EP1425785A2 - Method of fabricating a gate stack at low temperature - Google Patents
Method of fabricating a gate stack at low temperatureInfo
- Publication number
- EP1425785A2 EP1425785A2 EP20020798410 EP02798410A EP1425785A2 EP 1425785 A2 EP1425785 A2 EP 1425785A2 EP 20020798410 EP20020798410 EP 20020798410 EP 02798410 A EP02798410 A EP 02798410A EP 1425785 A2 EP1425785 A2 EP 1425785A2
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- European Patent Office
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- layer
- substrate
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- oxide
- reactant
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- the present invention relates to methods and equipment for forming dielectric stacks in integrated circuits, and particularly to forming a thin oxide interfacial layer under a high-k material.
- Gate dielectrics are formed of high quality silicon dioxide and are typically referred to as "gate oxide" layers. Such layers are typically grown from a single crystal silicon wafer or epitaxial silicon layer. The gate oxide capacitively couples the gate electrode to the channel region between the source and the drain regions in a typical transistor.
- ultra thin gate oxides e.g., less than 5 nm
- defect densities including pinholes, charge trapping states, and susceptibility to hot carrier injection effects.
- Such high defect densities lead to leakage currents through the gate dielectric and rapid device breakdown that is unacceptable for circuit designs with less than 0.25 ⁇ m gate spacing, i.e., sub-quarter-micron technology.
- incorporating materials with a higher permittivity than SiO 2 into the gate dielectric opens the door to further device scaling. Due to their higher dielectric constant, such materials can exhibit the same capacitance as a thinner silicon dioxide layer, such that a lower equivalent oxide thickness can be achieved without tunnel-limited behavior.
- Another advantage of some high dielectric materials is their diffusion barrier properties, such as resistance to boron penetration, and their high thermal conductivity.
- ALD atomic layer deposition
- one deposition cycle comprises exposing the substrate to a metal precursor, removing unreacted first reactant and reaction byproducts from the reaction chamber, exposing the substrate to an oxygen precursor followed by a second removal step.
- metal alkoxides which serve as both a metal and oxygen source in reacting with another metal compound
- the silicon surface Prior to thermally growing silicon oxide, the silicon surface is desirably cleaned to avoid contamination and produce superior electrical properties.
- the surface is generally cleaned of a naturally forming oxide known as "native oxide.”
- native oxide forms naturally over bare silicon surfaces even upon exposure to clean room environments at room temperature.
- native oxide comprises a few angstroms of silicon oxide and therefore makes up a substantial portion of the dielectric film to be formed.
- a thermal oxide can be grown through the native oxide to complete the desired dielectric layer, the quality and thickness of the native oxide are inconsistent across the silicon surface.
- the native oxide that results from long transportation and/or storage is typically contaminated with impurities.
- native oxide is often removed from the surface with dilute hydrofluoric acid (HF) baths or HF vapor etching. Dipping the wafers in a dilute HF bath cleans the silicon surface of native oxide and leaves the surface hydrogen terminated. HF vapor etching similarly cleans the silicon surface and terminates dangling silicon bonds, but the surface termination includes a substantial fluorine content. Hydrogen termination is not very stable, particularly at elevated temperatures. The hydrogen atoms readily desorb to leave the dangling silicon bonds that tend to attract atmospheric contaminants. Even with hydrogen and fluorine termination in place, atmospheric oxidants can still diffuse through the termination layer between the HF treatment and subsequent processing.
- HF hydrofluoric acid
- HF treatment cleans the wafer surface but leaves the surface inadequately protected for the period between cleaning and further processing.
- One manner in which a clean silicon surface can be maintained for longer periods of time is to quickly grow a thin silicon oxide layer after cleaning the silicon surface.
- an ultra thin Si0 2 layer can provide improved interface characteristics between a silicon structure and high dielectric permittivity (high-k dielectric) materials. Spontaneous oxide regrowth, such as by room temperature exposure to typical oxidants like air or water, results in a very slow reaction, which is unacceptable for commercial fabrication.
- thermal oxidation at temperatures greater than 500°C causes the hydrogen termination left by HF treatment to desorb well before temperatures reach the level at which significant oxidation takes place. In the interim, the silicon surface is left unprotected.
- thermal oxidation of the initially bare silicon substrate proceeds rapidly and by mechanisms that are not well understood, as compared to latter stages during which oxidants diffuse through an already-grown portion of the silicon oxide. Accordingly, when attempting to provide oxide thicknesses appropriate for interface improvement beneath high-k materials, the oxidation is not easily controlled and can easily exceed the desired thickness. Additionally, even if an ultra thin oxide layer is effectively formed as an interfacial layer, under typical growth conditions when the subsequent high-k material is deposited the oxide layer grows further. A silicon oxide interface that is too thick results in a lower overall dielectric constant.
- the thickness of the Si0 2 interface determines the minimum thickness for the gate oxide layer.
- such methods should be compatible with single-wafer processing systems and sub-quarter-micron technology, yet exhibit higher yield and throughput compared to conventional techniques.
- the present invention relates to a process for forming a gate dielectric on a semiconductor substrate by forming an interfacial dielectric oxide layer on the substrate and depositing a high-k layer over the interfacial dielectric.
- the high-k layer is preferably deposited under conditions such that the thickness of the interfacial dielectric layer does not substantially increase.
- the present invention relates to a method of forming a dielectric layer on a silicon substrate.
- the method preferably comprises growing a silicon oxide interface layer less than about 15 A thick on the substrate and depositing a high-k material on top of the interlace layer.
- depositing comprises maintaining the substrate at a temperature less than about 300°C and supplying water vapor as an oxidizing agent.
- Depositing the high-k material preferably grows the interface layer by less than about 15 A, more preferably by less than about 10 A and even more preferably by less than about 5 A.
- depositing comprises an ALD process.
- the ALD process may in turn comprise a plurality of cycles, with each cycle preferably comprising: contacting the substrate with a first reactant; removing the unreacted first reactant and possible reaction byproducts from the reaction chamber; contacting the substrate with water vapor; and removing the unreacted water vapor and possible reaction byproducts from the reaction chamber.
- Figure 1 shows a general process sequence for depositing an ultrathin interfacial dielectric material between the substrate and a high-k dielectric material in a gate dielectric.
- the present invention discloses a method of producing an ultra thin oxide interfacial layer between the substrate and a high-k material, wherein the thickness of the interfacial layer is maintained during the deposition of the high-k dielectric material.
- Figure 1 shows a general process sequence in accordance with the present invention.
- the substrate is first cleaned 10 to remove native oxide and contaminants.
- the surface may then optionally be modified 20 to facilitate the subsequent formation 30 of an ultra thin interfacial dielectric.
- the surface may be subject to optional modification 40 to facilitate the subsequent deposition of the high-k dielectric layer 50. Preferred methods are described in the embodiments below, requiring no modification of the oxide surface prior to high-k deposition.
- substrate refers to any surface on which a layer is to be deposited.
- thin oxide layers and high-k layers can be formed over metal surfaces.
- the preferred substrate is a semiconductor structure, such as an epitaxial silicon layer or the top surface of a monolithic silicon wafer. In this context, the skilled artisan will appreciate that the semiconductor substrate is the lowest level of semiconductor material from which devices are formed in an integrated circuit.
- the substrate is cleaned 10 to remove contaminants and naturally occurring or native oxide on the semiconductor structure.
- Cleaning of the substrate may be achieved by any method known in the art.
- wafer cleaning prior to gate oxide growth is conducted ex situ before the wafer is loaded into the process chamber.
- wafers may be cleaned in an HCI/HF wet etch bath.
- cleaning can be performed in situ.
- an integrated HF and acetic acid vapor clean can be conducted in a module within a cluster tool, reducing transport time and opportunity for recontamination or re-oxidation.
- a hydrogen bake step can be conducted within the chamber to sublimate native oxide. Small amounts of HCI vapor can be added to this step to aid in cleaning metal contaminants and the like during the hydrogen bake.
- plasma products can assist or conduct in situ cleaning, such as by substituting H radicals for hydrogen gas.
- use of activated or excited species can widen the process temperature window for adequate cleaning.
- the substrate surface may optionally be treated 20 in a way that moderates the subsequent oxidation of the substrate and the resulting growth of an interfacial dielectric oxide layer, as disclosed in copending application number 09/791 ,167, filed February 22, 2001, the disclosure of which is incorporated herein by reference.
- the dangling bonds at the silicon surface following cleaning have a strong tendency to bond with groups or radicals present in the ambient atmosphere.
- the silicon dangling bonds are practically completely terminated by atomic hydrogen or fluorine. Hydrogen is the smallest atom in existence and fluorine is the smallest haiide atom. They do not provide any significant barrier for the diffusion of the oxidant to the silicon surface.
- the hydrogen or fluorine termination can be replaced by a termination with a larger group.
- the surface is then partially blocked, and the diffusion of the oxidant towards the surface proceeds more slowly. This substantially dampens the oxidation rate, particularly during the initial stages of the growth, which typically proceeds relatively quickly.
- the permeability of the diffusion barrier can be tailored, the oxidation rate can be controlled, and the final oxide thickness can be adjusted.
- the increasing oxide thickness contributes to the overall diffusion barrier and the oxidation process has the tendency to be self-limiting in oxide thickness.
- exposure of the silicon surface to water vapor results in replacement of the hydrogen termination of the dangling bonds with an OH termination.
- the OH group is substantially larger than the H atom and thus already has a strong moderating effect on the oxidation rate.
- other effects like bonding strength, polarity, etc. will be of influence to the oxidation rate. Consequently the mere occupation of the dangling bonds by ligands can and will influence the oxidation rate.
- the ligands are OH groups formed by exposure to H 2 0.
- the interfacial dielectric is silicon oxide grown by exposure to a species that is reactive with the cleaned substrate, such as in thermal oxidation of the cleaned substrate.
- the oxidant source can comprise any number of known oxidants, particularly a volatile oxidant such as 0 2 , H 2 0, HCOOH, and HCI0 4 .
- oxidation rates are preferably enhanced by providing oxidants more reactive than oxygen and/or by elevating the oxidation temperature, preferably to a temperature between about 50°C and 400°C, more preferably between about 300°C and 400°C. Desirably, process temperatures are maintained below about 400°C during oxidation.
- a 5 A thick layer of Si0 2 may be grown on a cleaned substrate by exposure to O3 gas for 100 seconds at400°C.
- the oxidant has a stronger oxidizing effect than oxygen or water vapor alone. Oxidation with such oxidizers can be conducted at lower temperatures, preferably less than about 300°C, more preferably less than about 200°C.
- An exemplary strong oxidizer in accordance with this embodiment, is an ozone-containing gas. In an alternative embodiment, this ozone-containing gas is mixed with water vapor, oxygen or an inert gas like a noble gas or N 2 .
- Another exemplary strong oxidizer comprises a peroxide-containing gas.
- An oxygen-containing source gas may be provided to a remote plasma generator to provide excited species for oxidation.
- the growth of the interfacial dielectric may also include nitrogen incorporation (e.g., by oxidation with NO or N2O or by nitridation with NH3) to form, for example, an oxynitride interfacial dielectric.
- nitrogen incorporation e.g., by oxidation with NO or N2O or by nitridation with NH3
- an oxynitride interfacial dielectric after cleaning an interfacial dielectric is grown by introduction of about 1.5 slm NO gas while maintaining a 15 slm flow of N 2 , assuming pure NO oxidant gas.
- the flow rate may need adjustment for use of alternative oxidant gases (e.g., 0 2 , H 2 0, N2O, HCOOH, HCIO4, nitroalkanes such as CH3NO2, alkyl nitrates such as (CH3)2CHON02, mixtures or diluted oxidants).
- oxidant gases e.g., 0 2 , H 2 0, N2O, HCOOH, HCIO4, nitroalkanes such as CH3NO2, alkyl nitrates such as (CH3)2CHON02, mixtures or diluted oxidants.
- Temperature and pressure are maintained at about 780°C and 50 Torr, respectively, and the N2 flow is similarly maintained.
- a layer of silicon oxynitride grows from the substrate to a thickness of about 0.5 nm.
- Nitrogen and/or oxygen radicals can also be used for oxide, nitride or oxynitride growth.
- the outermost layer of silicon oxide is nitrided to form a nitride layer that resists further oxide growth.
- the interfacial dielectric layer preferably comprises SiO x , SiN y , or SiO x N y .
- the interfacial oxide layer may alternatively be produced by any other methods known in the art. For example it may be produced by controlled deposition rather than oxidation of the substrate. In one embodiment an interfacial dielectric layer of Si0 2 is deposited by atomic layer deposition (ALD). In another embodiment an interfacial dielectric layer of Si0 2 is grown by chemical oxidation of the substrate.
- ALD atomic layer deposition
- an interfacial dielectric layer such as a Si0 2 layer, with controlled thickness and optional -OH termination is followed by the deposition of a second thin dielectric layer in a manner that inhibits further growth of the underlying interfacial dielectric layer.
- the underlying dielectric layer grows by less than 10 A, on average, during the deposition of the second dielectric layer, more preferably by less than 5 A, on average, and even more preferably does not grow at all during deposition of the second dielectric layer.
- the layer deposited over the interfacial dielectric layer is a high-k dielectric material.
- the high-k material has a higher dielectric constant than silicon oxide, preferably has a dielectric constant greater than 5, and more preferably has a dielectric constant greater than 10.
- the high-k material deposited on the interfacial dielectric layer may be any high-k material that can be deposited without substantially growing the interfacial dielectric layer.
- a preferred high-k material is a metal oxide.
- high-k materials that can be used in the present invention are Zr0 2 , HfO ⁇ , AI2O3, Ta 2 Os, Ti0 2 , BST, ST, SBT, Nb 2 0 5 , and La 2 0 3 , as well as oxides of Sc, Y, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb or Lu, solid solutions of metal oxides and nanolaminates of metal oxides.
- Controlling the thickness of the underlying interfacial dielectric layer on a monolayer scale to achieve a target thickness of a few monolayers is particularly advantageous for such high-k applications, since the total thickness limits the achievable capacitance and thickness variations can have significant impact upon overall uniformity of the compound dielectric.
- Non-uniformity results in higher than necessary equivalent oxide thickness, since the minimum thickness to avoid leakage must be employed, such that the non-uniform oxide is excessively thick elsewhere.
- excessive gate dielectric variation can ultimately reduce production yield.
- any deposition process that does not further grow the interfacial oxide layer may be used to form the high-k dielectric layer.
- ALD, CVD, PVD, MOCVD, MBE or any other known method may be used to deposit the high-k material so long as conditions are maintained such that no further oxidation of the underlying layer occurs. These methods are preferably carried out at less than 400°C, more preferably less than about 300°C and even more preferably less than about 200°C.
- the second layer may contribute barrier characteristics and resistance to hot carrier effects at the same time as enabling overall scaling of the gate dielectric due to a higher dielectric constant.
- a further surface treatment can optionally be provided prior to deposition of the high-k material.
- excited species treatment may serve to modify the surface termination of the interfacial layer and promote subsequent deposition.
- the layer left by a pulse is self-terminated with a surface that is non-reactive with the remaining chemistry of that pulse. After the self-limiting reaction has gone to completion, the unreacted source chemical is removed from the reaction space and the substrate is exposed to the next reactant.
- Water vapor is preferably used as the oxygen source, replacing ligand termination of the previous pulse, because it does not substantially further grow the thin interfacial oxide at less than 300°C. Oxide regrowth is a particular concern during initial stages of the high-k deposition, since oxidants can readily diffuse through the few monolayers of high-k material and thin interfacial oxide.
- pulses of aluminum source gas or zirconium source gas are alternated with water vapor pulses, with intervening purge pulses.
- the second dielectric layer comprises AI2O3 deposited from trimethyl aluminum (TMA) and water.
- the temperature at which the high-k dielectric is deposited is preferably maintained low enough that the thickness of the interfacial dielectric layer does not increase.
- deposition of the high-k material is preferably carried out at a temperature below about 400°C. More preferably deposition is carried out at a temperature between about 70°C and 300°C, and most preferably between about 200°C and 300°C. In one embodiment, temperature is lowered from the temperature at which thermal oxidation was performed during interfacial dielectric growth to less than about 300°C during high-k dielectric deposition. Pressure during the processes is preferably maintained between about 1 Torr and 80 Torr, more preferably at about 10 Torr.
- Each pulsing cycle consists of four basic steps:
- the number of cycles determines the thickness of the layer.
- the growth rate of AI2O3 from (CH3)3AI and H2O is typically near 0.1 nm/cycle or 1 A/cycle at 300°C, or about 3-4 cycles/monolayer (AI2O3 has a bulk lattice parameter of about 3 A).
- the methyl terminations left by each TMA pulse self-terminate adsorption of each such pulse and also reduce the number of available chemisorption sites, such that less than a full monolayer forms with each pulse.
- the pulsing cycle is repeated sufficient times to produce the desired layer thickness.
- Aluminum oxide can serve as the only high-k material in the gate dielectric, or as a thin barrier layer prior to forming one or more additional dielectric layers.
- the average deposition rate is about 0.59 A/cycle at 300°C.
- the cycle of Table II, consisting of pulse A, purge A, pulse B, purge B, may be repeated as many times as necessary to produce a layer of the desired thickness. More generally, temperatures during the process preferably fall between about 200°C and 300°C.
- the metal monolayer formed by each ZrCI pulse is self-terminated with chloride, which does not readily react with excess ZrCI 4 under the preferred conditions.
- the preferred oxygen source gas reacts with or adsorbs upon the chloride-terminated surface during the oxygen phase in a ligand-exchange reaction limited by the supply of zirconium chloride complexes previously adsorbed. Moreover, oxidation leaves a hydroxyl and oxygen bridge termination that does not further react with excess oxidant in the saturative phase.
- sufficient cycles are conducted to grow between about 20 A and 60 A of Zr ⁇ 2. More preferably, sufficient cycles are conducted to grow between about 20 A and 40 A and most preferably about 30 A.
- the dielectric constant of the layer is between about 18 and 24.
- the deposited dielectric layer is optionally annealed to improve the quality of this layer.
- the deposited dielectric layer may be subjected to a high temperature oxygen anneal, crystallizing the layer and filling any oxygen vacancies which might otherwise leave essentially metallic leakage paths.
- An anneal step may be carried out in situ in a reactor designed to minimize the risk of explosive or otherwise undesirable reactions among sequential reactants.
- the anneal is carried out under conditions that prevent further growth of the interfacial oxide layer.
- an ALD process may be used to deposit the high-k layer wherein the ALD process uses two metal compounds, one of which is an oxygen source material that reacts well with another metal compound but which does not oxidize the substrate.
- the surface of the substrate is alternately reacted with a metal source material and an oxygen source material.
- the oxygen source material is preferably a metal alkoxide, a metal compound that has at least one organic ligand and where oxygen is bonded to at least one boron, silicon or metal atom.
- the metal alkoxide serves as both an oxygen and metal source when it reacts with a second metal compound, such as a metal halide, or a metal alkyl. In this process a high-k metal oxide can be deposited without further oxidation of the underlying substrate and thus without further growth of the interfacial oxide layer.
- the high-k material can be deposited by direct decomposition of metal precursors in the absence of oxygen.
- metal precursors preferably comprise both metal and oxygen and thus are able to form metal oxides without additional oxygen. In this case, the absence of an oxidizing agent would prevent further growth of the interfacial oxide layer.
- Preferred metal precursors are organic metal compounds. However, they may also be volatile anhydrous metal nitrates.
- the high-k material can be deposited by metal organic chemical vapor deposition (MOCVD).
- MOCVD metal organic chemical vapor deposition
- an oxidant is used that does not substantially further grow the interfacial oxide layer at the temperature at which the process is carried out.
- Dielectric deposition may be followed by formation of a transistor gate electrode over the dielectric stack.
- electrode formation may also be performed in situ. Accordingly, not only can a dielectric stack be formed in situ, but in the preferred embodiment the reactor and methods enable in situ processing of all steps in the formation of a transistor gate stack. Thus interfacial dielectric growth and second high-k dielectric deposition may be conducted in situ.
- any or all of wafer cleaning, depositing dielectric layers, annealing and forming electrodes can be conducted in situ, that is, in the same process chamber or cluster tool without exposure to the atmosphere between steps.
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- Formation Of Insulating Films (AREA)
- Insulated Gate Type Field-Effect Transistor (AREA)
Abstract
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Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US31656201P | 2001-08-31 | 2001-08-31 | |
US316562P | 2001-08-31 | ||
US227475 | 2002-08-22 | ||
PCT/US2002/027230 WO2003041124A2 (en) | 2001-08-31 | 2002-08-26 | Method of fabricating a gate stack at low temperature |
Publications (1)
Publication Number | Publication Date |
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EP1425785A2 true EP1425785A2 (en) | 2004-06-09 |
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ID=32312306
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP20020798410 Withdrawn EP1425785A2 (en) | 2001-08-31 | 2002-08-26 | Method of fabricating a gate stack at low temperature |
Country Status (2)
Country | Link |
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EP (1) | EP1425785A2 (en) |
TW (1) | TW559916B (en) |
-
2002
- 2002-08-26 EP EP20020798410 patent/EP1425785A2/en not_active Withdrawn
- 2002-08-28 TW TW91119485A patent/TW559916B/en not_active IP Right Cessation
Non-Patent Citations (1)
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See references of WO03041124A3 * |
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TW559916B (en) | 2003-11-01 |
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Inventor name: TUOMINEN, MARKO Inventor name: HUBERT MAES, JAN, WILLEM Inventor name: POMAREDE, CHRITOPHE, F. Inventor name: SHERO, ERIC Inventor name: HAUKKA, SUVI, P. |
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Inventor name: TUOMINEN, MARKO Inventor name: HUBERT MAES, JAN, WILLEM Inventor name: POMAREDE, CHRITOPHE, F. Inventor name: SHERO, ERIC Inventor name: HAUKKA, SUVI, P. |
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