CN110760818A - Process for growing alumina by using atomic layer deposition technology - Google Patents

Process for growing alumina by using atomic layer deposition technology Download PDF

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Publication number
CN110760818A
CN110760818A CN201911055242.XA CN201911055242A CN110760818A CN 110760818 A CN110760818 A CN 110760818A CN 201911055242 A CN201911055242 A CN 201911055242A CN 110760818 A CN110760818 A CN 110760818A
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atomic layer
layer deposition
introducing
trimethylaluminum
reactant
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刘佳晶
陈艳明
叶武阳
温丽娜
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Changchun Long Round Chen Microelectronic Technology Co Ltd
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Changchun Long Round Chen Microelectronic Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/40—Oxides
    • C23C16/403—Oxides of aluminium, magnesium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • C23C16/45525—Atomic layer deposition [ALD]
    • C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Formation Of Insulating Films (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention relates to a process for growing alumina by using an atomic layer deposition technology, which belongs to the field of semiconductor manufacturing. Meanwhile, the influence of high-temperature annealing on the early-stage process performance is inhibited, so that no heating process is needed in the material growth process, the energy consumption in the manufacturing process is greatly reduced, and the in-chip uniformity of the material can reach below 0.5%.

Description

Process for growing alumina by using atomic layer deposition technology
Technical Field
The invention relates to a process for growing aluminum oxide by using an atomic layer deposition technology, belonging to the field of semiconductor manufacturing.
Background
With the rapid development of large scale integrated circuit technology, the ALD atomic layer deposition method is used to grow the high-k gate dielectric material alumina Al2O3The leakage current of the gate can be effectively reduced. ALD can meet growth in a monoatomic layer control mode, accurately control the thickness at an angstrom level or a monoatomic layer level, and perform a continuous deposition reaction process. Too high or too low a temperature will reduce the growth rate of ALD and grow Al2O3Followed byAnnealing treatment is performed to eliminate the stress in the interface and the film, but the growth rate of the process mode is slower and the cost is higher.
Growth of alumina Al2O3Thin films, low temperatures can result in low growth rates and inability to achieve atomic layer deposition, while excessively high temperatures can result in thermal decomposition and chemisorption of precursors and affect the quality and properties of the thin film. In practical semiconductor application, the temperature for depositing the film is between 200 ℃ and 300 ℃, the annealing temperature is 500 ℃, however, some semiconductor early-stage process preparations cannot bear too high temperature in the subsequent process, and the too high temperature can greatly affect the performance of the electrode, so the annealing temperature can affect the property of the device, and the method also greatly limits the growth time and the cost.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a process for growing aluminum oxide by using an atomic layer deposition technology, which increases the temperature, can improve the growth rate of an aluminum oxide film, and cannot reduce the quality of the film due to overhigh temperature.
The technical scheme adopted by the invention for realizing the purpose is as follows: a process for growing alumina by atomic layer deposition technique, comprising the steps of:
setting the temperature of a reaction cavity of an atomic layer deposition system to be 320-380 ℃, and controlling the pressure value to be 1.19-1.3 torr;
step two, preparing the alumina film by utilizing an atomic layer deposition method, wherein the specific preparation process comprises the following steps:
① introducing a first reactant trimethylaluminum into the reaction cavity of the atomic layer deposition system, wherein the flow rate is 200 sccm-400 sccm, and the introduction time is 2 s-7 s;
② introducing nitrogen N2 to purge trimethylaluminum for 3-10 s;
③ introducing a second reactant ozone O3 for 10-35 s;
④ continuously introducing nitrogen N2 for 5-20 s;
steps ① to ④ form a cycle, and the cycle is repeated to obtain an alumina film.
Preferably, the temperature of the reaction chamber of the atomic layer deposition system in the first step is set to 350 ℃.
Preferably, the second step of preparing the alumina film by using the atomic layer deposition method comprises the steps of introducing a first reactant of trimethylaluminum at a flow rate of 300sccm for 5s, introducing nitrogen N2 to purge the trimethylaluminum for 7s, introducing a second reactant of ozone O3 for 20s, continuously introducing nitrogen N2 for 10s, and repeating the steps ① to ④ to form a cycle to obtain the alumina film.
Further, the cycle in the second step is repeated 178 times, and the thickness of the alumina film is
Figure BDA0002256379110000021
Through the design scheme, the invention can bring the following beneficial effects: the method takes trimethylaluminum (Al (CH3)3, TMA) as an aluminum source, ozone O3 as an oxygen source, nitrogen N2 as a carrier gas, a substrate as a silicon wafer, and the temperature of a reaction chamber of an atomic layer deposition system is set to be 320-380 ℃ to prepare the aluminum oxide film. Meanwhile, the influence of high-temperature annealing on the early-stage process performance is inhibited, so that no heating process is needed in the material growth process, the energy consumption in the manufacturing process is greatly reduced, and the in-chip uniformity of the material can reach below 0.5%.
Detailed Description
In order to more clearly illustrate the invention, the invention is further described below in connection with preferred embodiments. As will be appreciated by those skilled in the art. The following detailed description is to be construed as illustrative and not restrictive, and various changes may be made in the following parameters by a user without departing from the spirit and scope of the invention as set forth in the appended claims. Well-known methods and procedures have not been described in detail so as not to obscure the present invention.
The invention provides a process for growing alumina by using an atomic layer deposition technology, which takes trimethylaluminum (Al (CH3)3, TMA) as an aluminum source, ozone O3 as an oxygen source, nitrogen N2 as a carrier gas, a substrate as a silicon wafer, the temperature of a reaction cavity of an atomic layer deposition system is set to be 320-380 ℃, and an alumina film is prepared, and the process specifically comprises the following steps:
1. early preparation
① regulating the temperature of the reaction cavity of the atomic layer deposition system at the equipment end, namely measuring the temperature in the cavity from top to bottom in the reaction cavity of the atomic layer deposition system by using a single thermocouple device, heating to cooling, and recording a temperature curve to ensure that the temperature variation interval reaches +/-0.5 ℃;
② setting the temperature of reaction chamber of atomic layer deposition system at 320-380 deg.C and the pressure at 1.19-1.3 torr on the interface of process menu of atomic layer deposition system;
2. placing a silicon wafer on a machine table, and carrying out long film operation:
① introducing a first reactant of trimethylaluminum (Al (CH3)3, TMA), wherein the flow rate is 200 sccm-400 sccm, and the introduction time is 2 s-7 s;
② purging trimethylaluminum (Al (CH3)3, TMA) with N2 of nitrogen for 3-10 s to remove unabsorbed trimethylaluminum (Al (CH3)3, TMA) molecules;
③ introducing a second reactant ozone O3 for 10-35 s to ensure that a first reactant trimethylaluminum (Al (CH3)3, TMA) and a second reactant ozone O3 fully react on the surface of the silicon wafer;
④, continuously introducing nitrogen N2 to purge redundant unreacted ozone O3 and byproducts obtained by the reaction for 5-20 s;
steps ① to ④ form a cycle, and the cycle is repeated for a number of times depending on the film thickness, to obtain an alumina film.
3. And after the process is finished, taking out the silicon wafer with the aluminum oxide film, measuring the thickness, uniformity, stress and refractive index RI of the aluminum oxide film, and performing macroscopic and microscopic detection by using a microscope. The thickness variation of the film can be controlled
Figure BDA0002256379110000031
The uniformity can reach below 0.5 percent. The surface of the silicon chip is observed by a microscope without any damage and warpage.
Example 1
A process for growing alumina by atomic layer deposition technique comprises the following steps:
setting the temperature of a reaction cavity of an atomic layer deposition system to be 350 ℃, and controlling the pressure value to be 1.19-1.3 torr;
step two, the specific preparation process for preparing the alumina film by utilizing the atomic layer deposition method is as follows:
① introducing a first reactant trimethylaluminum into the reaction cavity of the atomic layer deposition system, wherein the flow rate is 300sccm, and the introduction time is 5 s;
② introducing nitrogen N2 to purge trimethylaluminum for 7 s;
③ introducing a second reactant ozone O3 for 20 s;
④ introducing nitrogen N2 for 10 s;
a cycle of ① to ④ is repeated 178 times to obtain an alumina film having a thickness of
Figure BDA0002256379110000041

Claims (4)

1. A process for growing alumina by atomic layer deposition technique, comprising the steps of:
setting the temperature of a reaction cavity of an atomic layer deposition system to be 320-380 ℃, and controlling the pressure value to be 1.19-1.3 torr;
step two, preparing the alumina film by utilizing an atomic layer deposition method, wherein the specific preparation process comprises the following steps:
① introducing a first reactant trimethylaluminum into the reaction cavity of the atomic layer deposition system, wherein the flow rate is 200 sccm-400 sccm, and the introduction time is 2 s-7 s;
② introducing nitrogen N2 to purge trimethylaluminum for 3-10 s;
③ introducing a second reactant ozone O3 for 10-35 s;
④ continuously introducing nitrogen N2 for 5-20 s;
steps ① to ④ form a cycle, and the cycle is repeated to obtain an alumina film.
2. The process of claim 1, wherein the temperature of the reaction chamber of the ald system is set to 350 ℃ in the first step.
3. The process of claim 1 or 2, wherein the second step of preparing the alumina film by the atomic layer deposition method comprises introducing trimethylaluminum as a first reactant at a flow rate of 300sccm for 5s, introducing N2 as nitrogen to purge trimethylaluminum for 7s, introducing ozone O3 as a second reactant for 20s, continuing to introduce N2 as nitrogen for 10s, and repeating the steps ① to ④ to form a cycle to obtain the alumina film.
4. A process according to claim 3, wherein the cycle in step two is repeated 178 times and the thickness of the alumina film is equal to
Figure FDA0002256379100000011
CN201911055242.XA 2019-10-31 2019-10-31 Process for growing alumina by using atomic layer deposition technology Pending CN110760818A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111517345A (en) * 2020-05-25 2020-08-11 上海交通大学 Three-dimensional structure micron aluminum oxide tube and preparation method thereof
CN112802734A (en) * 2020-12-30 2021-05-14 长春长光圆辰微电子技术有限公司 Method for depositing single-side film of silicon wafer
CN114959646A (en) * 2022-04-08 2022-08-30 普乐新能源科技(徐州)有限公司 Excellent ALD coating process
CN116682894A (en) * 2023-07-28 2023-09-01 无锡松煜科技有限公司 Method for improving batch-to-batch uniformity of ALD passivation films of TOPCON battery and application

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US6673701B1 (en) * 2002-08-27 2004-01-06 Micron Technology, Inc. Atomic layer deposition methods
CN101211759A (en) * 2006-12-28 2008-07-02 中芯国际集成电路制造(上海)有限公司 Capacitor, random memory cell and method for forming same
CN102201481A (en) * 2011-06-07 2011-09-28 合肥海润光伏科技有限公司 Novel N-type silicon hetero-junction battery with IBC (interdigitated back-contacted) structure and fabrication method thereof
CN102560419A (en) * 2011-11-29 2012-07-11 华东师范大学 Method for preparing alumina ultrathin film
US20130333835A1 (en) * 2012-06-14 2013-12-19 E I Du Pont De Nemours And Company Process for manufacturing gas permeation barrier material and structure

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
US6673701B1 (en) * 2002-08-27 2004-01-06 Micron Technology, Inc. Atomic layer deposition methods
CN101211759A (en) * 2006-12-28 2008-07-02 中芯国际集成电路制造(上海)有限公司 Capacitor, random memory cell and method for forming same
CN102201481A (en) * 2011-06-07 2011-09-28 合肥海润光伏科技有限公司 Novel N-type silicon hetero-junction battery with IBC (interdigitated back-contacted) structure and fabrication method thereof
CN102560419A (en) * 2011-11-29 2012-07-11 华东师范大学 Method for preparing alumina ultrathin film
US20130333835A1 (en) * 2012-06-14 2013-12-19 E I Du Pont De Nemours And Company Process for manufacturing gas permeation barrier material and structure

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111517345A (en) * 2020-05-25 2020-08-11 上海交通大学 Three-dimensional structure micron aluminum oxide tube and preparation method thereof
CN112802734A (en) * 2020-12-30 2021-05-14 长春长光圆辰微电子技术有限公司 Method for depositing single-side film of silicon wafer
CN114959646A (en) * 2022-04-08 2022-08-30 普乐新能源科技(徐州)有限公司 Excellent ALD coating process
CN116682894A (en) * 2023-07-28 2023-09-01 无锡松煜科技有限公司 Method for improving batch-to-batch uniformity of ALD passivation films of TOPCON battery and application
CN116682894B (en) * 2023-07-28 2023-11-17 无锡松煜科技有限公司 Method for improving batch-to-batch uniformity of ALD passivation films of TOPCON battery and application

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