CN111945133A - Method for improving performance of hafnium-based ferroelectric film and application - Google Patents
Method for improving performance of hafnium-based ferroelectric film and application Download PDFInfo
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- 229910052735 hafnium Inorganic materials 0.000 title claims abstract description 80
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000000151 deposition Methods 0.000 claims abstract description 49
- 239000000758 substrate Substances 0.000 claims abstract description 36
- 238000000137 annealing Methods 0.000 claims abstract description 19
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- QQIUEZPRJAABMK-UHFFFAOYSA-N hafnium(4+) oxygen(2-) zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4].[Hf+4] QQIUEZPRJAABMK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 239000010409 thin film Substances 0.000 claims description 55
- 239000010408 film Substances 0.000 claims description 54
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 42
- 230000008021 deposition Effects 0.000 claims description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 12
- 229910052737 gold Inorganic materials 0.000 claims description 12
- 239000010931 gold Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000003990 capacitor Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- DWCMDRNGBIZOQL-UHFFFAOYSA-N dimethylazanide;zirconium(4+) Chemical compound [Zr+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C DWCMDRNGBIZOQL-UHFFFAOYSA-N 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 238000002207 thermal evaporation Methods 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 17
- 230000010287 polarization Effects 0.000 abstract description 8
- 241001391944 Commicarpus scandens Species 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 description 17
- 230000005621 ferroelectricity Effects 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 229910000449 hafnium oxide Inorganic materials 0.000 description 6
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- ZYLGGWPMIDHSEZ-UHFFFAOYSA-N dimethylazanide;hafnium(4+) Chemical compound [Hf+4].C[N-]C.C[N-]C.C[N-]C.C[N-]C ZYLGGWPMIDHSEZ-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000007664 blowing Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- 238000004151 rapid thermal annealing Methods 0.000 description 4
- 239000012495 reaction gas Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000013077 target material Substances 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 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 3
- 230000007423 decrease Effects 0.000 description 3
- 230000027311 M phase Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000005669 field effect Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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Abstract
The invention belongs to the technical field of ferroelectric film materials, and discloses a method for improving the performance of a hafnium-based ferroelectric film, which comprises the following steps: (1) growing a TiN bottom electrode on the cleaned substrate; (2) depositing a hafnium oxide-zirconium oxide film on the TiN bottom electrode by an atomic deposition method; (3) depositing a zirconium oxide cover layer on the hafnium oxide-zirconium oxide film; (4) and (5) annealing.The method for improving the hafnium-based ferroelectric film by depositing the zirconium oxide cover layer on the atomic layer is accurate in control, and the formed film is good in uniformity and beneficial to large-area production. The zirconium oxide is adopted as the cover layer, so that the proportion of non-ferroelectric phase in the hafnium-based ferroelectric film is obviously reduced, the proportion of orthorhombic phase is improved, the remanent polarization value is doubled, meanwhile, the leakage current of the film is reduced, the film is not easy to break down, the reliability of the film is improved, and the ratio is 104After s the residual polarization still remains 85% of the initial value.
Description
Technical Field
The invention relates to the technical field of ferroelectric film materials, in particular to a method for improving the performance of a hafnium-based ferroelectric film and application thereof.
Background
The ferroelectric thin film material is an important material of a memory device, and particularly, during the last 5 to 10 years, the ferroelectric thin film material has been greatly developed in a plurality of application fields, such as a ferroelectric field effect transistor (FeFET), a ferroelectric random access memory (FeRAM), a Tunnel Field Effect Transistor (TFET), a resistive random access memory (ReRAM), and the like.
In 2011, people find ferroelectricity in a hafnium oxide thin film material for the first time, compared with traditional ferroelectric materials such as lead zirconate titanate and barium titanate, the hafnium-based ferroelectric material is compatible with a silicon-based semiconductor technology which is mainstream in an integrated circuit at present, the problem that the size of a traditional ferroelectric material memory cannot be further reduced is overcome due to outstanding miniaturization capability, and a preparation method mainly based on an atomic layer deposition technology is easy for large-scale production, so that the hafnium-based ferroelectric material has been widely concerned by academic circles and social industries since the discovery.
Under normal temperature and pressure, the bulk hafnium oxide material is a monoclinic phase without ferroelectricity, a hafnium-based ferroelectric film with a ferroelectric phase can be obtained by methods of element doping, stress action, high-temperature annealing, film thickness control and the like, and a phenomenon that a non-ferroelectric phase and a ferroelectric phase coexist commonly exists in the hafnium-based ferroelectric film, and meanwhile, the phases are transformed. Therefore, hafnium-based ferroelectric thin films have some problems to be solved: (1) the non-ferroelectric phase reduces the remanent polarization of the ferroelectric thin film; (2) the non-ferroelectric phase can increase the electric leakage of the film, so that the film is easy to break down and fail; (3) under the action of an electric field, an unstable ferroelectric phase in the film can be converted into a non-ferroelectric phase, and the service life of the film is influenced. For the purpose of improving the performance of the hafnium-based ferroelectric thin film and further application, reducing the proportion of non-ferroelectric phase in the hafnium-based ferroelectric thin film is a great challenge in academia and industry.
Disclosure of Invention
The invention aims to overcome the defect of high proportion of non-ferroelectric phase in the hafnium-based ferroelectric film in the prior art, and firstly provides a method for improving the performance of the hafnium-based ferroelectric film.
The second purpose of the invention is to provide the hafnium-based ferroelectric thin film material obtained by the method.
The third purpose of the invention is to provide the application of the ferroelectric thin film material.
The purpose of the invention is realized by the following technical scheme:
the invention firstly provides a method for improving the performance of a hafnium-based ferroelectric film, which comprises the following steps:
(1) growing a TiN bottom electrode on the cleaned substrate;
(2) depositing a hafnium oxide-zirconium oxide film on the TiN bottom electrode by an atomic deposition method;
(3) depositing a zirconium oxide cover layer on the hafnium oxide-zirconium oxide film;
(4) and (5) annealing.
Hafnium oxide (HfO)2) The crystal is a fluorite structure, the crystal structure is a monoclinic phase at normal temperature and normal pressure, the monoclinic phase can be converted into a tetragonal phase or a cubic phase with higher symmetry at high temperature, and the structures do not have ferroelectricity. In 2011, a hafnium-based ferroelectric thin film material having ferroelectricity, which is considered to occur as a metastable orthorhombic phase having asymmetry, was obtained by doping silicon element in hafnium oxide, and was verified both theoretically and experimentally.
The invention utilizes the stress action, and a layer of zirconia cover layer is added on the ferroelectric film, thereby greatly reducing the non-ferroelectric proportion of the hafnium-based ferroelectric film.
Since the bulk hafnium oxide is monoclinic, the monoclinic phase ratio in HZO gradually increases with the increase in thickness, resulting in a decrease in the ratio of orthorhombic phase, and thus in a decrease in ferroelectricity. According to the surface energy model, as the thickness is reduced, the formed stable phase is changed from the orthogonal phase to the tetragonal phase, and meanwhile, the ratio of the surface oxygen-deficient interface to the thickness is increased as the thickness is reduced, so that the transition from the orthogonal phase to the tetragonal phase is caused, and therefore, the optimization of the thickness of the HZO is an important method for obtaining the ferroelectricity of the HZO.
According to the method for improving the performance of the hafnium-based ferroelectric film, the thickness of the zirconia cover layer in the step (3) is 0.5-2 nm.
Preferably, the method for improving the performance of the hafnium-based ferroelectric thin film comprises the following operation in step (3): using tetra (dimethylamino) hafnium as hafnium source, tetra (dimethylamino) zirconium as zirconium source, O3Alternately depositing 19-94 cycles as an oxidant to obtain Hf: zr is 0.5-2: 1 the hafnium-based ferroelectric thin film.
Preferably, in the method for improving the performance of the hafnium-based ferroelectric thin film, the annealing operation in the step (4) is: and putting the film into a rapid annealing furnace, rapidly heating to 400-700 ℃, annealing in an inert gas atmosphere for 30-90 s, and cooling to room temperature.
The invention also provides the hafnium-based ferroelectric film obtained by the method.
The invention also provides a film capacitor containing the hafnium-based ferroelectric film.
The invention also provides a preparation method of the film capacitor, which comprises the following steps: and respectively depositing a nickel electrode and a gold electrode on the prepared hafnium-based ferroelectric film to obtain the film capacitor.
More preferably, the method for preparing the thin film capacitor comprises the steps of firstly depositing nickel as an intermediate layer and then depositing gold as a top electrode on the hafnium-based ferroelectric thin film by using a vacuum thermal evaporation technology, wherein the deposition rate is 0.02nm/s, the deposition is carried out under high vacuum, and the air pressure is 8 x 10 < -4 > Pa.
Compared with the prior art, the invention has the following beneficial effects:
the invention firstly provides a method for improving the performance of a hafnium-based ferroelectric film, which comprises the following steps: (1) growing a TiN bottom electrode on the cleaned substrate; (2) depositing a hafnium oxide-zirconium oxide film on the TiN bottom electrode by an atomic deposition method; (3) depositing a zirconium oxide cover layer on the hafnium oxide-zirconium oxide film; (4) and (5) annealing. The method for improving the hafnium-based ferroelectric film by depositing the zirconium oxide cover layer by the atomic layer is accurate in control, and the formed film is good in uniformity and beneficial to large-area production.
The zirconium oxide is adopted as the cover layer, so that the proportion of non-ferroelectric phase in the hafnium-based ferroelectric film is obviously reduced, the proportion of orthorhombic phase is improved, the remanent polarization value is doubled, meanwhile, the leakage current of the film is reduced, the film is not easy to break down, the reliability of the film is improved, and the ratio is 104After s the residual polarization still remains 85% of the initial value.
Drawings
FIG. 1 is a schematic structural diagram of a hafnium-based ferroelectric thin film capacitor with a zirconium oxide cap layer according to the present invention;
FIG. 2 is a low angle diffraction pattern of zirconia as a capping layer and an uncapping layer;
FIG. 3 is a P-V plot of zirconia as a capping layer and an uncapping layer;
FIG. 4 is a graph comparing leakage current density for zirconia as a capping layer and an uncapping layer;
FIG. 5 is a graph comparing retention times of zirconia as a capping layer and no capping layer;
FIG. 6 is a graph showing the effect of the thickness of a zirconia capping layer on the ferroelectricity of a hafnium-based ferroelectric thin film.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The test methods used in the following experimental examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are, unless otherwise specified, commercially available reagents and materials.
Example 1
A method for improving the performance of a hafnium-based ferroelectric thin film comprises the following steps:
(1) preparation of the substrate: selecting N <100> silicon, manufacturing a square slice with the size of 15mm multiplied by 15mm as a substrate, carrying out ultrasonic cleaning on the substrate, putting the substrate into acetone, isopropanol, deionized water and absolute ethyl alcohol for cleaning once to remove impurities such as organic matters on the surface, and then blowing the substrate with nitrogen to dry to ensure that the surface of the substrate is clean;
(2) preparation of bottom electrode: heating the substrate to 280 ℃, using Ti as a target material and N2Performing sputtering deposition under the power of 75W by using Ar as a reaction gas and a protective gas to obtain a TiN bottom electrode with the thickness of about 50 nm;
(3) preparation of hafnium-based thin films: placing into an atomic deposition chamber, heating the substrate to 280 deg.C, using tetrakis (dimethylamino) hafnium as the hafnium source, tetrakis (dimethylamino) zirconium as the zirconium source, and O3Alternate deposition of 20cycles as an oxidizing agent, yielding Hf: zr is 0.5: 1 a hafnium-based ferroelectric thin film having a thickness of about 20 nm;
(4) preparation of zirconia cap layer: depositing a 5cycles zirconia cover layer (with the thickness of 0.5nm) on the hafnium-based film by using the existing hafnium source oxygen source and keeping the temperature unchanged;
(5) annealing: the film deposited with the zirconia cover layer is put into a rapid thermal annealing furnace (RTP), the temperature is raised to 400 ℃ through fast reading, annealing is carried out for 60s under the protection of high-purity nitrogen atmosphere, and then cooling is carried out to the room temperature;
(6) preparing a top electrode: by using vacuum thermal evaporation and evaporation technology, depositing 3mm of nickel on the prepared film as an intermediate layer to increase the adhesion of a gold electrode, depositing 50nm of gold as a top electrode, controlling the deposition rate at 0.02nm/s, and performing deposition under vacuum at a pressure of 8 × 10-4Pa。
Example 2
A method for improving the performance of a hafnium-based ferroelectric thin film comprises the following steps:
(1) preparation of the substrate: selecting N <100> silicon, manufacturing a square slice with the size of 15mm multiplied by 15mm as a substrate, carrying out ultrasonic cleaning on the substrate, putting the substrate into acetone, isopropanol, deionized water and absolute ethyl alcohol for cleaning once to remove impurities such as organic matters on the surface, and then blowing the substrate with nitrogen to dry to ensure that the surface of the substrate is clean;
(2) preparation of bottom electrode: heating the substrate to 280 ℃, using Ti as a target material and N2Performing sputtering deposition under the power of 75W by using Ar as a reaction gas and a protective gas to obtain a TiN bottom electrode with the thickness of about 50 nm;
(3) preparation of hafnium-based thin films: placing into an atomic deposition chamber, heating the substrate to 280 deg.C, using tetrakis (dimethylamino) hafnium as the hafnium source, tetrakis (dimethylamino) zirconium as the zirconium source, and O3As an oxidizing agent, 75cycles were deposited alternately, yielding Hf: zr 1: 1 a hafnium-based ferroelectric thin film having a thickness of about 20 nm;
(4) preparation of zirconia cap layer: depositing a 10cycles zirconia cover layer (with the thickness of 1nm) on the hafnium-based film by using the existing hafnium source oxygen source and keeping the temperature unchanged;
(5) annealing: placing the film deposited with the zirconia cover layer into a rapid thermal annealing furnace (RTP), raising the temperature to 550 ℃ by fast reading, annealing for 30s under the protection of high-purity nitrogen atmosphere, and cooling to room temperature;
(6) preparing a top electrode: by using vacuum thermal evaporation and evaporation technology, depositing 3mm of nickel on the prepared film as an intermediate layer to increase the adhesion of a gold electrode, depositing 50nm of gold as a top electrode, controlling the deposition rate at 0.02nm/s, and performing deposition under vacuum at a pressure of 8 × 10-4Pa。
Example 3
A method for improving the performance of a hafnium-based ferroelectric thin film comprises the following steps:
(1) preparation of the substrate: selecting N <100> silicon, manufacturing a square slice with the size of 15mm multiplied by 15mm as a substrate, carrying out ultrasonic cleaning on the substrate, putting the substrate into acetone, isopropanol, deionized water and absolute ethyl alcohol for cleaning once to remove impurities such as organic matters on the surface, and then blowing the substrate with nitrogen to dry to ensure that the surface of the substrate is clean;
(2) preparation of bottom electrode: heating the substrate to 280 ℃, using Ti as a target material and N2Performing sputtering deposition under the power of 75W by using Ar as a reaction gas and a protective gas to obtain a TiN bottom electrode with the thickness of about 50 nm;
(3) preparation of hafnium-based thin films: placing into an atomic deposition chamber, heating the substrate to 280 deg.C, using tetrakis (dimethylamino) hafnium as the hafnium source, tetrakis (dimethylamino) zirconium as the zirconium source, and O394cycles were deposited alternately as an oxidizing agent, yielding Hf: zr is 2: 1 a hafnium-based ferroelectric thin film having a thickness of about 20 nm;
(4) preparation of zirconia cap layer: depositing a 20cycles zirconia cover layer (with the thickness of 2nm) on the hafnium-based film by using the existing hafnium source oxygen source and keeping the temperature unchanged;
(5) annealing: the film deposited with the zirconia cover layer is put into a rapid thermal annealing furnace (RTP), the temperature is raised to 700 ℃ through fast reading, annealing is carried out for 90s under the protection of high-purity nitrogen atmosphere, and then cooling is carried out to the room temperature;
(6) preparing a top electrode: by using vacuum thermal evaporation and evaporation technology, depositing 3mm of nickel on the prepared film as an intermediate layer to increase the adhesion of a gold electrode, depositing 50nm of gold as a top electrode, controlling the deposition rate at 0.02nm/s, and performing deposition under vacuum at a pressure of 8 × 10-4Pa。
Comparative example 1
A method for improving the performance of a hafnium-based ferroelectric thin film comprises the following steps:
(1) preparation of the substrate: selecting N <100> silicon, manufacturing a square slice with the size of 15mm multiplied by 15mm as a substrate, carrying out ultrasonic cleaning on the substrate, putting the substrate into acetone, isopropanol, deionized water and absolute ethyl alcohol for cleaning once to remove impurities such as organic matters on the surface, and then blowing the substrate with nitrogen to dry to ensure that the surface of the substrate is clean;
(2) preparation of bottom electrode: heating the substrate to 280 ℃, using Ti as a target material and N2Performing sputtering deposition under the power of 75W by using Ar as a reaction gas and a protective gas to obtain a TiN bottom electrode with the thickness of about 50 nm;
(3) preparation of hafnium-based thin films: placing into an atomic deposition chamber, heating the substrate to 280 deg.C, using tetrakis (dimethylamino) hafnium as the hafnium source, tetrakis (dimethylamino) zirconium as the zirconium source, and O3As an oxidizing agent, 75cycles were deposited alternately, yielding Hf: zr 1: 1 a hafnium-based ferroelectric thin film having a thickness of about 20 nm;
(4) annealing: putting the hafnium-based ferroelectric film into a rapid thermal annealing furnace (RTP), raising the temperature to 550 ℃ by fast reading, annealing for 30s under the protection of high-purity nitrogen atmosphere, and cooling to room temperature;
(5) preparing a top electrode: by using vacuum thermal evaporation and evaporation technology, 3mm of nickel is firstly deposited on the prepared film to be used as an intermediate layer, so that the adhesion of a gold electrode is increasedDepositing 50nm gold as top electrode at 0.02nm/s under vacuum pressure of 8 × 10-4Pa。
Diffraction was performed on the hafnium-based ferroelectric thin films prepared in examples 1 to 3 and comparative example 1, and the results are shown in fig. 2, and 4 curves from bottom to top in fig. 2: the m-phase peak intensity at 28.6 ° and the o-phase peak intensity change at 30.6 ° see: the hafnium-based ferroelectric thin film having a zirconium oxide cap layer has a strength of an orthorhombic phase gradually increased and a strength of a monoclinic phase significantly decreased as the thickness of the hafnium oxide cap layer is increased from 0nm to 2 nm. The non-ferroelectric m phase gradually decreased and the ferroelectric o phase gradually increased, indicating that the hafnium-based ferroelectric thin film with the zirconia capping layer has less non-ferroelectric phase and more ferroelectric phase.
As can be seen from fig. 3: the proportion of monoclinic phase decreases continuously and reaches a state of saturation at 1 nm. This is sufficient to show that the monoclinic phase in HZO is significantly suppressed and the proportion of the orthorhombic phase is significantly enhanced by the zirconia cap layer, i.e., good ferroelectricity can be obtained by the cap layer.
The P-V of the hafnium-based ferroelectric thin film prepared in example 2 is shown in FIG. 4, the magnitude of remanent polarization 2Pr can be generally used to represent the ferroelectric strength of the hafnium-based ferroelectric thin film, and it can be seen from FIG. 4 that the uncapped hafnium-based ferroelectric thin film 2Pr has only 20.5 μ C/cm at + -6 scan voltages2And the 2Pr of the hafnium-based ferroelectric film with the capping layer reaches 44.7 mu C/cm2The addition is doubled, and the fact that the ferroelectricity of the hafnium-based ferroelectric film can be greatly improved by taking the zirconium oxide as the cover layer is proved, and the ferroelectricity performance of the film is improved.
The leakage current density of the hafnium-based ferroelectric thin film prepared in example 2 is shown in fig. 5, and it can be seen that the thin film with the zirconia capping layer has smaller leakage current than the thin film without the capping layer, on one hand, the physical thickness of the thin film with the capping layer is increased, and the leakage current is reduced, on the other hand, the non-ferroelectric phase in the thin film with the capping layer is less, and the non-ferroelectric phase is more likely to cause leakage current than the ferroelectric phase, so that the hafnium-based ferroelectric thin film using zirconia as the capping layer can effectively reduce the leakage current of the thin film, and improve the leakage performance of.
FIG. 6 shows the retention time of the hafnium-based ferroelectric thin film prepared in example 2, which is an important reference index for the reliability of a memory, and the remanent polarization value P is measured after turning over the ferroelectric material0After a plurality of times, measuring the residual polarization value PsThrough Ps/P0To measure the reliability of the memory, it can be seen that the hafnium-based ferroelectric thin film without the cap layer is 104s is only 50% of the initial value, and the hafnium-based ferroelectric thin film with zirconium oxide as the cover layer is 104s is 85% of the initial value, so that the hafnium-based ferroelectric thin film using zirconium oxide as the capping layer has better reliability.
It will be appreciated by those skilled in the art that the use of the present invention is not limited to the specific applications described above. The invention is also not limited to the preferred embodiments thereof with respect to the specific elements and/or features described or depicted herein. It should be understood that the invention is not limited to the disclosed embodiment or embodiments, but is capable of numerous rearrangements, modifications and substitutions without departing from the scope of the invention as set forth and defined by the following claims.
Claims (8)
1. A method for improving the performance of a hafnium-based ferroelectric film is characterized by comprising the following steps:
(1) growing a TiN bottom electrode on the cleaned substrate;
(2) depositing a hafnium oxide-zirconium oxide film on the TiN bottom electrode by an atomic deposition method;
(3) depositing a zirconium oxide cover layer on the hafnium oxide-zirconium oxide film;
(4) and (5) annealing.
2. The method of claim 1, wherein the thickness of the zirconia cap layer in step (3) is 0.5-2 nm.
3. The method for improving the performance of a hafnium-based ferroelectric thin film as claimed in claim 1, wherein the operation of step (3) is: with tetra (dimethylamine)Based) hafnium as a source of hafnium, tetrakis (dimethylamino) zirconium as a source of zirconium, O3Alternately depositing 19-94 cycles as an oxidant to obtain Hf: zr is 0.5-2: 1 the hafnium-based ferroelectric thin film.
4. The method for improving the performance of a hafnium-based ferroelectric thin film as claimed in claim 1, wherein the annealing operation of step (4) is: and putting the film into a rapid annealing furnace, rapidly heating to 400-700 ℃, annealing in an inert gas atmosphere for 30-90 s, and cooling to room temperature.
5. A hafnium-based ferroelectric thin film obtained by the method of any one of claims 1 to 4.
6. A thin film capacitor comprising the hafnium-based ferroelectric thin film as claimed in claim 5.
7. The method for producing a thin film capacitor as claimed in claim 6, comprising the steps of: and respectively depositing a nickel electrode and a gold electrode on the prepared hafnium-based ferroelectric film to obtain the film capacitor.
8. The method for manufacturing a thin film capacitor as claimed in claim 7, wherein the deposition is performed under high vacuum at a pressure of 8 x 10 by depositing nickel as an intermediate layer and gold as a top electrode on the hafnium-based ferroelectric thin film by vacuum thermal evaporation and evaporation at a deposition rate of 0.02nm/s-4Pa。
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| CN114927526A (en) * | 2022-06-02 | 2022-08-19 | 北京超弦存储器研究院 | Ferroelectric memory, ferroelectric capacitor and preparation method thereof |
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| CN113178478A (en) * | 2021-03-15 | 2021-07-27 | 中国科学院微电子研究所 | Ferroelectric film and deposition method and application thereof |
| CN113363384A (en) * | 2021-06-06 | 2021-09-07 | 复旦大学 | HfO2Ferroelectric tunnel junction device and method for manufacturing the same |
| CN113363384B (en) * | 2021-06-06 | 2022-11-18 | 复旦大学 | HfO 2 Ferroelectric tunnel junction device and method for manufacturing the same |
| CN113668062A (en) * | 2021-08-20 | 2021-11-19 | 湘潭大学 | Orthorhombic phase hafnium oxide based ferroelectric film and preparation method and application thereof |
| CN114864558A (en) * | 2022-05-06 | 2022-08-05 | 西安电子科技大学 | Preparation process of hafnium oxide based ferroelectric film |
| CN114927526A (en) * | 2022-06-02 | 2022-08-19 | 北京超弦存储器研究院 | Ferroelectric memory, ferroelectric capacitor and preparation method thereof |
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| CN114990530B (en) * | 2022-06-02 | 2024-06-07 | 华东师范大学 | Method for preparing HZO ferroelectric film at low temperature and HZO ferroelectric film |
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| CN115261788B (en) * | 2022-09-07 | 2023-04-18 | 宁波大学 | Improve HfO 2 Method for ferroelectricity |
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