CN110190186A - A kind of construction method of the topological farmland array of high density polarization - Google Patents
A kind of construction method of the topological farmland array of high density polarization Download PDFInfo
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- G11C11/00—Digital stores characterised by the use of particular electric or magnetic storage elements; Storage elements therefor
- G11C11/21—Digital stores characterised by the use of particular electric or magnetic storage elements; Storage elements therefor using electric elements
- G11C11/22—Digital stores characterised by the use of particular electric or magnetic storage elements; Storage elements therefor using electric elements using ferroelectric elements
- G11C11/221—Digital stores characterised by the use of particular electric or magnetic storage elements; Storage elements therefor using electric elements using ferroelectric elements using ferroelectric capacitors
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- H—ELECTRICITY
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- H10B—ELECTRONIC MEMORY DEVICES
- H10B53/00—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory capacitors
Abstract
The invention discloses a kind of construction methods of the topological farmland array of high density polarization, belong to micro-nano structure technical field, and by pulsed laser deposition technology growth bismuth ferrite thin film, this material of bismuth ferrite is free of lead, are a kind of green, environmentally friendly materials；The sedimentary condition of low oxygen pressure ensure that the spontaneous presence of defect (such as Lacking oxygen).The microscopical needle point electric field action of piezoelectric forces can make charged defects generate displacement, influence the spontaneous existing topological domain structure that polarizes, to go out the topological farmland array of high-density center type polarization of dimension adjustable by needle point electric field configuration, single topology farmland is having a size of tens nanometers, these polarize, and topological farmland overturning is controllable, has good stability, and is suitable for preparation high density ferroelectric RAM.The preparation method that the present invention uses, pulsed laser deposition technique is mature, prepares film and does not need additional template auxiliary, the vector piezoelectricity scanning force microscopy based on scanning probe microscopy is easy to operate, has good practicability.
Description
Technical field
The invention belongs to micro-nano structure technical fields, and in particular to a kind of building side of the topological farmland array of high density polarization
Method.
Background technique
Ferroelectric memory is likely to become next-generation nonvolatile memory and causes extensive concern.It has low-power consumption, quickly
Write-in, (3.3V is more than 10 to much bigger erasable number16It is secondary) the advantages that, the disadvantage is that storage density is low.In recent years, with people couple
The requirement of device miniaturization is further strong, and market shows earnestly to expect to highdensity memory device.Based on topological farmland of polarizing
Ferroelectric RAM be exactly this high-density memory device representative.It is individually vortexed polarization in theoretical prediction in 2004
The size on topological farmland is 3.2nm, corresponding storage density reaches 60Tb/inch2Later, latest theories prediction in 2018 is single is vortexed
The topological farmland size that polarizes only has 0.77nm, storage density to be up to 103Tb/inch2.In addition to being vortexed, there are also anti-vortex, Skyrmion,
The topological structures such as radial centre type, they are all nanoscale, can be used for highdensity ferroelectric RAM.
Under the excitation of theoretical prediction, people start to find these topological structures in authentic material, occur successively
Some achievements, most of turbulent structure and its cyclic array to have good stability, such as in magnetic crystal, PbTiO3/
SrTiO3Multilayer film, PbTiO3/SrTiO3Superlattices in.However, these results without hearth electrode because do not carry out further
The research controllably overturn, simultaneously, it is also difficult to which the form of capacitor is integrated in device；The preparation process difficulty of these results is very
Height also rests in R&D units at present.Investigation finds that the Study on topology in ferroelectric is still single spark, returns
Because keeping polarization rotation difficult in the biggish lattice anisotropy of ferroelectric material.In smaller size of nano-dot matrix, tradition is used
Standard ferroelectric lead zirconate titanate (abbreviation PZT), vortex farmland only exist in a other nano dot；For lead-free ferroelectric material
BiFeO3The high density nanometer lattice row of (abbreviation BFO) preparation is capable of forming the topological domain structure of centre type, but because is logical
The acquisition of template ion beam etched film is crossed, template therein preparation, removal etc. make the slightly aobvious complexity of preparation process.
2016, the topological phase transition and topology of substance mutually obtained Nobel Prize in physics, in identity mathematics and physics perfection knot
While conjunction, also predictive of the application value of material and device in modern science and technology with topological structure, infused to researchers
Confidence and vigor are entered.Currently, the ferroelectricity storage based on topological farmland of polarizing faces two big challenges, first is that finding green, environment friend
The material and preparation process of good type are simple, second is that high density polarizes, topological farmland can controllably be overturn.2017, Ren Men
PbTiO3/SrTiO3Superlattices in realize the controllable overturning of ferroelectricity/vortex coexisting phase, but PbTiO3Containing volatile
Lead, and lead is toxic.In March, 2017, European Union have passed through the lead tolerance in legislation limitation electronic product, therefore, including it is famous
PZT including, leaded traditional ferroelectric material is doomed to will receive legal restriction, still, this to some preparations develop novel lead-free
Piezoelectricity, ferroelectric material provide good chance to substitute the company of PZT.
For the characterization on topological farmland of polarizing, polarized characterization can be carried out by having many methods.X-ray diffraction characterization can
The information of lattice direction is obtained, but is visualized not strong.Transmission electron microscope characterization can be disclosed by the gradient of unit cell
Polarization direction, but the data of a certain cross section of sample can only be provided, and sample preparation, characterization all have destructiveness to sample.With
They are compared, and piezoelectricity force microscope (Piezorespone force microscopy, PFM) is very suitable for iron electric polarization and opens up
Flutter the characterization on farmland: (1) it, which can not only characterize polarization outside face, can also characterize polarization in face, so as to be obtained by recombinating polarization
The three-dimensional domain structure of real space is obtained, the regulation to domain structure may be implemented by applying needle point electric field in (2)；(3) knot obtained
Fruit can also directly compare with the result of theoretical modeling.
In summary, it is necessary to propose a kind of new method, it is adjusted to construct iron electric polarization topology farmland array to realize
Control, and new Technology Ways are developed, realize the high density ferroelectric memory device preparation of environmentally protective, high quality, low cost.
Scientific and technical literature " Controllable conductive readout in self assembled,
Topologically confined ferroelectricdomain walls " (Nature Nanotechnology, 2018,
13 (10), 947-952) it finds that large area, high density and the ferroelectricity of self assembly may be implemented using the method for pulse laser deposition
BiFeO3Nano island has completely centripetal or centrifugation pintongs domain structure；The limited domain wall of this topology can be with electricity around it
Polarization Coupling, forms the domain wall conductance of the reversible regulation of vertical electric field, and changing value is up to 1000 times.This self-assembled nanometer island array
Unique growing method will also be expected to be generalized to other thin film systems, to reduce future feature material and high density microelectronics
The integrated manufacturing cost of device.
Summary of the invention
Goal of the invention: the purpose of the present invention is to provide a kind of construction methods of the topological farmland array of high density polarization, not only
Simple process, and can high-volume, preparation of industrialization.
Technical solution: to achieve the above object, the present invention adopts the following technical scheme:
A kind of construction method of the topological farmland array of high density polarization, includes the following steps:
S1, pulse laser sedimentation preparation of film sample；
S2, spontaneous polarization topology farmland is obtained using PFM characterization, reconstruct to film sample；
S3, ferroelectric thin film is overturn polarization direction outside face by the write-in of PFM needle point electric field in larger area；
S4, it is written, the topological farmland array of high density polarization is constructed in ferroelectric thin film and realized by PFM needle point pulse voltage
It is regulated and controled.
Further, in step S1, the pulse laser sedimentation preparation of film sample is that successively pulse swashs on substrate
Light deposition hearth electrode, ferroelectric layer, the substrate are SrTiO3, hearth electrode SrRuO3, the ferroelectric layer is BiFeO3。
Further, the hearth electrode SrRuO3With a thickness of 30~40nm；Ferroelectric layer BiFeO3With a thickness of 50~
60nm, pulse laser deposit ferroelectric layer BiFeO3Condition is that oxygen presses 2~3Pa, it is desirable that ferroelectric layer BiFeO3Layer is without miscellaneous phase.
Further, in step S2, there is conductive coating in the PFM needle point, the conductive coating is Pt/Ir.
Further, in step S2, the method for the characterization is first to acquire sample region using vector PFM technology
The PFM image of (vertical direction) outside face, PFM needle point driving frequency are 200~300KHz；Then sample is carried out relative to probe
The rotation of cantilever, and direction of rotation is mutually perpendicular to, i.e., 0 ° and 90 °；Find the same zone of the PFM image of acquisition vertical direction
Domain, acquires (horizontal direction) PFM image in 0 ° and 90 ° of face, and the PFM needle point driving frequency is 1.0~1.2MHz.
Further, in step S2, the method for the reconstruct is two level sides using Matlab program to acquisition
To PFM image data handled, obtain two-dimensional polarization vector figure；The PFM image data of joint vertical direction obtains three
The polarization vector of dimension.
Further, in step S3-S4, the method for the building is first to be written using direct current PFM needle point electric field scanning
Rectangular patterns (left side positive voltage, the right negative voltage, size need to be more than coercive voltage), in the larger area region of ferroelectric thin film
Polarize overturning outside interior realization face, and then needle point is fixed on to the position specified in writing area, apply direct current on PFM needle point
Press pulse write-in, the topological farmland array of building polarization.
The utility model has the advantages that compared with prior art, a kind of construction method of the topological farmland array of high density polarization of the invention is adopted
Thin film technique is prepared with low oxygen pressure, ensure that the presence of defect under the premise of no miscellaneous phase, while can efficiently prepare thin
Film, wherein ferroelectric layer is bismuth ferrite, and compared with traditional leaded ferroelectric material, this material is environmentally protective, polarization value is big, ferroelectricity
Property is good；The construction method utilizes piezoelectricity force microscope, technologically advanced, belongs to Environment Science；The high density polarization that building obtains
Topological farmland array is expected to the technical bottleneck low for the solution storage density that ferroelectric RAM part faces currently on the market
Offer scheme.
Detailed description of the invention
Fig. 1 is the ferroelectric thin film preparation process flow explanatory diagram of embodiment 1；
Fig. 2 is the X-ray diffractogram of ferroelectric thin film in embodiment 1；
Fig. 3 is the surface topography map of ferroelectric thin film in embodiment 1；
Fig. 4 is the PFM piezoelectric loop figure of ferroelectric thin film in embodiment 1；
Fig. 5 is the vector PFM analysis method schematic diagram of step S2 ferroelectric thin film in embodiment 1；
Fig. 6 is the vector PFM characterization result figure of step S2 ferroelectric thin film in embodiment 1；
Fig. 7 is that step S2 uses PFM analysis method, Matlab program processing result figure in embodiment 1；
Fig. 8 is the topological farmland array of figure of high density polarization that step S3 is constructed using PFM needle point electric field in embodiment 1.
Specific embodiment
In order to further illustrate the present invention, with reference to embodiments to a kind of topological farmland of high density polarization provided by the invention
The construction method of array is described in detail.It should be understood that these embodiments are merely to illustrate the present invention rather than limit this hair
Bright range.
Furthermore, it is to be understood that after reading the content taught by the present invention, those skilled in the art can make the present invention
Various changes or modification, these equivalent forms also fall within the scope of the appended claims of the present application.
A kind of construction method of the topological farmland array of high density polarization, includes the following steps:
S1, pulse laser sedimentation preparation of film sample；
S2, spontaneous polarization topology farmland is obtained using PFM characterization, reconstruct to film sample；
S3, it is written by PFM needle point electric field by the overturning that polarizes outside face to topological farmland is polarized；
S4, it is written, the topological farmland array of high density polarization is constructed in ferroelectric thin film and realized by PFM needle point pulse voltage
It is regulated and controled.
In step S1, pulse laser sedimentation preparation of film is pulse laser depositions of bottom electrode, ferroelectric layer on substrate, substrate
For SrTiO3, hearth electrode SrRuO3, pulse laser deposits ferroelectric layer BiFeO on hearth electrode surface3。
Wherein, hearth electrode SrRuO3With a thickness of 30~40nm；Ferroelectric layer BiFeO3With a thickness of 50~60nm, pulse swashs
Light deposition BiFeO3Condition is that oxygen presses 2~3Pa, it is desirable that ferroelectric layer BiFeO3Layer is without miscellaneous phase.
In step S2, the PFM needle point used has conductive coating, and the present invention is Pt/Ir using the conductive coating of PFM needle point.
Characterizing method is first to acquire the PFM image of sample region vertical direction using vector PFM technology, and PFM needle point drives
Dynamic frequency is 200~300KHz；Then the rotation relative to probe cantilever is carried out to sample, and direction of rotation is mutually perpendicular to,
I.e. 0 ° and 90 °；The same area for finding the PFM image of acquisition vertical direction, acquires 0 ° and 90 ° of horizontal direction PFM image,
PFM needle point driving frequency is 1.0~1.2MHz.
Reconstructing method is handled using PFM image data of the Matlab program to two horizontal directions of acquisition, is obtained
Obtain two-dimensional polarization vector figure；The PFM image data of joint vertical direction obtains three-dimensional polarization vector.
In step S3-S4, construction method is that rectangular patterns (left side positive electricity first is written using direct current PFM needle point electric field scanning
Pressure, the right negative voltage, size need to be more than coercive voltage), it polarizes and turns over outside realization face in the larger area region of ferroelectric thin film
Turn, then needle point is fixed on to the position specified in writing area, applies direct current voltage pulse write-in, building on PFM needle point
The topological farmland array of high density polarization.
Embodiment 1
As shown in figures 1-8, Fig. 1 is a kind of building flow diagram of the topological farmland array of high density polarization of the present invention.Below
In conjunction with Fig. 2-6, the present embodiment is described in detail.
High quality, high performance epitaxial ferroelectric film: X-ray diffraction θ -2 θ scanning characterization are prepared first, as shown in Fig. 2,
As a result the epitaxial structure for clearly providing STO/SRO/BFO, by face outside the lattice constant that is calculated of (002) peak show BFO film
For the structure of diamond shape phase；Atomic force microscope characterization provides pattern, as shown in figure 3, roughness (rms, root-mean-square value) is
0.5nm illustrates that film surface is smooth (Fig. 3 a), and three-dimensional appearance figure (Fig. 3 b) also demonstrates this point；Use " piezoelectricity-hysteresis " mould
Formula characterizes the PFM piezoelectric loop of sample, as shown in figure 4,180 ° of variation occurs for PFM phase diagram (Fig. 4 a), it is normalised
PFM amplitude image (Fig. 4 b) is butterfly-like piezoelectric loop, and the coercive field for providing BFO film is ± 4V, very symmetrical, illustrates sample ferroelectricity
Property is good.Then vector PFM characterization, analysis carried out to ferroelectric thin film, reconstruct the spontaneous topological domain structure of acquisition, finally, passing through
The topological farmland array of needle point electric field write-in building polarization simultaneously regulates and controls it.
According to step S1, pulsed laser deposition uses the BFO ceramic target of stoichiometry, by strict control oxygen pressure,
The parameters such as temperature, laser energy density, pulse frequency (being shown in Table lattice) preparation includes the STO/SRO/BFO structure of a certain concentration defect
Film.Pulse laser is the laser that the wavelength that KrF excimer laser issues is 248nm, deposits the preparation parameter of BFO film
It is given in Table 1:
1 pulse laser deposition parameter of table
After having deposited BFO film, it is cooled to room temperature under conditions of oxygen pressure is 500Pa.
According to step S2, the topological domain structure that polarizes is shown in Fig. 5 using vector PFM analysis, reconstructing method.Specifically, refer to
It is to obtain two-dimensional polarization by reconstructing (horizontal direction, lateral) polarization (Fig. 5 a, b) in the face of at least two vertical direction
Vector, black and white contrast illustrates that polarization direction is vertical with cantilevered orientation and is directed toward on the contrary, grey in 45 ° of schematic diagrames of Fig. 5 c in figure
Contrast shows that polarization direction is parallel with cantilevered orientation.The characterization on the spontaneous polarization topology farmland in film and reconstruct are in figure 6 and figure 7
It provides, acquires PFM phase diagram (lateral phase) in the face of 0 ° (Fig. 6 a) and 90 ° (Fig. 6 b) two vertical direction, make in advance
Being polarized with -6V the DC voltage for being more than coercive voltage to film, spontaneous polarization is distributed outside face to determine, selected to be used to reconstruct
Regional area and amplification (Fig. 6 c, d), the polarization direction information (arrow see Fig. 7 a, in b provided by amplification phase diagram is provided
Head is directed toward), two-dimentional polarization vector figure (Fig. 7 c) in processing reconstruct acquisition face is carried out to image data using Matlab program, then join
Conjunction face outer (vertical direction, vertical) (Fig. 7 d) polarization finally obtains the three-dimensional domain structure of ferroelectric thin film local, is that face is export-oriented
Under, the topological structure of center divergence form (schematic diagram below Fig. 7).
According to step S3, characterized using original state of the vector PFM method to ferroelectric thin film, respectively outside acquisition face
The PFM phase diagram of (Fig. 8 b) in (Fig. 8 a) and face carries out larger area to film using the+6V/-6V rectangular patterns being pre-designed
(~3 × 3 μm2) polarization overturning and characterization, (Fig. 8 c) PFM phase diagram, which can determine, outside face is written into the vertical direction of region
Polarization overturning completely, polarization direction is that the left side is downward, the right is upward；The PFM phase diagram of (Fig. 8 d) is more complicated in face, is formed
Banded domain structure.Needle point is fixed on certain position on film, applies pulse voltage on needle point, design parameter is in table 2
In provide, it should be pointed out that wherein sample local is punctured when+6V, 1000s.Then the feelings after pulse voltage write-in
Condition carries out vector PFM characterization, analysis, and the circular solids image that PFM phase (Fig. 8 e) provides outside face specifies the effect of needle point write-in
Fruit is fine, and the Polarization Coupling of needle point electric field and ferroelectric thin film obtains very well, what makes more sense is that, in face in PFM phase (Fig. 8 f) figure
Left dark/right half and half contrast distribution bright, that Zuo Liang/right side is dark illustrate head to head, tail to the polarization distribution of tail, pass through polarization reconstruct
The size of the final two kinds of polarization topology farmland array for obtaining center diverging, centre convergence, the size on topological farmland and pulse voltage, when
Between there is corresponding relationship, and both topological farmlands are present in same width figure and illustrate that it can regulate and control.It is this stabilization, controllable
Polarization topology farmland array can be used for highdensity ferroelectric memory device.
Table 2 applies alive size, Pulse-Time Parameters on PFM needle point
Claims (7)
- The construction method of topological farmland array 1. a kind of high density polarizes, characterized by the following steps:S1, pulse laser sedimentation preparation of film sample；S2, spontaneous polarization topology farmland is obtained using PFM characterization, reconstruct to film sample；S3, ferroelectric thin film is overturn polarization direction outside face by the write-in of PFM needle point electric field in larger area；S4, it is written, the topological farmland array of high density polarization is constructed in ferroelectric thin film and is realized to it by PFM needle point pulse voltage Regulation.
- The construction method of topological farmland array 2. a kind of high density according to claim 1 polarizes, it is characterised in that: step S1 In, the pulse laser sedimentation preparation of film sample is successively pulse laser depositions of bottom electrode, ferroelectric layer on substrate, described Substrate be SrTiO3, hearth electrode SrRuO3, the ferroelectric layer is BiFeO3。
- The construction method of topological farmland array 3. a kind of high density according to claim 2 polarizes, it is characterised in that: described Hearth electrode SrRuO3With a thickness of 30~40nm；Ferroelectric layer BiFeO3With a thickness of 50~60nm, pulse laser deposits ferroelectric layer BiFeO3Condition is that oxygen presses 2~3Pa.
- The construction method of topological farmland array 4. a kind of high density according to claim 1 polarizes, it is characterised in that: step S2 In, there is conductive coating in the PFM needle point, the conductive coating is Pt/Ir.
- The construction method of topological farmland array 5. a kind of high density according to claim 1 polarizes, it is characterised in that: step S2 In, the method for the characterization is first to acquire the PFM image of sample region vertical direction, PFM needle using vector PFM technology Sharp driving frequency is 200~300KHz；Then the rotation relative to probe cantilever is carried out to sample, and direction of rotation is mutually hung down Directly, i.e., 0 ° and 90 °；Find the same area of the PFM image of acquisition vertical direction, the horizontal direction PFM figure of 0 ° and 90 ° of acquisition Picture, the PFM needle point driving frequency are 1.0~1.2MHz.
- The construction method of topological farmland array 6. a kind of high density according to claim 1 polarizes, it is characterised in that: step S2 In, the method for the reconstruct is handled using PFM image data of the Matlab program to two horizontal directions of acquisition, Obtain two-dimensional polar plot；The PFM image data of joint vertical direction obtains three-dimensional polarization vector.
- The construction method of topological farmland array 7. a kind of high density according to claim 1 polarizes, it is characterised in that: step In S3-S4, the method for the building is first to realize to polarize outside face using direct current PFM needle point electric field scanning write-in rectangular patterns to turn over Turn, then needle point is fixed on to the position specified on sample, applies direct current voltage pulse write-in on PFM needle point, construct highly dense The topological farmland array of degree polarization.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110634871A (en) * | 2019-10-15 | 2019-12-31 | 淮阴工学院 | Periodic strip domain structure of ferroelectric film and characterization method thereof |
| CN111554683A (en) * | 2020-04-10 | 2020-08-18 | 华南师范大学 | Preparation method of novel photosensitive ferroelectric topological domain nano island |
| CN112420709A (en) * | 2019-08-23 | 2021-02-26 | 中国科学院物理研究所 | Conversion of PbTiO3/SrTiO3Method of vortex domain of superlattice material |
| CN112467025A (en) * | 2020-10-28 | 2021-03-09 | 淮阴工学院 | Method for constructing periodic strip domain in ferroelectric film by using needle-tip electric field |
| CN113594364A (en) * | 2021-08-06 | 2021-11-02 | 佛山湘潭大学绿色智造研究院 | Multi-vortex ferroelectric domain multi-logic-state storage unit and power regulation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112420709A (en) * | 2019-08-23 | 2021-02-26 | 中国科学院物理研究所 | Conversion of PbTiO3/SrTiO3Method of vortex domain of superlattice material |
| CN110634871A (en) * | 2019-10-15 | 2019-12-31 | 淮阴工学院 | Periodic strip domain structure of ferroelectric film and characterization method thereof |
| CN110634871B (en) * | 2019-10-15 | 2021-10-29 | 淮阴工学院 | Characterization method of periodic strip domain structure of ferroelectric film |
| CN111554683A (en) * | 2020-04-10 | 2020-08-18 | 华南师范大学 | Preparation method of novel photosensitive ferroelectric topological domain nano island |
| CN111554683B (en) * | 2020-04-10 | 2023-08-22 | 华南师范大学 | Preparation method of novel photosensitive ferroelectric topological domain nano island |
| CN112467025A (en) * | 2020-10-28 | 2021-03-09 | 淮阴工学院 | Method for constructing periodic strip domain in ferroelectric film by using needle-tip electric field |
| CN112467025B (en) * | 2020-10-28 | 2024-04-23 | 淮阴工学院 | Method for constructing periodic strip domain in ferroelectric film by utilizing needlepoint electric field |
| CN113594364A (en) * | 2021-08-06 | 2021-11-02 | 佛山湘潭大学绿色智造研究院 | Multi-vortex ferroelectric domain multi-logic-state storage unit and power regulation method |
| CN113594364B (en) * | 2021-08-06 | 2023-09-19 | 佛山湘潭大学绿色智造研究院 | Multi-logic state storage unit with multi-vortex ferroelectric domain and electric power regulation and control method |
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