CN110165053A - A kind of ALD preparation Hf towards ferroelectric memory application0.5Zr0.5O2The method of ferroelectric thin film - Google Patents
A kind of ALD preparation Hf towards ferroelectric memory application0.5Zr0.5O2The method of ferroelectric thin film Download PDFInfo
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- 239000010409 thin film Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000010408 film Substances 0.000 claims abstract description 41
- 238000000137 annealing Methods 0.000 claims abstract description 32
- 238000000231 atomic layer deposition Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 229910052735 hafnium Inorganic materials 0.000 claims abstract description 10
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims abstract description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 9
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003860 storage Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 229910052681 coesite Inorganic materials 0.000 claims description 21
- 229910052906 cristobalite Inorganic materials 0.000 claims description 21
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 229910052682 stishovite Inorganic materials 0.000 claims description 21
- 229910052905 tridymite Inorganic materials 0.000 claims description 21
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000003990 capacitor Substances 0.000 claims description 12
- 230000005621 ferroelectricity Effects 0.000 claims description 11
- 229910010037 TiAlN Inorganic materials 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 238000000059 patterning Methods 0.000 claims description 8
- 238000000206 photolithography Methods 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 claims description 5
- -1 methylethylamino Chemical group 0.000 claims description 4
- 238000000992 sputter etching Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 2
- 238000004377 microelectronic Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 4
- 229910052742 iron Inorganic materials 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 230000010287 polarization Effects 0.000 abstract description 3
- 230000010354 integration Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 10
- 239000010703 silicon Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000000151 deposition Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000001341 grazing-angle X-ray diffraction Methods 0.000 description 4
- 229910000449 hafnium oxide Inorganic materials 0.000 description 4
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- 230000009471 action Effects 0.000 description 3
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- 238000004321 preservation Methods 0.000 description 3
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
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- 239000013078 crystal Substances 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- INIGCWGJTZDVRY-UHFFFAOYSA-N hafnium zirconium Chemical compound [Zr].[Hf] INIGCWGJTZDVRY-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
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- 238000004528 spin coating Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FIWXUAGPOBLSIJ-UHFFFAOYSA-N [Hf].[Zr].[O] Chemical compound [Hf].[Zr].[O] FIWXUAGPOBLSIJ-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000003032 molecular docking Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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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
- 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
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/405—Oxides of refractory metals or yttrium
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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
- 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
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L28/00—Passive two-terminal components without a potential-jump or surface barrier for integrated circuits; Details thereof; Multistep manufacturing processes therefor
- H01L28/40—Capacitors
- H01L28/55—Capacitors with a dielectric comprising a perovskite structure material
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10B—ELECTRONIC MEMORY DEVICES
- H10B53/00—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory capacitors
- H10B53/30—Ferroelectric RAM [FeRAM] devices comprising ferroelectric memory capacitors characterised by the memory core region
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- Mechanical Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Computer Hardware Design (AREA)
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Abstract
The invention discloses a kind of ALD towards ferroelectric memory application to prepare Hf0.5Zr0.5O2The method of ferroelectric thin film, including technique for atomic layer deposition is used, using hafnium source and zirconium source as precursors, ozone or water as oxygen source, cavity temperature is 250 ~ 280 DEG C, and precursors heating temperature is 75 ~ 80 DEG C, prepares ferroelectric thin film.Ferroelectric thin film prepared by the present invention, compared to the ferroelectric thin film for the perovskite structure that traditional handicraft obtains, it is easier to compatible with standard semiconductor fabrication techniques, integration is high, and Thin-film anneal temperature is low, and annealing rate is high, annealing time is short, ferroelectric layer thickness is small, through the excessively high resulting film of annealing rate heat treatment process, has the excellent properties that remanent polarization is big, dielectric constant is big, leakage current is small.Preparation method repeatability of the present invention is high, and thin-film ferroelectric is uniform, is advantageously implemented ferroelectric thin film in fields broad application prospects such as information storage, integrated circuits.
Description
Technical field
The invention belongs to conductive material technical fields, and in particular to a kind of ALD preparation towards ferroelectric memory application
Hf0.5Zr0.5O2The method of ferroelectric thin film.
Background technique
HfO_2 film is a kind of high dielectric constant (High-K) material, has wide band gap and and CMOS
(Complementary Metal-Oxide-Semiconductor Transistor) technique has preferable compatibility etc. excellent
Point is widely used in preparing dielectric insulation material in microelectronic component.In recent years successively studies have found that this dielectric material
HfO2Ferroelectricity can be generated after adulterating different elements, can be used to prepare hafnium based ferroelectric film.And the Pb of traditional perovskite structure
(Zr,Ti)O3 (PZT)、SrBi2Ta2O9(SBT) etc. ferroelectric thin films, heat treatment leads to ferroelectricity when by film dimensions effect, crystallization
Sexual involution, with gap are narrow, limit the development of ferroelectric memory with factors such as the interface mismatches of Si, so that it faces high system for a long time
Cause the development obstacles of this and low storage density.
At present the technology of preparation method of more mature ferroelectric thin film be mainly also to rely on magnetron sputtering, collosol and gel,
The technologies such as pulse laser deposition.The process that these technologies prepare film is more complicated, inaccurate for the thickness control of film,
And the size of substrate is limited, preparation cost is relatively high, be not suitable for large scale preparation thin-film material, film it is uniform
Property is not good enough, and dielectric properties are undesirable.Traditional ferroelectric material needs certain thickness just to have ferroelectricity, and high temperature is needed to move back
Fire, thermal losses is larger, and the device size made in this way is big, the trend of device microminiaturization is not met, using atomic layer deposition
(ALD) technology prepares ferroelectric thin film, can accurately control the thickness of film, and the shape of large area deposition film, substrate is unrestricted
System.
And hafnium base ferroelectric material is ferroelectric material and the trending selection that semiconductor technology combines, to realize ferroelectricity device
The microminiaturization of part provides may.
Summary of the invention
It is an object of the invention to overcome the problems of the prior art, provide it is a kind of towards ferroelectric memory application
ALD prepares Hf0.5Zr0.5O2The method of ferroelectric thin film.The present invention is based on the hafnium oxide based ferroelectric film ferroelectricities of doping zr element
The induced conversion of phase is studied, and ALD(atomic layer deposition is passed through) technology and high annealing rate heat treatment process, compared with low temperature thermal oxidation
With the hafnium zirconium oxygen ferroelectric thin film for obtaining function admirable in short annealing time.
The purpose of the present invention is achieved by the following technical programs:
A kind of ALD preparation Hf towards ferroelectric memory application0.5Zr0.5O2The method of ferroelectric thin film, including use atomic layer deposition
Product technology, uses hafnium source and zirconium source as precursors, ozone or water as oxygen source, and cavity temperature is 250 ~ 280 DEG C, reaction
Presoma heating temperature is 75 ~ 80 DEG C, and the molar ratio of Hf:Zr is 0.2 ~ 0.8:02 ~ 0.8, prepares ferroelectric thin film, ferroelectric thin film
Molecular formula be HfxZr1-xO2, wherein 0 < x < 1.
First with ALD grow ferroelectric thin film, can ultra-clean chamber integration realize technique docking, while ALD growth
Film, can have preferable compactness and uniformity, and ingredient is uniform.
Film is prepared in vacuum environment ald chamber body, the method has the characteristics that using easy, film thickness is easily controllable, and
And the final thickness of film can be controlled by the cycle period of ALD.
High annealing rate heat treatment process provided by the invention, by being rapidly heated, ultra-short Time heat preservation, Temperature fall
Method is realized compared with low temperature induction of ferroelectricity phase transition and high-speed is annealed, and simplifies preparation process flow and shortens preparation time,
With practical application value.
Preferably, atomic layer deposition processing in, control ferroelectric thin film growth with a thickness of 3 ~ 25nm.
Preferably, hafnium source is four methylethylamino hafniums or four diformazan ammonia hafniums；Zirconium source is four methylethylamino zirconiums or four diformazan ammonia zirconiums.
Present invention simultaneously provides a kind of Si/SiO2The preparation method of the mim structure capacitor of/TiN/HZO/TiN, including such as
Lower step:
S1. it prepares hearth electrode: TiAlN thin film being grown for Ti as target using magnetron sputtering, according to Si/SiO2/ TiN is successively assembled
At the first substrate；
S2. by ferroelectric thin film described in the first substrate over-assemble claim 1, the top growth TiN is carried out according still further to the method for step S1
Electrode obtains Si/SiO2/TiN/HZO/TiN；
S3. high annealing rate heat treatment: by Si/SiO2/ TiN/HZO/TiN is carried out at the high annealing rate heat under nitrogen atmosphere
Reason, 450 ~ 550 DEG C of annealing temperature, the retention time is 20 ~ 60 s；
The Si/SiO is obtained after S4, photolithography patterning and ion etching2The mim structure capacitor of/TiN/HZO/TiN.
Preferably, in step S1, base reservoir temperature is heated to 270 ~ 350 DEG C in magnetron sputtering, and sputtering current is 0.3 ~ 0.35
A first sputters Ti target under argon atmosphere and is cleaned, then passes to nitrogen, Ar/N2Flow-rate ratio is 15:1, is sputtered 5 minutes.
Preferably, Ti is in 8*10-4 TiAlN thin film is grown under the vacuum of Pa.
450 ~ 550 DEG C are carried out to film using quick anneal oven (RTP), the retention time is 20 ~ 60 s, in nitrogen atmosphere
High annealing rate heat treatment is carried out so that the hafnium oxide dielectric film of doping zr element becomes ferroelectric thin film, annealing process master
It is divided into three phases: heats up in nitrogen atmosphere high speed rate, ultra-short Time heat preservation and Temperature fall.
To guarantee that temperature significantly changes in annealing process, so that intermediate ferroelectric film thermally expands, push up
The transformation from dielectric material to ferroelectric material occurs under the stress clamping action of hearth electrode.
The thickness of top electrode and hearth electrode is consistent, and growth conditions is consistent.
The substrate of selection is silicon substrate, has rigidity characteris, is the most common material in semiconductor industry, can be preparation
Ferroelectric memory provides convenience.
Compared with prior art, the present invention has following technical effect that
The silicon chip substrate that the present invention chooses is easy to combine with semiconductor technology, ferroelectric thin film prepared by the present invention, compared to biography
The ferroelectric thin film for the perovskite structure that system technique obtains, size is small, has good ferroelectric properties.At excessively high annealing rate heat
Resulting film is managed, there are the excellent properties that dielectric constant is big, leakage current is small.High annealing rate provided by the invention is heat-treated work
Skill is heated up by high-speed, ultra-short Time heat preservation, the method for Temperature fall, induction of ferroelectricity phase transition, is realized compared with low temperature and fast
Fast annealing simplifies preparation process flow, has practical application value.Preparation process repeatability of the present invention is high, thin-film ferroelectric
Uniformly, it is advantageously implemented and is with a wide range of applications in ferroelectric thin film in fields such as information storage, integrated circuits.
Detailed description of the invention
Fig. 1 is the schematic diagram of long each layer film on Si base substrate.
Fig. 2 is in Si/SiO2Hf is grown with ALD on/TiN substrate0.5Zr0.5O2The AFM phenogram of film.
Fig. 3 is Si/SiO2/TiN/Hf0.5Zr0.5O2Film is after the TiN for depositing a flood in quick anneal oven (RTP) 550
DEG C, the GIXRD phenogram measured after the heat treatment of 30 s high annealing rates.
Fig. 4 is Si/SiO2/TiN/Hf0.5Zr0.5O2/ TiN sample carries out electric leakage performance to sample after photolithography patterning
Measurement.
Fig. 5 is Si/SiO2/TiN/Hf0.5Zr0.5O2/ TiN sample through excessively high annealing rate heat treatment and photolithography patterning at
Ferroelectricity P-V test after reason.
Fig. 6 is Si/SiO2/TiN/Hf0.5Zr0.5O2/ TiN sample through excessively high annealing rate heat treatment and photolithography patterning into
Row C-V (capacitance-voltage) tests obtained curve graph.
Fig. 7 is Si/SiO2/TiN/Hf0.5Zr0.5O2The flow diagram of/TiN progress assembled formation.
Specific embodiment
It to make the object, technical solutions and advantages of the present invention clearer, combined with specific embodiments below will with comparative example
Technical solution of the present invention is described in detail.Obviously, the described embodiment is only a part of the embodiment of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of obtained all other embodiment, belong to the range protected of the present invention.
Except specified otherwise, equipment used in the present embodiment is routine experiment equipment, and reagent used is that analysis is pure
Reagent.
Embodiment 1
As shown in fig. 7, the present invention prepares Si/SiO2The mim structure capacitor method of/TiN/HZO/TiN is as follows:
1. handling substrate: choosing 15 mm15mm has 100 nm SiO2The silicon wafer of layer successively uses acetone, isopropyl as substrate
Alcohol, deionized water are cleaned by ultrasonic 15 minutes, remove surface impurity, are finally dried up with nitrogen gun, toast 5 minutes for 60 degree on hot plate.
2. prepared by hearth electrode: washed substrate is put into magnetron sputtering chamber, Ti(99.995%) it is used as target in 8*10-4
TiAlN thin film is grown under the vacuum of Pa, base reservoir temperature is heated to 350 DEG C, and sputtering current is 0.35 A.First sputtered under argon atmosphere
5 minutes cleaning targets of Ti target, then pass to nitrogen, Ar/N2Flow-rate ratio is 15:1, is sputtered 5 minutes, waiting temperature is down to room temperature
Taking-up multimeter measurement resistance is 45 Ω afterwards.
3. preparing Hf0.5Zr0.5O2(HZO) dielectric layer film: Hf is prepared using technique for atomic layer deposition (ALD)0.5Zr0.5O2
Dielectric layer film, using TDMAHf (four diformazan ammonia hafniums) and TDMAZr (four diformazan ammonia zirconiums) respectively as precursors, ozone
As oxygen source, cavity temperature is 280 DEG C, and the heating temperature of precursor source is 75 DEG C, and it is 1:1(molar ratio that hafnium zirconium, which grows ratio,
Example), 50 circulations are grown, with a thickness of the Hf of 12 nm0.5Zr0.5O2Film.HZO represents Hf in the present invention0.5Zr0.5O2。
Specific preparation process is as follows:
Using technique for atomic layer deposition, the reaction chamber being first passed through gaseous first presoma pulse where the bottom electrode layer,
So that the first presoma is sufficiently adsorbed on bottom electrode layer surface, leads to inert gas later and purged, then oxygen source is with impulse form
Into reaction chamber, is sufficiently reacted with the surface of the first presoma absorption, be passed through inert gas extra ozone and by-product
It takes reaction chamber out of, forms first layer presoma reactive deposition atomic layer in first electrode layer surface；It then will be before gaseous second
It drives body pulse and is passed through above-mentioned reaction chamber, the second presoma is made sufficiently to be adsorbed on the first precursor thin-film layer surface, lead to inertia later
Gas is purged, and oxygen source enters reaction chamber with impulse form, is sufficiently reacted with the surface of the second presoma absorption, then be passed through lazy
Property gas the by-product that extra ozone and reaction generate taken out of reaction chamber, form the in the first precursor thin-film layer surface
The atomic layer of two precursor reactive depositions；Repeat above-mentioned steps, pass through the stacking of hafnium oxide and zirconium oxide atomic layer respectively,
Hf required for preparingxZr1-xO2Film layer.(the first presoma is that perhaps the second presoma of zirconium source is hafnium source or zirconium in hafnium source
Source, 250 ~ 280 DEG C of growth temperature, 75 ~ 80 DEG C of presoma heating temperature.The ratio of hafnium and zirconium is 1:1)
4. preparing top electrode film: by Si/SiO2/TiN/Hf0.5Zr0.5O2Substrate and one piece of clean silicon wafer for carrying out step are put
Enter in sputtering chamber, carries out growth TiAlN thin film according to the method for step 2；TiN uses general thickness range: 10-200 nm may be used
With the thickness of electrode is related with electric conductivity, and too thin thickness electric conductivity is poor.
5. the calibration of thickness of electrode: demarcating the thickness of TiAlN thin film to the silicon wafer for having done step with step instrument；
6. high annealing rate heat treatment: by Si/SiO2/ TiN/HZO/TiN structure sample be put into quick anneal oven (RTP) into
High annealing rate heat treatment under row nitrogen atmosphere, 550 DEG C of annealing temperature, the retention time is 30 s.
7, photolithography patterning and ion etching: sample surfaces spin coating photoresist toasts 1 minute on 90 DEG C of hot plate,
Then it is put into the glass mask plate uv-exposure that alignment on litho machine is printed on circular hole electrode, is subsequently placed in developer solution and develops, and
It is placed in deionized water and cleans, then sample is placed on 115 DEG C of hot plates and is toasted 1 minute.The good sample of photoetching is placed on ion
It is 7*10 in vacuum degree in etching cavity-4 Argon gas is passed through when Pa, setting sample stage rotates, and etches after parameter is arranged to sample
The photoresist of sample surfaces after etching is cleaned up with acetone, obtains Si/SiO by 732 s2The MIM of/TiN/HZO/TiN is tied
Structure capacitor.
Compliance test result:
1, GIXRD is tested: the sample after annealing being carried out GIXRD test, analyzes Hf0.5Zr0.5O2The crystal transfer of film；
Measuring TiN thickness of electrode by step instrument is 60 nm, under room temperature environment, using X-ray diffractometer to high annealing
Treated Hf0.5Zr0.5O2Film carries out GIXRD test, O (200) orthorhombic phase is produced as shown in Figure 3, it can thus be appreciated that quickly
Annealing furnace (RTP) carries out lower 550 DEG C of nitrogen atmosphere, after the high annealing rate heat treatment of 30 s to sample, intermediate Hf0.5Zr0.5O2
Film can induce phase transition, form with ferroelectric orthorhombic phase under the action of TiN cap rock stress clamps.
2, it under room temperature in vacuo environment, is leaked electricity using Agilent B1500 A high-precision semiconductor analyzer to device
Test.This Si/SiO2The capacitor of the mim structure of/TiN/HZO/TiN, in 2.5 V and -2.5 V, leakage current 10-7 The A order of magnitude, while ferroelectricity test is carried out to it using Radiant ferroelectricity analyzer, by loading ± 3 V voltages, obtain it
Corresponding remanent polarization PrFor 17.3224 μ C/cm2, coercive voltage VcFor 1.6057 V, sample is surveyed by impedance analyzer
Examination, the Hf prepared0.5Zr0.5O2Film has the typical butterfly curve of ferroelectric material, it was demonstrated that this method is successfully prepared zirconium
The hafnium oxide base ferroelectric material of doping.
Mim structure shown in FIG. 1 is measurement Hf0.5Zr0.5O2The structure of ferroelectric thin film electric property, wherein hearth electrode and top
Electrode is all TiN electrode, and electrode radius has 20 μm respectively, and 40 μm, 80 μm, 100 μm, the electrode combination of different radii can
With more comprehensively measurement Hf0.5Zr0.5O2Ferroelectric thin film electric property.
Hf in Fig. 20.5Zr0.5O2The surface Root Mean Square roughness RMS of film=555.445 pm, film crystal grain is small, surface
It is smooth and non-porous, be conducive to the growth of latter layer film.
Fig. 4 is Si/SiO2/TiN/Hf0.5Zr0.5O2/ TiN sample carries out electric leakage performance to sample after photolithography patterning
Measurement.
From fig. 4, it can be seen that in the case where voltage is+2.5 V effect, electric current 1.577*10-7A, when voltage is -2.5 V, electric current
For 4.4815*10-7 A, crystalline property is preferable, and defect is less.
See from Fig. 5, Hf0.5Zr0.5O2For film when voltage is added to 3 V, remanent polarization Pr is 17.3224 μ C/
cm2, coercive voltage is 1.6057 V.
See from Fig. 6, at TiN top and bottom electrode clamping action and 550 DEG C, the high annealing rate heat of 30 s nitrogen atmospheres
It after reason, is tested by impedance analyzer, Hf0.5Zr0.5O2The C-V curve of film shows the distinctive butterfly curve of ferroelectric material,
Film is demonstrated with ferroelectricity, and is had excellent performance.
Embodiment 2:
1. handling substrate: choosing 15 mm15 mm are without SiO2Layer the heavily doped silicon wafer of P or N-type as substrate, successively use acetone,
Isopropanol, deionized water are cleaned by ultrasonic 15 minutes, sour with HF with the impurity of the mixed liquor clean the surface of the concentrated sulfuric acid and hydrogen peroxide
Remove the SiO that silicon chip surface is formed2, finally dried up with nitrogen gun, it is dry to be placed in 60 degree of bakings on hot plate；
2. preparing Hf0.5Zr0.5O2(HZO) dielectric layer film: Hf is prepared using technique for atomic layer deposition (ALD)0.5Zr0.5O2Dielectric
Layer film, using TDMAHf (four diformazan ammonia hafniums) and TDMAZr (four diformazan ammonia zirconiums) respectively as precursors, ozone conduct
Oxygen source, cavity temperature are 280 DEG C, and the heating temperature in source is 75 DEG C, and it is 1:1(molar ratio that hafnium zirconium, which grows ratio), grow 50
Circulation, with a thickness of the Hf of 12 nm0.5Zr0.5O2Film.HZO represents Hf in the present invention0.5Zr0.5O2。
3. preparing top electrode film: the clean silicon wafer that p++Si//HZO substrate and one piece carry out step is put into sputtering chamber
It is interior, growth TiAlN thin film is carried out according to the method for step 2；The calibration of thickness of electrode: the silicon wafer for having done step is demarcated with step instrument
The thickness of TiAlN thin film；
4. high annealing rate heat treatment: p++Si/HZO/TiN structure sample being put into quick anneal oven (RTP) and carries out nitrogen atmosphere
Lower high annealing rate heat treatment is enclosed, 550 DEG C of annealing temperature, the retention time is 30 s.
5. photolithography patterning and ion etching: sample surfaces spin coating photoresist toasts 1 minute on 90 DEG C of hot plate,
Then it is put into the glass mask plate uv-exposure that alignment on litho machine is printed on circular hole electrode, is subsequently placed in developer solution and develops, and
It is placed in deionized water and cleans, then sample is placed on 115 DEG C of hot plates and is toasted 1 minute.The good sample of photoetching is placed on ion
It is 7*10 in vacuum degree in etching cavity-4 Argon gas is passed through when Pa, setting sample stage rotates, and etches after parameter is arranged to sample
732 s clean up the photoresist of the sample surfaces after etching with acetone, obtain the mim structure capacitor of p++Si/HZO/TiN
Device.
Hearth electrode: heavy doping silicon wafer or Pt, the metal electrodes such as Au or metal nitride such as TiN electrode
Top electrode: TiN electrode.
Claims (10)
1. a kind of ALD towards ferroelectric memory application prepares Hf0.5Zr0.5O2The method of ferroelectric thin film, which is characterized in that including
Using technique for atomic layer deposition, use hafnium source and zirconium source as precursors, ozone or water as oxygen source, cavity temperature is
250 ~ 280 DEG C, precursors heating temperature is 75 ~ 80 DEG C, and the molar ratio of Hf:Zr is 0.2 ~ 0.8:02 ~ 0.8, prepares iron
Conductive film, the molecular formula of ferroelectric thin film are HfxZr1-xO2, wherein 0 < x < 1.
2. the preparation method for the ferroelectric thin film that can be used for storing according to claim 1, which is characterized in that at atomic layer deposition
In reason, control ferroelectric thin film growth with a thickness of 3 ~ 25nm.
3. a kind of ALD towards ferroelectricity storage application prepares Hf according to claim 10.5Zr0.5O2Ferroelectric thin film, feature
It is, hafnium source is four methylethylamino hafniums or four diformazan ammonia hafniums；Zirconium source is four methylethylamino zirconiums or four diformazan ammonia zirconiums.
4. one kind that the preparation method of any ferroelectric thin film that can be used for storing of claims 1 to 3 is prepared is towards iron
The Hf of electricity storage application0.5Zr0.5O2Ferroelectric thin film.
5. the ferroelectric thin film that can be used for storing described in claim 4 is preparing the application in microelectronic component.
6. a kind of Si/SiO2The preparation method of the mim structure capacitor of/TiN/HZO/TiN, which is characterized in that including walking as follows
It is rapid:
S1. according to Si/SiO2/ TiN is successively assembled into the first substrate；
S2. by ferroelectric thin film described in the first substrate over-assemble claim 1, TiN top electrode is grown on this basis, obtains Si/
SiO2/TiN/HZO/TiN；
S3. high annealing rate heat treatment: by Si/SiO2/ TiN/HZO/TiN is carried out at the high annealing rate heat under nitrogen atmosphere
Reason, 450 ~ 550 DEG C of annealing temperature, the retention time is 20 ~ 60 s；
The Si/SiO is obtained after S4, photolithography patterning and ion etching2The mim structure capacitor of/TiN/HZO/TiN.
7. Si/SiO according to claim 62The preparation method of the mim structure capacitor of/TiN/HZO/TiN, feature exist
In in step S1, using magnetron sputtering using Ti as target growth TiAlN thin film.
8. Si/SiO according to claim 72The preparation method of the mim structure capacitor of/TiN/HZO/TiN, feature exist
In base reservoir temperature is heated to 270 ~ 350 DEG C in magnetron sputtering, and sputtering current is 0.3 ~ 0.35 A, first sputters under argon atmosphere
Ti target is cleaned, and nitrogen, Ar/N are then passed to2Flow-rate ratio is 15:1, is sputtered 5 minutes.
9. Si/SiO according to claim 62The preparation method of the mim structure capacitor of/TiN/HZO/TiN, feature exist
In Ti is in 8*10-4TiAlN thin film is grown under the vacuum of Pa.
10. Si/SiO according to claim 62The preparation method of the mim structure capacitor of/TiN/HZO/TiN, feature exist
In the thickness of TiN is consistent in top electrode TiN and step S1 in step S2, and growth conditions is consistent.
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