US20020106898A1 - Methods for removing silicon-oxy-nitride layer and wafer surface cleaning - Google Patents
Methods for removing silicon-oxy-nitride layer and wafer surface cleaningDownload PDFInfo
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- US20020106898A1 US20020106898A1US09/776,738US77673801AUS2002106898A1US 20020106898 A1US20020106898 A1US 20020106898A1US 77673801 AUS77673801 AUS 77673801AUS 2002106898 A1US2002106898 A1US 2002106898A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/311—Etching the insulating layers by chemical or physical means
- H01L21/31105—Etching inorganic layers
- H01L21/31111—Etching inorganic layers by chemical means
Definitions
- the present inventionrelates to methods for removing a silicon-oxy-nitride layer from a semiconductor substrate and wafer surface cleaning, and more particularly to methods for removing a silicon-oxy-nitride layer without residual oxide and wafer surface cleaning.
- Silicon-oxy-nitride (SiO X N Y ) layers formed over polysilicon layers used as gate electrodes in semiconductor devicesare commonly used as bottom anti-reflective coating (BARC) layers.
- BARC layersare formed over the polysilicon layers before forming photoresist layers used to define the gate electrodes, and they prevent reflection of actinic light used to expose the photoresist layers from their surfaces.
- the processing set forthis extremely crucial for the manufacturing techniques of very large scale integrated circuit (VLSI) and ultra large scale integrated circuit (ULSI) .
- the silicon-oxy-nitride layeris removed by using a dry etching process or a wet etching process used a heated phosphorus acid (H 3 PO 4 ) solution.
- H 3 PO 4heated phosphorus acid
- the silicon-oxy-nitride layermust be removed completely by using the heated H 3 PO 4 solution.
- the silicon-oxy-nitride layeris usually difficult to remove completely as they contain oxide composition therein.
- plasma of the dry etching processmay cause undesired damages that may induce device failure. Therefore, it is very necessary to provide a new option to remove the silicon-oxy-nitride layers without the problems mentioned above.
- SC 1Standard clean 1
- SC 2standard clean 2
- SC 1standard clean 1
- SC 2standard clean 2
- SC 1standard clean 1
- SC 2standard clean 2
- the SC 1 solutioncomprises a hot aqueous mixture of ammonium hydroxide, hydrogen peroxide, and water (1:1:5 of 30% H 2 O 2 , 28% NH 4 OH and H 2 O)
- the SC 2 solutioncomprises a hot acid mixture of hydrogen peroxide, hydrochloric acid and water (1:1:5 of 30% H 2 O 2 , 37% HC 1 and H 2 O)
- Both the SC 1 and SC 2 solutionscontain hydrogen peroxide, which easily react with silicon atoms of the wafer surface to form chemical oxide layers.
- these chemical oxide layersare removed by using dilute hydrofluoric (DHF) acid, but the DHF acid causes the formation of a hydrogen-terminated or hydrogen-passivated layer.
- DHFdilute hydrofluoric
- the undesired hydrogen-terminated layeris hydrophobic and susceptible to particle contamination which will result in defects of the following formed films.
- the hydrogen-passivated layereasily causes the formation of a native oxide layer when a wafer is exposed in the atmosphere. Especially during wafer transport in the clean room or reactor pump down, silicon atoms of the wafer surface having dangling bonds will adsorb hydrogen atoms to form a hydrophobic hydrogen-terminated surface. In this manner, oxygen will bond with silicon atoms to form an undesired native oxide layer.
- FIG. 1Ashows the growth of the native oxide layer on a hydrogen-terminated surface of a silicon wafer exposed in the atmosphere.
- hydroxyl or oxygen atomwill bond with silicon atoms of the wafer surface to form an oxygen-terminated or hydroxyl-terminated layer as shown in FIG. 1B.
- Silicon-hydroxyl groups formed by physically adsorbed water molecules undergoing dissociative chemisorption on silicon atomsact as adsorption sites for additional water molecules and result in further oxidation.
- EGethylene glycol
- HFhydrogen fluoride
- a mixture solution of ethylene glycol and hydrogen fluorideto replace the conventional one used a solution of HF and H 2 O (Dilute HF Solution) to effectively reduce the formation of undesired hydrophobic hydrogen-terminated layers on the wafer surface, therefore avoid particle contaminations and water absorption.
- the inventionuse utilizes a solution of ethylene glycol and hydrogen fluoride to completely remove the silicon-oxy-nitride layer from a substrate without residual oxide.
- the method for wafer surface cleaningalso uses a solution of ethylene glycol and hydrogen fluoride to remove chemical oxide or native oxide from wafer surfaces and an ethylene glycol solvent to rinse the wafer surfaces.
- FIG. 1Ashows the growth of a native oxide layer on a hydrogen-terminated surface of a silicon wafer exposed in the atmosphere
- FIG. 1Bshows a native oxide layer on a oxygen-terminated and hydroxyl-terminated surface of a silicon wafer
- FIG. 2shows the process flow diagram of the wafer surface cleaning of this invention.
- the inventionuses a mixture solution of ethylene glycol and hydrogen fluoride as a new etching solution of a silicon-oxy-nitride layer and a new wafer surface cleaning solution in modern semiconductor process.
- a mixture solution of ethylene glycol and hydrogen fluoridecan completely remove a deposited silicon-oxy-nitride layer from a semiconductor substrate whereas the conventional heated phosphorus acid solution can not. Because the silicon-oxy-nitride layer always contains oxide which can not be effectively removed by the heated phosphorus acid solution.
- the mixture solution of ethylene glycol and hydrogen fluoride of the inventionis used to replace the dilute hydrofluoric acid solution used to remove a native oxide layer and a chemical oxide layer. It is found that ethylene glycol can vary the hydroxyl radical and dissolved oxygen concentrations, which are known to affect the oxidation kinetics of hydrophobic hydrogen-terminated layers, and is expected to aid the creation of a uniform, oxide-free surface since ethylene glycol is an effective wetting agent.
- the silicon-oxy-nitride layeris used as a bottom anti-reflective coating layer also known as a BARC layer.
- the BARC layeris deposited on a semiconductor substrate having a conductive layer thereon used as a gate electrode to improve the critical dimension control of the gate electrode in a photolithography process.
- the semiconductor substrateis preferably a silicon substrate with a ⁇ 100> crystal orientation.
- the conductive layeris preferably a polysilicon layer.
- the silicon-oxy-nitride layercan be formed by using a conventional chemical vapor deposition (CVD) process, and is preferably a plasma enhanced chemical vapor deposition (PECVD) process.
- CVDchemical vapor deposition
- PECVDplasma enhanced chemical vapor deposition
- a photoresist layeris formed on the silicon-oxy-nitride layer.
- the gate electrodecan be defined by using a conventional photolithography process. After defining the gate electrode, the photoresist layer is firstly stripped. Then the BARC layer must be removed completely for further processing. The BARC layer is removed by immersing the semiconductor substrate in a mixture solution of ethylene glycol and hydrogen fluoride. Ethylene glycol is used as a solvent and hydrogen fluoride is a solute.
- the concentration of hydrogen fluorideis about 2 to about 6 percent by volume, and is preferably about 4 percent.
- the etching temperatureis in the range of about 30° C. to about 90° C. It is found that as the concentration of hydrogen fluoride increases, the etching rate of oxide in the silicon-oxy-nitride layer also raises.
- the solution of ethylene glycol and hydrogen fluoride of the inventionis used to clean wafers.
- the wafer surface cleaning proceduresby using the standard cleaning recipes SC 1 and SC 2 leave the cleaned wafer surface with an undesired chemical oxide layer of about 15 angstroms, which is harmful to the sequential growth of an epitaxial silicon layer or a silicon dioxide layer and usually lead to a high contact resistance and device failures.
- a dilute hydrofluoric acid (DHF) aqueous solution with a mixing ratio of 1:100is utilized to remove the chemical oxide layer before performing a further process.
- DHFdilute hydrofluoric acid
- the DHF solution treatmentalways leaves the treated wafer with a hydrogen-terminated surface, which is hydrophobic and susceptible to adsorb contaminant particles. It is found that the growth of the hydrogen-terminated surface strongly depends on the concentrations of hydroxyl and dissolved oxygen and ethylene glycol can effectively vary the hydroxyl and dissolved oxygen concentrations and hence affect the oxidation kinetics of a hydrogen-terminated surface. Also, the solution of ethylene glycol and hydrogen fluoride provides less hydrogen-termination than the aqueous DHF solution. In addition, fluoric ions in the solution of ethylene glycol and hydrogen fluoride can react with hydrogen fluoride to form HF 2 ⁇ which is thought to play a role in the uniformity of silicon dioxide etching. Thus the treatment of wafer surfaces by using the solution of ethylene glycol and hydrogen fluoride produces silicon surfaces that are smoother and less prone to particulate contamination.
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Abstract
Description
- 1. Field of the Invention[0001]
- The present invention relates to methods for removing a silicon-oxy-nitride layer from a semiconductor substrate and wafer surface cleaning, and more particularly to methods for removing a silicon-oxy-nitride layer without residual oxide and wafer surface cleaning.[0002]
- 2. Description of the Related Art[0003]
- Silicon-oxy-nitride (SiO[0004]XNY) layers formed over polysilicon layers used as gate electrodes in semiconductor devices are commonly used as bottom anti-reflective coating (BARC) layers. The BARC layers are formed over the polysilicon layers before forming photoresist layers used to define the gate electrodes, and they prevent reflection of actinic light used to expose the photoresist layers from their surfaces. The processing set forth is extremely crucial for the manufacturing techniques of very large scale integrated circuit (VLSI) and ultra large scale integrated circuit (ULSI) . After the lithography process defined the gate electrodes, the silicon-oxy-nitride layer is removed by using a dry etching process or a wet etching process used a heated phosphorus acid (H3PO4) solution. In addition, when the quality of the deposited silicon-oxy-nitride layer is unqualified, the silicon-oxy-nitride layer must be removed completely by using the heated H3PO4solution. However, the silicon-oxy-nitride layer is usually difficult to remove completely as they contain oxide composition therein. Furthermore, plasma of the dry etching process may cause undesired damages that may induce device failure. Therefore, it is very necessary to provide a new option to remove the silicon-oxy-nitride layers without the problems mentioned above.
- Standard clean[0005]1 (SC1) or RCA1 and standard clean2 (SC2) or RCA2 are almost the standard cleaning techniques and recipes throughout the integrated circuit processing. The SC1 solution comprises a hot aqueous mixture of ammonium hydroxide, hydrogen peroxide, and water (1:1:5 of 30% H2O2, 28% NH4OH and H2O) and the SC2 solution comprises a hot acid mixture of hydrogen peroxide, hydrochloric acid and water (1:1:5 of 30% H2O2, 37% HC1 and H2O) Both the SC1 and SC2 solutions contain hydrogen peroxide, which easily react with silicon atoms of the wafer surface to form chemical oxide layers. Usually, these chemical oxide layers are removed by using dilute hydrofluoric (DHF) acid, but the DHF acid causes the formation of a hydrogen-terminated or hydrogen-passivated layer. The undesired hydrogen-terminated layer is hydrophobic and susceptible to particle contamination which will result in defects of the following formed films.
- The hydrogen-passivated layer easily causes the formation of a native oxide layer when a wafer is exposed in the atmosphere. Especially during wafer transport in the clean room or reactor pump down, silicon atoms of the wafer surface having dangling bonds will adsorb hydrogen atoms to form a hydrophobic hydrogen-terminated surface. In this manner, oxygen will bond with silicon atoms to form an undesired native oxide layer. FIG. 1A shows the growth of the native oxide layer on a hydrogen-terminated surface of a silicon wafer exposed in the atmosphere. Besides, as a wafer is immersed in water or rinsed by deionized (DI) water, hydroxyl or oxygen atom will bond with silicon atoms of the wafer surface to form an oxygen-terminated or hydroxyl-terminated layer as shown in FIG. 1B. Silicon-hydroxyl groups formed by physically adsorbed water molecules undergoing dissociative chemisorption on silicon atoms act as adsorption sites for additional water molecules and result in further oxidation.[0006]
- After performing wafer surface cleaning procedures by using the SC[0007]1 and SC2 solutions to clean wafers or the DHF acid to remove the native oxide and the chemical oxide, DI water is often used sequentially by the semiconductor industry to rinse the wafers. According to the phenomenon mentioned above, a native oxide layer is very likely formed again after performing the standard or conventional wafer surface cleaning procedures. Moreover, in the following dry procedure, however, undesired contaminations, such as water marks, particles and even silicon powders may be induced. Therefore, it is necessary to provide a new wafer surface cleaning method to replace the conventional one without the problems set forth.
- It is therefore an object of the invention to provide a mixture solution of ethylene glycol (EG) and hydrogen fluoride (HF) to replace the conventional wet etching solution to completely remove a silicon-oxy-nitride layer containing oxide.[0008]
- It is another object of this invention to provide a wet etching process used a mixture solution of ethylene glycol and hydrogen fluoride to replace the conventional dry etching process to remove silicon-oxy-nitride layer without plasma damages.[0009]
- It is a further object of this invention to provide a method for wafer surface cleaning used a mixture solution of ethylene glycol and hydrogen fluoride to replace the conventional one used a solution of HF and H[0010]2O (Dilute HF Solution) to effectively reduce the formation of undesired hydrophobic hydrogen-terminated layers on the wafer surface, therefore avoid particle contaminations and water absorption.
- It is another object of this invention to provide a method for wafer surface cleaning used a mixture solution of ethylene glycol and hydrogen fluoride to replace the conventional one used a solution of HF and H[0011]2O to reduce wafer surface roughness and prevent water marks.
- To achieve these objects, and in accordance with the purpose of the invention, the invention use utilizes a solution of ethylene glycol and hydrogen fluoride to completely remove the silicon-oxy-nitride layer from a substrate without residual oxide. Moreover, the method for wafer surface cleaning also uses a solution of ethylene glycol and hydrogen fluoride to remove chemical oxide or native oxide from wafer surfaces and an ethylene glycol solvent to rinse the wafer surfaces.[0012]
- It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.[0013]
- The foregoing aspects and many of the attendant advantages of this invention will become more readily appreciated as the same becomes better understood by reference to the following detailed description, when taken in conjunction with the accompanying drawings, wherein:[0014]
- FIG. 1A shows the growth of a native oxide layer on a hydrogen-terminated surface of a silicon wafer exposed in the atmosphere;[0015]
- FIG. 1B shows a native oxide layer on a oxygen-terminated and hydroxyl-terminated surface of a silicon wafer; and[0016]
- FIG. 2 shows the process flow diagram of the wafer surface cleaning of this invention.[0017]
- The invention uses a mixture solution of ethylene glycol and hydrogen fluoride as a new etching solution of a silicon-oxy-nitride layer and a new wafer surface cleaning solution in modern semiconductor process. As an etching solution of a silicon-oxy-nitride layer, the mixture solution of ethylene glycol and hydrogen fluoride can completely remove a deposited silicon-oxy-nitride layer from a semiconductor substrate whereas the conventional heated phosphorus acid solution can not. Because the silicon-oxy-nitride layer always contains oxide which can not be effectively removed by the heated phosphorus acid solution.[0018]
- As a wafer surface cleaning solution, the mixture solution of ethylene glycol and hydrogen fluoride of the invention is used to replace the dilute hydrofluoric acid solution used to remove a native oxide layer and a chemical oxide layer. It is found that ethylene glycol can vary the hydroxyl radical and dissolved oxygen concentrations, which are known to affect the oxidation kinetics of hydrophobic hydrogen-terminated layers, and is expected to aid the creation of a uniform, oxide-free surface since ethylene glycol is an effective wetting agent.[0019]
- In modern deep-submicron integrated circuit process, the application of the solution of ethylene glycol and hydrogen fluoride as a new etching solution of a silicon-oxy-nitride layer will be described hereinafter. In this embodiment, the silicon-oxy-nitride layer is used as a bottom anti-reflective coating layer also known as a BARC layer. The BARC layer is deposited on a semiconductor substrate having a conductive layer thereon used as a gate electrode to improve the critical dimension control of the gate electrode in a photolithography process. The semiconductor substrate is preferably a silicon substrate with a <100> crystal orientation. The conductive layer is preferably a polysilicon layer. The silicon-oxy-nitride layer can be formed by using a conventional chemical vapor deposition (CVD) process, and is preferably a plasma enhanced chemical vapor deposition (PECVD) process. To define the gate electrode, a photoresist layer is formed on the silicon-oxy-nitride layer. The gate electrode can be defined by using a conventional photolithography process. After defining the gate electrode, the photoresist layer is firstly stripped. Then the BARC layer must be removed completely for further processing. The BARC layer is removed by immersing the semiconductor substrate in a mixture solution of ethylene glycol and hydrogen fluoride. Ethylene glycol is used as a solvent and hydrogen fluoride is a solute. The concentration of hydrogen fluoride is about 2 to about 6 percent by volume, and is preferably about 4 percent. The etching temperature is in the range of about 30° C. to about 90° C. It is found that as the concentration of hydrogen fluoride increases, the etching rate of oxide in the silicon-oxy-nitride layer also raises.[0020]
- The embodiment set forth is an example only, and it should not be treated as confinements of the scope and spirit of the invention. In stead, the solution of ethylene glycol and hydrogen fluoride of the invention can be used to etch or completely remove any silicon-oxy-nitride layer in semiconductor processes.[0021]
- In another embodiment, the solution of ethylene glycol and hydrogen fluoride of the invention is used to clean wafers. According to the description of the related art, the wafer surface cleaning procedures by using the standard cleaning recipes SC[0022]1 and SC2 leave the cleaned wafer surface with an undesired chemical oxide layer of about 15 angstroms, which is harmful to the sequential growth of an epitaxial silicon layer or a silicon dioxide layer and usually lead to a high contact resistance and device failures. Conventionally, a dilute hydrofluoric acid (DHF) aqueous solution with a mixing ratio of 1:100 is utilized to remove the chemical oxide layer before performing a further process. The DHF solution treatment always leaves the treated wafer with a hydrogen-terminated surface, which is hydrophobic and susceptible to adsorb contaminant particles. It is found that the growth of the hydrogen-terminated surface strongly depends on the concentrations of hydroxyl and dissolved oxygen and ethylene glycol can effectively vary the hydroxyl and dissolved oxygen concentrations and hence affect the oxidation kinetics of a hydrogen-terminated surface. Also, the solution of ethylene glycol and hydrogen fluoride provides less hydrogen-termination than the aqueous DHF solution. In addition, fluoric ions in the solution of ethylene glycol and hydrogen fluoride can react with hydrogen fluoride to form HF2− which is thought to play a role in the uniformity of silicon dioxide etching. Thus the treatment of wafer surfaces by using the solution of ethylene glycol and hydrogen fluoride produces silicon surfaces that are smoother and less prone to particulate contamination.
- The application of the wafer surface cleaning procedure of the invention will be described hereinafter. In a common wafer-cleaning recipe, after performing the RCA clean process on a silicon wafer by using the SC[0023]1 and SC2 solutions, the silicon wafer is rinsed by using DI water. Then the wafer is immersed in the solution of ethylene glycol and hydrogen fluoride to remove the oxide layer. The concentration of hydrogen fluoride is about 2 to about 6 percent by volume, and is preferably about 4 percent. The clean temperature is about 20° C. to 30° C. Next an ethylene glycol solvent is used to rinse the wafer. In this manner, the invention provides the cleaned wafer with a smooth surface, meanwhile, less particles and no water mark appear. The process flow is shown in FIG. 2.
- Other embodiments of the invention will appear to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples to be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.[0024]
Claims (14)
1. A method for removing a silicon-oxy-nitride layer, said method comprising:
providing a substrate having a silicon-oxy-nitride layer thereon;
and immersing said substrate in a solution of ethylene glycol and hydrogen fluoride at a temperature.
2. The method according toclaim 1 , wherein said solution comprises about 2 percent to about 6 percent hydrogen fluoride by volume.
3. The method according toclaim 1 , wherein said solution comprises about 94 percent to about 98 percent ethylene glycol by volume.
4. The method according toclaim 1 , wherein said temperature is in a range of about 30° C. to about 90° C.
5. A method for wafer surface cleaning, said method comprising:
providing a wafer surface;
rinsing said wafer surface by using deionized water;
immersing said wafer surface in a solution of ethylene glycol and hydrogen fluoride;
displacing said wafer surface from said solution; and
rinsing said wafer surface by using a ethylene glycol solvent.
6. The method according toclaim 5 , wherein said wafer surface is a silicon wafer surface.
7. The method according toclaim 5 , wherein said solution comprises about 2 percent to about 6 percent hydrogen fluoride by volume.
8. The method according toclaim 5 , wherein said solution comprises about 94 percent to about 98 percent ethylene glycol by volume.
9. A method for wafer surface cleaning, said method comprising:
providing a wafer surface;
cleaning said wafer surface by using a first solution;
rinsing said wafer surface by using deionized water;
cleaning said wafer surface by using a second solution;
rinsing said wafer surface by using deionized water;
immersing said wafer surface in a solution of ethylene glycol and hydrogen fluoride;
displacing said wafer surface from said solution; and
rinsing said wafer surface by using a ethylene glycol solvent.
10. The method according toclaim 9 , wherein said wafer surface is a silicon wafer surface.
11. The method according toclaim 9 , wherein said first solution is a standard clean 1 solution.
12. The method according toclaim 9 , wherein said second solution is a standard clean 2 solution.
13. The method according toclaim 9 , wherein said solution comprises about 2 percent to about 6 percent hydrogen fluoride by volume.
14. The method according toclaim 9 , wherein said solution comprises about 94 percent to about 98 percent ethylene glycol by volume.
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| US20120027956A1 (en)* | 2010-07-29 | 2012-02-02 | International Business Machines Corporation | Modification of nitride top layer |
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| US20150214068A1 (en)* | 2014-01-24 | 2015-07-30 | United Microelectronics Corp. | Method of performing etching process |
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| US5939336A (en)* | 1998-08-21 | 1999-08-17 | Micron Technology, Inc. | Aqueous solutions of ammonium fluoride in propylene glycol and their use in the removal of etch residues from silicon substrates |
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- 2001-02-05USUS09/776,738patent/US6444582B1/ennot_activeExpired - Lifetime
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| US20120027956A1 (en)* | 2010-07-29 | 2012-02-02 | International Business Machines Corporation | Modification of nitride top layer |
| US20150214068A1 (en)* | 2014-01-24 | 2015-07-30 | United Microelectronics Corp. | Method of performing etching process |
| US9385000B2 (en)* | 2014-01-24 | 2016-07-05 | United Microelectronics Corp. | Method of performing etching process |
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| CN116759295A (en)* | 2023-08-14 | 2023-09-15 | 天府兴隆湖实验室 | Silicon wafer cleaning method and silicon wafer cleaning equipment |
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| US6444582B1 (en) | 2002-09-03 |
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