CN108447770B - Preparation method of silicon dioxide film - Google Patents
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- CN108447770B CN108447770B CN201810190973.4A CN201810190973A CN108447770B CN 108447770 B CN108447770 B CN 108447770B CN 201810190973 A CN201810190973 A CN 201810190973A CN 108447770 B CN108447770 B CN 108447770B
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- H01L21/02164—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon oxide, e.g. SiO2
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- 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
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- 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
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- H01L21/02238—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor silicon in uncombined form, i.e. pure silicon
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Abstract
The invention provides a preparation method of a silicon dioxide film. First, a silicon substrate is provided. Secondly, the silicon substrate is placed into an oxidation furnace, and the temperature in the oxidation furnace is 1000-1200 ℃. Then, oxygen is introduced into the oxidation furnace, and the flow rate of the oxygen is 9slm/min-10 slm/min. And introducing oxygen into the oxidation furnace for 4-6 min, introducing hydrogen into the oxidation furnace and igniting, wherein the flow of the hydrogen is 14-14.6 slm/min, and forming a first silicon dioxide layer on the surface of the silicon substrate.
Description
Technical Field
The invention relates to an electronic semiconductor process, in particular to a preparation method of a silicon dioxide film.
Background
In semiconductor manufacturing technology, oxidation and Chemical Vapor Deposition (CVD) are commonly used for the preparation of thin films. The thermal oxidation method is a method of forming a silicon dioxide film on the surface of a silicon wafer at a high temperature. The purpose of the thermal oxidation is to produce a silicon dioxide film with certain quality requirements on a silicon wafer, and the silicon dioxide film plays roles of protecting, passivating, insulating, buffering a medium and the like on the silicon wafer or a device.
In the existing semiconductor device manufacturing process, a wet oxygen process is commonly used, i.e. a silicon dioxide film is grown on a silicon substrate by carrying high-temperature water vapor with oxygen. In the wet oxygen process, the purity of high-temperature water vapor has an important influence on the process quality, and the low purity of the water vapor can cause the high impurity content of the silicon dioxide film and the poor film quality. To increase the purity of water, high purity water is often produced by combustion of hydrogen with oxygen (oxyhydrogen synthesis). In addition, the flow rate of oxygen and the flow rate of hydrogen also have important effects on the generation rate of the silica film and the uniformity of the silica film during the silica film preparation process.
Disclosure of Invention
In view of the above, it is necessary to provide a method for preparing a silica thin film, which can improve the growth rate and uniformity of the silica thin film.
The invention provides a preparation method of a silicon dioxide film, which comprises the following steps:
s100, providing a silicon substrate;
s200, putting the silicon substrate into an oxidation furnace, and heating the temperature in the oxidation furnace to a reaction temperature of 1000-1200 ℃;
s300, introducing oxygen into the oxidation furnace, wherein the flow rate of the oxygen is 9slm/min-10 slm/min; and
s400, introducing oxygen into the oxidation furnace for 4-6 min, introducing hydrogen into the oxidation furnace and igniting, wherein the flow rate of the hydrogen is 14-14.6 slm/min, and forming a first silicon dioxide layer on the surface of the silicon substrate.
In one embodiment, the S400 includes:
s410, introducing oxygen into the oxidation furnace for 4-6 min, and then beginning to introduce hydrogen into the oxidation furnace, wherein the flow rate of the hydrogen is 4-8 slm/min;
and S420, introducing hydrogen into the oxidation furnace for 0.5-1.5 min, adjusting the flow of the hydrogen to 14-14.6 slm/min, and forming a first silicon dioxide layer on the surface of the silicon substrate.
In one embodiment, in S300, the oxygen flow rate is 9.53 slm/min.
In one embodiment, in S400, the hydrogen flow rate is 14.3 slm/min.
In one embodiment, the S200 includes:
the S200 includes:
s210, providing an oxidation furnace, heating the oxidation furnace to a pretreatment temperature, wherein the pretreatment temperature is 800-900 ℃;
s220, after the temperature of the oxidation furnace is raised to the pretreatment temperature, putting the silicon substrate into the oxidation furnace, and introducing nitrogen into the oxidation furnace;
s230, keeping the pretreatment temperature for 20-40 min, cutting off nitrogen and raising the temperature in the oxidation furnace from the pretreatment temperature to a reaction temperature, wherein the reaction temperature is 1000-1200 ℃.
In one embodiment, the S300 includes:
s310, when the temperature in the oxidation furnace is increased from the pretreatment temperature to the reaction temperature, introducing oxygen into the oxidation furnace, wherein the flow rate of the oxygen is 10slm/min-15 slm/min;
s320, after the temperature in the oxidation furnace is increased to the reaction temperature, adjusting the flow of the oxygen to be 9slm/min-10slm/min, and forming a second silicon dioxide layer on the surface of the silicon substrate, wherein the second silicon dioxide layer is arranged between the first silicon oxide layer and the silicon substrate.
In one embodiment, after S400, S500 is further included, hydrogen is cut off, oxygen is continuously introduced into the oxidation furnace, the flow rate of the oxygen is 9slm/min to 10slm/min, and a third silicon dioxide layer is formed on the surface of the first silicon dioxide layer away from the silicon substrate.
In one embodiment, S100 is followed by S110, and the silicon substrate is cleaned by a cleaning solution.
In one embodiment, the cleaning liquid is H2SO4\H2O2Mixed solution of (3), NH4OH\H2O2\H2O mixed solution, HC L \ H2O2\H2One or more of an O mixed solution and an HF solution.
In one embodiment, the method further comprises S600, and after the first silicon dioxide layer is prepared, the temperature in the oxidizing furnace is reduced to 800-900 ℃ for 60-70 min.
In the preparation method of the silicon dioxide film provided by the invention, high-purity water vapor is generated by the reaction of oxygen with the flow rate of 9slm/min-10slm/min and hydrogen with the flow rate of 14slm/min-14.6slm/min at the reaction temperature of 1000-1200 ℃. And the water vapor reaches the surface of the silicon substrate in a diffusion mode and reacts with silicon on the surface of the silicon substrate rapidly to generate a first silicon dioxide layer. The hydrogen is in the flow of 14slm/min-14.6slm/min, the flow rate of the hydrogen and the oxygen is proper when the oxygen is in the flow of 9slm/min-10slm/min, and a better reaction atmosphere is arranged in the oxidation furnace, so that the first silicon dioxide layer can be quickly and efficiently prepared, and the uniformity of the prepared first silicon dioxide layer is greatly improved.
Drawings
FIG. 1 is a flow chart of a method for forming a silicon dioxide film according to an embodiment of the present invention;
FIG. 2 is a schematic process reaction diagram of a method for preparing a silicon dioxide film according to an embodiment of the present invention;
FIG. 3 is a schematic process reaction diagram of a method for preparing a silicon dioxide film according to another embodiment of the present invention;
FIG. 4 is a schematic process reaction diagram of a method for preparing a silicon dioxide film according to an embodiment of the present invention;
FIG. 5 is a schematic process reaction diagram of a method for preparing a silicon dioxide film according to an embodiment of the present invention;
FIG. 6 is a schematic temperature process diagram of a method for forming a silicon dioxide film according to an embodiment of the present invention.
Description of the reference numerals
110: silicon substrate
120: first silicon dioxide layer
130: second silicon dioxide layer
140: a third silicon dioxide layer
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the following will explain in detail the preparation method of the silicon dioxide thin film of the present invention by way of examples, with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The following describes the method for preparing a silica film according to an embodiment of the present invention in detail with reference to the accompanying drawings.
Referring to fig. 1 and 2, an embodiment of the present invention provides a method for preparing a silicon dioxide thin film, which includes the following steps:
s100, providing a silicon substrate 110;
s200, putting the silicon substrate 110 into an oxidation furnace, and heating the temperature in the oxidation furnace to a reaction temperature, wherein the reaction temperature is 1000-1200 ℃;
s300, introducing oxygen into the oxidation furnace, wherein the flow rate of the oxygen is 9slm/min-10 slm/min; and
s400, introducing oxygen into the oxidation furnace for 4-6 min, introducing hydrogen into the oxidation furnace and igniting, wherein the flow rate of the hydrogen is 14-14.6 slm/min, and forming a first silicon dioxide layer 120 on the surface of the silicon substrate 110.
In S100, the silicon substrate 110 may be a P-type silicon wafer or an N-type silicon wafer. The size, thickness and shape of the silicon substrate 110 are not limited and can be selected according to actual needs. In one embodiment, the silicon substrate 110 is 400-600 um thick.
In the S200, the oxidation furnace is an apparatus for preparing a silica thin film. The oxidation furnace comprises an ignition furnace, an ignition gun, a synthesis chamber and a thermocouple group. The main body of the synthesis chamber is arranged in the ignition furnace, and the gas outlet end of the synthesis chamber extends to the outside of the ignition furnace and is communicated with the quartz tube. The gas inlet end of the synthesis chamber extends to the outside of the ignition furnace and is sleeved with an ignition gun, and the gas inlet end of the ignition gun is provided with a hydrogen gas inlet pipe. The gas inlet end of the synthesis chamber is provided with an oxygen inlet pipe, and the thermocouple component is arranged on an ignition furnace and an ignition gun.
In S200, the silicon substrate 110 is placed in the oxidation furnace. The temperature in the oxidation furnace is the reaction temperature, which is 1000-1200 ℃, preferably 1050 ℃. The reaction temperature is increased, the reaction speed is accelerated, and the production rate of the silicon dioxide film can be improved.
In S400, the first silicon dioxide layer 120 is a wet oxygen layer of a silicon dioxide thin film prepared by an oxyhydrogen synthesis method. And after oxygen is introduced into the oxidation furnace for 4-6 min and the measurement reading of a meter for measuring the oxygen flow tends to be stable, introducing hydrogen into the oxidation furnace and igniting, wherein the flow of the hydrogen is 4-8 slm/min. Therefore, explosion caused by overlarge hydrogen-oxygen ratio due to inaccurate flow measurement when the flowmeter is started instantly can be avoided, and the preparation process of the silicon dioxide film can be ensured to have higher safety.
In this embodiment, the method for preparing the silica thin film generates high-purity water vapor by reacting oxygen with a flow rate of 9slm/min to 10slm/min and hydrogen with a flow rate of 14slm/min to 14.6slm/min at a reaction temperature of 1000 ℃ to 1200 ℃. The water vapor can diffuse to the surface of the silicon substrate 110 to react with silicon to form a first silicon dioxide layer 120. When the flow rate of the hydrogen is 14slm/min to 14.6slm/min and the flow rate of the oxygen is 9slm/min to 10slm/min, the hydrogen can react with the oxygen to generate more water vapor, so that a stable water vapor environment can be rapidly formed in the oxidation furnace, and thus the first silicon dioxide layer 120 with better uniformity can be efficiently prepared, and the uniformity of the prepared silicon dioxide film is greatly improved.
In one embodiment, the S400 includes:
s410, introducing oxygen into the oxidation furnace for 4-6 min, and then beginning to introduce hydrogen into the oxidation furnace, wherein the flow rate of the hydrogen is 4-8 slm/min; and
and S420, introducing hydrogen into the oxidation furnace for 0.5-1.5 min, adjusting the flow of the hydrogen to 14-14.6 slm/min, and forming the first silicon dioxide layer 120 on the surface of the silicon substrate 110.
In the embodiment, oxygen is firstly introduced, the flow rate of the oxygen is 9slm/min-10slm/min, and hydrogen is introduced after the oxygen is introduced for 4min-6 min. The hydrogen reacts with the oxygen to generate water vapor, and the water vapor diffuses to the surface of the silicon substrate 110 to react with silicon to form the first silicon dioxide layer 120. The flow of the hydrogen is 4slm/min-8slm/min, and after the hydrogen with the flow of 4slm/min-8slm/min is introduced for 0.5min-1.5min and the measurement reading of the flowmeter is stable, the flow of the hydrogen is adjusted to 14slm/min-14.6 slm/min. Therefore, explosion caused by overlarge hydrogen-oxygen ratio due to inaccurate flow measurement when the flowmeter is started instantly can be effectively avoided, and the preparation process of the first silicon dioxide layer 120 can be ensured to have higher safety.
In one embodiment, in S300, the oxygen flow rate is 9.53 slm/min.
In this embodiment, the flow rate of the oxygen is 9.53slm/min, and the flow rate of the hydrogen is 14slm/min to 14.6slm/min, preferably 14.3 slm/min. The flow rates of the hydrogen and the oxygen are proper, and the hydrogen and the oxygen can react to generate more water vapor, so that a stable water vapor environment can be quickly formed in the oxidation furnace, and the first silicon dioxide layer 120 with better uniformity can be prepared.
In one embodiment, in S400, the flow rate of the hydrogen gas is 14.3 slm/min.
In this embodiment, the flow rate of the oxygen is 9.53slm/min, and the flow rate of the hydrogen is 14.3 slm/min. The hydrogen and the oxygen can react to generate a large amount of water vapor, and a stable water vapor environment can be quickly formed in the oxidation furnace, so that the silicon dioxide film with better uniformity is prepared, and the uniformity of the silicon dioxide film can reach within +/-2%.
Referring to Table 1, in one embodiment, a film with a thickness of 37.5min and 20min can be grown under the conditions of an oxygen flow of 9.53slm/min and a hydrogen flow of 14.3slm/min
And
a silicon dioxide thin film of (2). As can be seen from the data in Table 1, the uniformity of the silica film prepared under the conditions of hydrogen flow rate of 14.3slm/min and oxygen flow rate of 9.53slm/min was good and was within + -2%.
TABLE 137.5 min and 20min Process parameters and uniformity of the grown silicon dioxide films
| Time of day | Temperature (. degree.C.) | H2Flow rate | O2Flow rate | In-chip uniformity | Uniformity between sheets |
| 37.5 |
1050 | 14.3 | 9.53 | ≤±0.97％ | ±0.34％ |
| 20min | 1050 | 14.3 | 9.53 | ≤±1.35％ | ±0.7％ |
In one embodiment, the S200 includes:
s210, providing an oxidation furnace, heating the oxidation furnace to a pretreatment temperature, wherein the pretreatment temperature is 800-900 ℃;
s220, after the temperature of the oxidation furnace is raised to the pretreatment temperature, putting the silicon substrate 110 into the oxidation furnace, and introducing nitrogen into the oxidation furnace; and
s230, keeping the pretreatment temperature for 20-40 min, cutting off nitrogen and raising the temperature in the oxidation furnace from the pretreatment temperature to a reaction temperature, wherein the reaction temperature is 1000-1200 ℃.
In this embodiment, the temperature of the oxidation furnace is raised to a pretreatment temperature of 800 to 900 ℃, which can improve reaction efficiency in the production of a silica film. The silicon substrate 110 is placed in the oxidation furnace, and nitrogen gas, or other inert gas, may be introduced into the oxidation furnace, which is not limited herein. The nitrogen is used for blowing out impurities in the oxidation furnace so as to ensure the high purity of the silicon dioxide film. The oxidation furnace keeps the pretreatment temperature at 800-900 ℃ for about 20-40 min, and after the temperature in the oxidation furnace is constant and reaches a stable state, the oxidation furnace is heated to the reaction temperature, wherein the reaction temperature is 1000-1200 ℃. When the temperature in the oxidation furnace is increased to the reaction temperature of 1000 ℃ to 1200 ℃, the preparation of the second silicon dioxide layer 130 can be ensured to be carried out in a better temperature range, so that the second silicon dioxide layer 130 can be ensured to be rapidly prepared.
In one embodiment, the S300 includes:
s310, when the temperature in the oxidation furnace is increased from the pretreatment temperature to the reaction temperature, introducing oxygen into the oxidation furnace, wherein the flow rate of the oxygen is 10slm/min-15 slm/min;
s320, after the temperature in the oxidation furnace is raised to the reaction temperature, adjusting the flow rate of the oxygen gas to 9slm/min to 10slm/min, and forming a second silicon dioxide layer 130 on the surface of the silicon substrate 110, wherein the second silicon dioxide layer 130 is disposed between the first silicon oxide layer 120 and the silicon substrate 110.
Referring to fig. 3 and 4, in this embodiment, when the temperature in the oxidation furnace is increased from 800 ℃ to 900 ℃ to 1000 ℃ to 1200 ℃, oxygen is introduced during the process of increasing the temperature from the pretreatment temperature to the reaction temperature, so as to perform the synthesis process of the second silicon dioxide layer 130. The second silicon oxide layer 130 is a first dry oxygen layer of a silicon oxide thin film. The oxygen gas diffuses to the surface of the silicon substrate 110 to react with silicon, thereby generating a second silicon dioxide layer 130. In this embodiment, the silicon dioxide film may be completely composed of the second silicon dioxide layer 130 prepared by oxygen gas diffusing to the surface of the silicon substrate 110 to react with silicon, or may be composed of the first silicon dioxide layer 120 and the second silicon dioxide layer 130, which is not limited herein.
In this embodiment, the second silicon oxide layer 130 is prepared with an oxygen flow rate of 10slm/min to 15 slm/min. Thus, the oxidizing furnace has a stable oxygen atmosphere, and the synthesis reaction of the second silicon dioxide layer 130 can be well performed, so that the second silicon dioxide layer 130 with better uniformity can be prepared. And after the temperature in the oxidation furnace rises to the reaction temperature, adjusting the flow of the oxygen to be 9slm/min-10 slm/min. Therefore, the first silicon dioxide layer 120 can be prepared by the reaction of the oxygen at the optimal temperature of 1000-1200 ℃ and the flow rate of 9-10 slm/min, the preparation time of the first silicon dioxide layer 120 is greatly shortened, and the uniformity of the prepared silicon dioxide film is greatly improved.
In one embodiment, the method further includes S500, turning off hydrogen, continuing to introduce oxygen into the oxidation furnace, wherein the flow rate of the oxygen is 9slm/min to 10slm/min, and forming a third silicon dioxide layer 140 on the surface of the first silicon dioxide layer 120 away from the silicon substrate 110.
Referring to fig. 5 and 6, in the present embodiment, after the first silicon dioxide layer 120 is completely prepared, the hydrogen is cut off, and the oxygen is continuously introduced to prepare the third silicon dioxide layer 140, where the third silicon dioxide layer 140 is a second dry oxygen layer of a silicon dioxide film.
In one embodiment, the silica film obtained by the method is a dry-wet-dry layered structure. The silicon dioxide thin film is composed of a first silicon dioxide layer 120, a second silicon dioxide layer 130, and a third silicon dioxide layer 140. The first dry oxygen layer 130 and the second dry oxygen layer 140 can increase the denseness of the silica thin film. The growth rate of the first dry oxygen layer 130 and the second dry oxygen layer 140 is relatively slow compared to the growth rate of the wet oxygen layer 120, and the thickness of the second dry oxygen layer 140 and the first dry oxygen layer 130 is preferably not more than 700 angstroms in consideration of the manufacturing cost of the silicon oxide thin film. Therefore, when the thickness of the second dry oxygen layer 140 and the first dry oxygen layer 130 is not more than 700 angstroms, the silica thin film has better denseness and the silica thin film is manufactured at a lower cost.
In this embodiment, the third silicon dioxide layer 140 is prepared at an oxygen flow rate of 9slm/min to 10slm/min, preferably 9.53 slm/min. The preparation of the third silicon oxide layer 140 is continued on the surface of the first silicon oxide layer 120, which can increase the compactness of the silicon oxide thin film.
In one embodiment, S100 is followed by S110, and the silicon substrate 110 is cleaned by a cleaning solution.
There is a possibility that contamination impurities including organic and inorganic substances may exist on the surface of the silicon substrate 110. These impurities exist in an atomic state, an ionic state, a thin film form, or a particle form on the surface of the silicon substrate 110. In order to thoroughly remove these impurities and to form a high purity silicon dioxide film, the silicon substrate 110 is cleaned with a cleaning solution in this embodiment.
In one embodiment, the cleaning fluid comprises H2SO4\H2O2Mixed solution of (3), NH4OH\H2O2\H2O mixed solution, HC L \ H2O2\H2One or more of an O mixed solution and an HF solution.
In this embodiment, the selection of the cleaning liquid is selected according to the removal of different types of impurities. H2SO4\H2O2The mixed solution of (2) can be used for removing heavy organic impurities. NH (NH)4OH\H2O2\H2The O mixed solution can be used for removing organic matters, inorganic matters and metal ions HC L \ H2O2\H2O mixed solutionCan be used for removing metal ions such as aluminum, iron, sodium and the like. The HF solution can be used to remove metal ions and native oxide layers.
In one embodiment, after the step S600, after the preparation of the silicon dioxide film is completed, the temperature in the oxidation furnace is reduced to 800-900 ℃ for 60-70 min.
Referring to fig. 6, in this embodiment, after S600, the temperature in the oxidation furnace is decreased from 1000-1200 ℃ to 800-900 ℃ after the preparation of the silica film is completed. In the process of reducing the reaction temperature from 1000-1200 ℃ to 800-900 ℃, nitrogen can be introduced for reducing the temperature, and other inert gases can also be introduced, which are not limited herein. By reducing the temperature in the oxidation furnace, potential safety hazards caused by too high temperature in the reaction furnace can be avoided.
The features of the above-described embodiments may be arbitrarily combined, and for the sake of clarity of description, all possible combinations of the features in the above-described embodiments are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. A method for preparing a silica film, comprising:
s100, providing a silicon substrate (110);
s200, putting the silicon substrate (110) into an oxidation furnace, and heating the temperature in the oxidation furnace from a preset temperature to a reaction temperature, wherein the reaction temperature is 1000-1200 ℃;
s310, before the temperature in the oxidation furnace is increased to the reaction temperature from the preset temperature, introducing oxygen into the oxidation furnace, wherein the flow rate of the oxygen is 10slm/min-15slm/min, forming a second silicon dioxide layer (130) on the surface of the silicon substrate (110), and arranging the second silicon dioxide layer (130) on the surface of the silicon substrate (110);
s320, after the temperature in the oxidation furnace is increased to the reaction temperature, adjusting the flow of the oxygen to be 9slm/min-10 slm/min;
s410, introducing oxygen into the oxidation furnace for 4-6 min, then starting to introduce hydrogen into the oxidation furnace, and igniting, wherein the flow rate of the hydrogen is 4-8 slm/min;
and S420, introducing hydrogen into the oxidation furnace for 0.5-1.5 min, adjusting the flow of the hydrogen to 14-14.6 slm/min, and forming a first silicon dioxide layer (120) on the surface of the second silicon dioxide layer (130).
2. The method for preparing a silica film according to claim 1, wherein the flow rate of the oxygen gas in S320 is 9.53 slm/min.
3. The method according to claim 2, wherein in S420, the flow rate of the hydrogen gas is 14.3 slm/min.
4. The method for preparing a silica thin film according to claim 1, wherein the S200 comprises:
s210, providing an oxidation furnace, heating the oxidation furnace to a pretreatment temperature, wherein the pretreatment temperature is 800-900 ℃;
s220, after the temperature of the oxidation furnace is raised to the pretreatment temperature, putting the silicon substrate (110) into the oxidation furnace, and introducing nitrogen into the oxidation furnace;
s230, keeping the pretreatment temperature for 20-40 min, cutting off nitrogen and raising the temperature in the oxidation furnace from the pretreatment temperature to a reaction temperature, wherein the reaction temperature is 1000-1200 ℃.
5. The method for preparing a silica film according to claim 1, further comprising: and S500, cutting off hydrogen, continuously introducing oxygen into the oxidation furnace, wherein the flow of the oxygen is 9slm/min-10slm/min, and forming a third silicon dioxide layer (140) on the surface of the first silicon dioxide layer (120) far away from the silicon substrate (110).
6. The method for producing a silica film according to claim 1, further comprising, after S100, S110 of cleaning the silicon substrate (110) with a cleaning solution.
7. The method for producing a silica film according to claim 6, wherein the cleaning liquid is H2SO4\H2O2Mixed solution of (3), NH4OH\H2O2\H2O mixed solution, HC L \ H2O2\H2One or more of an O mixed solution and an HF solution.
8. The method for producing a silica thin film according to any one of claims 1 to 7, further comprising:
s600, after the first silicon dioxide layer is prepared, the temperature in the oxidation furnace is reduced to 800-900 ℃, and the temperature reduction time is 60-70 min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1131691A (en) * | 1997-05-14 | 1999-02-02 | Fuji Electric Co Ltd | Method for forming thermal oxidized film for silicon carbide semiconductor device |
| CN101866851A (en) * | 2010-05-12 | 2010-10-20 | 上海宏力半导体制造有限公司 | Oxidizing layer manufacture method |
| CN103871861A (en) * | 2014-03-24 | 2014-06-18 | 上海华力微电子有限公司 | Method for improving uniformity of large-size silicon wafer device performance |
| CN104561928A (en) * | 2014-12-24 | 2015-04-29 | 浙江大学 | Method for depositing silicon dioxide film on glass substrate |
Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW471068B (en) * | 1997-03-05 | 2002-01-01 | Hitachi Ltd | Method for fabricating semiconductor integrated circuit device with insulation film |
| TW451361B (en) * | 2000-07-26 | 2001-08-21 | Promos Technologies Inc | Method of preventing oxidation |
| US7087536B2 (en) * | 2004-09-01 | 2006-08-08 | Applied Materials | Silicon oxide gapfill deposition using liquid precursors |
| US7645709B2 (en) * | 2007-07-30 | 2010-01-12 | Applied Materials, Inc. | Methods for low temperature oxidation of a semiconductor device |
| CN101728239B (en) * | 2009-11-10 | 2013-01-30 | 上海宏力半导体制造有限公司 | Removal method of water vapor on crystal wafer surface |
| JP5813303B2 (en) * | 2009-11-20 | 2015-11-17 | 株式会社日立国際電気 | Semiconductor device manufacturing method, substrate processing method, and substrate processing apparatus |
| CN102136425A (en) * | 2010-01-22 | 2011-07-27 | 北大方正集团有限公司 | P-channel depletion MOS (metal oxide semiconductor) transistor and preparation method thereof |
| CN103377902B (en) * | 2012-04-28 | 2016-05-04 | 无锡华润上华科技有限公司 | Thermal oxide wafer generates the method for oxide layer |
| CN102931128B (en) * | 2012-11-28 | 2015-01-07 | 上海华力微电子有限公司 | Method for rounding edge corner of shallow groove separation |
| CN103681456A (en) * | 2013-10-23 | 2014-03-26 | 上海华力微电子有限公司 | Method for reducing critical dimension loss in HARP (High Aspect Ratio Process) film annealing |
| CN103715067B (en) * | 2013-12-31 | 2016-11-02 | 北京七星华创电子股份有限公司 | A kind of method improving into film uniformity |
| CN107591314A (en) * | 2016-07-08 | 2018-01-16 | 上海新昇半导体科技有限公司 | It is a kind of to form oxide layer and the method for epitaxial layer |
-
2018
- 2018-03-08 CN CN201810190973.4A patent/CN108447770B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1131691A (en) * | 1997-05-14 | 1999-02-02 | Fuji Electric Co Ltd | Method for forming thermal oxidized film for silicon carbide semiconductor device |
| CN101866851A (en) * | 2010-05-12 | 2010-10-20 | 上海宏力半导体制造有限公司 | Oxidizing layer manufacture method |
| CN103871861A (en) * | 2014-03-24 | 2014-06-18 | 上海华力微电子有限公司 | Method for improving uniformity of large-size silicon wafer device performance |
| CN104561928A (en) * | 2014-12-24 | 2015-04-29 | 浙江大学 | Method for depositing silicon dioxide film on glass substrate |
Non-Patent Citations (1)
| Title |
|---|
| "3D silicon Transformation using hydrogenannealing";Ming-Chang M.Lee等;《Solid-state sensor,Actuator and Microsystems》;20040610;第19-22页 * |
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