CN116759297A - Method for reducing wafer surface temperature in continuous preparation of low-temperature silicon nitride film - Google Patents
Method for reducing wafer surface temperature in continuous preparation of low-temperature silicon nitride film Download PDFInfo
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- CN116759297A CN116759297A CN202311061976.5A CN202311061976A CN116759297A CN 116759297 A CN116759297 A CN 116759297A CN 202311061976 A CN202311061976 A CN 202311061976A CN 116759297 A CN116759297 A CN 116759297A
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- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 95
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 123
- 238000006243 chemical reaction Methods 0.000 claims abstract description 74
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 33
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 76
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 48
- 229910000077 silane Inorganic materials 0.000 claims description 48
- 229910052757 nitrogen Inorganic materials 0.000 claims description 44
- 239000007789 gas Substances 0.000 claims description 41
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 39
- 229910052710 silicon Inorganic materials 0.000 claims description 39
- 239000010703 silicon Substances 0.000 claims description 39
- 229910021529 ammonia Inorganic materials 0.000 claims description 32
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 claims description 32
- 238000000151 deposition Methods 0.000 claims description 28
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 26
- 229910052786 argon Inorganic materials 0.000 claims description 13
- 230000008021 deposition Effects 0.000 claims description 13
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 claims description 10
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 9
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 9
- -1 fluoride ions Chemical class 0.000 claims description 8
- 150000002829 nitrogen Chemical class 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims 2
- 238000001816 cooling Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 239000012495 reaction gas Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 76
- 230000001276 controlling effect Effects 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 9
- 238000010924 continuous production Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 238000010494 dissociation reaction Methods 0.000 description 5
- 230000005593 dissociations Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 230000004075 alteration Effects 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—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
- H01L21/02112—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
- H01L21/02123—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
- H01L21/0217—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 nitride not containing oxygen, e.g. SixNy or SixByNz
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- 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
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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
- C23C16/22—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
- C23C16/34—Nitrides
- C23C16/345—Silicon nitride
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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
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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
- C23C16/52—Controlling or regulating the coating process
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- 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
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
- H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
- H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]
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Abstract
The application discloses a method for reducing the surface temperature of a wafer in continuously preparing a low-temperature silicon nitride film, which is characterized in that the temperature of nitrogen gas in atmosphere is controlled in the process of continuously forming the low-temperature silicon nitride film, the initial nitrogen gas temperature is limited to be 20-25 ℃, after the temperature of the surface of the wafer is detected to rise by a certain value, the nitrogen gas temperature is adjusted downwards in a mode of cooling the nitrogen gas, and the formed low-temperature atmosphere can take away heat generated on the surface of the wafer after being introduced into a vacuum reaction chamber, so that the effect of reducing the surface temperature of the wafer is achieved, and the components of reaction gas are not influenced, so that the film is stable. Therefore, the efficiency of the equipment can be improved, and the device is better protected.
Description
Technical Field
The application relates to the technical field of low-temperature silicon nitride film preparation, in particular to a method for reducing the surface temperature of a wafer in continuously preparing a low-temperature silicon nitride film.
Background
Because of the need for low temperature devices, silicon nitride thin film processes below 100 ℃ need to be developed. In the prior art, silane, ammonia and nitrogen react in a plasma atmosphere to generate silicon nitride, and the temperature of a base and the whole cavity are mainly controlled to achieve low-temperature reaction, but in the actual production process, as the reaction times are increased, the temperature of a wafer gradually rises along with the plasma reaction, the temperature difference with the base is larger and larger, and even in certain reaction times, the surface temperature of the wafer exceeds the upper limit temperature of 100 ℃. Thereby causing the difference of film coating on the surface of the wafer and affecting the performance of the film.
The existing method for reducing the surface temperature of the wafer mainly reduces the temperature of the base by introducing mixed liquid with a certain temperature into the heating disc, thereby achieving the purpose of stabilizing the surface temperature of the wafer. The method can effectively reduce the surface temperature of the wafer to a certain extent, but the effect of reducing the surface temperature of the wafer is obviously deteriorated when the number of continuous reactions is too large.
Disclosure of Invention
In order to overcome the defects in the prior art, the application aims to provide a method for reducing the surface temperature of a wafer in continuously preparing a low-temperature silicon nitride film.
In order to solve the technical problems, the application is realized by adopting the following technical scheme:
the application provides a method for reducing the surface temperature of a wafer in continuously preparing a low-temperature silicon nitride film, which comprises the following steps:
s1, controlling the temperature of a vacuum reaction chamber of PECVD equipment to be 60-80 ℃, then removing impurities in the chamber, and fluorinating an upper polar plate of the vacuum reaction chamber to form aluminum fluoride;
s2, introducing silicon-containing gas silane and ammonia into the vacuum reaction chamber for pretreatment; then continuously introducing silicon-containing gas silane and ammonia gas into the vacuum reaction chamber, simultaneously introducing nitrogen gas, controlling the radio frequency power to be 400-900W, and depositing a silicon nitride film on the surface of the chamber;
s3, placing the wafer on a base in a vacuum reaction chamber, and introducing silicon-containing gas silane and ammonia into the vacuum reaction chamber for pretreatment; then continuously introducing silicon-containing gas silane and ammonia into the vacuum reaction chamber, and simultaneously introducing nitrogen to deposit a silicon nitride film on the surface of the wafer;
s4, after the wafer with the silicon nitride film deposited is taken out, repeating the steps S1-S3, and preparing the silicon nitride film deposited on the surface of the wafer next time;
in the steps S2 and S3, the temperature of the introduced nitrogen is the initial nitrogen temperature, and the initial nitrogen temperature is 20-25 ℃;
when the temperature of the surface of the wafer for preparing the low-temperature silicon nitride film for the nth time is detected to be higher than the temperature of the surface of the wafer for preparing the low-temperature silicon nitride film for the first time by more than or equal to a set value, the temperature of the nitrogen gas introduced in the steps S2 and S3 is correspondingly reduced.
Preferably, in the reducing the temperature of the nitrogen gas introduced in the steps S2 and S3, the specific reduction value of the temperature of the nitrogen gas introduced is calculated by the following formula:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
Preferably, in the steps S2 and S3, the flow rate of the nitrogen gas is 5000-20000 sccm.
Preferably, the ratio of the flow rate of the nitrogen to the flow rate of the silicon-containing gas silane is 1:25.
Preferably, in step S1, the specific steps of removing the impurities in the cavity and fluorinating the upper plate of the vacuum reaction chamber to form aluminum fluoride are as follows: introducing 2000-6000 sccm of fluorinated nitrogen and 4000-12000 sccm of argon which are dissociated into fluoride ions outside the chamber, wherein the introducing time is 30-60 s, and the pressure in the vacuum reaction chamber is kept at 1-10 torr.
Preferably, the ratio of the nitrogen fluoride to the argon is 1:2.
Preferably, in step S2 and step S3, the specific steps of introducing silicon-containing gas silane and ammonia gas into the vacuum reaction chamber to perform pretreatment are as follows: 200-800 sccm of silicon-containing gas silane and 100-400 sccm of ammonia gas are introduced into the vacuum reaction chamber for 5-10 s.
Preferably, in step S2 and step S3, the ratio of the silicon-containing gas silane to ammonia gas is 1:2.
Preferably, in step S2, in the step of depositing the silicon nitride film on the surface of the cavity, the pressure in the vacuum reaction chamber is kept at 1-10 torr, the flow rate of the silane gas containing silicon and the ammonia gas is the same as the flow rate of the pretreatment, the deposition time is 10-20S, and the thickness of the deposited silicon nitride film is 200-1000A.
Preferably, in step S3, in the step of depositing the silicon nitride film on the surface of the wafer, the pressure in the vacuum reaction chamber is kept at 1-10 torr, the flow rate of the silane gas containing silicon and the ammonia gas is the same as the flow rate of the pretreatment, the deposition time is 3-120S, and the thickness of the deposited silicon nitride film is 200-8000A.
Preferably, the set point is 2 ℃.
Compared with the prior art, the application has the following beneficial effects:
1) According to the application, the temperature of the nitrogen gas in the atmosphere is controlled in the process of continuously forming the low-temperature silicon nitride film, the initial nitrogen gas temperature is limited to be 20-25 ℃, after a certain value of the rise of the surface temperature of the wafer is detected, the nitrogen gas temperature is adjusted downwards in a mode of cooling the nitrogen gas, and the formed low-temperature atmosphere gas is introduced into the vacuum reaction chamber to take away heat generated on the surface of the wafer, so that the effect of reducing the surface temperature of the wafer is achieved, and the components of the reaction gas are not influenced, so that the film is stable.
2) The application further precisely adjusts the specific temperature value of the introduced low-temperature atmosphere gas nitrogen by a specific method, so that the surface temperature of the wafer is not increased and always tends to be stable in the process of continuously producing the low-temperature silicon nitride film, thereby improving the efficiency of equipment and better protecting devices.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 shows the results of the wafer surface temperature and susceptor temperature variations measured at different reaction times in the method of continuously preparing a low temperature silicon nitride film of comparative example 1;
FIG. 2 shows the results of the wafer surface temperature and susceptor temperature variations measured at different reaction times in the method of continuously preparing a low temperature silicon nitride film according to example 1;
FIG. 3 shows the linear relationship between the nitrogen temperature reduction and the wafer surface temperature reduction in the method for continuously preparing a low temperature silicon nitride film under different conditions in example 2.
Description of the embodiments
The advantages and various effects of the present application will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the application, not to limit the application.
Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. In case of conflict, the present specification will control.
Unless specifically indicated otherwise, the various raw materials, reagents, instruments, equipment, and the like used in the present application are commercially available or may be prepared by existing methods.
Before the research of the application, in the existing method for preparing the low-temperature silicon carbide film, silicon-containing gas silane and ammonia gas are generally adopted as reaction source gases, normal-temperature nitrogen is introduced to deposit the silicon nitride film, and in the continuous production process, the temperature of the surface of a wafer is gradually increased along with the increase of the reaction times, and the difference between the surface of the wafer and the temperature of a base is larger. Therefore, a method for reducing and stabilizing the surface temperature of the wafer needs to be developed, so that the efficiency of equipment is improved, and the electrical property of a device is better protected.
In order to achieve the above object, the present application provides a method for continuously preparing a low temperature silicon nitride film to reduce the surface temperature of a wafer, the method comprising the steps of:
1. the method comprises the steps of taking aluminum (Al) as a material of a cavity wall, controlling the temperature of a PECVD vacuum reaction chamber with an aluminum Al low-temperature base to be 60-80 ℃, keeping the temperature unchanged in each subsequent step, and preparing a low-temperature silicon nitride film at the temperature; the temperature range is controlled to be any point value or small range of 65-75 ℃. The control temperature may be any one or a range of values between any two of 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃, 69 ℃, 70 ℃, 71 ℃, 72 ℃, 73 ℃, 74 ℃, 75 ℃, 76 ℃, 77 ℃, 78 ℃, 79 ℃, 80 ℃, and the application is not particularly limited and has little influence on the performance of the finally produced low-temperature silicon nitride film.
2. Introducing 2000-6000 sccm of nitrogen fluoride (after dissociation into fluoride ions outside the chamber) and 4000-12000 sccm of argon, wherein the introducing time is 30-60 s, and removing impurities in the chamber under the environment under the condition that the pressure in the PECVD vacuum reaction chamber is kept at 1-10 torr, so that an upper polar plate of the vacuum reaction chamber forms aluminum fluoride; according to the size of the chamber, the flow range of the introduced nitrogen fluoride can be arbitrarily regulated within 2000-6000 sccm, and the flow of argon is correspondingly regulated according to the ratio of the nitrogen fluoride to the argon (mainly, after the fluoride ion treatment, the upper polar plate is fluorinated, and the concentration of effective fluoride ions is optimal when the ratio of the nitrogen fluoride (NF 3) to the Argon (AR) is 1:2).
3. Introducing 200-800 sccm of silicon-containing gas silane (SIH 4) and 100-400 sccm of ammonia (NH 3) into the PECVD vacuum reaction chamber for 5-10s; then under the condition of keeping the pressure in the PECVD vacuum chamber at 1-10 torr, continuing to introduce 200-800 sccm of silicon-containing gas silane (SIH 4) and 100-400 sccm of ammonia (NH 3), and introducing 5000-20000 sccm of nitrogen (N2) output by a cooling device, controlling the radio frequency power at 400-900W, and the deposition time at 10-20 s, depositing a silicon nitride film on the reaction surface of the vacuum chamber, wherein the thickness is about 200-1000A, and the PECVD vacuum chamber mainly plays a role in protecting the chamber. The flow rate of the silane and the ammonia can be adjusted in the flow rate ranges, and the flow rate ratio of the silane to the ammonia is preferably 1:2; the flow rate of the nitrogen can be adjusted within the flow rate range, and the flow rate ratio of the nitrogen to the silane is preferably 1:25 so as to ensure the pressure to be stable;
4. then placing a substrate (a 12-inch wafer) on a base of the vacuum reaction chamber, and introducing 200-800 sccm of silicon-containing gas silane (SIH 4) and 100-400 sccm of ammonia (NH 3) into the PECVD vacuum chamber for 5-10s; and continuing to introduce 200-800 sccm of silicon-containing gas silane (SIH 4) and 100-400 sccm of ammonia (NH 3) under the condition that the pressure in the PECVD vacuum chamber is kept at 1-10 torr, introducing 5000-20000 sccm of nitrogen (N2) output by a cooling device, controlling the radio frequency power to be 400-900W, and depositing a silicon nitride film on the surface of the 12-inch wafer for 3-120 s, wherein the thickness is about 200-8000A. The flow rate of the silane and the ammonia can be adjusted in the flow rate ranges, and the flow rate ratio of the silane to the ammonia is preferably 1:2; the flow rate of the nitrogen can be adjusted within the flow rate range, and the flow rate ratio of the nitrogen to the silane is preferably 1:25 so as to ensure the pressure to be stable;
5. and (3) taking out the wafer deposited with the silicon nitride film, repeating the steps 1-4, and preparing the silicon nitride film deposited on the surface of the wafer next time, thereby carrying out continuous production.
In the production process, the surface temperature of the wafer is detected, and the surface temperature of the wafer measured by preparing the silicon nitride film for the first time is used as the initial surface temperature of the wafer. In the first deposition of the silicon nitride film, the temperature of the introduced nitrogen is controlled to be 20-25 ℃ in the steps 3 and 4, and the temperature is used as the initial nitrogen temperature. When the temperature of the surface of the wafer for preparing the low-temperature silicon nitride film for the nth time is detected to be higher than or equal to a set value compared with the initial temperature of the surface of the wafer, the set value is preferably 2 ℃ (such as 2 ℃, 3 ℃, 4 ℃ or 5 ℃ and the like), and the nitrogen is cooled by a cooling device to correspondingly reduce the temperature of the nitrogen introduced in the steps S2 and S3. In the reducing step S2 and S3, the reducing value of the temperature of the nitrogen is calculated by adopting the following formula:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
Examples
The method for forming a low temperature silicon nitride film according to the present application will be described in detail with reference to examples and experimental data.
Comparative example 1
The comparative example provides a method for continuously forming a low-temperature silicon nitride film, which comprises the following specific steps:
1) The Al is used as a material of a cavity wall, the Al is used as a PECVD vacuum reaction chamber of a low-temperature base, the temperature of the vacuum reaction chamber is controlled to be 80 ℃, and the temperature is kept unchanged in each subsequent step;
2) Introducing 4000 sccm of nitrogen fluoride (after dissociation into fluoride ions outside the chamber) and 8000 sccm of argon, wherein the introducing time is 40 s, and removing impurities in the chamber under the environment under the condition that the pressure in the PECVD vacuum reaction chamber is kept at 5 torr, so that an upper polar plate of the vacuum reaction chamber forms aluminum fluoride;
3) Introducing silicon-containing gas Silane (SIH) into the PECVD vacuum reaction chamber 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, with a charging time of 8 s; then, while keeping the pressure in the PECVD vacuum chamber at 5 torr, continuing to introduce silicon-containing gas silane (SIH 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, and nitrogen gas (N) without cooling treatment was introduced 2 10000 sccm at 25 deg.c, controlling the radio frequency power to 600W and depositing time to 15 s, depositing silicon nitride film on the reaction surface of the vacuum cavity with thickness of 500A to protect the cavityBody function;
4) Then placing a 12 inch wafer on the base of the vacuum reaction chamber, introducing silicon-containing gas Silane (SIH) into the PECVD vacuum chamber 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, with a charging time of 8 s; then, under the condition of keeping the pressure in the PECVD vacuum chamber at 5 torr, continuing to introduce silicon-containing gas Silane (SIH) 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, and nitrogen gas (N) without cooling treatment was introduced 2 10000 sccm at about 25 deg.c, 600W rf power control, 50 s deposition time, and about 2000A thickness of silicon nitride film deposited on the 12 inch wafer surface.
5) And (3) taking out the wafer deposited with the silicon nitride film, repeating the steps 1-4, and preparing the silicon nitride film deposited on the surface of the wafer next time, thereby carrying out continuous production. In the production process, the temperature of the introduced nitrogen is not adjusted, the surface temperature of the wafer and the temperature of the base are detected, and the results of the surface temperature of the wafer and the temperature of the base measured in the 1 st, 10 th, 15 th, 20 th and 25 th times of reaction are shown in fig. 1. As can be seen from fig. 1, the temperature of the wafer surface has gradually increased from about 95 ℃ for the 1 st reaction to above 100 ℃ for the 25 th reaction, while the temperature of the wafer surface has exceeded the upper temperature limit of 100 ℃ at this time, although the temperature of the susceptor has stabilized at 80 ℃.
Example 1
The embodiment provides a method for continuously forming a low-temperature silicon nitride film, which comprises the following specific steps:
1) The Al is used as a material of a cavity wall, the Al is used as a PECVD vacuum reaction chamber of a low-temperature base, the temperature of the vacuum reaction chamber is controlled to be 80 ℃, and the temperature is kept unchanged in each subsequent step;
2) Introducing 4000 sccm of nitrogen fluoride (after dissociation into fluoride ions outside the chamber) and 8000 sccm of argon, wherein the introducing time is 40 s, and removing impurities in the chamber under the environment under the condition that the pressure in the PECVD vacuum reaction chamber is kept at 5 torr, so that an upper polar plate of the vacuum reaction chamber forms aluminum fluoride;
3) Vacuum reacting to the PECVDIntroducing silicon-containing gas Silane (SIH) into the chamber 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, with a charging time of 8 s; then, while keeping the pressure in the PECVD vacuum chamber at 5 torr, continuing to introduce silicon-containing gas silane (SIH 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, and nitrogen gas (N) outputted from the cooling device was introduced 2 ) 10000 sccm, controlling the radio frequency power to be 600W, the deposition time to be 15 s, depositing a silicon nitride film on the reaction surface of the vacuum cavity, and having the thickness of about 500A, and mainly playing a role in protecting the cavity;
4) Then placing a 12 inch wafer on the base of the vacuum reaction chamber, introducing silicon-containing gas Silane (SIH) into the PECVD vacuum chamber 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, with a charging time of 8 s; then, under the condition of keeping the pressure in the PECVD vacuum chamber at 5 torr, continuing to introduce silicon-containing gas Silane (SIH) 4 ) 400 sccm and ammonia (NH) 3 ) 200 sccm, and nitrogen gas (N) outputted from the cooling device was introduced 2 ) 10000 sccm, controlling the radio frequency power to 600W, depositing 50 s, and depositing a silicon nitride film on the surface of the 12 inch wafer to a thickness of about 2000A.
5) And (3) taking out the wafer deposited with the silicon nitride film, repeating the steps 1-4, and preparing the silicon nitride film deposited on the surface of the wafer next time, thereby carrying out continuous production. In the production process, the surface temperature of the wafer is detected, and the surface temperature of the wafer measured by preparing the silicon nitride film for the first time is used as the initial surface temperature of the wafer. In the first deposition of the silicon nitride film, the temperature of the introduced nitrogen gas is controlled to be 25 ℃ in the steps 3 and 4, and the initial nitrogen gas temperature is used. And detecting the surface temperature of the wafer and the temperature of the base, and when the surface temperature of the wafer is detected to be 2 ℃ higher than the initial surface temperature of the wafer when the silicon nitride film is prepared for the nth time, correspondingly reducing the temperature of the nitrogen gas introduced when the silicon nitride film is prepared for the nth time through a cooling device. In the reducing step S2 and S3, the reducing value of the temperature of the nitrogen is calculated by adopting the following formula:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
The results of the wafer surface temperature and the susceptor temperature measured at the 1 st, 10 th, 15 th, 20 th and 25 th times of the reaction (i.e., the number of times of preparing the silicon nitride film) are shown in fig. 2. As can be seen from fig. 2, the susceptor temperature was always stabilized at 80 c and the wafer surface temperature was also almost always stabilized at 90 c. Compared with the method of comparative example 1, in the method of this example, in continuously forming a low temperature silicon nitride film, the wafer surface temperature was significantly lowered, and the temperature was kept substantially stable after 25 times of reaction.
Example 2
The embodiment provides a method for continuously forming a low-temperature silicon nitride film, and particularly discusses the relationship between the surface temperature change of a wafer and the nitrogen temperature change by adopting nitrogen with different reduced temperatures to continuously produce for 10 times. The specific procedure is substantially the same as in example 1, except that: each 10 times of continuous production was used as one experimental group, and each experimental group was continuously produced 50 times in total using nitrogen gas at the same temperature. In addition, the method of continuously forming the low-temperature silicon nitride film by adopting the nitrogen gas temperature of 25 ℃ is used as a comparison experiment group, and the surface temperature of the wafer is measured respectively at 10 times, 20 times, 30 times, 40 times and 50 times. The experimental conditions of the specific groups are shown in table 1.
TABLE 1
In table 1, the wafer surface temperature decrease value of the experiment group 1 compared with the comparison experiment group is the difference between the 10 th wafer surface temperature measured in the experiment group 1 and the wafer surface temperature when the low-temperature silicon nitride film is prepared for the 10 th time in the comparison experiment group, the wafer surface temperature decrease value of the experiment group 2 compared with the comparison experiment group is the difference between the 20 th wafer surface temperature measured in the experiment group 2 and the wafer surface temperature when the low-temperature silicon nitride film is prepared for the 20 th time in the comparison experiment group, and so on.
And drawing a correlation curve by taking the nitrogen temperature reduction value (x) adopted by each experimental group as an abscissa and the wafer surface temperature reduction value (y) as an ordinate, and obtaining a correlation linear equation as shown in the result of fig. 3: y=4.3822x+0.2095.
As can be seen from the test results of this example, the temperature of the wafer surface can be reduced linearly by reducing the nitrogen temperature. From this result, it can be deduced that: when the surface temperature of the wafer is increased, in order to reduce the surface temperature of the wafer, a nitrogen temperature reduction value can be correspondingly obtained through the linear equation, so that the temperature of the introduced nitrogen is reduced, and the effect of reducing the surface temperature of the wafer is achieved.
The formula from which the drop in temperature of the specific incoming nitrogen is deduced is:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
Example 3
The embodiment provides a method for continuously forming a low-temperature silicon nitride film, which comprises the following specific steps:
1) The Al is used as a material of a cavity wall, the Al is used as a PECVD vacuum reaction chamber of a low-temperature base, the temperature of the vacuum reaction chamber is controlled to be 70 ℃, and the temperature is kept unchanged in each subsequent step;
2) Introducing 2000 sccm of nitrogen fluoride (after dissociation into fluoride ions outside the chamber) and 4000 sccm of argon, wherein the introducing time is 60 s, and removing impurities in the chamber under the environment under the condition that the pressure in the PECVD vacuum reaction chamber is kept at 8 torr, so that an upper polar plate of the vacuum reaction chamber forms aluminum fluoride;
3) Introducing silicon-containing gas Silane (SIH) into the PECVD vacuum reaction chamber 4 ) 800 sccm and ammonia (NH) 3 ) 400 sccm, 5 s inlet time; then, while keeping the pressure in the PECVD vacuum chamber at 5 torr, continuing to introduce silicon-containing gas silane (SIH 4 ) 800 sccm and ammonia (NH) 3 ) 400 sccm, and nitrogen gas (N) output from the cooling device was introduced 2 ) 20000 sccm, controlling the radio frequency power to 900W, depositing a silicon nitride film on the reaction surface of the vacuum cavity with the deposition time of 10s and the thickness of about 600A, and mainly playing a role in protecting the cavity;
4) Then placing a 12 inch wafer on the base of the vacuum reaction chamber, introducing silicon-containing gas Silane (SIH) into the PECVD vacuum chamber 4 ) 800 sccm and ammonia (NH) 3 ) 400 sccm, 5 s inlet time; then, under the condition of keeping the pressure in the PECVD vacuum chamber at 5 torr, continuing to introduce silicon-containing gas Silane (SIH) 4 ) 800 sccm and ammonia (NH) 3 ) 400 sccm, and nitrogen gas (N) output from the cooling device was introduced 2 ) 20000 sccm, controlling the rf power to 900W, depositing a silicon nitride film on the 12 inch wafer surface for a deposition time of 20s a thickness of about 500a A a.
5) And (3) taking out the wafer deposited with the silicon nitride film, repeating the steps 1-4, and preparing the silicon nitride film deposited on the surface of the wafer next time, thereby carrying out continuous production. In the production process, the surface temperature of the wafer is detected, and the surface temperature of the wafer measured by preparing the silicon nitride film for the first time is used as the initial surface temperature of the wafer. In the first deposition of the silicon nitride film, the temperature of the introduced nitrogen gas is controlled to be 23 ℃ in the steps 3 and 4, and the initial nitrogen gas temperature is used. And detecting the surface temperature of the wafer and the temperature of the base, and when the surface temperature of the wafer is detected to be 2 ℃ higher than the initial surface temperature of the wafer when the silicon nitride film is prepared for the nth time, correspondingly reducing the temperature of the nitrogen gas introduced when the silicon nitride film is prepared for the nth time through a cooling device. The specific temperature drop value of the introduced nitrogen is calculated by adopting the following formula:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
The wafer surface temperatures measured after 25 times of reaction were all stabilized at 80 ℃.
Example 4
The embodiment provides a method for continuously forming a low-temperature silicon nitride film, which comprises the following specific steps:
1) The Al is used as a material of a cavity wall, the Al is used as a PECVD vacuum reaction chamber of a low-temperature base, the temperature of the vacuum reaction chamber is controlled to be 60 ℃, and the temperature is kept unchanged in each subsequent step;
2) Introducing 6000 sccm of nitrogen fluoride (after dissociation into fluoride ions outside the chamber, introducing) and 12000 sccm of argon, wherein the introducing time is 30 s, and removing impurities in the chamber under the environment under the condition that the pressure in the PECVD vacuum reaction chamber is kept at 3 torr, so that an upper polar plate of the vacuum reaction chamber forms aluminum fluoride;
3) Introducing silicon-containing gas Silane (SIH) into the PECVD vacuum reaction chamber 4 ) 200 sccm and ammonia (NH) 3 ) 100 sccm, and the charging time is 10s; then, while keeping the pressure in the PECVD vacuum chamber at 3 torr, continuing to introduce silicon-containing gas silane (SIH 4 ) 200 sccm and ammonia (NH) 3 ) 100 sccm, and nitrogen (N) output from the cooling device was introduced 2 ) 5000 sccm, controlling the radio frequency power to be 400W, depositing the silicon nitride film on the reaction surface of the vacuum cavity for 20s, and forming a silicon nitride film with the thickness of about 800A, wherein the silicon nitride film mainly plays a role in protecting the cavity;
4) Then placing a 12 inch wafer on the base of the vacuum reaction chamber, introducing silicon-containing gas Silane (SIH) into the PECVD vacuum chamber 4 ) 200 sccm and ammonia (NH) 3 ) 100 sccm, and the charging time is 10s; then, keeping the pressure in the PECVD vacuum chamber at 3 torr, continuing to introduce silicon-containing gas Silane (SIH) 4 ) 200 sccm and ammonia (NH) 3 ) 100 sccm, and nitrogen (N) output from the cooling device was introduced 2 ) 5000 sccm, controlling the radio frequency power to 400W, depositing the silicon nitride film on the surface of the 12 inch wafer for 100 s hours, and the thickness of the silicon nitride film is about 4000A.
5) And (3) taking out the wafer deposited with the silicon nitride film, repeating the steps 1-4, and preparing the silicon nitride film deposited on the surface of the wafer next time, thereby carrying out continuous production. In the production process, the surface temperature of the wafer is detected, and the surface temperature of the wafer measured by preparing the silicon nitride film for the first time is used as the initial surface temperature of the wafer. In the first deposition of the silicon nitride film, the temperature of the introduced nitrogen gas is controlled to be 22 ℃ in the steps 3 and 4, and the initial nitrogen gas temperature is used. And detecting the surface temperature of the wafer and the temperature of the base, and correspondingly reducing the temperature of the nitrogen gas introduced in the process of preparing the silicon nitride film for the nth time through a cooling device when the surface temperature of the wafer is 3 ℃ higher than the initial surface temperature of the wafer in the process of preparing the silicon nitride film for the nth time. The specific temperature drop value of the introduced nitrogen is calculated by adopting the following formula:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
The wafer surface temperatures measured after 25 times of reaction were all stabilized at 70 ℃.
Finally, it is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present application 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. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (11)
1. A method for continuously preparing a low-temperature silicon nitride film to reduce the surface temperature of a wafer, which is characterized by comprising the following steps:
s1, controlling the temperature of a vacuum reaction chamber of PECVD equipment to be 60-80 ℃, then removing impurities in the chamber, and fluorinating an upper polar plate of the vacuum reaction chamber to form aluminum fluoride;
s2, introducing silicon-containing gas silane and ammonia into the vacuum reaction chamber for pretreatment; then continuously introducing silicon-containing gas silane and ammonia gas into the vacuum reaction chamber, simultaneously introducing nitrogen gas, controlling the radio frequency power to be 400-900W, and depositing a silicon nitride film on the surface of the chamber;
s3, placing the wafer on a base in a vacuum reaction chamber, and introducing silicon-containing gas silane and ammonia into the vacuum reaction chamber for pretreatment; then continuously introducing silicon-containing gas silane and ammonia into the vacuum reaction chamber, and simultaneously introducing nitrogen to deposit a silicon nitride film on the surface of the wafer;
s4, after the wafer with the silicon nitride film deposited is taken out, repeating the steps S1-S3, and preparing the silicon nitride film deposited on the surface of the wafer next time;
in the steps S2 and S3, the temperature of the introduced nitrogen is the initial nitrogen temperature, and the initial nitrogen temperature is 20-25 ℃;
when the temperature of the surface of the wafer for preparing the low-temperature silicon nitride film for the nth time is detected to be higher than the temperature of the surface of the wafer for preparing the low-temperature silicon nitride film for the first time by more than or equal to a set value, the temperature of the nitrogen gas introduced in the steps S2 and S3 is correspondingly reduced.
2. The method for continuously preparing low-temperature silicon nitride film according to claim 1, wherein the decreasing value of the temperature of the introduced nitrogen in the decreasing steps S2 and S3 is calculated by the following formula:
a=（b-0.2095）/ 4.3822
wherein a is the decrease value of the temperature of the introduced nitrogen, and the decrease value is the decrease value of the temperature; b is the rise in the wafer surface temperature, which is the rise in the temperature in degrees celsius.
3. The method for continuously preparing low-temperature silicon nitride film according to claim 1, wherein the flow rate of nitrogen gas in steps S2 and S3 is 5000-20000 sccm.
4. The method for continuously preparing low temperature silicon nitride film according to claim 3, wherein the ratio of the flow rate of nitrogen to the flow rate of silane containing silicon is 1:25.
5. The method for continuously preparing low-temperature silicon nitride film according to claim 1, wherein in step S1, the specific steps of removing the impurities in the chamber and fluorinating the upper plate of the vacuum reaction chamber to form aluminum fluoride are as follows: introducing 2000-6000 sccm of fluorinated nitrogen and 4000-12000 sccm of argon which are dissociated into fluoride ions outside the chamber, wherein the introducing time is 30-60 s, and the pressure in the vacuum reaction chamber is kept at 1-10 torr.
6. The method for continuously preparing low temperature silicon nitride film according to claim 5, wherein the ratio of nitrogen fluoride to argon is 1:2.
7. The method for continuously preparing low-temperature silicon nitride film according to claim 1, wherein in step S2 and step S3, the specific steps of introducing silicon-containing gas silane and ammonia gas into the vacuum reaction chamber for pretreatment are as follows: 200-800 sccm of silicon-containing gas silane and 100-400 sccm of ammonia gas are introduced into the vacuum reaction chamber for 5-10 s.
8. The method for continuously preparing low temperature silicon nitride film according to claim 7, wherein in step S2 and step S3, the ratio of the silicon-containing gas silane to ammonia is 1:2.
9. The method according to claim 1, wherein in the step S2, the pressure in the vacuum reaction chamber is maintained at 1-10 torr, the flow rate of the silane and ammonia gas introduced into the vacuum reaction chamber is the same as the flow rate of the pretreatment, the deposition time is 10-20S, and the thickness of the deposited silicon nitride film is 200-1000A.
10. The method according to claim 1, wherein in the step S3, the pressure in the vacuum reaction chamber is maintained at 1-10 torr, the flow rate of the silane and ammonia gas introduced into the vacuum reaction chamber is the same as the flow rate of the pretreatment, the deposition time is 3-120S, and the thickness of the deposited silicon nitride film is 200-8000A.
11. The method for continuously preparing low temperature silicon nitride film according to claim 1, wherein the set value is 2 ℃.
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