CN109979811A - A kind of preparation method of tantalum doping hafnium oxide novel ferroelectric material - Google Patents
A kind of preparation method of tantalum doping hafnium oxide novel ferroelectric material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 29
- 229910000449 hafnium oxide Inorganic materials 0.000 title claims abstract description 13
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 11
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 11
- CJNBYAVZURUTKZ-UHFFFAOYSA-N hafnium(IV) oxide Inorganic materials O=[Hf]=O CJNBYAVZURUTKZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 230000008021 deposition Effects 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 239000010408 film Substances 0.000 abstract description 19
- 239000010409 thin film Substances 0.000 abstract description 17
- 230000005621 ferroelectricity Effects 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 5
- 239000007772 electrode material Substances 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000001259 photo etching Methods 0.000 description 2
- 229920002120 photoresistant polymer Polymers 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000001052 transient effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000005620 antiferroelectricity Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/083—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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
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- H01L29/40—Electrodes ; Multistep manufacturing processes therefor
- H01L29/401—Multistep manufacturing processes
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Abstract
The invention belongs to Material Fields, and in particular to a kind of preparation method of tantalum doping hafnium oxide novel ferroelectric material.Present invention firstly provides donor dopings, to prepare HfO2Ferroelectric thin-flim materials provides a kind of new path；Ta doping HfO is avoided using Pt electrode2Material is reacted with electrode material, and the HfO of alms giver Ta doping is obtained in the way of pulse laser deposition, short annealing etc.2Ferroelectric thin film, it was demonstrated that donor element can also be used for promoting HfO by doping2Film generates ferroelectricity.Donor doping HfO2The realization of ferroelectric thin film can help us to understand doped chemical chemical valence to HfO2The influence of thin-film ferroelectric, to preferably using HfO2Ferroelectric thin film generates positive impetus.
Description
Technical field
The invention belongs to Material Fields, and in particular to a kind of preparation method of tantalum doping hafnium oxide novel ferroelectric material,
Tantalum doping hafnium oxide ferroelectric thin film is prepared with pulse laser (PLD) method, so that preparation has abnormal Dielectric and ferroelectric properties
Novel ferroelectric material.
Background technique
For hafnium oxide as a kind of by numerous studies and the material used, most important purposes is in semicon industry
As high-k dielectric material, as high-g value, dielectric constant is its key parameter, and adulterating is that adjusting dielectric constant is non-usually
With with effective mode.After hafnium oxide in 2011 is found to have ferroelectricity, do not have because having traditional ferroelectric material
Can several nano thickness still have ferroelectricity, with the advantages such as semiconductor technology compatibility have as ferroelectric memory new material and
It is concerned.
And hafnium oxide to be made to generate ferroelectricity, one of them very important mode is exactly to adulterate, and scholars have found to lead to
Overdoping different type, various dose element can make hafnium oxide have different parameters ferroelectricity.But so far
Only oligo-element adulterates HfO2The ferroelectric properties of film is explored, and mainly the acceptor of+2 ,+3 and+4 valence elements or is waited
Valence doping；There are also the chanzas of a great number of elements (whether how can generate ferroelectricity, ferroelectric properties) not to be studied, and adulterates and promote
Make HfO2Film generates that ferroelectric mechanism is not clear, therefore explores and new can make HfO2Film generates ferroelectric doping
Element and the performance for understanding the ferroelectric thin film that it is generated are extremely important, for generating the HfO of different ferroelectric properties2Ferroelectric thin film,
Understand doping and promotes HfO2Film generates ferroelectric mechanism and preferably applies HfO2Ferroelectric thin film has critically important value.
In conclusion doping can make the property of hafnium oxide, great changes will take place, its can be made to generate dielectricity, ferroelectricity
Property, anti-ferroelectricity etc., but adulterate HfO2Thin film study also needs many needs of work to complete.
Summary of the invention
In view of the above problems or insufficient, the present invention provides a kind of tantalum doping hafnium oxide novel ferroelectric materials
Preparation method adulterates HfO based on+5 valence element T a of alms giver2Film realizes thin-film dielectric exception and ferroelectric film preparation side
Method.For HfO2Ferroelectric thin film preparation provides a kind of new route.
Specifically includes the following steps:
Step 1: using pulse laser deposition (PLD) to Ta2O5Target, HfO2The mode that target is alternately practiced shooting is in Pt/Si substrate
Deposit the HfO of 10~25nm thickness Ta doping2Noncrystal membrane mixes the ratio of the target practice number of two targets to control Ta by control
Miscellaneous content obtains the Ta:HfO that doping content is 15~25mol%2Film.
Step 2: in Ta:HfO prepared by step 12The Pt top electrode of 70~90nm thickness is prepared on film.
Step 3: using short annealing RTA technology, the resulting sample of step 2, which is carried out short annealing, makes its crystallization.Using
99.999% nitrogen, air pressure are maintained at 2Torr, are warming up to 600~800 DEG C, keep the temperature 1 minute, the annealing of cooled to room temperature
Condition.
Present invention firstly provides donor dopings, to prepare HfO2Ferroelectric thin-flim materials provides a kind of new path.This
Invention avoids Ta doping HfO using Pt electrode2Material is reacted with electrode material, utilizes pulse laser deposition, short annealing
Etc. modes obtain alms giver Ta doping HfO2Ferroelectric thin film, it was demonstrated that donor element can also be used for promoting HfO by doping2It is thin
Film generates ferroelectricity.Donor doping HfO2The realization of ferroelectric thin film can help us to understand doped chemical chemical valence to HfO2It is thin
The ferroelectric influence of film, to preferably using HfO2Ferroelectric thin film generates positive impetus.
Detailed description of the invention
Fig. 1 is preparation flow figure of the present invention；
Fig. 2 is the XRD spectrum of embodiment；
Fig. 3 is the C-V characteristic map of embodiment；
Fig. 4 is the I-V characteristic map of embodiment；
Fig. 5 is the ferroelectric hysteresis loop characteristic map of embodiment；
Fig. 6 is the transient state IV characteristic map of embodiment；
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and examples.
It is 20nm with film thickness, tantalum content is the ferroelectricity HfO of 15.8mol.%2Film is embodiment in the present invention
Specific steps are described in detail.
Specific steps are as shown in Fig. 1, this process is described in detail in we herein:
Step 1: growing the Ta doping HfO of 20nm in Pt/Si substrate using pulse laser deposition (PLD) technology2Film.
Specifically:
Pt substrate is placed in vacuum chamber above target, target-substrate distance is fixed as 55mm, and substrate temperature is increased to 150 DEG C；
99.999% oxygen is passed through after heating, control oxygen is pressed in 1Pa, wavelength is used to burn for the laser (KrF) of 248nm
Lose the target material surface of rotation, laser energy 2.5J/cm2, carry out HfO2Target and tantalum oxide Ta2O5Target exchange is practiced shooting, wherein
Laser hits HfO2The pulse frequency of target is 5Hz, under strike 50；The pulse frequency of strike oxidation tantalum target is 5Hz, strike 5
Under.So circulation 5 times obtains with a thickness of 20nm, and tantalum content is the amorphous HfO of 15.8mol.%2Film.
Step 2: using sputtering technology, the amorphous made from step 1 mixes the HfO of yttrium2The area of growth 80nm is on film
The Pt top electrode of 25 25 μm of μ ms.Specifically:
To step 1 prepare sample dry 5-10min in 120 DEG C of heating plate, with glue spreader rotation using 1000 turns/
The revolving speed spin coating AZ5216 photoresist of min 10s (prerotation), 3000 turns/min 30s (real-turn), dry in 100 DEG C of heating plate
Dry 60s is dried using contact photoetching machine exposure 1.6s (litho pattern is 25 μ m, 25 μm of squares) in 120 DEG C of heating plates
Dry 90s is cleaning 1min in deionized water then in developing liquid developing 45s with the general exposure 45s of litho machine.
After photoetching, sample is placed in vacuum chamber above target, 99.999% argon gas is passed through, air pressure is maintained at
0.5Pa sputters Ti target 35s using radio-frequency power 100W, grows 2nmTi film as adhesion layer, then arrives air pressure adjustment
1Pa sputters Pt target 8min using dc power 50W, grows 80nmPt electrode.
It has grown and sample is sequentially placed into acetone, alcohol, deionized water after Pt electrode, sample has been removed.It will exposure
Photoresist, Ti, the Pt in area are removed, and the Pt top electrode for 25 μm of 25 μ m is obtained.
Step 3: using short annealing RTA technology, sample obtained in step 2 is placed in quick anneal oven, is passed through
99.999% nitrogen, air pressure are maintained at 2Torr, and 30s is warming up to 600 DEG C, keep the temperature 1 minute, cooled to room temperature.Take out sample
Product obtain having ferroelectric polycrystalline HfO2Film.
To HfO made from embodiment2Ferroelectric material carries out structure and electrical testing.
HfO obtained2The XRD of metal-dielectric-metal (MIM) structure test results are shown in figure 2.It can be with from Fig. 2
Find out, HfO obtained2Film crystallizes, and 31 ° or so of peak value should be with ferroelectric orthorhombic phase, electricity below
Film occurs for characteristic, and there is ferroelectricity to demonstrate this point.
HfO obtained2Mim structure C-V characteristic test result it is as shown in Figure 3.From figure 3, it can be seen that the material
Polarizability and application electric field are not linear relationships, produce the butterfly shape C-V curve of ferroelectric material.
HfO obtained2The I-V characteristic of mim structure test results are shown in figure 4.Polarization reversal electricity from being marked 1. from Fig. 4
The material known to stream is ferroelectric material.
HfO obtained2Mim structure ferroelectric hysteresis loop characteristic test result it is as shown in Figure 5.From figure 5 it can be seen that should
The ferroelectric hysteresis loop of material indicates that the material should be the biggish ferroelectric material of electric leakage.
HfO obtained2Mim structure transient state IV curve it is as shown in Figure 6.2. partial polarization reverse current is marked from Fig. 6
Know that the material is ferroelectric material.
By above-mentioned test it can be proved that Ta prepared by the present invention adulterates HfO2Material is ferroelectric material, has tradition HfO2
The abnormal Dielectric and ferroelectric properties that dielectric material does not have.It can be used for memory, ferroelectricity logical device etc.；And it is first to doping is understood
Plain chemical valence is to HfO2The influence of thin-film ferroelectric, preferably to apply HfO2Ferroelectric thin film generates positive impetus.
Claims (2)
1. a kind of preparation method of tantalum doping hafnium oxide novel ferroelectric material, comprising the following steps:
Step 1: using pulse laser deposition PLD to Ta2O5Target, HfO2The mode that target is alternately practiced shooting deposits 10 in Pt/Si substrate
The HfO of~25nm thickness Ta doping2Noncrystal membrane controls Ta doping by controlling the ratio to the target practice number of two targets and contains
Amount obtains the Ta:HfO that doping content is 15~25mol%2Film；
Step 2: in Ta:HfO prepared by step 12The Pt top electrode of 70~90nm thickness is prepared on film；
Step 3: using short annealing RTA technology, the resulting sample of step 2, which is carried out short annealing, makes its crystallization.
2. the preparation method of tantalum doping hafnium oxide novel ferroelectric material as described in claim 1, it is characterised in that: described quick
Annealing uses 99.999% nitrogen, and air pressure is maintained at 2Torr, is warming up to 600~800 DEG C, keeps the temperature 1 minute, naturally cools to room
The annealing conditions of temperature.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106463513A (en) * | 2014-05-20 | 2017-02-22 | 美光科技公司 | Polar, chiral, and non-centro-symmetric ferroelectric materials, memory cells including such materials, and related devices and methods |
| US20170103988A1 (en) * | 2015-10-09 | 2017-04-13 | University Of Florida Research Foundation, Inc. | Doped ferroelectric hafnium oxide film devices |
| US20180331113A1 (en) * | 2017-05-09 | 2018-11-15 | Micron Technology, Inc. | Semiconductor structures, memory cells and devices comprising ferroelectric materials, systems including same, and related methods |
| CN109100900A (en) * | 2018-07-23 | 2018-12-28 | 电子科技大学 | A kind of HfO2The application method of base ferroelectric material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106463513A (en) * | 2014-05-20 | 2017-02-22 | 美光科技公司 | Polar, chiral, and non-centro-symmetric ferroelectric materials, memory cells including such materials, and related devices and methods |
| US20170103988A1 (en) * | 2015-10-09 | 2017-04-13 | University Of Florida Research Foundation, Inc. | Doped ferroelectric hafnium oxide film devices |
| US20180331113A1 (en) * | 2017-05-09 | 2018-11-15 | Micron Technology, Inc. | Semiconductor structures, memory cells and devices comprising ferroelectric materials, systems including same, and related methods |
| CN109100900A (en) * | 2018-07-23 | 2018-12-28 | 电子科技大学 | A kind of HfO2The application method of base ferroelectric material |
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