CN104103752A - Method of preparing oxide film material with shape memory effects and application thereof - Google Patents
Method of preparing oxide film material with shape memory effects and application thereof Download PDFInfo
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Abstract
A method of preparing an oxide film material with shape memory effects comprises steps: the pulse laser deposition technology is used for preparing a two-phase-coexistence BiFeO3 film on a high-quality mismatch single-crystal substrate; and a focusing ion beam etching technology is used for preparing a pure-phase nano structure on the two-phase-coexistence BiFeO3 film prepared in the former step. The invention also discloses the application of the film nano structure. The method and the application of the invention have the effects that a ferroelectric oxide material with huge shape memory effects is successfully prepared by using the epitaxial growth technology and the focusing ion beam etching technology. An electric field, the temperature and the stress can all have effects on the shape memory strain of the material, and the maximal reversible strain can be as high as 14%. As regulation on the shape memory effects of the material can also be realized by the electric field, the working frequency is higher than that of the traditional alloy material, and in addition, as the shape strain is realized in the nano scale, the material can replace the traditional alloy material to be applied to sensing, driving and the like in the small size.
Description
Technical field
The present invention relates to oxide film material field, particularly a kind of preparation method and application thereof with the oxide film material of shape memory effect.
Background technology
Ferroic material typically refers to those functional material systems with ferroelectric, iron bullet, the order parameter such as ferromagnetic, comprises ferroelectric/piezoelectrics, magnetostrictive material and marmem.They have huge application potential at many functional structures and device in as sensing driving etc.Piezoelectric is as (1-x) [Pb (Mg
1/3nb
2/3) O
3]-x[PbTiO
3] conventionally under electric field, show high mechanical response, can be for driver or transducer (Fuetal., Nature403,281 (2000); Liuetal., Phys.Rev.Lett.103,257602 (2009); Kutnjak et al., Nature441,956 (2006)).In these function application, vital effect is often played in mechanical strain.Yet in piezoelectricity PZN-8%PT, maximum can realize 1.7% electric field induced strain (Parketal., J.Appl.Phys.82,1804, (1997)), at ferroelectric BaTiO
3middle maximum also can realize 0.75% reversible strain (Renetal., Nat.Mater.3,91 (2004)).Yet in ferroelastic marmem, under environmental stimuli, (stress, magnetic field etc.) can realize recoverable 0.5%-8% conventionally strain (Renetal., Nature389,579 (1997); Cahnetal., Nature374,120 (1995)).Generally believe at present the martensite phase transformation (Bhattacharyaetal., Nature428,55 (2004)) that this huge physical mechanism of remembering deformation behind causes for factors such as heat, stress, magnetic fields.Owing to existing superior mechanical response, marmem is such as damping device, mechanical joint, even the aspect such as biology and aerospace engineering all has very large application space (Morgan et al., Mater.Sci.Eng.A378,16 (2004)), its application often has irreplaceable effect.
Recently, although can realize the reversible strain (Chmielus et al., Nat.Mater.8,863 (2009)) up to 8% in alloy, the step of the larger mechanical response of people's pursuit in decades does not still stop recently.And, although block alloy material can produce huge mechanical effect, under nanoscale, (～100 nanometer) these alloy materials just start to lose shape memory effect, and in addition, the stability of material has also been subject to challenge (as metal material oxidation and large surperficial can grade) under small size.And current marmem normally temperature or magnetic field controls that realize can recovery strain, the response frequency that this must reduce structure, is unfavorable for frequency applications (Yangetal., Scripta Mater.60,493 (2009) of device; Bouville et al., Acta Mater.56,3558 (2009)).Solution is such as stability, the effective ways of the difficult problems such as small size in nanoscale oxide material and structure, realize electric field controlled, be greater than 10% huge shape memory effect, this is the blank in this field at present.
BiFeO
3be a kind of ferroelectric multi-ferroic material, its ground state is rhombus phase structure (Wang et al., Science299,1719 (2003)).Due to its superior ferroelectric and magneto-electric coupled performance extensively receive publicity (Chuetal., Nat.Mater.7,478 (2008)).Utilize the abundant Phase Diagram Structures of this material and high epitaxy technology in recent years, it is found that effect of stress can be at BiFeO
3the nanoscale of realizing two kinds of crystal structures in material coexist (<100 nanometer), be rhombus phase and Tetragonal (Zeches et al., Science326,977 (2009)), at two-phase intersection, can obtain huge piezoelectric response (Zhang et al. simultaneously, Nat.Nanotechnol.6,98 (2011)).Yet at BiFeO
3in system, can realize by pure four directions and mix mutually the Structure Transformation to pure rhombus phase through four directions/rhombus by certain means? that is to say whether can utilize and mix phase BiFeO
3at nanoscale, realize class shape memory effect? what can produce at present huge shape memory effect is substantially all alloy material, do not have oxide stable, and relative oxide, in alloy, cannot realize high-quality thin film epitaxial growth preparation, this is just unfavorable for realizing micro-(receiving) motor application (MEMS, NMES) of huge shape memory effect.
In addition, mixing phase BiFeO
3in the process of Structure Transformation, can realize great can recovery strain, can be greater than 10% in marmem? huge can normally the generation in bulk alloy by recovery strain that martensite phase transformation at present causes, once alloy material size is dropped to nanoscale, shape memory effect is just subject to severe inhibition conventionally.This is for applying and proposed challenge under small scale.
Due to BiFeO
3it is ferroelectric substance, can substitute temperature with electric field and realize regulation and control? in order to realize shape memory effect, marmem is all in temperature at present, stress, under the effect in magnetic field, realization can recovery strain, the work period that this must improve material and device, be unfavorable for that device applies under higher response frequency.With respect to temperature and magnetic field, electric field can be realized higher response frequency conventionally.
At present in existing all functions material, ferroelectric material can realize 0.75% can recovery strain, in relaxation ferroelectric, can realize 1.7% can recovery strain, magnetostrictive material can be less than 0.5% by recovery strain, therefore utilize existing technology, in functional material system, shape memory and gold is can recovery strain maximum, up to 8%.The bottleneck of tremendous strains in this functional material that seems that Here it is for many years.
Therefore, the problem existing for prior art, having to be solved is in the oxide material of stable nonhazardous, to realize huge shape memory effect, and is under nanoscale, the huge Shape Memory Effect that implementation structure phase transformation drives; Except stress and temperature, electric field is regulated and controled shape memory oxide as a new regulation and control degree of freedom; And realize nanoscale shape memory oxide material can recovery strain up to 14%.
Summary of the invention
Technical problem solved by the invention is to provide a kind of preparation method with the oxide film material of shape memory effect; The method can be prepared the ferroelectric oxide material with huge shape memory effect, and its shape strain can be realized under nanoscale, thereby likely substitutes the sensing of traditional alloy material under small size, the application such as driving.In the oxide material of stable nonhazardous, realize huge shape memory effect, and be under nanoscale, the huge Shape Memory Effect that implementation structure phase transformation drives; Except stress and temperature, electric field is regulated and controled shape memory oxide as a new regulation and control degree of freedom; And realize nanoscale shape memory oxide material and can be greater than 8% strain in alloy material by recovery strain.
For solving the problems of the technologies described above, the technical solution used in the present invention is to provide a kind of preparation method with the oxide film material of shape memory effect, comprises the steps:
(1) utilize pulsed laser deposition technique in high lattice mismatch single crystalline substrate, to prepare the BiFeO of two-phase coexistent
3film;
(2) utilize the BiFeO of the two-phase coexistent that focused-ion-beam lithography technology makes in upper step
3in film, prepare pure rhombus phase nanostructure.
Preferably, described in step (1), pulsed laser deposition technique refers to, prepares the BiFeO of described two-phase coexistent
3the film growth temperature of film is 600-800 ℃, and growth air pressure is 1-25Pa, and laser energy density is 1-5J/cm
2, growth rate is 0.5-5 nm/minute, and annealing is carried out under an atmospheric oxygen pressure condition, and temperature is from growth temperature to room temperature, with the speed cooling of 1-20 ℃/min.
Preferably, in order to realize huge shape memory effect, the BiFeO described in step 1)
3film thickness is 150-250 nanometer.
Preferably, the two-phase in described two-phase coexistent is rhombus phase and Tetragonal, and described rhombus phase is of a size of 30-100 nanometer, and described Tetragonal is of a size of 30-100 nanometer.
Preferably, described high lattice mismatch single crystalline substrate is LaAlO
3crystal or there is LaAlO
3/ SrTiO
3the Si substrate of resilient coating, at described Grown (La, Sr) MnO
3, (La, Sr) CoO
3or LaNiO
3deng oxide, as hearth electrode, thickness of electrode is 3-10 nanometer.
Preferably, step 2) described focused-ion-beam lithography is used 30keV Ga
+double-beam ion source, ion beam current is controlled at 10-50pA.
Preferably, step 2) time of described focused-ion-beam lithography is 2-10 minute.
Preferably, step 2) described focused-ion-beam lithography 10 seconds in the end, adopt the ion beam current of 10pA.
The application of the oxide film material that second technical problem to be solved by this invention has shape memory effect described in being under electric field action, adopting nanoscale atomic force microscope conducting probe is top electrode, polarizing voltage is up to 15-20 volt.
The application of the oxide film material that the 3rd technical problem to be solved by this invention has shape memory effect described in being under temperature action, is characterized in that: temperature range be 300K to 673K, rate temperature change is 5～20K/ minute.
Effect of the present invention is to utilize growth technology and focused-ion-beam lithography means, successfully prepares a kind of ferroelectric oxide material with huge shape memory effect.Epitaxial growth can be prepared two-phase coexistent BiFeO3, focused-ion-beam lithography is prepared into pure rhombus phase structure (as shown in Figure 1, 2) by two-phase coexistent BiFeO3, and then in this etching rhombus phase structure out, electric field, temperature, stress can be to this material shape memory strain generation effect, realize by the reversible conversion between pure rhombus phase and pure Tetragonal.Its maximum reversible strain can be up to 14%, as shown in Figure 3,4, and far above the record of the maximum 8% reversible strain that can realize in current alloy material.This huge shape memory effect derives from BiFeO simultaneously
3reversible conversion in crystal between the pure rhombus phase of nanoscale and pure Tetragonal (as Fig. 4 (a) with (b)), for electronic device is integrated and small size under the application such as sensing, driving lay the first stone.Because the effect of electric field makes the realization of this shape memory effect increase a kind of control measures, make its operating frequency higher than traditional alloy material.
Accompanying drawing explanation
Fig. 1 is the BiFeO at the two-phase coexistent that utilizes pulsed laser deposition technique to prepare
3in film, utilize the micro-nano structure of focused ion beam technology etching;
Fig. 2 is utilizing focused ion beam technology etching to mix phase BiFeO
3in process, occur by STRESS VARIATION, caused by transmission electron microscope (TEM) figure mixing mutually to pure rhombus inversion of phases;
Fig. 3 is at the BiFeO that utilizes focused ion beam technology etching
3on the micro-nano structure of film, by electric field, caused by pure rhombus mutually to the reversible conversion schematic diagram that is accompanied by 14% reversible strain of pure Tetragonal;
Fig. 4 is pure rhombus phase BiFeO after etching
3under thermal stimulus by pure rhombus mutually to the reversible conversion schematic diagram that is accompanied by 14% reversible strain of pure Tetragonal.
Embodiment
Below in conjunction with accompanying drawing 1-4 and embodiment, the present invention is further illustrated.
Embodiment
A preparation method with the oxide film material of shape memory effect, comprises the steps:
(1) utilize pulsed laser deposition technique, at high lattice mismatch single crystalline substrate LaAlO
3upper preparation is greater than the BiFeO that 150nm is thick
3film.All film growth temperature are 700 ℃, and growth air pressure is 13Pa, and laser energy density is 1.5J/cm
2, growth rate is 2.5 nm/minute, what form that rhombus phase coexists with Tetragonal mixes phase BiFeO
3.In general, mix phase BiFeO
3counter stress is very responsive, thus film thickness be increased to 150 nanometers when above basic phase structure be pure rhombus phase.Therefore want thicker mixing phase film, it is the mixing phase film success epitaxial growth that thickness is greater than 150 nanometers, we have adopted a kind of high oxygen pressure, slow annealing method, under an atmospheric oxygen pressure condition, temperature is from 700 ℃ to room temperature, with the speed cooling of 5 ℃/min, to guarantee that the stress of sull sample does not discharge completely, thickness is still keeping mixing phase structure more than 150 nanometers.In order to realize electricity performance measurement, at growth BiFeO
3before, oxide conducting material as thin as a wafer can be used as hearth electrode, equally in order to prevent Stress Release, keep mixing phase structure, in order to guarantee its conductivity, the thickness of oxide electrode must be controlled between 3-5 nanometer again, that in the present embodiment, adopt is (La, Sr) MnO
3as oxide electrode.
(2) utilize focused-ion-beam lithography technology, mixing phase BiFeO
3in film, prepare nanostructure, the nanostructure of preparing as shown in Figure 1.Before etching, in order to guarantee that sample is not destroyed by high energy ion beam, utilize electron beam evaporation method that the materials such as carbon and platinum are deposited to film surface as protective layer.In the process of etching, use 30keV Ga
+double-beam ion source, ion beam current is controlled at 50pA, to guarantee etch rate and to guarantee that sample is not damaged.According to the nanostructure of different sizes; etch period is 2.5-3.5 minute, and the final stage of all nanostructure etchings, in order to protect the degree of crystallinity of nanostructure; adopt 10 seconds of ion beam current bombardment sample of 10pA, by surperficial amorphous layer and other pollutant removals.
BiFeO prepared by the present invention
3film is at electric field, temperature, and the strain effect under effect of stress is as shown in Fig. 2,3 and 4.In all etching processes, in order to protect sample, do not adopt ion beam to observe the pattern of etching structure.But utilize 30keV Ga
+the accelerating voltage of ion, under the prerequisite not being destroyed, is etched into nanostructure by sample in film thickness direction, and utilizes the intrafascicular probe of focused ion that thin slice is fixed on copper mesh.Further etching sample has adopted respectively 16keV and 8keV Ga
+ion source, last all samples surface is by 5keV and 2eV Ga
+ion source Bombardment and cleaning, to reduce the damage in preparation process.Can observe huge strain effect with in situ TEM by scan-probe is micro-.Scanning probe microscopy measurement is to utilize under the atomic force microscope that conducting probe (platinum/silicon) is housed to obtain.Surface topography and strain analysis are scanned and are obtained by contact mode.Sweep speed is 0.2Hz, not breakdown in order to guarantee sample in detection process, and polarized electric field is up to 15-20 volt.Transmission electron microscope measurement is by the in situ TEM with temperature control, and temperature probe and thermocouple integrated in Electronic Speculum are realized, between temperature-varying zone for 300K is to 673K.Heating and cooling speed is 5～20K/ minute.
What Fig. 1 represented is to utilize focused-ion-beam lithography technology, is mixing phase BiFeO
3the nanostructure realizing in material.
What Fig. 2 represented is the shape memory effect being caused by STRESS VARIATION, utilizes focused ion beam technology etching to mix phase BiFeO
3, find can make the epitaxial stress of film be discharged by nanostructure, and then realize the regulation and control to material phase structure, from Tetragonal and the mixture of rhombus phase, become pure rhombus phase.Wherein etched area, left side is for mixing phase, and etched area, right side is pure rhombus phase.The nanostructure that proof forms by corrasion can affect substrate constraint effect (epitaxial stress), and then can regulate and control out huge change of shape.
What Fig. 3 represented is the huge shape memory effect realizing on etching structure being caused by electric field, the reset condition that wherein (a) is material, (b) 14% the shape memory strain for realizing under 20V voltage, (c) under-10V voltage, 14% shape strain is returned to initial state completely, realize the reversible regulation and control of its strain, (d) being the height change of material before and after electric field action, is the quantitative measurment to huge shape memory effect.
That Fig. 4 represents is the pure rhombus phase BiFeO under the Stress Release after etching being caused by temperature
3phase transformation and the huge shape strain of material between room temperature and 450 degrees Celsius, wherein (a) is room temperature diffraction spot, the pure rhombus phase structure that shows material under room temperature, (b) be the diffraction spot under 450 degree, the structure that shows material becomes pure tetragonal phase structure, (c) shows material pattern at room temperature, (d) shows that material exists huge shape strain under 450 degree, its height change is obvious, and deformation quantity is up to 14%.
Claims (10)
1. a preparation method with the oxide film material of shape memory effect, is characterized in that, comprises the steps:
(1) utilize pulsed laser deposition technique in high lattice mismatch single crystalline substrate, to prepare the BiFe0 of two-phase coexistent
3film;
(2) utilize the BiFeO of the two-phase coexistent that focused-ion-beam lithography technology makes in upper step
3in film, prepare nanostructure.
2. according to a kind of preparation method with the oxide film material of shape memory effect described in claim l, it is characterized in that: described in step (1), pulsed laser deposition technique refers to, prepares the BiFeO of described two-phase coexistent
3the film growth temperature of film is 600-800 ° of C, and growth air pressure is 1-25Pa, and laser energy density is 1-5J/cm
2, growth rate is 0.5-5 nm/minute, is annealed under an atmospheric oxygen pressure condition, temperature is from growth temperature to room temperature, with the speed cooling of 1-20 ° of C/ minutes.
3. a kind of preparation method with the oxide film material of shape memory effect according to claim 1, is characterized in that: step 1) described BiFeO
3film thickness is 150-250 interior rice.
4. a kind of preparation method with the oxide film material of shape memory effect according to claim 1, it is characterized in that: the two-phase in described two-phase coexistent is rhombus phase and Tetragonal, described rhombus phase is of a size of rice in 30 1 lOO, and described Tetragonal is of a size of 30-100 interior rice.
5. a kind of preparation method with the oxide film material of shape memory effect according to claim 1, is characterized in that: described high lattice mismatch single crystalline substrate is LaAl0
3crystal or there is LaAl0
3/ SrTi0
3the Si substrate of resilient coating, at described Grown (La, Sr) Mn0
3, (La, Sr) CoO
3or LaNiO
3deng oxide, as hearth electrode, thickness of electrode is 3-10 nanometers.
6. a kind of preparation method with the oxide film material of shape memory effect according to claim 1, is characterized in that: step 2) described focused-ion-beam lithography use 30kev Ga
+xX beam ion source, ion beam current is controlled at 10-50pA.
7. a kind of preparation method with the oxide film material of shape memory effect according to claim 1, is characterized in that: step 2) time of described focused-ion-beam lithography is 2-10 minute.
8. a kind of preparation method with the oxide film material of shape memory effect according to claim 1, is characterized in that: step 2) described focused-ion-beam lithography 10 seconds in the end, adopt the ion beam current of 10pA.
9. the application of a kind of oxide film material with shape memory effect claimed in claim 1 under electric field action, is characterized in that: adopting nanoscale atomic force microscope conducting probe is top electrode, and polarizing voltage is up to 15-20 volts.
10. the application of the oxide film material that a kind of described in claim l has a shape memory effect under temperature action, is characterized in that: temperature range be 300K to 673K, rate temperature change is 5～20K/ minute.
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| CN105859273A (en) * | 2016-03-29 | 2016-08-17 | 陕西科技大学 | 2-2 type BiFeO3-CuFe2O4 composite film and preparation method therefor |
| CN106431382A (en) * | 2016-09-08 | 2017-02-22 | 苏州大学 | Method for preparing ferrite epitaxial thin film with indoor temperature broadband big magnetocapacitance effect |
| CN108565336A (en) * | 2018-03-12 | 2018-09-21 | 华南师范大学 | A kind of BiFeO3Film and preparation method thereof |
| CN109208069A (en) * | 2018-07-18 | 2019-01-15 | 华南师范大学 | A method of induction bismuth ferrite thin film phase transformation |
| CN111926295A (en) * | 2020-09-01 | 2020-11-13 | 深圳大学 | Huge tetragonal phase PbTiO3Method for producing thin film |
| CN112592206A (en) * | 2020-12-09 | 2021-04-02 | 中国科学技术大学 | Method for obtaining large pseudo plastic deformation of ferroelectric material |
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| CN105859273A (en) * | 2016-03-29 | 2016-08-17 | 陕西科技大学 | 2-2 type BiFeO3-CuFe2O4 composite film and preparation method therefor |
| CN105859273B (en) * | 2016-03-29 | 2019-07-30 | 陕西科技大学 | A kind of 2-2 type BiFeO3-CuFe2O4 laminated film and preparation method thereof |
| CN106431382A (en) * | 2016-09-08 | 2017-02-22 | 苏州大学 | Method for preparing ferrite epitaxial thin film with indoor temperature broadband big magnetocapacitance effect |
| CN106431382B (en) * | 2016-09-08 | 2020-05-01 | 苏州大学 | Method for preparing ferrite epitaxial film with room-temperature wide-frequency large-magnetic capacitance effect |
| CN108565336A (en) * | 2018-03-12 | 2018-09-21 | 华南师范大学 | A kind of BiFeO3Film and preparation method thereof |
| CN108565336B (en) * | 2018-03-12 | 2022-01-04 | 华南师范大学 | BiFeO3Film and preparation method thereof |
| CN109208069A (en) * | 2018-07-18 | 2019-01-15 | 华南师范大学 | A method of induction bismuth ferrite thin film phase transformation |
| CN111926295A (en) * | 2020-09-01 | 2020-11-13 | 深圳大学 | Huge tetragonal phase PbTiO3Method for producing thin film |
| CN111926295B (en) * | 2020-09-01 | 2022-08-09 | 深圳大学 | Huge tetragonal phase PbTiO 3 Method for producing thin film |
| CN112592206A (en) * | 2020-12-09 | 2021-04-02 | 中国科学技术大学 | Method for obtaining large pseudo plastic deformation of ferroelectric material |
| CN112592206B (en) * | 2020-12-09 | 2022-03-01 | 中国科学技术大学 | Method for obtaining large pseudo plastic deformation of ferroelectric material |
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