Concentration is that the 0.04-0.08mol/lBi+Sr+Ta mixed sols is stand-by;
(3) adopt usual method to prepare SrBi 2Ta 2O 9Film.
2. a kind of inorganic salt raw material liquid chemical method as claimed in claim 1 prepares SrBi 2Ta 2O 9Ferroelectric ceramic thin film is characterized in that: the method for the preparation of above-mentioned (one) soluble inorganic salt raw material is:
(1) system Bi salt brine solution: take by weighing Bi (NO 3) 35H 2O raw material 20-30 gram, the 30%-40% of adding 20-30ml
Salpeter solution, be heated to 40-50 ℃, stir 20-30 minute to solution clarification, add water 100-120ml
Be diluted to 0.35-0.5mol/l concentration, the cooling back is stand-by;
(2) preparation fluorotantalic acid solution: accurately take by weighing Ta powder 5-6 gram, join in about 40% hydrofluoric acid solution of 5ml,
At room temperature dissolved 1-2 days, and treated that it all after the dissolving, added water 50-60ml and be diluted to 0.5-0.6mol/l
Concentration;
(3) preparation Sr salts solution: accurate weighing Sr (NO 3) 2Raw material 20-25 gram is dissolved in it in 200-250ml water,
Form 0.4-0.6mol/l concentration solution.
3. a kind of inorganic salt raw material liquid chemical method as claimed in claim 1 prepares SrBi 2Ta 2O 9Ferroelectric ceramic thin film is characterized in that above-mentioned (three) preparation SrBi 2Ta 2O 9Film process is:
(1) adopt dip-coating method film forming or rotation to apply film forming;
(2) drying process: the sol pellicle for preparing was toasted about 15-20 minute under 100 ℃ of-150 ℃ of temperature, to remove wherein moisture content and part organic solvent;
(3) thermal treatment: the film after will drying is warming up to 300 ℃-400 ℃ with the speed of 3-5 ℃/min, is incubated 20-40 minute, removes wherein organic complex group and other volatile matter;
(4) sintering: the film of above-mentioned preparation is warmed up to the speed of 5-8 ℃/min under 700 ℃-850 ℃ the temperature and under mobile oxygen condition, carries out sintering, be incubated 20-40 minute, form and have that certain crystallization phases is formed and the film of even compact;
(5) repetitive operation: the operating process of repetition above (1) to (4) 5-8 time, form film until obtaining the thick SBT of 400-600nm.
4. prepare SrBi as claim 1 or 3 described a kind of inorganic salt raw material liquid chemical methods 2Ta 2O 9Ferroelectric ceramic thin film is characterized in that: above-mentioned (three) SrBi 2Ta 2O 9Rotation coating film is in (1) of the preparation of film: with cleaned Si/SiO 2/ Ti/Pt substrate adheres to the center of equal glue machine support pallet, after splashing into the SBT colloidal sol for preparing previously on the substrate, under the drive of turning axle, apply 20-30 second with the about 2000-4000 of rotating speed rev/min speed rotation, thereby form certain thickness dissolved glue film.
5. prepare SrBi as claim 1 or 3 described a kind of inorganic salt raw material liquid chemical methods 2Ta 2O 9Ferroelectric ceramic thin film is characterized in that: above-mentioned (three) SrBi 2Ta 2O 9The dip-coating method film-forming technology process is in (1) of the preparation of film: clamp substrate through cleaning with the pulling machine dop, slowly immerse among the colloidal sol, static 5-10 is after second, and 0.4-0.6m/min lifts out from colloidal sol with average rate.
CN 03100039 2003-01-07 2003-01-07 Preparation of SrBi2Ta2O9 ferroelectric ceramic film by inorganic salt rawmaterial liquid-phase chemical method Expired - Fee Related CN1223548C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100358626C (en) * 2004-08-30 2008-01-02 南京大学 Preparation method of high specific surface tantalate and niobate photo catalyst
CN100450969C (en) * 2006-04-25 2009-01-14 清华大学 Process for preparing submicro-crystal piezoelectric ceramics
CN102898133A (en) * 2012-10-23 2013-01-30 中国科学技术大学 Six-layer structure bismuth titanium-ferrum-nickelate ceramic material with multiferroic performance and preparation method thereof
CN107935590A (en) * 2017-12-08 2018-04-20 安阳工学院 Microwave sintering prepares the method for Aurivillius phase SrBiFeCoTiO materials and the product of preparation
CN110164694A (en) * 2019-05-22 2019-08-23 东北大学 One kind having ultra-high dielectric coefficient organic/inorganic Ferroelectric Composites, preparation method and application

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100358626C (en) * 2004-08-30 2008-01-02 南京大学 Preparation method of high specific surface tantalate and niobate photo catalyst
CN100450969C (en) * 2006-04-25 2009-01-14 清华大学 Process for preparing submicro-crystal piezoelectric ceramics
CN102898133A (en) * 2012-10-23 2013-01-30 中国科学技术大学 Six-layer structure bismuth titanium-ferrum-nickelate ceramic material with multiferroic performance and preparation method thereof
CN107935590A (en) * 2017-12-08 2018-04-20 安阳工学院 Microwave sintering prepares the method for Aurivillius phase SrBiFeCoTiO materials and the product of preparation
CN110164694A (en) * 2019-05-22 2019-08-23 东北大学 One kind having ultra-high dielectric coefficient organic/inorganic Ferroelectric Composites, preparation method and application
CN110164694B (en) * 2019-05-22 2020-09-29 东北大学 Organic/inorganic ferroelectric composite material with ultrahigh dielectric constant, preparation method and application thereof

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