CN102194685A - Method for regulating energy band compensation between Ge substrate and TixAlyO film - Google Patents
Method for regulating energy band compensation between Ge substrate and TixAlyO film Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000001105 regulatory effect Effects 0.000 title abstract description 6
- 238000000151 deposition Methods 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 230000008021 deposition Effects 0.000 claims abstract description 20
- 238000000137 annealing Methods 0.000 claims abstract description 12
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 27
- 229910052732 germanium Inorganic materials 0.000 claims description 26
- 239000010408 film Substances 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 16
- 239000002184 metal Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000005137 deposition process Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 6
- 239000010409 thin film Substances 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- 230000033228 biological regulation Effects 0.000 claims description 3
- 239000004065 semiconductor Substances 0.000 abstract description 10
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 3
- 229910052593 corundum Inorganic materials 0.000 abstract 3
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Abstract
The invention discloses a method for regulating energy band compensation between a Ge substrate and a TixAlyO film, comprising the steps of: cleaning and drying the Ge substrate; putting the Ge substrate in an ALD (Atom Layer Deposition) reaction chamber to deposit with Al2O3 as a beginning layer by alternating the deposition circulation of Al2O3 and TiO2, wherein the mol ratio of Al to Ti in a finally deposited film is 1: (1.2-4.5); and annealing the Ge substrate deposited with the film to obtain a finished product. In the method, when the ratio of Al to Ti is decreased, the accumulated capacitance is increased; and the leakage current is increased. Along with the increment of the ratio of Al to Ti, the valence band and conduction band compensations of Al2O3/TiO2 on Ge and the band gaps are increased synchronously. These results show that the ALDAl2O3/TiO2 nanometre lamination structure can be used for effectively regulating the interface quality and the energy band structure between the grid medium and the Ge so as to modify the working performance of the MOS (Metal Oxide Semiconductor) device. The method has important application foreground in the Ge-based MOSFET (Metal-Oxide -Semiconductor Field Effect Transistor) preparation.
Description
Technical field
The present invention relates to technique for atomic layer deposition, specifically is to regulate the method that can be with skew between gate medium TixAlyO film and the substrate Ge in the preparation process of Ge base MOSFET device.
Background technology
High
kMaterial has been obtained many progress in the research in traditional si-substrate integrated circuit field, but faces the physics of a series of sternnesses and the challenge of technical problem.One of them main chronic illness is exactly high
kThe introducing of gate medium and metal gate material, when reducing the high power consumption of small scale complementary CMOS device, also bring the deterioration at channel material/gate dielectric material interface, owing to reasons such as Coulomb scattering, phon scatterings, cause the obvious decline of channel mobility, greatly affected the raising of CMOS logical device speed.So, adopt novel semiconductor channel material such as Ge and GaAs to replace traditional Si material to become another attractive solution of preparation high-performance New-type CMOS device with high mobility.Compare with silicon, Ge has higher electronics and hole mobility, low doping activationary temperature.In history, Ge once was one of most important semiconductor, and first transistor of success making and first integrated circuit all are that preparation is on the Ge semiconductor chip in the world.
Along with semiconductor process techniques continue to advance, the key of person's technology that the lifting of constantly the dwindling of chip size and live width, function becomes the semiconductor manufacturing industry wherein day by day raises for the thickness evenness of thin-film technique and the requirement of quality.Atomic layer deposition (ALD) is the gas-solid phase reaction that utilizes between reacting gas and the substrate, finishes the demand of technology, owing to can finish the higher technology of precision, therefore is regarded as one of development key link of sophisticated semiconductor technology.Its cardinal principle is that reaction chambers are injected in two kinds of vapor precursor ALT pulses, between by the inert gas exhaust, rear a kind of precursor generates the solid phase film with the front a kind of reaction that is adsorbed on the surface.ALD has from restriction (Self-limiting) self-saturating characteristics, and excellent three-dimensional stickiness (conformality) and large-area uniformity; Accurately, simple film thickness monitoring (only relevant) with the reaction cycle number of times; (RT-400 for low depositing temperature
oC); Low deposition rate (1-2nm/min).It does the many group members' that are fit to modifying interface and preparation nanoscale layer structure (Nanlaminates) especially.
Many oxides such as HfO
2, ZrO
2, Al
2O
3Deng just being studied widely as candidate's semi-conducting material.But they all can not satisfy replacement SiO fully
2Requirement.TiO
2Have very high dielectric constant (k=80), but because TiO
2Can be with too little (3.5 eV), and crystallization temperature also lower (400
oC); And Al
2O
3Has bigger energy gap (8.8 eV), higher crystallization temperature.For this reason, the applicant adopts ald in conjunction with these two kinds of oxides advantage separately, has successfully deposited the Ti-Al-O composite nano film of different Ti/Al ratio, can be with skew to it, and electricity and interfacial property are studied.
Summary of the invention
Technical problem to be solved by this invention provides the ald TixAl that can be with compensation between a kind of Ge of regulation and control semiconductor and gate medium
yThe O method, this method is by regulating the Ti/Al ratio in the Ti-Al-O composite nano film, effectively regulated and to be with compensation between Ge substrate and the gate dielectric membrane, make conduction band offset between film and Ge substrate greater than 1 eV, effectively reduced leakage current, the method technology is simple, and MOSFET has important application prospect at the Ge base.
The above-mentioned adjustable Ge base MOSFET preparation of devices method that can be with skew, it may further comprise the steps:
1) substrate cleans: at first with germanium substrate in acetone, methyl alcohol ultrasonic cleaning 2-10 minute successively, remove the greasy dirt on Ge surface, then the germanium substrate is moved on in the hydrofluoric acid aqueous solution, cleaned 1-3 minute under the room temperature, then steeped 1-3 minute with deionized water, repeated several times dries up the germanium substrate at last with high pure nitrogen;
2) ALD Al
2O
3/ TiO
2The nano-stack thin-film technique: the germanium substrate after the step 1) processing is put into the ALD reative cell, carry out the deposition of gate dielectric layer, the ALD deposition parameter of wherein setting is: reaction chamber temperature: 200 ~ 300 ℃; Reaction source: depositing Al
2O
3Adopt source metal Al (CH
3)
3And H
2The O reaction, Al (CH
3)
3The source temperature is room temperature; Depositing Ti O
2Adopt source metal Ti (OC
3H
7)
4And H
2The O reaction, Ti (OC
3H
7)
4The source temperature is 40 ~ 80
oC;
Deposition process: with Al
2O
3Be beginning layer, alternately Al
2O
3And TiO
2Deposition cycle, in the deposition process, the pulse at source metal and water source all is 0.1 ~ 0.4 s, according to want deposition medium layer thickness strobe pulse number of times, and the molar ratio of Al/Ti is Al:Ti=1:1.2-4.5 in the film of final deposition; After each source pulse, all and then clean 1 ~ 10 s with high pure nitrogen, wash out byproduct of reaction and residual source;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N
2Protection down, in 400 ~ 600 ℃ of short annealing 30 ~ 180 s to room temperature.
Above-mentioned steps 1) the percentage by weight 2-5% of hydrofluoric acid aqueous solution in.
In this method, when the molar ratio of Al/Ti was reduced to 1:4.5 from 1:1.2, accumulation attitude electric capacity increased; Leakage current rises.And, along with the Al/Ti ratio increases, Al
2O
3/ TiO
2Valence band on Ge and conduction band compensation and band gap all can increase simultaneously.These presentation of results: ALD Al
2O
3/ TiO
2The nano-stack structure can be regulated interface quality and the band structure between gate medium and the Ge effectively, thereby improves the service behaviour of MOS device.Show that the method has important application prospects in Ge base MOSFET.
Description of drawings
Fig. 1 is the photoelectron spectroscopy figure of different Ti/Al percentage of T i-Al-O composite nano film, and wherein Fig. 1 (a) is Al 2p, and Fig. 1 (b) is Ti 2p.
Fig. 2 is the O1s electron energy loss spectroscopy (EELS) figure of different Ti/Al percentage of T i-Al-O composite nano film.
The valence band spectrogram of Fig. 3 different Ti/Al percentage of T i-Al-O composite nano film and Ge substrate.
Can be with between Fig. 4 different Ti/Al percentage of T i-Al-O composite nano film and the Ge substrate is offset schematic diagram.
Capacitance density-the voltage curve of Fig. 5 different Ti/Al percentage of T i-Al-O composite nano film.
Current density-the voltage curve of Fig. 6 different Ti/Al percentage of T i-Al-O composite nano film.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
One, backing material: commercial monocrystalline germanium wafer, N type, orientation (100), resistivity 0.2-0.5Wcm.
Two, technological process:
Embodiment 1:
1) substrate cleans: at first with the successively ultrasonic cleaning 2 minutes in acetone, methyl alcohol of germanium substrate, remove the greasy dirt on Ge surface, then the germanium substrate is moved on in the hydrofluoric acid aqueous solution of percentage by weight 2%, cleaned 1 minute under the room temperature, then steeped 1 minute with deionized water, repeat 3 times, at last the germanium substrate is dried up with high pure nitrogen;
2) ALD Al
2O
3/ TiO
2The nano-stack thin-film technique: the germanium substrate after the step 1) processing is put into the ALD reative cell, carry out the deposition of gate dielectric layer, the ALD deposition parameter of wherein setting is: reaction chamber temperature: 200 ℃; Reaction source: depositing Al
2O
3Adopt source metal Al (CH
3)
3And H
2The O reaction, Al (CH
3)
3The source temperature is room temperature; Depositing Ti O
2Adopt source metal Ti (OC
3H
7)
4And H
2The O reaction, Ti (OC
3H
7)
4The source temperature is 40
oC;
Deposition process: with Al
2O
3Be beginning layer, alternately Al
2O
3And TiO
2Deposition cycle, in the deposition process, the pulse at source metal and water source is 0.1 s all, obtain Al-Ti-O (ATO) sample (i) that thickness is about 18 nm: its structural parameters are (1:5)-ATO:[Al
2O
3(1 cycle)+TiO
2(5 cycles)], basic laminated construction is one deck Al
2O
3+ five layers of TiO
2, as the thickness of hierarchical element cycling deposition 18 nm.The molar ratio of Al/Ti is Al:Ti=1:1.2 among this embodiment; After each source pulse, all and then clean 4 s with high pure nitrogen, wash out byproduct of reaction and residual source;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N
2Protection is lower, in 400 ℃ of short annealing 120s.
Embodiment 2:
1) substrate cleans: at first with the successively ultrasonic cleaning 10 minutes in acetone, methyl alcohol of germanium substrate, remove the greasy dirt on Ge surface, then the germanium substrate is moved on in the hydrofluoric acid aqueous solution of percentage by weight 2%, cleaned 3 minutes under the room temperature, then steeped 3 minutes with deionized water, repeat 3 times, at last the germanium substrate is dried up with high pure nitrogen;
2) ALD Al
2O
3/ TiO
2The nano-stack thin-film technique: the germanium substrate after the step 1) processing is put into the ALD reative cell, carry out the deposition of gate dielectric layer, the ALD deposition parameter of wherein setting is: reaction chamber temperature: 300 ℃; Reaction source: depositing Al
2O
3Adopt source metal Al (CH
3)
3And H
2The O reaction, Al (CH
3)
3The source temperature is room temperature; Depositing Ti O
2Adopt source metal Ti (OC
3H
7)
4And H
2The O reaction, Ti (OC
3H
7)
4The source temperature is 80
oC;
Deposition process: with Al
2O
3Be beginning layer, alternately Al
2O
3And TiO
2Deposition cycle, in the deposition process, the pulse at source metal and water source is 0.4 s all, obtain Al-Ti-O (ATO) sample (ii) that thickness is about 18 nm: its structural parameters are (1:5)-ATO:[Al
2O
3(1 cycle)+TiO
2(5 cycles)], basic laminated construction is one deck Al
2O
3+ ten layers of TiO
2, as the thickness of hierarchical element cycling deposition 18 nm.The molar ratio of Al/Ti is Al:Ti=1:2 among this embodiment; After each source pulse, all and then clean 10 s with high pure nitrogen, wash out byproduct of reaction and residual source;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N
2Protection is lower, in 500 ℃ of short annealing 30s.
Embodiment 3:
1) substrate cleans: at first with the successively ultrasonic cleaning 5 minutes in acetone, methyl alcohol of germanium substrate, remove the greasy dirt on Ge surface, then the germanium substrate is moved on in the hydrofluoric acid aqueous solution of percentage by weight 2%, cleaned 2 minutes under the room temperature, then steeped 2 minutes with deionized water, repeat 3 times, at last the germanium substrate is dried up with high pure nitrogen;
2) ALD Al
2O
3/ TiO
2The nano-stack thin-film technique: the germanium substrate after the step 1) processing is put into the ALD reative cell, carry out the deposition of gate dielectric layer, the ALD deposition parameter of wherein setting is: reaction chamber temperature: 250 ℃; Reaction source: depositing Al
2O
3Adopt source metal Al (CH
3)
3And H
2The O reaction, Al (CH
3)
3The source temperature is room temperature; Depositing Ti O
2Adopt source metal Ti (OC
3H
7)
4And H
2The O reaction, Ti (OC
3H
7)
4The source temperature is 60
oC;
Deposition process: with Al
2O
3Be beginning layer, alternately Al
2O
3And TiO
2Deposition cycle, in the deposition process, the pulse at source metal and water source is 0.2 s all, obtain Al-Ti-O (ATO) sample (iii) that thickness is about 18 nm: its structural parameters are (1:20)-ATO:[Al
2O
3(1 cycle)+TiO
2(20 cycles)], basic laminated construction is one deck Al
2O
3+ two ten layers of TiO
2, as the thickness of hierarchical element cycling deposition 18 nm.The molar ratio of Al/Ti is Al:Ti=1:4.5 among this embodiment; After each source pulse, all and then clean 4 s with high pure nitrogen, wash out byproduct of reaction and residual source;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N
2Protection is lower, in 600 ℃ of short annealing 180s.
Three, sample test analysis and conclusion
Electrode material: magnetron sputtering top electrode platinum, elargol is as hearth electrode.
Test characterizes: the Surface Physical Chemistry structure after the germanium substrate processing is measured with x X-ray photoelectron spectroscopy X instrument, thickness and the interfacial property of gate dielectric membrane characterize with transmission electron microscope, I-E characteristic is measured with high precision electro potential source/Pi Anbiao, and capacitance-voltage characteristics is measured with accurate electric impedance analyzer.
1. different Ti/Al molar ratios is to the impact in conjunction with energy of Al2p and Ti2p.
By XPS analysis, sample (1:5)-ATO, (1:10)-the Al/Ti molar ratio of ATO and (1:20)-ATO is respectively 1:1.2,1:2 and 1:4.5.Fig. 1 (a) has showed the Al 2p photoelectron spectroscopy figure of three kinds of different Ti/Al percentage of T i-Al-O composite nano films.When the Ti/Al molar ratio is 4.5:1(x=0.9) time, the binding energy of Al 2p and Ti 2p is respectively 74.1 and 458.9 eV.Can find out obviously that from figure along with the raising of Al content in film, the binding energy of Al 2p reduces, and the binding energy of Ti 2p increases.Formed the Ti-Al-O key in this proof annealing rear film.This is because in the Ti-Al-O key that forms, the electronegativity of Al is bigger than the electronegativity of Ti, so Al obtains electronics from Ti, thereby binding energy descends.
2. different Ti/Al molar ratios is to the impact that can be with of Ti-Al-O composite nano film
In principle, can produce two kinds of energy losses in the process that light activated electronics process medium escapes out, a kind of because excitation of plasma causes that another is owing to electronics causes from the valence to the conduction band.For general high dielectric constant material, will be by the energy loss that excitation of plasma causes much larger than other one.So the energy gap of high dielectric constant material can be by determining with its distance of original position at energy loss peak.The O 1s electron energy loss spectroscopy (EELS) figure of Fig. 2 different Ti/Al percentage of T i-Al-O composite nano film.We can find that along with the content increase of Al, the band gap of film is also along with increase.When the molar ratio of Al/Ti was 1:1.2, the band gap of film was 5.06 eV.
In order to obtain conduction band offset (△ Ec), we must obtain the data of valence band offset (△ Ev) according to formula △ Ec=Eg (TAO)-Eg (Ge)-△ Ev.Therefore we have surveyed the valence band spectrum on different Ti/Al percentage of T i-Al-O composite nano film and Ge surface with XPS, and data as shown in Figure 3.By linear extrapolation, the valence band that we obtain the Ge surface is 0.09 eV, and the valence band of three kinds of different Ti/Al percentage of T i-Al-O composite nano films is respectively 3.08 eV, 2.92 eV, 2.70 eV.And △ Ev=EVBM (TAO) – EVBM (Ge), therefore working as the Ti/Al ratio is 7:6,2:1, during 4.5:1, conduction band offset is respectively 1.40 eV, 1.21 eV, 1.04 eV.
The band gap of considering the Ge substrate is 0.67 eV, and according to the data that obtain above, Fig. 4 has provided can be with between different Ti/Al percentage of T i-Al-O composite nano film and the Ge substrate and has been offset schematic diagram.
3. different Ti/Al molar ratios is to the influence of Ti-Al-O composite nano film electrical properties
Fig. 5 has showed capacitance density-voltage (C-V) curve of different Ti/Al percentage of T i-Al-O composite nano film.Measuring frequency is 1MHz.As can be seen from the figure along with the increase of the content of Al in the film, the electric capacity of accumulation attitude slowly descends.When x=0.7, its oxide equivalent thickness is 2.3 nm.
Fig. 6 has shown the leakage current curve of the film correspondence among Fig. 5.As can be seen from the figure along with the increase of the content of Al in the film, the leakage current of film slowly descends.At voltage be+during 1V, its leakage current density is respectively 7.41 * 10-7A/cm
2, 1. 12 * 10-5A/cm
2, 2. 69 * 10-5A/cm
2
Claims (2)
1. regulate and control the method that can be with compensation between Ge substrate and TixAlyO film for one kind, it is characterized in that may further comprise the steps:
1) substrate cleans: at first with germanium substrate in acetone, methyl alcohol ultrasonic cleaning 2-10 minute successively, remove the greasy dirt on Ge surface, then the germanium substrate is moved on in the hydrofluoric acid aqueous solution, cleaned 1-3 minute under the room temperature, then steeped 1-3 minute with deionized water, repeated several times dries up the germanium substrate at last with high pure nitrogen;
2) ALD Al
2O
3/ TiO
2The nano-stack thin-film technique: the germanium substrate after the step 1) processing is put into the ALD reative cell, carry out the deposition of gate dielectric layer, the ALD deposition parameter of wherein setting is: reaction chamber temperature: 200 ~ 300 ℃; Reaction source: depositing Al
2O
3Adopt source metal Al (CH
3)
3And H
2The O reaction, Al (CH
3)
3The source temperature is room temperature; Depositing Ti O
2Adopt source metal Ti (OC
3H
7)
4And H
2The O reaction, Ti (OC
3H
7)
4The source temperature is 40 ~ 80
oC;
Deposition process: with Al
2O
3Be beginning layer, alternately Al
2O
3And TiO
2Deposition cycle, in the deposition process, the pulse at source metal and water source all is 0.1 ~ 0.4 s, according to want deposition medium layer thickness strobe pulse number of times, and the molar ratio of Al/Ti is Al:Ti=1:1.2-4.5 in the film of final deposition; After each source pulse, all and then clean 1 ~ 10 s with high pure nitrogen, wash out byproduct of reaction and residual source;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N
2Protection down, in 400 ~ 600 ℃ of short annealing 30 ~ 180 s to room temperature.
2. can be with the method for compensation between regulation and control Ge substrate according to claim 1 and TixAlyO film, it is characterized in that the percentage by weight 2-5% of step 1) hydrofluoric acid aqueous solution.
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|---|---|---|---|---|
| CN103274435A (en) * | 2013-05-22 | 2013-09-04 | 复旦大学 | Titanium aluminum oxide thin film and preparation method and application thereof |
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| CN103215643B (en) * | 2013-03-29 | 2015-06-24 | 太原理工大学 | Method for preparing monocrystal oxide film on Ge substrate |
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2011
- 2011-04-08 CN CN2011100876977A patent/CN102194685B/en not_active Expired - Fee Related
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| CN1416156A (en) * | 2002-09-27 | 2003-05-07 | 上海华虹（集团）有限公司 | Structure of grid medium with high dielectric and its preparation method |
| CN1424744A (en) * | 2003-01-02 | 2003-06-18 | 上海华虹（集团）有限公司 | High dielectric grid laminating structure |
| US7138680B2 (en) * | 2004-09-14 | 2006-11-21 | Infineon Technologies Ag | Memory device with floating gate stack |
| CN102005380A (en) * | 2010-10-12 | 2011-04-06 | 复旦大学 | Method for depositing AlN (Aluminum Nitride)/high-k grid medium double-layer structure by adopting atom layer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274435A (en) * | 2013-05-22 | 2013-09-04 | 复旦大学 | Titanium aluminum oxide thin film and preparation method and application thereof |
| CN103274435B (en) * | 2013-05-22 | 2015-01-07 | 复旦大学 | Titanium aluminum oxide thin film and preparation method and application thereof |
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