CN115786855A - Epitaxial yttrium-doped hafnium-based ferroelectric film material and growth method thereof - Google Patents
Epitaxial yttrium-doped hafnium-based ferroelectric film material and growth method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 28
- 229910052735 hafnium Inorganic materials 0.000 title claims abstract description 22
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 34
- 229910000449 hafnium oxide Inorganic materials 0.000 claims abstract description 14
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010409 thin film Substances 0.000 claims description 41
- 239000010408 film Substances 0.000 claims description 38
- 239000013077 target material Substances 0.000 claims description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 229910002182 La0.7Sr0.3MnO3 Inorganic materials 0.000 claims description 13
- 229910002367 SrTiO Inorganic materials 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 8
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 4
- 230000008685 targeting Effects 0.000 claims description 3
- 229910002075 lanthanum strontium manganite Inorganic materials 0.000 abstract description 16
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010009 beating Methods 0.000 description 2
- 230000005621 ferroelectricity Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 101100353526 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) pca-2 gene Proteins 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 231100000053 low toxicity Toxicity 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention belongs to the field of materials, and particularly relates to an epitaxial yttrium-doped hafnium-based ferroelectric film material and a growth method thereof. According to the method, the STO is used as a substrate, the LSMO is used as a buffer layer, and the epitaxial orientation of YHO on the same substrate is regulated and controlled by changing the growth process of YHO, so that a pure cross-phase (002) epitaxial yttrium-doped hafnium oxide ferroelectric film material and a dual-orientation YHO ferroelectric film material containing an orthorhombic phase (111) and an orthorhombic phase (002) are respectively obtained. The yttrium-doped hafnium oxide ferroelectric film material provided by the invention has the advantages that the YHO ferroelectric film material is subjected to orientation control through a specific process, the problem that the application of an epitaxial yttrium-doped hafnium-based ferroelectric film is limited because the epitaxial yttrium-doped hafnium-based ferroelectric film can only grow on a specific substrate in a single orientation is solved, the growth mechanism of the epitaxial yttrium-doped hafnium-based ferroelectric film material can be further explored, and the development and application of corresponding ferroelectric devices can be improved.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to an epitaxial yttrium-doped hafnium-based ferroelectric film material and a growth method thereof.
Background
The ferroelectric material is an important functional material, has the important characteristics of excellent dielectricity, piezoelectricity, pyroelectric property, ferroelectricity, electro-optic effect, acousto-optic effect, photorefractive effect, nonlinear optical effect and the like, and has wide application prospect in the fields of ferroelectric memories, spatial light modulators, optical waveguides, dielectric phase shifters and the like. Among them, hafnium-based ferroelectric materials are promising candidates for new ferroelectric materials due to their superior performance such as superior miniaturization capability, larger band gap, higher remanent polarization, simple chemical composition, low toxicity, and compatibility with Complementary Metal Oxide Semiconductor (CMOS) processes.
The hafnium-based oxide is stable in the form of monoclinic phase (P2) at room temperature 1 The/c, m phase), other common high temperature, high pressure phases, namely the tetragonal phase (P4) 2 The/nmc, the t phase) and the cubic phase (Fm 3m, the c phase), can be stabilized at room temperature by doping or nanostructures. The research proves that the ferroelectricity can be derived from non-centrosymmetric polar orthogonal phase (Pca 2) 1 O phase). Most research is based on polycrystalline thin films, with great progress being made in preparing, understanding the structure and ferroelectric properties of hafnium oxide, and in device fabrication. Epitaxial films, which are typically nucleated on the surface of a single crystal or bottom epitaxial layer, are much less studied than if bulk crystallization by poly crystalline annealing were performed. Therefore, the mechanism of stabilization of the hafnium oxide ferroelectric phase in the epitaxial film is significantly different from that of the polycrystalline film, thereby providing an opportunity for stabilization of film quality and concomitant better functional characteristics.
Researchers at the university of tokyo industries, japan, 2015, first reported epitaxial growth of doped hafnium oxide ferroelectric thin films. Since then, research on the epitaxial hafnium-based ferroelectric thin film has been exponentially increased, and it has been demonstrated that the epitaxially grown hafnium-based ferroelectric thin film exhibits a more ordered domain structure and superior ferroelectric properties.
Regarding the research of epitaxial yttrium-doped hafnium oxide ferroelectric film, due to the problem of lattice constant matching, only pure cross-phase YHO (111) or pure cross-phase YHO (002) can be grown on a specific substrate in the industry; and based on the category of epitaxial growth YHO (111) and YHO (002), the substrate lattice-matched with the epitaxial growth YHO (111) needs to be selected one to one. For example, kiliha Katayama in ZrO 2 -Y 2 O 3 An epitaxial YHO (002) ferroelectric film is grown on a (YSZ) (002) substrate, yu Yun is on SrTiO 3 An epitaxial YHO (111) ferroelectric thin film was grown on a (STO) (001) substrate.
The epitaxial dual-orientation ferroelectric film has two different lattice constants, so that the material interface matching is wider, the process expandability of heterogeneous ferroelectric device stacking is increased, and a new idea is provided for the development of a future interface reconfigurable ferroelectric device. However, due to the development of modern technology, interdisciplinary applications, and the trend of highly integrated technology development, the pure phase growth of epitaxial thin films, specific requirements of YHO (111) and YHO (002) on the substrate, limited the development of epitaxial YHO ferroelectric thin films.
Disclosure of Invention
Aiming at the problems or the defects, the invention provides an epitaxial yttrium-doped hafnium-based ferroelectric thin film material and a growth method thereof, aiming at solving the problem that the application of the existing epitaxial yttrium-doped hafnium-based ferroelectric thin film is limited because the epitaxial yttrium-doped hafnium-based ferroelectric thin film can only be grown in a single orientation on a specific substrate, and the epitaxial yttrium-doped hafnium oxide ferroelectric thin film material with pure cross phase (002) and a bi-orientation material containing orthogonal phase (111) and orthogonal phase (002) are respectively obtained on the same substrate by changing the growth process by adopting a pulse laser deposition method.
An epitaxial yttrium-doped hafnium-based ferroelectric thin film material sequentially comprises the following components from top to bottom: srTiO 3 (STO) substrate, la 0.7 Sr 0.3 MnO 3 A (LSMO) buffer layer and a yttrium doped hafnium oxide (YHO) ferroelectric thin film.
The La 0.7 Sr 0.3 MnO 3 The (LSMO) buffer layer has a thickness of 30-45 nm.
The yttrium-doped hafnium oxide (YHO) ferroelectric film is a YHO film containing an orthorhombic phase (111) and an orthorhombic phase (002) simultaneously, or a YHO film containing an orthorhombic phase (002); the thickness is 10-25 nm.
The growth method of the epitaxial yttrium-doped hafnium-based ferroelectric film material comprises the following steps:
step 1, adopting a pulse laser deposition technology to deposit SrTiO 3 Growing La on (STO) substrate 0.7 Sr 0.3 MnO 3 (LSMO) thin films as buffer layers.
The method comprises the following specific steps: mixing SrTiO 3 Placing the (STO) substrate in a vacuum chamber, and raising the temperature of the substrate to 650-750 ℃; after the temperature rise is finished, oxygen is introduced, the oxygen pressure is controlled to be 30-40 Pa, and then laser (such as KrF) is adopted to ablate the surface of the rotating target material (the laser energy is 1.4-1.6J/cm) 2 ) Obtaining La with the thickness of 30-45 nm 0.7 Sr 0.3 MnO 3 (LSMO) buffer layers.
Step 2, adopting a pulse laser deposition technology to prepare the La prepared in the step 1 0.7 Sr 0.3 MnO 3 And growing an epitaxial YHO ferroelectric film on the (LSMO) buffer layer film.
If the orthogonal phase (111) and the orthogonal phase (002) are bi-oriented YHO ferroelectric thin film is grown, the specific steps are as follows:
raising the temperature of the substrate to 750-800 ℃; after the temperature rise is finished, oxygen is introduced, the oxygen pressure is controlled to be 10-15Pa, and laser (such as KrF) is adopted to ablate the surface of the rotating target material (the laser energy is 1.8-2.2J/cm) 2 ) HfO is performed according to the doping amount of Y 2 Target material and Y 2 O 3 The target was switched and hit to obtain a YHO film having a thickness of 10 to 25nm and containing an orthorhombic phase (111) and an orthorhombic phase (002).
If the YHO ferroelectric thin film of the orthorhombic phase (002) is grown, the method specifically comprises the following steps:
adjusting the temperature of the substrate to 625-700 ℃; introducing oxygen after the temperature rise is finished, controlling the oxygen pressure at 0.05-1Pa, and ablating the surface of the rotating target material by laser (such as KrF) (the laser energy is 1.8-2.2J/cm) 2 ) HfO is performed according to the doping amount of Y 2 Target material and Y 2 O 3 Target material exchange target shooting is carried out to obtain YHO (002) film with the thickness of 10-25 nm.
The invention uses SrTiO 3 (STO) is a substrate, la 0.7 Sr 0.3 MnO 3 The (LSMO) is used as a buffer layer, and an yttrium doped hafnium oxide (YHO) ferroelectric film is grown at a high temperature. The epitaxial orientation of YHO on the same substrate is regulated and controlled by changing the growth process of YHO, and the epitaxial yttrium-doped hafnium oxide ferroelectric film material with pure cross phase (002) and the dual-orientation YHO ferroelectric film material containing orthogonal phase (111) and orthogonal phase (002) are respectively obtained. The epitaxial dual-orientation ferroelectric film has two different lattice constants, so that the material has interface matching propertyThe process has the advantages of increasing the process expandability of the heterogeneous ferroelectric device stacking, and providing a new idea for the development of the interface reconfigurable ferroelectric device in the future.
In conclusion, the yttrium-doped hafnium oxide ferroelectric thin film material provided by the invention has the advantages that the YHO ferroelectric thin film material is subjected to orientation control through a specific process, the problem that the application of an epitaxial yttrium-doped hafnium-based ferroelectric thin film is limited due to the fact that the epitaxial yttrium-doped hafnium-based ferroelectric thin film can only grow on a specific substrate in a single orientation is solved, and the growth mechanism of the epitaxial yttrium-doped hafnium-based ferroelectric thin film material can be further explored, and the development and application of corresponding ferroelectric devices can be improved.
Drawings
FIG. 1 shows XRD theta-2 theta scales for structural characterization of epitaxial YHO dual-orientation ferroelectric thin film.
FIG. 2 is a P-V characteristic diagram of structural characterization of an epitaxial YHO dual-orientation ferroelectric thin film.
FIG. 3 shows XRD theta-2 theta scales of o (002) structural characterization of epitaxial YHO ferroelectric thin film material.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples.
Example 1
The preparation method of the epitaxial YHO dual-orientation ferroelectric film comprises the following specific steps:
step 1, adopting a pulse laser deposition technology to form SrTiO 3 Growth of La on (STO) substrates 0.7 Sr 0.3 MnO 3 (LSMO) thin film.
The method specifically comprises the following steps: mixing SrTiO 3 The (STO) substrate is placed in a vacuum chamber, the target spacing is fixed at 60mm, and the substrate temperature is raised to 750 ℃; introducing 99.999% oxygen after heating, controlling oxygen pressure at 30Pa, ablating the surface of the rotating target material by using laser (KrF) with wavelength of 248nm and laser energy of 1.5J/cm 2 Wherein the laser strikes La 0.7 Sr 0.3 MnO 3 The pulse frequency of the (LSMO) target material is 5Hz, and the LSMO thin film with the thickness of 45nm is obtained under the impact of 4000 Hz.
And 2, growing a 15nm epitaxial YHO ferroelectric film on the LSMO film prepared in the step 1 by adopting a pulse laser deposition technology.
The method specifically comprises the following steps: the target pitch was fixed at 55mm,the temperature of the substrate is 770 ℃; introducing 99.999 percent oxygen after the temperature rise is finished, controlling the oxygen pressure at 15Pa, ablating the surface of the rotating target material by adopting laser (KrF) with the wavelength of 248nm and the laser energy of 2J/cm 2 Performing HfO 2 Target material and Y 2 O 3 Target exchange targeting, in which the laser strikes the HfO 2 The pulse frequency of the target material is 5Hz, and the target material is hit under 48 Hz; beating Y 2 O 3 The pulse frequency of the target material is 2Hz, and the target material is hit under 1. This was repeated 16 times to give a YHO film with a thickness of 15nm, which was incubated for 10 minutes and subsequently allowed to cool to room temperature at 10 ℃ per minute.
And 3, step 3: and (3) growing a Pt electrode with the thickness of 25nm and the diameter of 35 mu m on the sample prepared in the step (2) by adopting a pulse laser deposition method.
The method specifically comprises the following steps: keeping the prepared epitaxial YHO ferroelectric film at normal temperature, adjusting the target spacing to 40mm, ablating the surface of the rotating target material by using laser (KrF) with the wavelength of 248nm and the laser energy of 2.5J/cm 2 And the pulse frequency of the laser hitting the Pt target material is 5Hz.
Example 2
The preparation of the epitaxial YHO ferroelectric thin film material o (002) comprises the following steps:
step 1, adopting a pulse laser deposition technology to deposit SrTiO 3 Growth of La on (STO) substrates 0.7 Sr 0.3 MnO 3 (LSMO) thin films.
The method comprises the following specific steps: srTiO 2 3 The (STO) substrate is placed in a vacuum chamber, the target spacing is fixed at 60mm, and the substrate temperature is raised to 700 ℃; introducing 99.999 percent oxygen after the temperature rise is finished, controlling the oxygen pressure at 30Pa, ablating the surface of the rotating target material by adopting laser (KrF) with the wavelength of 248nm and the laser energy of 1.5J/cm 2 Wherein the laser strikes La 0.7 Sr 0.3 MnO 3 The pulse frequency of the (LSMO) target material is 5Hz, and the LSMO thin film with the thickness of 45nm is obtained under the impact of 4000 Hz.
And 2, growing a 15nm epitaxial YHO ferroelectric film on the LSMO film prepared in the step 1 by adopting a pulse laser deposition technology.
The method specifically comprises the following steps: the target spacing was fixed at 55mm and the substrate temperature was raised to 700 ℃; introducing 99.999 percent oxygen after the temperature rise is finished, controlling the oxygen pressure at 0.05Pa,ablating the surface of the rotating target material by using laser (KrF) with the wavelength of 248nm and the laser energy of 2J/cm 2 Performing HfO 2 Target material and Y 2 O 3 Target exchange targeting, in which laser hits HfO 2 The pulse frequency of the target material is 5Hz, and the target material is hit under 48 Hz; beating Y 2 O 3 The pulse frequency of the target material is 2Hz, and the target material is hit under 1. The above steps are circulated for 16 times to obtain an epitaxial YHO ferroelectric thin film with the thickness of 15nm, the temperature is kept for 10 minutes, and then the temperature is reduced to room temperature at 10 ℃/minute.
And step 3: and (3) growing a Pt electrode with the thickness of 25nm and the diameter of 35 mu m on the sample prepared in the step (2) by adopting a pulse laser deposition method.
The method specifically comprises the following steps: keeping the prepared epitaxial YHO ferroelectric film at normal temperature, adjusting the target spacing to 40mm, ablating the surface of the rotating target material by using laser (KrF) with the wavelength of 248nm and the laser energy of 2.5J/cm 2 Wherein the pulse frequency of the laser hitting the Pt target material is 5Hz.
HfO obtained for examples 1 and 2 2 The ferroelectric material was subjected to structural and electrical testing.
The XRD results of the obtained epitaxial YHO bi-oriented ferroelectric thin film are shown in FIG. 1. As can be seen from fig. 1, the bragg peak of YHO film o (111) appeared at about 30 °, the bragg peak of YHO film o (002) appeared at about 34 °, and the P-V characteristic test results are shown in fig. 2. As can be seen from FIG. 2, the material has residual polarization of 2Pr =16 μ C/cm 2 。
The XRD result of the obtained epitaxial YHO ferroelectric thin film material o (002) is shown in FIG. 3. As can be seen from fig. 3, the bragg peak of YHO film o (002) appears around 34 °.
As can be seen from the above examples and corresponding tests, the present invention is applied to SrTiO 3 (STO) and La 0.7 Sr 0.3 MnO 3 The orientation of the epitaxial YHO ferroelectric film is effectively regulated and controlled through the process and specific parameters on (LSMO), the electrical characteristics are represented, the relationship between the orientation structure and the ferroelectric properties can be known, the problem that the current epitaxial yttrium-doped hafnium-based ferroelectric film can only grow in a single orientation on a specific substrate to cause application limitation is solved, the growth mechanism is further explored, and the generation rate of corresponding ferroelectric devices is improvedAnd (5) displaying the application.
Claims (2)
1. An epitaxial yttrium-doped hafnium-based ferroelectric thin film material is characterized in that: srTiO is arranged from top to bottom in sequence 3 (STO) substrate, la 0.7 Sr 0.3 MnO 3 (LSMO) buffer layer and yttrium doped hafnium oxide (YHO) ferroelectric thin film;
the La 0.7 Sr 0.3 MnO 3 The thickness of the (LSMO) buffer layer is 30-45 nm;
the yttrium-doped hafnium oxide (YHO) ferroelectric film is a YHO film containing an orthorhombic phase (111) and an orthorhombic phase (002) simultaneously, or a YHO film containing an orthorhombic phase (002); the thickness is 10-25 nm.
2. The method for growing an epitaxial yttrium doped hafnium-based ferroelectric thin film material of claim 1, comprising the steps of:
step 1, adopting a pulse laser deposition technology to deposit SrTiO 3 Growing La on (STO) substrate 0.7 Sr 0.3 MnO 3 (LSMO) thin films as buffer layers;
the method comprises the following specific steps: srTiO 2 3 Placing the (STO) substrate in a vacuum chamber, and raising the temperature of the substrate to 650-750 ℃; introducing oxygen after the temperature rise is finished, controlling the oxygen pressure at 30-40 Pa, and then ablating the surface of the rotating target material by adopting laser to obtain La with the thickness of 30-45 nm 0.7 Sr 0.3 MnO 3 (LSMO) buffer layer with laser energy of 1.4-1.6J/cm 2 ；
Step 2, adopting a pulse laser deposition technology to prepare the La prepared in the step 1 0.7 Sr 0.3 MnO 3 Growing an epitaxial YHO ferroelectric thin film on the (LSMO) buffer layer thin film;
if the orthogonal phase (111) and the orthogonal phase (002) are bi-oriented YHO ferroelectric thin film is grown, the specific steps are as follows:
raising the temperature of the substrate to 750-800 ℃; introducing oxygen after the temperature rise is finished, controlling the oxygen pressure at 10-15Pa, ablating the surface of the rotating target material by adopting laser, and carrying out HfO according to the doping amount of Y 2 Target material and Y 2 O 3 Target exchange targeting to obtain a target containing orthorhombic phase (111) and orthorhombic phase (002) with a thickness of 10-25 nm) The YHO film of (1) and the laser energy is 1.8 to 2.2J/cm 2 ；
If the YHO ferroelectric thin film of the orthorhombic phase (002) is grown, the method specifically comprises the following steps:
adjusting the temperature of the substrate to 625-700 ℃; introducing oxygen after the temperature rise is finished, controlling the oxygen pressure to be 0.05-1Pa, ablating the surface of the rotating target material by adopting laser, and carrying out HfO according to the doping amount of Y 2 Target material and Y 2 O 3 Target material exchange and target shooting are carried out to obtain a YHO (002) film with the thickness of 10-25 nm and the laser energy of 1.8-2.2J/cm 2 。
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| 艾婉蕾: "外延Y掺杂HfO2铁电薄膜研究", 中国优秀硕士学位论文全文数据库工程科技Ⅰ辑, 15 April 2024 (2024-04-15) * |
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