CN108103440A - A kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film - Google Patents
A kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film Download PDFInfo
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- CN108103440A CN108103440A CN201711193698.3A CN201711193698A CN108103440A CN 108103440 A CN108103440 A CN 108103440A CN 201711193698 A CN201711193698 A CN 201711193698A CN 108103440 A CN108103440 A CN 108103440A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
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Abstract
The invention discloses a kind of preparation methods of negative poisson's ratio lanthanum-strontium-manganese-oxygen film, belong to electric thin technical field.After substrate used is cleaned with La0.7Sr0.3MnO3Target is put into togerther in pulsed laser deposition equipment, and the vacuum state of pulsed laser deposition equipment, substrate heating temperature, flowing oxygen pressure are controlled, deposition operation is carried out and obtains La0.7Sr0.3MnO3‑δFilm.The present invention passes through in SrTiO3Grown film acts on film tension stress, while makes La0.7Sr0.3MnO3‑δThe manganese oxygen octahedra of film expands, and obtains the La of negative poisson's ratio0.7Sr0.3MnO3‑δFilm.In addition laser energy used in this method is relatively low, and simple process and low cost is honest and clean, efficient, workable.
Description
Technical field
Invention is related to a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film, belongs to electric thin technical field.
Background technology
Since 1987, scientist Lakes heated polyurethane foam, cools down and relaxation processes etc., is had
After negative poisson's ratio is -0.7 material, people open the widely studied of this field.Negative poisson's ratio material refers to material tension
Lateral expansion occurs when stretching in elastic range, transverse compression occurs when compressed in elastic range.In usual thin-film material
In and find no the presence of Negative poisson's ratio, the modulus of shearing of negative poisson's ratio material energy strengthening material increases plane strain
Fracture toughness, increase resistance to indentation etc..These unusual properties cause negative poisson's ratio material to have wide application value.Than
There is Ni Ru commercialized3Al monocrystal materials, because it has -0.81 negative poisson's ratio, so as to possess high intensity and anti-fractureing property,
It is equipped on the blade of aero-engine.
At present, negative poisson's ratio material is mainly found in macromolecule polymeric material, but macromolecule negative poisson's ratio material is as gathered
Ethylene, polyurethane material etc., which do not have perovskite structure, has Electrical transport, therefore has a greatly reduced quality in commercial Application.Calcium
Perovskite like structure La0.7Sr0.3MnO3Material has unique structure and physical property, such as giant magnetoresistance effect, magnetic order, track are in order
Characteristic becomes the research hotspot in the fields such as physics, material and engineering in recent years.La0.7Sr0.3MnO3Film is real in many directions
Existing device, magnetic head, magnetoresistive memory, Magnetic Sensor and the magnetic refrigeration side being used as at present in information storage system
Face, and the change of the lower easy recurring structure that influences in external condition of these devices and performance.Device La0.7Sr0.3MnO3It is thin
The Poisson's ratio of film is typically positive, it is difficult to meet industrial requirement, therefore prepare the La of negative poisson's ratio at this stage0.7Sr0.3MnO3
Film can effectively solve the problems, such as these.
The content of the invention
1. goal of the invention：
In order to be directed to above-mentioned present situation, a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film is proposed.
2. technical solution：
A kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film, the described method includes：
(1) substrate used is cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state, vacuum degree reach after to substrate into
Row heating, heating temperature are 720~740 DEG C；
(4) flowing oxygen cycle operation is carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)；
(5) deposition operation is carried out to the pulsed laser deposition equipment in step (4), obtains different-thickness
La0.7Sr0.3MnO3-δFilm；
(6) XRD tests are carried out to gained film, obtains lattice parameter afilm、cfilm；
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3-δThe Poisson's ratio of film；
A in formulafilm、cfilm、abulkThe respectively lattice parameter of film a axis, c-axis and target, wherein target lattice parameter
Preferably, step (1) described substrate is SrTiO3(001) substrate, substrate lattice parameter must be more than La0.7Sr0.3MnO3
Target lattice parameter, and error range is
Preferably, the vacuum degree of step (3) described high vacuum state is 1 × 10-3~1 × 10-5Pa；
Preferably, the oxygen pressure of step (4) the flowing oxygen cycle operation is 1 × 10-2~1 × 10-4Pa；
Preferably, the process conditions of step (5) described pulsed laser deposition are that laser pulse width is 10ns, laser energy 150
~200 mJ, 1~5Hz of laser frequency, a length of 5~25min during deposition；
Preferably, step (5) La0.7Sr0.3MnO3Film thickness scope is 10~70nm；
The present invention is using pulsed deposition coating technique, in SrTiO3Substrate, the oxygen pressure of cycle operation are 1 × 10-2~1 ×
10-4Pa, film thickness are 10~70nm, prepare the La of negative poisson's ratio0.7Sr0.3MnO3-δFilm, principle are in SrTiO3Lining
The effect of film tension stress when being grown on bottom, the oxygen pressure of cycle operation is low oxygen pressure (10-2~10-4Pa it) can obtain anoxic
La0.7Sr0.3MnO3-δFilm, because La during anoxic0.7Sr0.3MnO3-δOxygen content is reduced in film, to ensure that electricity price balances Mn4+Turn
Become Mn3+, and Mn3+Ionic radius be more than Mn4+Ionic radius, expand manganese oxygen octahedra, so as to obtain negative pool
The film of loose ratio；And when thickness is more than 70nm, La0.7Sr0.3MnO3-δRelaxation, no negative poisson's ratio characteristic can occur for film；
3. advantageous effect：
Roughness of film prepared by the present invention is low, and required laser energy is relatively low, and simple process and low cost is honest and clean, efficiency
Height, workable, the La of gained0.7Sr0.3MnO3-δFilm negative poisson's ratio material has very big potential in field of electronic devices
Application value.
Description of the drawings
Fig. 1 is the La that embodiment 1 arrives embodiment 50.7Sr0.3MnO3-δFilm XRD diagram；
Fig. 2 is the La of embodiment 30.7Sr0.3MnO3-δFilm RSM schemes；
Specific embodiment
Below by embodiment, the present invention will be described in detail, these embodiments are only because the mesh that exemplary illustrates
, and it is not intended to limit the present invention.
Embodiment 1
(1) by SrTiO used3(001) substrate is cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state for 1 × 10-4Pa, vacuum degree reach
Substrate is heated afterwards, heating temperature is 720 DEG C；
(4) flowing oxygen cycle operation, oxygen pressure are carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)
For 1 × 10-2Pa；
(5) deposition operation, laser pulse width 10ns, laser energy are carried out to the pulsed laser deposition equipment in step (4)
180 mJ, laser frequency 3Hz；A length of 5min during deposition obtains the La that thickness is 10nm0.7Sr0.3MnO3-δFilm；
(6) XRD tests are carried out to gained film, XRD spectrum is shown in Fig. 1, obtains lattice parameter afilmForcfilm
For
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3-δThe Poisson's ratio of film；
A in formulafilm、cfilm、abulkThe respectively lattice parameter of film a axis, c-axis and target, wherein target lattice parameter
Its negative poisson's ratio is -0.2.
Embodiment 2
As different from Example 1：
(1) by SrTiO used3(001) substrate is cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state for 1 × 10-4Pa, vacuum degree reach
Substrate is heated afterwards, heating temperature is 730 DEG C；
(4) flowing oxygen cycle operation, oxygen pressure are carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)
For 1 × 10-2Pa；
(5) deposition operation, laser pulse width 10ns, laser energy are carried out to the pulsed laser deposition equipment in step (4)
180 mJ, laser frequency 3Hz；A length of 15min during deposition obtains the La that thickness is 68nm0.7Sr0.3MnO3-δFilm；
(6) XRD tests are carried out to gained film, XRD spectrum is shown in Fig. 1, obtains lattice parameter afilmFor
cfilmFor
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3-δThe Poisson's ratio of film；
A in formulafilm、cfilm、abulkThe respectively lattice parameter of film a axis, c-axis and target, wherein target lattice parameter
Its negative poisson's ratio is -2.22.
Embodiment 3
As different from Example 1：
(1) by SrTiO used3(001) substrate is cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state for 1 × 10-4Pa, vacuum degree reach
Substrate is heated afterwards, heating temperature is 730 DEG C；
(4) flowing oxygen cycle operation, oxygen pressure are carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)
For 1 × 10-2Pa；
(5) deposition operation, laser pulse width 10ns, laser energy are carried out to the pulsed laser deposition equipment in step (4)
150mJ, laser frequency 3Hz；A length of 25min during deposition obtains the La that thickness is 78nm0.7Sr0.3MnO3-δFilm；
(6) XRD tests are carried out to gained film, XRD spectrum is shown in Fig. 1, obtains lattice parameter afilmFor
cfilmFor
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3The Poisson's ratio of film；
Thickness is the La of 78nm0.7Sr0.3MnO3It is as shown in Figure 2 that relaxation occurs for film.
Embodiment 4
As different from Example 1：
(1) by LaAlO used3(001) substrate is cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state for 1 × 10-4Pa, vacuum degree reach
Substrate is heated afterwards, heating temperature is 740 DEG C；
(4) flowing oxygen cycle operation, oxygen pressure are carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)
For 1 × 10-2Pa；
(5) deposition operation, laser pulse width 10ns, laser energy are carried out to the pulsed laser deposition equipment in step (4)
150 mJ, laser frequency 3Hz；A length of 10min during deposition obtains the La that thickness is 40nm0.7Sr0.3MnO3-δFilm；
(6) XRD tests are carried out to gained film, XRD spectrum is shown in Fig. 1, obtains lattice parameter afilmFor
cfilmFor
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3-δThe Poisson's ratio of film；
A in formulafilm、cfilm、abulkThe respectively lattice parameter of film a axis, c-axis and target, wherein target lattice parameter
Its substrate used is LaAlO3, because LaAlO3The lattice parameter of substrate isLess than La0.7Sr0.3MnO3Target
The lattice parameter of materialIn LaAlO3The effect of Grown compression chord, no negative poisson's ratio characteristic.
Embodiment 5
As different from Example 1：
(1) (La, Sr) (Al, Ta) O by used in3(LSAT) (001) substrate is successively in acetone, absolute ethyl alcohol, deionized water
In be cleaned by ultrasonic；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state for 1 × 10-4Pa, vacuum degree reach
Substrate is heated afterwards, heating temperature is 730 DEG C；
(4) flowing oxygen cycle operation, oxygen pressure are carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)
For 1 × 10-2Pa；
(5) deposition operation, laser pulse width 10ns, laser energy are carried out to the pulsed laser deposition equipment in step (4)
200 mJ, laser frequency 3Hz；A length of 10min during deposition obtains the La that thickness is 41nm0.7Sr0.3MnO3-δFilm；
(6) XRD tests are carried out to gained film, XRD spectrum is shown in Fig. 1, obtains lattice parameter afilmFor
cfilmFor
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3-δThe Poisson's ratio of film；
A in formulafilm、cfilm、abulkThe respectively lattice parameter of film a axis, c-axis and target, wherein target lattice parameter
Its substrate used is LSAT, because the lattice parameter of LSAT substrates isLess than La0.7Sr0.3MnO3Target
Lattice parameterIn the effect of LSAT Grown compression chords, no negative poisson's ratio characteristic.
La is can be seen that from the XRD of Fig. 10.7Sr0.3MnO3-δFilm is made in LAO, LSAT Grown compression chord
Used time diffraction maximum obtains lattice parameter c in the left side of substratefilmLarger, the Poisson's ratio being calculated by formula 1 is positive value,
When STO Growns tension stress acts on, diffraction maximum obtains lattice parameter c in the left side of substratefilmIt is smaller, by formula 1
The Poisson's ratio being calculated is negative value.
The Qx of film and the Qx of substrate are can be seen that not in straight line from the RSM of Fig. 2, illustrate that this film is relaxed
Henan.
Comparative example prepares different-thickness in various substrates (STO, LAO, LSAT) and on STO substrates respectively
La0.7Sr0.3MnO3-δThe results are shown in Table 1 for the Poisson's ratio of film：
The La of 1 different-thickness of table and substrate0.7Sr0.3MnO3-δFilm Poisson's ratio result
Embodiment described above only expresses the preferred embodiment of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, several deformations can also be made, improves and substitutes, these belong to this hair
Bright protection domain.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film, which is characterized in that the described method includes：
(1) substrate used is cleaned by ultrasonic in acetone, absolute ethyl alcohol, deionized water successively；
(2) by La0.7Sr0.3MnO3Substrate in target and step (1) is put into pulsed laser deposition equipment；
(3) vacuum operation is carried out to pulsed laser deposition equipment, reaches high vacuum state, vacuum degree adds substrate after reaching
Heat, heating temperature are 720~740 DEG C；
(4) flowing oxygen cycle operation is carried out to the pulsed laser deposition equipment of gained high vacuum state in step (3)；
(5) deposition operation is carried out to the pulsed laser deposition equipment in step (4), obtains the La of different-thickness0.7Sr0.3MnO3-δ
Film；
(6) XRD tests are carried out to gained film, obtains lattice parameter afilm、cfilm；
(7) according to the lattice parameter of film, La is calculated according to formula (1)0.7Sr0.3MnO3-δThe Poisson's ratio of film；
A in formulafilm、cfilm、abulkThe respectively lattice parameter of film a axis, c-axis and target, wherein target lattice parameter
2. a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film according to claim 1, it is characterised in that：Step (1)
The substrate is SrTiO3(001) substrate, substrate lattice parameter must be more than La0.7Sr0.3MnO3Target lattice parameter, and error model
Enclose for
3. a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film according to claim 1, it is characterised in that：Step (3)
The vacuum degree of the high vacuum state is 1 × 10-3~1 × 10-5Pa。
4. a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film according to claim 1, it is characterised in that：Step (4)
The oxygen pressure of the flowing oxygen cycle operation is 1 × 10-2~1 × 10-4Pa。
5. a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film according to claim 1, it is characterised in that：Step (5)
The process conditions of the pulsed laser deposition are that laser pulse width is 10ns, 150~200mJ of laser energy, 1~5Hz of laser frequency
A length of 5~25min during deposition.
6. a kind of preparation method of negative poisson's ratio lanthanum-strontium-manganese-oxygen film according to claim 1, it is characterised in that：Step (5)
The La0.7Sr0.3MnO3-δFilm thickness scope is 10~70nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115139512A (en) * | 2022-07-26 | 2022-10-04 | 西北工业大学 | Three-dimensional negative Poisson ratio structure 3D printing method and system |
| CN117568755A (en) * | 2024-01-15 | 2024-02-20 | 华中科技大学 | Low-resistance lanthanum strontium manganese oxygen electrode film and preparation method thereof |
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| CN102586747A (en) * | 2012-03-13 | 2012-07-18 | 浙江理工大学 | Preparation method of (BiFe03) m/(La0.7Sr0.3Mn03)n multi-layer film |
| CN106591781A (en) * | 2017-01-10 | 2017-04-26 | 河北大学 | Improvement method for interface dead layer of ultrathin lanthanum-strontium-manganese oxide film |
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2017
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Patent Citations (2)
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| CN102586747A (en) * | 2012-03-13 | 2012-07-18 | 浙江理工大学 | Preparation method of (BiFe03) m/(La0.7Sr0.3Mn03)n multi-layer film |
| CN106591781A (en) * | 2017-01-10 | 2017-04-26 | 河北大学 | Improvement method for interface dead layer of ultrathin lanthanum-strontium-manganese oxide film |
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| M.CESARIA,ET AL.: "Optical response of oxygen deficient La0.7Sr0.3MnO3 thin films deposited by pulsed laser deposition", 《THIN SOLID FILMS》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115139512A (en) * | 2022-07-26 | 2022-10-04 | 西北工业大学 | Three-dimensional negative Poisson ratio structure 3D printing method and system |
| CN115139512B (en) * | 2022-07-26 | 2023-05-02 | 西北工业大学 | Three-dimensional negative poisson ratio structure 3D printing method and system |
| CN117568755A (en) * | 2024-01-15 | 2024-02-20 | 华中科技大学 | Low-resistance lanthanum strontium manganese oxygen electrode film and preparation method thereof |
| CN117568755B (en) * | 2024-01-15 | 2024-03-26 | 华中科技大学 | Low-resistance lanthanum strontium manganese oxygen electrode film and preparation method thereof |
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