CN112824559A - Method for depositing silicon-carbon-nitrogen-oxygen molecular film at low temperature - Google Patents
Method for depositing silicon-carbon-nitrogen-oxygen molecular film at low temperature Download PDFInfo
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- CN112824559A CN112824559A CN201911138117.5A CN201911138117A CN112824559A CN 112824559 A CN112824559 A CN 112824559A CN 201911138117 A CN201911138117 A CN 201911138117A CN 112824559 A CN112824559 A CN 112824559A
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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
- C23C16/308—Oxynitrides
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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
- C23C16/44—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
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Abstract
The invention discloses a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at low temperature, which comprises the steps of conveying a first precursor to a reaction chamber, wherein the first precursor is contacted with at least part of the surface of a substrate in the reaction chamber and reacts to generate an amino compound film; removing the unreacted first precursor on the surface of the substrate; conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film; and removing the unreacted second precursor, cooling the SiCON film in the reaction chamber to room temperature, and taking out the SiCON film, thereby achieving the technical effects of good quality, high stability, realization of low-temperature deposition and strong wet etching resistance of the SiCON film deposited on the high aspect ratio structure by adopting a molecular layer, and solving the technical problems of poor quality, poor stability and poor shape-preserving coverage of the structure of the film on the high aspect ratio structure in the prior art.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at low temperature.
Background
The deposition of thin films on the surface of substrates is a very important process step in many industrial processes. Silicon carbon nitrogen oxygen (SiCNO) thin film materials are often used as etch stop layers during semiconductor device fabrication due to their low dielectric constant. When the current semiconductor process node is reduced to below 10 nanometers, the requirement on the uniform shape-retaining property of a nano-scale film deposited on a high-aspect-ratio structure is higher and higher, and the silicon-carbon-oxygen-nitrogen film shows excellent shape-retaining coverage on the structure in this respect. However, the conventional methods for depositing the silicon-carbon-oxygen-nitrogen film have some defects in quality. For example, the use of a furnace tube to deposit a silicon-carbon-oxygen-nitrogen film requires a higher temperature (above 550 ℃), the deposited film cannot have a better composition ratio, and the deposited film has poor bondability with the underlying material, which affects the electrical performance stability and the wet etching resistance of the film material during FEOL heating cycles. Plasma Enhanced Chemical Vapor Deposition (PECVD) can be used to deposit SiCNO films at lower temperatures, but because of the directional deposition of the plasma during deposition, the conformal coverage of high aspect ratio structures is poor.
Disclosure of Invention
The embodiment of the invention provides a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at low temperature, which is used for solving the technical problems of poor quality, poor stability and poor coverage protection capability of a film structure on a high aspect ratio structure in the prior art, and achieves the technical effects of depositing a SiCON film with good quality on the high aspect ratio structure, high stability and strong wet etching resistance.
In order to solve the above problem, an embodiment of the present invention provides a method for depositing a silicon carbon nitrogen oxygen molecular film at a low temperature, where the method includes: conveying a first precursor to a reaction chamber, wherein the first precursor is in contact with at least part of the surface of a substrate in the reaction chamber and reacts to generate an amino compound film; removing the unreacted first precursor on the surface of the substrate; conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film; and removing the unreacted second precursor, cooling the SiCON film to room temperature in the reaction chamber, and taking out.
Preferably, the removing of the unreacted first precursor from the substrate surface includes: and introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber and the surface of the substrate, and removing the unreacted first precursor on the surface of the substrate.
Preferably, the removing of the unreacted second precursor includes: and introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber, and removing the unreacted second precursor.
Preferably, after the first precursor is conveyed to the reaction chamber, the surface of the substrate for generating the amine-based compound film is heated for the first time.
Preferably, after the second precursor is conveyed to the reaction chamber, the surface of the substrate for generating the SiCON film is heated for the second time.
Preferably, the temperature ranges of the first heating and the second heating are both 30-300 ℃.
Preferably, the first precursor contains a multifunctional amine group, wherein the molecular formula of the multifunctional amine group is
Wherein n in the molecular formula of the multifunctional amino is a positive integer.
Preferably, the second precursor contains a precursor of silicon atom, wherein the molecular formula of the second precursor is
Wherein n in the molecular formula of the second precursor is a positive integer, and y is an integer not greater than 3.
Preferably, the pressure of the reaction chamber is 0Torr to 300 Torr.
Preferably, the substrate is any one of silicon, silicon dioxide, SOI, germanium, gallium arsenide, glass, sapphire, or metal.
One or more technical solutions in the embodiments of the present invention at least have one or more of the following technical effects:
the embodiment of the invention provides a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at low temperature, which comprises the following steps: conveying a first precursor to a reaction chamber, wherein the first precursor is in contact with at least part of the surface of a substrate in the reaction chamber and reacts to generate an amino compound film; removing the unreacted first precursor on the surface of the substrate; conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film; and removing the unreacted second precursor, cooling the SiCON film to room temperature in the reaction chamber, and taking out. The method comprises the steps of reacting at least part of the surface of a substrate with a first precursor to generate an amino compound film, removing the unreacted first precursor, introducing a second precursor to react with the amino compound film to generate a SiCON film, wherein the SiCON film deposited by a molecular layer on a high aspect ratio structure has good quality and does not have directional deposition, so that the SiCON film has high stability, the heating temperature is 30-300 ℃ in the deposition process, the low-temperature deposition is realized, the technical effect of strong wet etching resistance is achieved, and the technical problems of poor quality, poor stability and poor shape-preserving covering capability of the structure of the film on the high aspect ratio structure in the prior art are solved.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
FIG. 1 is a flow chart of a method for low temperature deposition of silicon carbon nitrogen oxygen molecular films in an embodiment of the present disclosure.
Detailed Description
The embodiment of the invention provides a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at low temperature, which is used for solving the technical problems of poor quality, poor stability and poor coverage protection capability of a film structure on a high aspect ratio structure in the prior art, and achieves the technical effects of depositing a SiCON film with good quality on the high aspect ratio structure, high stability and strong wet etching resistance.
According to the technical scheme, a first precursor is conveyed to a reaction chamber, and the first precursor is contacted with at least part of the surface of a substrate in the reaction chamber and reacts to generate an amino compound film; removing the unreacted first precursor on the surface of the substrate; conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film; and removing the unreacted second precursor, cooling the SiCON film in the reaction chamber to room temperature, and taking out the SiCON film, so that the technical effects of depositing the SiCON film with good quality on a high aspect ratio structure, high stability and strong wet etching resistance are achieved.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
The embodiment of the present invention provides a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at a low temperature, please refer to fig. 1, which includes steps 110 to 140:
step 110: and conveying a first precursor to a reaction chamber, wherein the first precursor is in contact with at least part of the surface of the substrate in the reaction chamber and reacts to generate the amino compound film.
Step 120: and removing the unreacted first precursor on the surface of the substrate.
Further, after the first precursor is conveyed to the reaction chamber, the surface of the substrate for generating the amino compound film is heated for the first time. Further, the temperature ranges of the first heating and the second heating are both 30-300 ℃. Further, the removing the unreacted first precursor from the substrate surface includes: and introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber and the surface of the substrate, and removing the unreacted first precursor on the surface of the substrate. Further, the first precursor contains multifunctional amine group, wherein the molecular formula of the multifunctional amine group is
Wherein n in the molecular formula of the multifunctional amino is a positive integer. Further, the pressure of the reaction chamber is 0Torr to 300 Torr. Further, the substrate is any one of silicon, silicon dioxide, SOI, germanium, gallium arsenide, glass, sapphire, or metal.
Specifically, the method for depositing the silicon carbon nitrogen oxygen molecular film at the low temperature in the embodiment of the application deposits the SiCNO film by using a molecular layer deposition technology. Molecular layer deposition was originally used to deposit organic polymeric materials such as polyimides, polyamides, polyureas. For example, 1, 4-diisocyanatobutane is reacted in turn with various amine-based compounds such as ethylenediamine and tris (2-aminoethyl) amine in sequence to form a polyurea film. In addition, the silicon precursor containing reactive moieties of isocyanate groups, aldehyde or ketone groups, acid chloride groups and anhydride groups in the examples of this application are reacted alternately with various amines (e.g., ethylene diamine) to form molecular layer deposited films.
First, the isocyanate group-containing compound is reacted with an amine-based compound as follows:
secondly, the reaction of the compound containing aldehyde or ketone groups and amino groups is as follows:
third, the reaction of the acid chloride group with the amine compound is as follows:
fourth, the reaction of the compound containing an anhydride group with an amine group is as follows:
according to the embodiment of the application, two precursors are alternately introduced into the reaction chamber to react with the surface of the substrate, so that the film of the compound with the network structure containing silicon, carbon, oxygen and nitrogen elements is generated. That is, first, a first precursor containing a multifunctional amine group is delivered into the reaction chamber, and the first precursor and at least a part of the surface of the first precursor in the reaction chamber adsorb to form a layer of amine groups (NH)2) And a compound film, wherein after the first precursor is conveyed to the reaction chamber, the surface of a substrate for generating the amino compound film is subjected to first heating, and the first heating temperature range is 30-300 ℃. The pressure in the reaction chamber is controlled to be 0Torr to 300 Torr. The substrate refers to a surface formed by SiCON film in the deposition preparation process, and is selected from any one of silicon, silicon dioxide, SOI, germanium, gallium arsenide, glass, sapphire or metal. And introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber and the surface of the substrate, and removing the redundant first precursor containing the amino compound which is not deposited on the surface of the substrate.
Step 130: conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film;
step 140: and removing the unreacted second precursor, cooling the SiCON film to room temperature in the reaction chamber, and taking out.
Further, after the second precursor is conveyed to the reaction chamber, the surface of the substrate for generating the SiCON film is heated for the second time. Further, the removing the unreacted second precursor includes: and introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber, and removing the unreacted second precursor. Further, the second precursor contains a precursor of silicon atom, wherein the molecular formula of the second precursor is
Wherein n in the molecular formula of the second precursor is a positive integer, and y is an integer not greater than 3.
Specifically, a second precursor containing silicon atoms is delivered to the reaction chamber, and the second precursor is contacted with the amine-based compound film to react to form a new CN chemical bond, namely a SiCNO film. And (3) after the second precursor is conveyed to the reaction chamber, heating the surface of the substrate for the second time, wherein the temperature range of the second heating is 30-300 ℃. The pressure in the reaction chamber is controlled to be 0Torr to 300 Torr. And introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber, removing the unreacted second precursor containing silicon in the reaction chamber, and circulating the steps for many times, namely alternately introducing the first precursor and the second precursor, and purging the reaction chamber by using the inert gas or the nitrogen, so that the SiCNO film with the ideal thickness can be obtained at a lower temperature. And cooling the SiCON film to room temperature in the reaction chamber, and taking the SiCON film out of the reaction chamber.
The technical scheme provided in the embodiment of the application at least has the following technical effects or advantages:
the embodiment of the invention provides a method for depositing a silicon-carbon-nitrogen-oxygen molecular film at low temperature, which comprises the following steps: conveying a first precursor to a reaction chamber, wherein the first precursor is in contact with at least part of the surface of a substrate in the reaction chamber and reacts to generate an amino compound film; removing the unreacted first precursor on the surface of the substrate; conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film; and removing the unreacted second precursor, cooling the SiCON film to room temperature in the reaction chamber, and taking out. The method comprises the steps of reacting at least part of the surface of a substrate with a first precursor to generate an amino compound film, removing the unreacted first precursor, introducing a second precursor to react with the amino compound film to generate a SiCON film, wherein the SiCON film deposited by a molecular layer on a high aspect ratio structure has good quality and does not have directional deposition, so that the SiCON film has high stability, the heating temperature is 30-300 ℃ in the deposition process, the low-temperature deposition is realized, the technical effect of strong wet etching resistance is achieved, and the technical problems of poor quality, poor stability and poor shape-preserving covering capability of the structure of the film on the high aspect ratio structure in the prior art are solved.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made in the embodiments of the present invention without departing from the spirit or scope of the embodiments of the invention. Thus, if such modifications and variations of the embodiments of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to encompass such modifications and variations.
Claims (10)
1. A method for depositing a silicon carbon nitrogen oxygen molecular film at low temperature is characterized by comprising the following steps:
conveying a first precursor to a reaction chamber, wherein the first precursor is in contact with at least part of the surface of a substrate in the reaction chamber and reacts to generate an amino compound film;
removing the unreacted first precursor on the surface of the substrate;
conveying a second precursor to the reaction chamber, wherein the second precursor is in contact with the amino compound film and reacts to generate a SiCON film;
and removing the unreacted second precursor, cooling the SiCON film to room temperature in the reaction chamber, and taking out.
2. The method of claim 1, wherein the removing of the unreacted first precursor from the substrate surface comprises:
and introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber and the surface of the substrate, and removing the unreacted first precursor on the surface of the substrate.
3. The method of claim 1, wherein the removing of the unreacted second precursor comprises:
and introducing inert gas or nitrogen into the reaction chamber to purge the reaction chamber, and removing the unreacted second precursor.
4. The method of claim 1, wherein the surface of the substrate on which the amine-based compound film is formed is heated for a first time after the first precursor is delivered to the reaction chamber.
5. The method of claim 4, wherein the second heating of the surface of the substrate on which the SiCON film is formed is performed after the second precursor is delivered to the reaction chamber.
6. The method of claim 5, wherein the first heating and the second heating are both at a temperature ranging from 30 ℃ to 300 ℃.
7. The method of claim 1, wherein the first precursor comprises a multifunctional amine group, wherein the multifunctional amine group has the formula
Wherein n in the molecular formula of the multifunctional amino is a positive integer.
8. The method of claim 1, wherein the second precursor comprises a precursor of silicon atoms, wherein the second precursor has a formula of
Wherein n in the molecular formula of the second precursor is a positive integer, and y is an integer not greater than 3.
9. The method of claim 1, wherein the pressure in the reaction chamber is 0to 300 Torr.
10. The method of claim 1, wherein the substrate is any one of silicon, silicon dioxide, SOI, germanium, gallium arsenide, glass, sapphire, or metal.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160024647A1 (en) * | 2014-07-26 | 2016-01-28 | Applied Materials, Inc. | Low Temperature Molecular Layer Deposition Of SiCON |
| US20160099146A1 (en) * | 2014-10-03 | 2016-04-07 | Applied Materials, Inc. | Precursors Suitable For High Temperature Atomic Layer Deposition Of Silicon-Containing Films |
| TW201614713A (en) * | 2014-07-19 | 2016-04-16 | Applied Materials Inc | Carbon and/or nitrogen incorporation in silicon-based films using silicon precursors with organic co-reactants by pe-ald |
| US20170323775A1 (en) * | 2016-05-06 | 2017-11-09 | Applied Materials, Inc. | Methods of Depositing SiCON with C, O and N Compositional Control |
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- 2019-11-20 CN CN201911138117.5A patent/CN112824559A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW201614713A (en) * | 2014-07-19 | 2016-04-16 | Applied Materials Inc | Carbon and/or nitrogen incorporation in silicon-based films using silicon precursors with organic co-reactants by pe-ald |
| US20160024647A1 (en) * | 2014-07-26 | 2016-01-28 | Applied Materials, Inc. | Low Temperature Molecular Layer Deposition Of SiCON |
| TW201610204A (en) * | 2014-07-26 | 2016-03-16 | 應用材料股份有限公司 | Low temperature molecular layer deposition of SiCON |
| US20160099146A1 (en) * | 2014-10-03 | 2016-04-07 | Applied Materials, Inc. | Precursors Suitable For High Temperature Atomic Layer Deposition Of Silicon-Containing Films |
| US20170323775A1 (en) * | 2016-05-06 | 2017-11-09 | Applied Materials, Inc. | Methods of Depositing SiCON with C, O and N Compositional Control |
| TW201816166A (en) * | 2016-05-06 | 2018-05-01 | 應用材料股份有限公司 | Methods of depositing SiCON with c, o and n compositional control |
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