CN102194685B - 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 PDF

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CN102194685B
CN102194685B CN2011100876977A CN201110087697A CN102194685B CN 102194685 B CN102194685 B CN 102194685B CN 2011100876977 A CN2011100876977 A CN 2011100876977A CN 201110087697 A CN201110087697 A CN 201110087697A CN 102194685 B CN102194685 B CN 102194685B
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film
substrate
source
deposition
ald
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CN102194685A (en
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李学飞
李爱东
付盈盈
刘晓杰
李辉
吴迪
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Nanjing University
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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

Can be with the method for compensation between regulation and control Ge substrate and TixAlyO film
Technical field
The present invention relates to technique for atomic layer deposition, specifically is in Ge base MOSFET preparation of devices process, to regulate the method that can be with skew between gate medium TixAlyO film and the substrate Ge.
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 influenced 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 and first integrated circuit of success making all are to be prepared 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, accomplishes the demand of technology, owing to can accomplish 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 through the inert gas exhaust, a kind of precursor in back be adsorbed on the surface before a kind of reaction generate the solid phase film.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 layer structure (Nanlaminates) that is fit to modifying interface and many group members of preparation nanoscale especially.
Many oxides such as HfO 2, ZrO 2, Al 2O 3Deng as candidate's semi-conducting material just by widely research.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 combines these two kinds of oxides advantage separately, adopts ald, has successfully deposited different Ti/Al percentage of T i-Al-O composite nano film, 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 through regulating the Ti/Al ratio in the Ti-Al-O composite nano film; Regulated effectively and can be with compensation between Ge substrate and the gate dielectric membrane, made conduction band offset between film and Ge substrate, reduced leakage current effectively greater than 1 eV; The method technology is simple, on Ge base MOSFET, has important application prospects.
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 a 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, wash out byproduct of reaction and residual source with high pure nitrogen;
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 when 1:1.2 is reduced to 1:4.5, accumulation attitude electric capacity increases; 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 MOS working performance of devices.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.
Between Fig. 4 different Ti/Al percentage of T i-Al-O composite nano film and the Ge substrate can be with the skew sketch map.
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
further describe the present invention below in conjunction with specific embodiment.
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 ultrasonic cleaning 2 minutes successively 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 a 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, the thickness of cycling deposition 18 nm as the lamination unit.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, wash out byproduct of reaction and residual source with high pure nitrogen;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N 2Under the protection, in 400 ℃ of short annealing 120s.
Embodiment 2:
1) substrate cleans: at first with the ultrasonic cleaning 10 minutes successively 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 a 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 that thickness is about 18 nm (ii): 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, the thickness of cycling deposition 18 nm as the lamination unit.The molar ratio of Al/Ti is Al:Ti=1:2 among this embodiment; After each source pulse, all and then clean 10 s, wash out byproduct of reaction and residual source with high pure nitrogen;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N 2Under the protection, in 500 ℃ of short annealing 30s.
Embodiment 3:
1) substrate cleans: at first with the ultrasonic cleaning 5 minutes successively 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 a 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 that thickness is about 18 nm (iii): 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, the thickness of cycling deposition 18 nm as the lamination unit.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, wash out byproduct of reaction and residual source with high pure nitrogen;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, at N 2Under the protection, 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 appearance; The thickness and the interfacial property of gate dielectric membrane characterize with transmission electron microscope; I-E characteristic is measured with high-accuracy voltage source/Pi Anbiao, and capacitance-voltage characteristics is measured with accurate electric impedance analyzer.
1. different Ti/Al molar ratio is to the influence of the binding energy of Al2p and Ti2p.
Through XPS analysis, sample (1:5)-ATO, (1:10)-ATO with (1:20)-the Al/Ti molar ratio of 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 was 4.5:1 (x=0.9), the binding energy of Al 2p and Ti 2p was respectively 74.1 and 458.9 eV.From figure, can find out obviously that 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 influence 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 is escaped away, a kind of owing to excitation of plasma causes, a kind of in addition 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 confirming 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 different Ti/Al percentage of T i-Al-O composite nano film and the surperficial valence band spectrum of Ge with XPS, and data are as shown in Figure 3.Through 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, according to the top data that obtain, Fig. 4 provided between different Ti/Al percentage of T i-Al-O composite nano film and the Ge substrate can be with the skew sketch map.
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 corresponding leakage current curve of the film 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 ald TixAlyO 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 of germanium substrate 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) 3With water reaction, Al (CH 3) 3The source temperature is a room temperature; Depositing Ti O 2Adopt source metal Ti (OC 3H 7) 4With water 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, wash out byproduct of reaction and residual source with high pure nitrogen;
Annealing: the germanium substrate behind the deposit film is put in the quick anneal oven, under nitrogen protection, in 400 ~ 600 ℃ of short annealing 30 ~ 180 s to room temperature.
2. can be with the ald TixAlyO method of 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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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103215643A (en) * 2013-03-29 2013-07-24 太原理工大学 Method for preparing monocrystal oxide film on Ge substrate

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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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CN1424744A (en) * 2003-01-02 2003-06-18 上海华虹（集团）有限公司 High dielectric grid laminating structure
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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