CN108118293B - Negative Poisson ratio perovskite type thin film material and preparation method thereof - Google Patents

Negative Poisson ratio perovskite type thin film material and preparation method thereof Download PDF

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CN108118293B
CN108118293B CN201611086729.0A CN201611086729A CN108118293B CN 108118293 B CN108118293 B CN 108118293B CN 201611086729 A CN201611086729 A CN 201611086729A CN 108118293 B CN108118293 B CN 108118293B
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陈朗
李晓文
黄传威
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Southwest University of Science and Technology
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    • C04B35/4682—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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Abstract

The invention relates to a negative poisson ratio perovskite type thin film material and a preparation method thereof. The chemical component of the perovskite type film material is BaTiO3Of perovskite type ABO3The structure of (1). Experiments show that the perovskite type thin film material has a negative Poisson ratio and is a material with a negative Poisson ratio characteristic.

Description

Negative Poisson ratio perovskite type thin film material and preparation method thereof
Technical Field
The invention relates to the technical field of metamaterials, in particular to a negative Poisson ratio perovskite type thin film material and a preparation method thereof.
Background
Metamaterials have a special microstructure with many unusual properties in electromagnetic, acoustic, plasmonic, mechanical, and thermal aspects. The poisson ratio of a material refers to the ratio of the absolute value of transverse positive strain and axial positive strain of the material when the material is unidirectionally pulled or pressed, and is also called a transverse deformation coefficient, which is an elastic constant reflecting transverse deformation of the material. The materials with different Poisson ratios show different mechanical properties, compared with the traditional material with the positive Poisson ratio characteristic, the material with the negative Poisson ratio characteristic has better physical properties, and the mechanical properties of the material with the negative Poisson ratio, including shear rigidity, anti-nicking, anti-fatigue and other properties, can be obviously improved compared with the material with the positive Poisson ratio. Therefore, the material with the negative Poisson ratio characteristic can be applied to many fields, and particularly has good application prospect in the fields of space, biomedicine, weapons, intelligent materials and the like.
However, in conventional materials, the poisson's ratio of the incompressible liquid is typically 0.5, i.e., the liquid does not change volume under load. The poisson's ratio of gas and cork is close to 0, that is gas and cork are compressible objects. Whereas for solid and functional oxides the poisson ratio is typically 0.1 to 0.3. Although theoretically the theoretical poisson's ratio of isotropic materials can vary from-1 to 0.5, no experiment has been done to date to observe the negative poisson's ratio phenomenon of solid materials. Perovskite type material (molecular general formula is ABO) in metamaterial3) Is a novel inorganic non-metallic material with unique physical and chemical properties, and the physical properties thereof have been studied by people in a large quantity, but most of the ABOs are considered3The poisson's ratio of the oxides of the structure is approximately 0.3 and a systematic approach to producing negative poisson's ratio perovskite-type materials has not been found.
Disclosure of Invention
Based on the above, it is necessary to provide a negative poisson ratio perovskite thin film material and a preparation method thereof.
The negative Poisson ratio perovskite type thin film material comprises BaTiO as a chemical component3The perovskite thin film material has a negative Poisson's ratio.
In one embodiment, the negative poisson's ratio perovskite thin film material has a poisson's ratio of-0.421 to-0.225.
The preparation method of the negative Poisson ratio perovskite thin film material comprises the following steps:
providing a target material, wherein the chemical component of the target material is BaTiO3；
Placing the target material in pulsed laser deposition equipment, and in an oxygen atmosphere, controlling the laser energy density to be 1.5J/cm2～2.5J/cm2Bombarding the target material by laser with the laser frequency of 1.5 Hz-2.5 Hz, so that the target material is melted to generate plasma; and
and depositing the plasma on a substrate with the temperature of 500-700 ℃ to form the negative Poisson ratio perovskite thin film material.
In one embodiment, the target material is prepared by the following method:
mixing BaCO3And TiO2Mixing to obtain a mixture;
ball-milling the mixture to obtain a first powder material;
presintering the first powder for 9-11 h at 850-950 ℃ to obtain a presintering material;
ball-milling the pre-sintered material to obtain a second powder material;
and pressing and molding the second powder, and sintering for 9-11 h at 1000-1200 ℃ to obtain the target material.
In one embodiment, the oxygen pressure in the oxygen atmosphere is 0.5Pa to 10 Pa.
In one embodiment, the BaCO in the mixture3With the TiO mentioned2The mass ratio of (A) to (B) is 0.8-1.2: 1.
in one embodiment, the BaCO in the mixture3With the TiO mentioned2The mass ratio of (1): 1.
in one embodiment, the step of drying the mixture at 80 ℃ to 120 ℃ is further included before the step of ball milling the mixture.
In one embodiment, the operation of ball milling the pre-sintering material is specifically to put the pre-sintering material into a ball mill for ball milling for 4 to 6 hours.
In one embodiment, the negative poisson's ratio perovskite thin film material is formed to have a thickness of 50nm to 150 nm.
The inventor conducts a great deal of research on perovskite type materials to prepare a negative Poisson ratio perovskite type thin film material. The chemical component of the film material is BaTiO3Of perovskite type ABO3The structure of (1). Experiments show that the perovskite type thin film material has a negative Poisson ratio and is a material with a negative Poisson ratio characteristic.
Drawings
FIG. 1 is a flow chart of a method for preparing a negative Poisson's ratio perovskite thin film material according to an embodiment;
FIG. 2 is a flow chart of a method of preparing a target according to one embodiment;
FIG. 3 is a schematic diagram of the principle of the Poisson's ratio experiment for determining perovskite thin film material.
Detailed Description
The following mainly refers to the accompanying drawings and specific examples to further explain the negative poisson ratio perovskite thin film material and the preparation method thereof in detail.
An embodiment of the negative poisson's ratio perovskite thin film material has a chemical composition of BaTiO3(barium titanate) having a negative poisson's ratio.
Experiments show that the perovskite type thin film material has a Poisson ratio of less than 0, the Poisson ratios measured in multiple directions are negative numbers, and the perovskite type thin film material has the mechanical properties of a negative Poisson ratio material.
Specifically, the Poisson ratio of the perovskite thin film material is-0.421 to-0.225.
The results of multi-directional poisson's ratio measurements on the perovskite thin film materials of the examples show that the perovskite thin film materials have the characteristics of a negative poisson's ratio, wherein the poisson's ratio is between-0.421 and-0.225, and is less than 0.
In one embodiment, the thickness of the perovskite thin film material is 50nm to 150 nm.
The chemical component of the perovskite thin film material is BaTiO3Of perovskite type ABO3The structure of (1). Experiments show that the perovskite type thin film material has a negative Poisson ratio and is a material with a negative Poisson ratio characteristic. Can be applied to the fields of space, biomedicine, weapons, intelligent materials and the like.
The invention also provides a preparation method of the negative Poisson ratio perovskite thin film material.
Referring to fig. 1, a method for preparing a negative poisson' S ratio perovskite thin film material according to an embodiment includes the following steps S110 to S130.
S110, providing a target material, wherein the chemical component of the target material is BaTiO3。
The chemical component of the target material is BaTiO3Pulse and vesselAfter laser deposition, BaTiO can be formed3A film of (2).
S120, placing the target obtained in the step S110 in pulsed laser deposition equipment, and in an oxygen atmosphere, enabling the laser energy density to be 1.5J/cm2～2.5J/cm2And the laser with the laser frequency of 1.5 Hz-2.5 Hz bombards the target material, so that the target material is melted to generate plasma.
In this embodiment, a Pulsed Laser Deposition (PLD) method is used to prepare the perovskite thin film. Bombarding the target material by using laser, melting the target material to generate plasma, and depositing the plasma on the substrate to obtain the film.
Specifically, the energy density of the laser is 1.5J/cm2～2.5J/cm2And the laser frequency is 1.5 Hz-2.5 Hz.
In one embodiment, the laser has an energy density of 2J/cm2～2.5J/cm2And the laser frequency is 1.5 Hz-2 Hz.
In another embodiment, the laser has an energy density of 1.5J/cm2～2J/cm2And the laser frequency is 2 Hz-2.5 Hz.
Specifically, the time of laser bombardment on the target material is 30-90 min, so that the target material is melted to generate plasma.
Specifically, the oxygen atmosphere refers to introducing pure oxygen into the pulsed laser deposition equipment, and the oxygen pressure of the oxygen atmosphere is 0.5-10 Pa. Bombarding the target material with laser in oxygen atmosphere, which is favorable for melting the target material to generate plasma, and depositing the plasma on a substrate with the temperature of 500-700 ℃ to form the negative Poisson ratio perovskite type thin film material.
In one embodiment, the oxygen atmosphere has an oxygen pressure of 1 Pa.
And S130, depositing the plasma obtained in the step S120 on a substrate with the temperature of 500-700 ℃ to form the negative Poisson ratio perovskite type thin film material.
The target material is melted to generate plasma, and the plasma is emitted and deposited on the substrate, so that the perovskite type thin film material is formed on the substrate.
In general, the temperature of the substrate can be controlled to be 500 to 700 ℃ by connecting a heater to the substrate. The substrate has a certain temperature, and when the plasma is deposited on the substrate, the temperature is not quenched, so that the deposited perovskite type thin film material has a specific microstructure and thus has a negative Poisson ratio characteristic.
In one embodiment, the substrate may be a silicon wafer. The silicon wafer has good high temperature resistance and can bear the temperature required by pulsed laser deposition.
Specifically, the thickness of the negative Poisson ratio perovskite thin film material obtained by deposition is 50nm to 150 nm. Of course, it will be appreciated that in other embodiments, the deposition time may also be adjusted to obtain different thicknesses of negative poisson's ratio perovskite thin film materials.
The preparation method of the negative Poisson's ratio perovskite type thin film material can prepare BaTiO chemical composition by improving parameters of pulse laser deposition3The perovskite thin film material has a negative Poisson's ratio characteristic.
Referring to fig. 2, in one embodiment, the target is prepared by the following steps S210 to S250.
S210, mixing BaCO3And TiO2Mixing to obtain a mixture.
In particular, BaCO3The purity of the (barium carbonate) is more than 99.99%. TiO 22The purity of the titanium dioxide is more than 99.99 percent.
In one embodiment, the mixture comprises BaCO3With TiO2The mass ratio of (A) to (B) is 0.8-1.2: 1.
further, BaCO in the mixture3With TiO2The mass ratio of (1): 1.
in one embodiment, the operation of ball milling the mixture further comprises drying the mixture at 80 ℃ to 120 ℃. Specifically, the mixture may be baked in an oven set at 100 ℃ for about 10 hours to remove moisture.
S220, ball-milling the mixture obtained in the S210 to obtain a first powder material.
Specifically, the mixture can be placed in a ball mill for ball milling for 4 to 6 hours, so thatBaCO3And TiO2And (4) changing into powder to obtain first powder.
S230, pre-burning the first powder obtained in the step S220 for 9 to 11 hours at the temperature of 850 to 950 ℃ to obtain a pre-burned material.
Pre-burning BaCO at 850-950 deg.C3And TiO2Of mixed powder of, BaCO3With TiO2Reaction to produce BaTiO3Therefore, the chemical component in the pre-sintering material is BaTiO3。
Specifically, the first powder is pre-sintered for 10 hours at the temperature of 900 ℃ to obtain a pre-sintered material.
S240, ball-milling the pre-sintered material obtained in the S230 to obtain second powder.
Pre-sintering to produce BaTiO3And further ball milling to change the pre-sintered material into powder to obtain second powder.
Specifically, the operation of ball milling the pre-sintering material is to put the pre-sintering material into a ball mill for ball milling for 4 to 6 hours. And the pre-sintered material is changed into powder after ball milling to obtain second powder.
S250, pressing and forming the second powder obtained in the step S240, and sintering for 9-11 hours at the temperature of 1000-1200 ℃ to obtain the target material.
Specifically, the second powder may be pressed into various desired shapes as required.
In this embodiment, the target material is obtained by sintering at 1200 ℃ for 10 hours.
The preparation method of the target material adopts BaCO3And TiO2As reaction raw materials, the BaTiO chemical component is prepared by the processes of ball milling, presintering, ball milling again, sintering and the like3The target material has good uniformity. After deposition of the pulse laser, the target material can be melted to generate plasma to be deposited on the substrate, so that the perovskite thin film material with the negative Poisson's ratio characteristic is obtained.
The preparation method of the perovskite thin film material can prepare BaTiO with chemical components3The perovskite thin film material of (1). Experiments show that the Poisson ratio of the perovskite thin film material is negative.
The following are specific examples.
In the following examples, BaCO is not particularly specified3Has a purity of 99.99% or more, TiO2The purity of (A) is 99.99% or more. The pulsed laser deposition apparatus was purchased from compax corporation, laser emitter model compax pro102F, chamber model BRM-133.
The prepared perovskite type thin film material is measured according to the conventional method for the Poisson's ratio of the perovskite type thin film material. The specific test principle is shown in fig. 3, the material to be tested is placed in a nanoindenter, and the elastic modulus of the material under a coordinate (x, y, z) is measured by a mechanical probe. Calculating a rigidity matrix of the material under the current coordinate system according to the elastic modulus of the material, and solving an inverse matrix according to the rigidity matrix to obtain the flexibility tensor S of the material under the current coordinate systemijkl. Rotating the material to be measured at the current coordinate (x, y, z) by a certain angle around the origin to obtain a new coordinate (x ', y', z '), measuring the elastic modulus of the material under the coordinate (x', y ', z'), calculating the rigidity matrix of the material under the rotated coordinate system according to the elastic modulus of the material, and obtaining the flexibility tensor S 'of the material under the new coordinate according to the inversion matrix of the rigidity matrix'ijkl. The poisson ratio (V) may be expressed as:
Figure BDA0001167389590000061
wherein i, j, k, l is 1,2, 3.
Example 1
Mixing BaCO with the mass ratio of 1:13And TiO2Mixing to obtain a mixture. The mixture is baked at 100 ℃ for about 10h to remove water. Then ball milling is carried out for 5 hours in a ball mill to obtain first powder. And after the ball milling is finished, pre-burning the first powder for 10 hours at 900 ℃ to obtain a pre-sintered material. And placing the pre-sintered material in a ball mill for ball milling for 5 hours to obtain second powder. Pressing and molding the second powder, and sintering for 10 hours at 1200 ℃ to obtain BaTiO powder with the chemical component3The target of (1). Placing the target material in a pulsed laser deposition device, and under the condition of oxygen pressure of 1Pa, controlling the laser energy density to be 2J/cm2Laser bombardment target with laser frequency of 2HzMelting the target material for 60min to generate plasma. Plasma deposition is carried out on a substrate with the temperature of 600 ℃ to form the perovskite type thin film material with the thickness of about 100 nm.
The prepared perovskite type thin film material is placed in a nanoindentor, the elastic modulus is measured in different directions through a mechanical probe, and the Poisson ratio of the material in each direction is calculated to be negative and is between-0.421 and-0.225.
Example 2
Mixing BaCO with the mass ratio of 0.8:13And TiO2Mixing to obtain a mixture. The mixture is baked at 80 ℃ for about 10h to remove water. Then ball milling is carried out for 4 hours in a ball mill to obtain first powder. After the ball milling is finished, pre-burning the first powder for 11 hours at 850 ℃ to obtain a pre-sintered material. And placing the pre-sintered material in a ball mill for ball milling for 4 hours to obtain second powder. Pressing and molding the second powder, and sintering for 9 hours at 1000 ℃ to obtain BaTiO powder with a chemical component3The target of (1). Placing the target material in a pulsed laser deposition device, and under the condition of 0.5Pa oxygen pressure, controlling the laser energy density to be 1.5J/cm2And bombarding the target material for 30min by laser with the laser frequency of 2.5Hz, so that the target material is melted to generate plasma. Plasma deposition is carried out on a substrate with the temperature of 500 ℃ to form the perovskite type thin film material with the thickness of about 50 nm.
The prepared perovskite type thin film material is placed in a nanoindentor, the elastic modulus is measured in different directions through a mechanical probe, and the Poisson ratio of the material in each direction is calculated to be negative and is between-0.421 and-0.225.
Example 3
Mixing BaCO with the mass ratio of 1.2:13And TiO2Mixing to obtain a mixture. The mixture was baked at 120 ℃ for about 10 hours to remove water. Then ball milling is carried out for 6 hours in a ball mill to obtain first powder. And after the ball milling is finished, pre-burning the first powder for 9 hours at 950 ℃ to obtain a pre-sintered material. And placing the pre-sintered material in a ball mill for ball milling for 6 hours to obtain second powder. Pressing and molding the second powder, and sintering for 11 hours at 1100 ℃ to obtain BaTiO powder with the chemical composition3The target of (1). Placing the target material in a pulsed laser deposition deviceUnder the condition of 10Pa oxygen pressure, the laser energy density is 2.5J/cm2And bombarding the target material for 90min by laser with the laser frequency of 1.5Hz, so that the target material is melted to generate plasma. Plasma deposition is carried out on a substrate with the temperature of 700 ℃ to form the perovskite type thin film material with the thickness of about 150 nm.
The prepared perovskite type thin film material is placed in a nanoindentor, the elastic modulus is measured in different directions through a mechanical probe, and the Poisson ratio of the material in each direction is calculated to be negative and is between-0.421 and-0.225.
Experiments show that the Poisson ratio of the cork is close to 0 by using the same method, which indicates that the testing method is feasible. The perovskite thin film material prepared by the invention has the Poisson ratio of-0.421 to-0.225, and is a material with the negative Poisson ratio characteristic.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (8)

1. The negative Poisson ratio perovskite type thin film material is characterized in that the chemical component of the perovskite type thin film material is BaTiO3The perovskite type thin film material has a negative Poisson ratio, and the thickness of the perovskite type thin film material with the negative Poisson ratio is 50 nm-150 nm.
2. The negative poisson's ratio perovskite thin film material according to claim 1, wherein the poisson's ratio of the perovskite thin film material is-0.421 to-0.225.
3. The method for preparing the negative poisson's ratio perovskite thin film material as claimed in any one of claims 1-2, characterized by comprising the following steps:
providing a target material, wherein the chemical component of the target material is BaTiO3；
Placing the target material in pulsed laser deposition equipment, and in an oxygen atmosphere, controlling the laser energy density to be 1.5J/cm2～2.5J/cm2Bombarding the target material for 30-90 min by laser with the laser frequency of 1.5-2.5 Hz to melt the target material to generate plasma, wherein the oxygen pressure in the oxygen atmosphere is 0.5-10 Pa; and
and depositing the plasma on a substrate with the temperature of 500-700 ℃ to form the negative Poisson's ratio perovskite thin film material, wherein the substrate is a silicon wafer.
4. The method for preparing the negative poisson's ratio perovskite thin film material according to claim 3, wherein the target material is prepared by adopting the following method:
mixing BaCO3And TiO2Mixing to obtain a mixture;
ball-milling the mixture to obtain a first powder material;
presintering the first powder for 9-11 h at 850-950 ℃ to obtain a presintering material;
ball-milling the pre-sintered material to obtain a second powder material;
and pressing and molding the second powder, and sintering for 9-11 h at 1000-1200 ℃ to obtain the target material.
5. The method of claim 4, wherein the BaCO in the mixture is present in the form of a thin film of negative Poisson's ratio perovskite material3With the TiO mentioned2The mass ratio of (A) to (B) is 0.8-1.2: 1.
6. the method for preparing a negative Poisson's ratio perovskite thin film material according to claim 4 or 5, wherein the BaCO in the mixture3With the TiO mentioned2The mass ratio of (1): 1.
7. the method for preparing a negative poisson's ratio perovskite thin film material according to claim 4, wherein the step of drying the mixture at 80-120 ℃ is further included before the step of ball milling the mixture.
8. The preparation method of the negative poisson's ratio perovskite thin film material according to claim 4, wherein the operation of ball milling the pre-sintering material is specifically to put the pre-sintering material into a ball mill for ball milling for 4-6 h.
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不同厚度BaTiO3薄膜的铁电隧道结电学性质的研究;温嘉红;《中国优秀硕士学位论文全文数据库 基础科学辑》;20150215(第02期);正文第17页，图2-2、2-3 *

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