CN100393625C - Neodymium doped bismuth titanate nano line array ferro-electric storage material and its synthetic method - Google Patents
Neodymium doped bismuth titanate nano line array ferro-electric storage material and its synthetic method Download PDFInfo
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- CN100393625C CN100393625C CNB2006100184833A CN200610018483A CN100393625C CN 100393625 C CN100393625 C CN 100393625C CN B2006100184833 A CNB2006100184833 A CN B2006100184833A CN 200610018483 A CN200610018483 A CN 200610018483A CN 100393625 C CN100393625 C CN 100393625C
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Abstract
The present invention relates to a neodymium doped bismuth titanate <(Bi, Nd)4, Ti3O12, BNT> nano line array ferro-electric storage material and a synthetic method thereof, and the neodymium doped bismuth titanate nano line array ferro-electric storage materials grow from chips and are directed by a high c axis. The present invention firstly chooses chips matched with BNT material crystal lattices, and adopts a magnetron sputtering method for sputtering Au or Pt quantum dots to the chips as catalysts. Precursor solution containing Bi<3+>, Nd<3+> and Ti<4+> is prepared, and then the chips and the precursor solution are put into a high pressure reactor. Technological conditions of hydrothermal synthesis (such as temperature, pressure intensity, reaction time, etc.) are strictly controlled, and the neodymium doped bismuth titanate nano line array ferro-electric storage materials which are directed by the high c axis grow and are synthesized. A nano line array vertical recording mode is used for greatly improving storage capacity of the unit areas of the materials, and therefore, the size of devices are further reduced. The nano line array ferro-electric storage materials can be used for replacing the use of ferro-electric films on ferro-electric storage mediums and become the new ferro-electric storage mediums.
Description
Technical field
The present invention relates to a kind of novel ferroelectric storage medium, particularly a kind of Nd-doped bismuth titanate that the high c axle of oriented growth is orientated on substrate [(Bi, Nd)
4Ti
3O
12, BNT] and nano line array ferro-electric storage material and synthetic method thereof.
Background technology
The ferroelectric memory material is the important materials that aspects such as modern microelectronics, MEMS (micro electro mechanical system), information storage are used, wherein bismuth titanates (Bi
4Ti
3O
12) be the simplest a kind of ferroelectric material of structure in the bismuth layer-like compound, have excellent electricity, optics and photoelectronics performance, at aspects such as modern microelectronics, MEMS (micro electro mechanical system), information storage wide application prospect is arranged, become the focus of current new function material research.Reported that at present employing MOCVD, Sol-Gel, RF-Sputtering, methods such as Plus Laser Deposition (PLD), ECRPlasmas Deposition prepare Bi
4Ti
3O
12Ferroelectric membranc, but adopt these methods all must pass through the high temperature crystallization process, for a long time the high temperature crystallization process can make the interface generation mutual diffusion mutually between substrate material and film, film and the electrode, sometimes even chemical reaction takes place, and, institute's synthetic material piezoelectric activity is low, and coercive field Ec height is unfavorable for polarization.Kind and method such as the A position doping orientation that change sample of people such as U.Chon by changing substrate prepared comparatively significantly BNT ferroelectric membranc of a, b orientation, and the ferroelectric properties of material obtains certain raising.Above-mentioned a, b orientation is flush type, because there is the critical size effect in the crystal grain of film, this will limit the raising of ferroelectric film memory storage density greatly, is difficult to satisfy the requirement of current high-density ferroelectric memory development.How further improving the storage density of ferroelectric memory, is the ardent targets of pursuing of people.
Summary of the invention
The neodymium doped bismuth titanate nano line array ferro-electric storage material and the growth synthetic method thereof that the purpose of this invention is to provide a kind of high storage density.
Synthetic method of the present invention is:
One, preparation contains Bi
3+, Nd
3+And Ti
4+Precursor solution, its prescription is:
1, bismuth oxide or its nitrate 0.04～0.12mol/L,
2, neodymium nitrate 0.016～0.025mol/L,
3, titanium oxide or its titaniferous salt 0.05～0.09mol/L,
4, mineralizer 1.0～6.0mol/L,
5, organic formwork agent 0.005～0.1mol/L,
6, water 55.5mol/L,
Wherein, bismuth oxide and nitrate thereof are: bismuth oxide (Bi
2O
3), Bismuth trinitrate (Bi (NO
3)
35H
2O);
Titanium oxide or its titaniferous salt are: tetrabutyl titanate (Ti (OC
4H
9)
4), titanium tetrachloride (TiCl
4) or titanium dioxide (TiO
2);
Mineralizer is: sodium hydroxide (NaOH), potassium hydroxide (KOH);
Organic formwork agent is: polyoxyethylene glycol (PEG, molecular-weight average 9000-12500), polyvinyl alcohol (PVA-124), cetyl trimethylammonium bromide (CTAB, C
19H
42BrN), thymus nucleic acid (DNA).
Two, select monocrystal chip
Strontium titanate (the SrTiO that selects lattice parameter and BNT lattice parameter to be complementary
3) or ruthenic acid strontium (SrRuO
3) monocrystal chip, the surface is cleaned, and with magnetron sputtering method sputter gold (Au) or platinum (Pt) quantum dot on substrate.
Three, oriented growth
1, precursor solution for preparing and the monocrystal chip of handling well are put into high-pressure reaction vessel;
2, Heating temperature is 175 ℃, pressure 2～3MPa;
3, through 24～96 hours hydro-thermal reactions.
Four, remove high pressure and take out substrate, washed 30 minutes with deionized water and dehydrated alcohol respectively, under 50～80 ℃ of conditions, dried by the fire 2～8 hours, characterize the performance of the high c axle orientation nano array ferro-electric storage material of growth.
When above-mentioned precursor solution is pressed formulated, should be through stirring fully and the ultra-sonic dispersion processing, the adding mineralizer is the crystallization that helps product, uses organic formwork agent can make Bi
3+, Nd
3+And Ti
4+Precursor solution mix, play " soft mode " effect simultaneously, be beneficial to the oriented growth of product under the condition of hydro-thermal.The raw material of above-mentioned prescription should be chemical pure or analytical pure.
This method growth synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material, its nanowire diameter is relevant with the size that sputters at on-chip Au or Pt quantum dot, is generally 10～50 nanometers; The length of nano wire is relevant with the time of carrying out hydro-thermal reaction, is generally 1 micron～5 microns.
The present invention's synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material of growing is a high c axle orientation, is implemented in large area deposition nano-wire array on the substrate, the product purity height of acquisition, and reduce the crystallization temperature of material greatly.As ferroelectric storage media, utilize the perpendicular recording pattern of nano-wire array can improve storage capacity on the device unit surface greatly it, its storage density can reach 1 terabit/cm
2Thereby, device size is further reduced, will become ferro-electric storage material of new generation.
Embodiment
The prescription and the processing parameter (reactor volume 50ml, compactedness is 80%) of the synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material of growth are described with embodiment below.
Embodiment one: with Bi (NO
3)
3, Nd (NO
3)
3And Ti (OC
4H
9)
4Be main raw material
By the synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material of aforementioned manner growth.
Embodiment two: with Bi
2O
3, Nd (NO
3)
3And TiO
2Be main raw material
By the synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material of aforementioned manner growth.
Embodiment three: with Bi (NO
3)
3, Nd (NO
3)
3And TiCl
4Be main raw material
By the synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material of aforementioned manner growth.
Embodiment four: with Bi
2O
3, Nd (NO
3)
3And TiCl
4Be main raw material
By the synthetic neodymium doped bismuth titanate nano line array ferro-electric storage material of aforementioned manner growth.
In above-mentioned prescription and the processing parameter, sequence number 1,2 and 3 is main raw materials, and corresponding ionic concn should be controlled in certain scope, and too high meeting causes that the product crystallization is incomplete; Cross to hang down and then can not effectively synthesize the BNT nano wire, and in this prescription (Bi, Nd)
3+And Ti
4+Concentration should be controlled at 0.05～0.12mol/L.Sequence number 4 mineralizer for adding in the reaction, the amount of its type and interpolation will influence the crystallization degree of product, and the type and the addition of different main raw material requirement mineralizers are also different, such as with Bi (NO
3)
35H
2O, Nd (NO
3)
3And Ti (OC
4H
9)
4During for main raw material, the NaOH that selects 1mol/L is as mineralizer, and with Bi
2O
3, Nd (NO
3)
3And TiO
2During for main raw material, the KOH that then selects 5mol/L is as mineralizer etc.Sequence number 5 is to be used for hydro-thermal synthetic reaction medium, and the cumulative volume that finally is mixed with precursor solution should not surpass 80% of reactor volume.Sequence number 6 organic formwork agent for selecting, what of its kind and addition are very big to the oriented growth influence of nano wire.PVA and PEG in this prescription, CTAB plays similar template action to DNA respectively in synthetic, so add identical amount respectively.For the processing parameter in the hydrothermal reaction process, different main raw materials requires different temperature, pressure and reaction times.
Claims (2)
1. the growth synthetic method of a neodymium doped bismuth titanate nano line array ferro-electric storage material, the synthetic method that it is characterized in that growing is:
One, preparation contains Bi
3+, Nd
3+And Ti
4+Precursor solution, its prescription is:
1) bismuth oxide or Bismuth trinitrate 0.04～0.12mol/L
2) neodymium nitrate 0.016～0.025mol/L
3) titanium oxide or titaniferous salt 0.05～0.09mol/L
4) mineralizer 1.0～6.0mol/L
5) organic formwork agent 0.005～0.1mol/L
6) water 55.5mol/L
Wherein, titaniferous salt is: tetrabutyl titanate or titanium tetrachloride;
Mineralizer is: sodium hydroxide or potassium hydroxide;
Organic formwork agent is: polyoxyethylene glycol, molecular-weight average 9000-12500, or polyvinyl alcohol, perhaps cetyl trimethylammonium bromide, perhaps thymus nucleic acid;
Two, select monocrystal chip
Strontium titanate or the ruthenic acid strontium monocrystal chip of selecting lattice parameter and Nd-doped bismuth titanate lattice parameter to be complementary clean the surface, and with magnetron sputtering method sputter gold or platinum quantum dot on substrate;
Three, oriented growth
1) precursor solution for preparing and the monocrystal chip of handling well are put into high-pressure reaction vessel;
2) Heating temperature is 175 ℃, pressure 2～3MPa;
3) through growth response in 24～96 hours;
Four, remove high pressure and take out substrate, washed 30 minutes with deionized water and dehydrated alcohol respectively, under 50～80 ℃ of conditions, dried by the fire 2～8 hours, characterize the performance of the high c axle orientation nano array ferro-electric storage material of growth.
2. neodymium doped bismuth titanate nano line array ferro-electric storage material that growth synthetic method according to claim 1 is made, it is characterized in that on strontium titanate or ruthenic acid strontium monocrystal chip it being by high c axle oriented growth of nanowires array, its nanowire diameter is 10～50 nanometers, and length is 1～5 micron.
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| CN100393625C true CN100393625C (en) | 2008-06-11 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100427431C (en) * | 2007-04-29 | 2008-10-22 | 湘潭大学 | Method for preparing lanthanide series rare earth ions doped with bismuth titanate non-plumbum ferroelectric nano-wire |
| CN101186737B (en) * | 2007-06-19 | 2010-09-01 | 东南大学 | Method for preparing ferric oxide ultra-fine rod array |
| CN102039149B (en) * | 2010-11-10 | 2013-02-06 | 武汉理工大学 | Self-assembly method of precious metal quantum dot/one-dimensional titanate nanoribbon heterojunction material |
| CN104525940A (en) * | 2014-12-31 | 2015-04-22 | 中国地质大学（武汉） | Bismuth micron particle and manufacturing method thereof |
| CN105271380A (en) * | 2015-10-31 | 2016-01-27 | 西安科技大学 | Preparation method of gadolinium-doped bismuth titanate with nano-sheet cluster structure |
| CN108531176B (en) * | 2018-03-30 | 2021-07-16 | 常州大学 | Self-assembly preparation method of nano cubic fence fluorescent material |
| CN108660544B (en) * | 2018-03-30 | 2020-10-02 | 常州大学 | Preparation method of semiconductor nano-fiber |
| CN109483087B (en) * | 2018-12-17 | 2021-07-23 | 安徽升鸿电子有限公司 | High-performance bismuth titanate welding material and preparation method thereof |
| CN111498896B (en) * | 2020-04-24 | 2023-05-30 | 山东国瓷功能材料股份有限公司 | Nanometer barium titanate material with low K value and high refractive index and dispersion liquid prepared from nanometer barium titanate material |
| CN116371398B (en) * | 2023-04-11 | 2023-11-10 | 中南大学 | BIT-Nd block piezoelectric photocatalyst and preparation method and application thereof |
Citations (3)
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|---|---|---|---|---|
| CN1288981A (en) * | 2000-09-18 | 2001-03-28 | 南京大学 | Low-electric field inducting control method to orient film prepared through a wet chemical process |
| JP2005071963A (en) * | 2003-08-28 | 2005-03-17 | Seiko Epson Corp | Ferroelectric film, method of manufacturing the same, ferroelectric memory and semiconductor device |
| WO2006013826A1 (en) * | 2004-08-06 | 2006-02-09 | Japan Science And Technology Agency | Bi LAYERED COMPOUND NANOPLATE, ARRAY THEREOF, PROCESS FOR PRODUCING THEM, AND APPARATUS UTILIZING THE SAME |
-
2006
- 2006-03-06 CN CNB2006100184833A patent/CN100393625C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288981A (en) * | 2000-09-18 | 2001-03-28 | 南京大学 | Low-electric field inducting control method to orient film prepared through a wet chemical process |
| JP2005071963A (en) * | 2003-08-28 | 2005-03-17 | Seiko Epson Corp | Ferroelectric film, method of manufacturing the same, ferroelectric memory and semiconductor device |
| WO2006013826A1 (en) * | 2004-08-06 | 2006-02-09 | Japan Science And Technology Agency | Bi LAYERED COMPOUND NANOPLATE, ARRAY THEREOF, PROCESS FOR PRODUCING THEM, AND APPARATUS UTILIZING THE SAME |
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