Disclosure of Invention
The invention aims to provide a method for detecting the adhesiveness of a PECVD cavity wall deposited film, which is characterized in that the film of the cavity wall with poor adhesiveness can fall off through plasma bombardment, the adhesiveness of the film is reversely pushed by monitoring the quantity of particles generated by film peeling, the macroscopic adhesiveness stability of the PECVD cavity wall film can be rapidly evaluated, the method is particularly suitable for preventive maintenance in a mass production environment, and the problem of low film forming quality caused by poor film adhesiveness is avoided.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
The invention provides a method for detecting adhesion of a PECVD cavity wall deposited film, which comprises the following steps:
Providing a PECVD cavity with a film deposited on the cavity wall;
Transferring the particle sheet into a PECVD cavity, performing first vacuumizing treatment on the PECVD cavity, pumping the PECVD cavity to a first pressure, transferring the particle sheet out of the PECVD cavity, measuring the pre-particle value of the particle sheet, and transferring the particle sheet into the PECVD cavity again;
and carrying out second vacuumizing treatment on the PECVD cavity, pumping the PECVD cavity to a third pressure, then transferring the particle sheet out of the PECVD cavity, detecting the particle post-value on the particle sheet, and judging the film adhesiveness.
According to the invention, the pre-particle value of the particle sheet is measured in advance, the PECVD cavity deposited with the film is vacuumized, the particle sheet is transferred into the PECVD cavity, nitrogen is introduced to avoid residual gas in the cavity from interfering with subsequent plasma bombardment, the pressure in the cavity is in a proper range, and the plasma of the stable gas generated by radio frequency is started to bombard the film on the cavity wall. The plasma of the stable gas can generate high-energy ions/free radicals to bombard the cavity wall film, the film is close to the stress in the actual process, the film with poor adhesion can be peeled off due to the bombardment, and particles are carried to the surface of a particle sheet (such as a silicon sheet or a quartz sheet) by the airflow for deposition. And then, vacuumizing treatment is carried out to remove residual stable gas and suspended particles in the cavity, so that no extra pollution is caused when the particle sheet is transmitted, the post-particle value of the particle sheet is detected, the adhesiveness of the film on the cavity wall is judged according to the pre-particle value and the post-particle value, and the more the number of particles/the larger the size, the worse the adhesiveness of the film.
The particle sheet disclosed by the invention does not form a film, so that if the particle rear value is lower after use, the particle sheet can be reused, and the particle front value can be redetermined before reuse, so that the detection cost can be greatly reduced, the influence of particles generated by a process can be eliminated, and the detection result is better and more accurate.
Preferably, the film is made by:
And introducing a gaseous deposition source into the PECVD cavity to reach target pressure, starting a radio frequency to perform deposition treatment, and depositing a film on the wall of the PECVD cavity.
The thin film is the same as the thin film to be deposited after detection, and the conventional silicon-containing thin film is adopted.
Preferably, the film is a silicon nitride film, the gaseous deposition source includes nitrogen, ammonia and silane, and the flow rate of the nitrogen is 350 sccm-4500 sccm, for example: 3500sccm, 3800sccm, 4000sccm, 4200sccm, 4500sccm, etc., not only the values listed but also other values not listed in the range of values are applicable, and the flow rate of the ammonia gas is 80sccm to 140sccm, for example: the flow rate of the silane is 250sccm to 350sccm, such as 250sccm, 280sccm, 300sccm, 320sccm, or 350sccm, which are not limited to the recited values, the high-frequency power is 600W to 1000W, such as 600W, 700W, 800W, 900W, or 1000W, which are not limited to the recited values, the other non-recited values within the range are similarly applied, the electrode gap is 350mil to 450mil, such as 350mil, 380mil, 400mil, 420mil, or 450mil, which are not limited to the recited values, the deposition temperature is 200 DEG to 400 DEG, such as 200 DEG, 250 DEG, 300 DEG, 350 DEG, or 400 DEG, which are similarly applied, and the deposition temperature is 4.r, such as 4.r, which are not limited to the recited values within the range, such as 4.r, 4 r, or 4 r, which are not limited to the recited values.
Preferably, the film is a silicon oxide film, the gaseous deposition source includes nitrous oxide and silane, and the flow rate of the nitrous oxide is 2000sccm to 2500sccm, for example: 2000sccm, 2200sccm, 2300sccm, 2400sccm, 2500sccm, etc., are not limited to the recited values, other non-recited values within the range are equally applicable, the flow rate of the silane is 70sccm to 130sccm, for example, 70sccm, 80sccm, 90sccm, 100sccm, 130sccm, etc., other non-recited values within the range are equally applicable, the high frequency power is 200W to 300W, for example, 200W, 220W, 250W, 280W, 300W, etc., not only the recited values, other non-recited values within the range are equally applicable, the electrode spacing is 350mil to 450mil, for example, 350mil, 380mil, 400mil, 420mil, 450mil, etc., other non-recited values within the range are equally applicable, the deposition temperature is 200 ℃ to 400 ℃, for example, 200 ℃ to 250 ℃ to 300 ℃ to 350 ℃ or 400 ℃ are equally applicable, the range is not limited to the recited values within the range is equal to the recited values, for example, the range is equal to the range is not limited to the recited values within the range is equal to 350mil to the other non-recited values, the range is equal to the target is not recited within the range is 2 r 2, for example, the range is equal to the non-recited within the range is equal to the range is not recited, and the target is equal to the non-recited within the range is equal to the range to the non-recited.
According to the invention, the film suitable for subsequent measurement can be prepared by controlling the target pressure, if the target pressure is too low, the film is denser (enhanced by ion bombardment), but high internal stress (compression or stretching) can be introduced, so that the subsequent peeling risk is increased, the number of particles detected by the particle sheets can be increased, and the difficulty in subsequent detection of the post-particle values of the particle sheets is increased and the accuracy is reduced due to the fact that peeled particles can be finer. Excessive target pressure can result in loose films, poor adhesion, but lower stress, large particle flaking is more easily detected.
The conditions of the deposition treatment are controlled in the range, so that the bonding strength of a film-substrate interface can be improved, and the influence on the detection accuracy caused by the falling of overlarge area or fine particles in the subsequent bombardment process is avoided.
Preferably, the first pressure is <20mtorr.
Preferably, the pellet sheet is placed on a heating plate and the front surface of the pellet sheet is disposed separately from the film.
The front surface of the particle sheet is separated from the film, namely the front surface of the particle sheet is not contacted with the film, so that the risk of damage of fragments or hardware is avoided, the bombardment conditions are consistent, the dropping positions of particles are basically consistent, the particle sheet is arranged at the position where the particles want to drop, and the dropped particles are ensured to be completely dropped on the particle sheet as much as possible.
The particle sheet used in the invention is a silicon wafer and/or a quartz sheet with a smooth surface, the surface of the particle sheet is smooth, the adsorption and counting of particles are facilitated, the particle sheet can be reused, but the pre-particle value of the particle sheet needs to be measured and recorded before the particle sheet is used.
Preferably, the second pressure is 2torr to 5torr, for example, 2torr, 2.5torr, 3torr, 4torr, 5torr, etc., not limited to the values recited, and other values not recited in the range are equally applicable.
The second pressure (i.e. the pressure of the introduced stable gas) can influence the detection accuracy, if the pressure of the introduced stable gas is too low, the mean free path of ions is long, the ion energy is high, the bombardment intensity is high, the film is possibly damaged unexpectedly due to excessive bombardment, the detection accuracy is reduced, and if the pressure of the introduced stable gas is too high, the generated plasma energy is low, the density of the plasma is high, the bombardment effect is poor, the sensitivity is reduced, and the film adhesiveness cannot be accurately judged.
Preferably, the high frequency power of the bombardment treatment is 600W to 1000W, for example, 350mil, 380mil, 400mil, 420mil or 450mil, etc., not limited to the listed values, other non-listed values in the range are equally applicable, the flow rate of the stable gas is 3500sccm to 4500sccm, for example, 3500sccm, 3800sccm, 4000sccm, 4200sccm or 4500sccm, etc., not limited to the listed values, other non-listed values in the range are equally applicable, the electrode spacing is 350mil to 450mil, for example, 350mil, 380mil, 400mil, 420mil or 450mil, etc., not limited to the listed values, other non-listed values in the range are equally applicable, the deposition temperature is 200 ℃ to 400 ℃, for example, 200 ℃ 250 ℃, 300 ℃, 350 ℃ or 400 ℃, etc., not limited to the listed values, other non-listed values in the range are equally applicable, and the stable gas also includes nitrogen.
The power of the bombardment treatment can influence the detection accuracy, if the power of the bombardment treatment is too low, the ion density is low, the bombardment energy is weak, the detection accuracy is reduced, if the power of the bombardment treatment is too high, the ion density is high, the energy is strong, sputtering and secondary deposition can be possibly caused, and the sputtering of a film or a substrate material can pollute a cavity and interfere with the subsequent detection analysis.
Helium and/or argon can be adopted as the stable gas, but the argon is heavier than the nitrogen, and the argon plasma has strong capability of etching the film and produces more particles under the same radio frequency power. Helium is relatively light in comparison with nitrogen, and argon plasma is weak in film etching capability under the same radio frequency power, and few particles are generated. The nitrogen cooperates with the radio frequency power to enable the detection result to be accurate. Argon and helium can be matched with proper radio frequency power to obtain the same detection effect.
Preferably, the third pressure is <20mtorr.
Preferably, the judging of the film adhesion includes:
and obtaining particle increment according to the difference value between the post-particle value and the pre-particle value, wherein the particle increment=0, and the pull-off strength of the film is more than or equal to 30MPa.
The grain increment=1-5, and the pull-off strength of the film is less than or equal to 20MPa and is less than 30MPa.
The grain increment=6-20, and the pull-off strength of the film is less than or equal to 15MPa and less than 20MPa.
The grain increment=21-50, and the pull-off strength of the film is less than or equal to 12MPa and less than 15MPa.
The grain increment=51-100, and the pull-off strength of the film is less than or equal to 10MPa and less than 12MPa.
The grain increment is more than 100, and the pull-off strength of the film is less than 10MPa.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, through plasma bombardment, the cavity wall film with poor adhesion can drop, the adhesion of the film is reversely pushed by monitoring the particle quantity generated by film peeling, the macroscopic adhesion stability of the PECVD cavity wall film can be rapidly evaluated, and a peeling high-incidence area is positioned, so that the method is particularly suitable for preventive maintenance in a mass production environment, and the problem of low film forming quality caused by poor film adhesion is avoided.
(2) According to the invention, the particle change of particle sheets before and after deposition is measured by simulating the deposition process, firstly, the particle front value of the particle sheets is measured before the particle sheets are transferred into a cavity, the particle sheets are positioned on a heating disc, then, stable gas plasmas are used for bombarding a film on the cavity, only the plasmas are used for bombarding, the main deposition process is not carried out, then, the particle rear value of the particle sheets is measured after vacuumizing, and the adhesiveness of the film is judged by comparing the particle front value with the particle rear value. The conventional main deposition may generate extra particles, the main deposition is not performed, and the stable gas is adopted for plasma bombardment, so that the interference of the particles with increased reaction is avoided, and the result is more accurate.
(2) The method can accurately and rapidly judge the adhesiveness and pull-off strength of the deposited film on the PECVD cavity wall according to the particle increment, does not need to damage the film, monitors the quantity of particles generated by peeling the film to reversely push the adhesiveness of the film, can rapidly evaluate the macroscopic adhesion stability of the PECVD cavity wall film, is particularly suitable for preventive maintenance in a mass production environment, and avoids the problem of low film forming quality caused by poor film adhesiveness.
Detailed Description
The technical scheme of the invention is further described by the following specific embodiments. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof.
The PECVD cavity provided by the embodiment of the invention is used for depositing a silicon nitride film by the following method:
Introducing a gaseous deposition source into the PECVD cavity according to the flow rate of nitrogen being 4000sccm, the flow rate of ammonia being 120sccm and the flow rate of silane being 300sccm until the pressure in the PECVD cavity reaches 4.5torr;
And (3) turning on the radio frequency, and depositing the film under the conditions that the high-frequency power is 800W, the electrode spacing is 400mil and the deposition temperature is 300 ℃ to obtain the silicon nitride film.
The PECVD cavity provided by the embodiment of the invention is used for depositing a silicon oxide film by the following method:
introducing a gaseous deposition source into the PECVD cavity according to the flow rate of nitrous oxide of 2200sccm and the flow rate of silane of 120sccm until the pressure in the PECVD cavity reaches 2.5torr;
And (3) turning on the radio frequency, and depositing the film under the conditions that the high-frequency power is 250W, the electrode spacing is 400mil and the deposition temperature is 300 ℃ to obtain the silicon oxide film.
Example 1
The embodiment provides a method for detecting adhesion of a PECVD cavity wall deposited film, which comprises the following steps:
measuring the pre-particle value of the particle sheet, and determining parameters such as the position, the number and the like of particles on the particle sheet;
vacuumizing the PECVD cavity deposited with the silicon nitride film, pumping to a pressure of <20mtorr, introducing the particle sheet into the PECVD cavity, introducing nitrogen into the cavity to a pressure of 4torr, starting a radio frequency, and bombarding the film under the conditions that the high-frequency power is 800W, the nitrogen flow rate is 4000sccm, the electrode spacing is 400mil and the deposition temperature is 300 ℃;
And vacuumizing the PECVD cavity again, after vacuumizing until the pressure is less than 20mtorr, transferring the particle sheet out of the PECVD cavity, detecting the particle post-value on the particle sheet, and judging the adhesiveness of the film.
Example 2
The embodiment provides a method for detecting adhesion of a PECVD cavity wall deposited film, which comprises the following steps:
measuring the pre-particle value of the particle sheet, and determining parameters such as the position, the number and the like of particles on the particle sheet;
vacuumizing the PECVD cavity deposited with the silicon nitride film, pumping to a pressure of <20mtorr, introducing the particle sheet into the PECVD cavity, introducing nitrogen into the cavity to a pressure of 5torr, starting a radio frequency, and bombarding the film under the conditions that the high-frequency power is 1000W, the nitrogen flow rate is 4500sccm, the electrode spacing is 450mil and the deposition temperature is 400 ℃;
And vacuumizing the PECVD cavity again, after vacuumizing until the pressure is less than 20mtorr, transferring the particle sheet out of the PECVD cavity, detecting the particle post-value on the particle sheet, and judging the adhesiveness of the film.
Example 3
The embodiment provides a method for detecting adhesion of a PECVD cavity wall deposited film, which comprises the following steps:
measuring the pre-particle value of the particle sheet, and determining parameters such as the position, the number and the like of particles on the particle sheet;
Vacuumizing the PECVD cavity deposited with the silicon nitride film, pumping to a pressure of <20mtorr, introducing the particle sheet into the PECVD cavity, introducing nitrogen into the cavity to a pressure of 2torr, starting a radio frequency, and bombarding the film under the conditions that the high-frequency power is 600W, the nitrogen flow rate is 3500sccm, the electrode spacing is 350mil and the deposition temperature is 200 ℃;
And vacuumizing the PECVD cavity again, after vacuumizing until the pressure is less than 20mtorr, transferring the particle sheet out of the PECVD cavity, detecting the particle post-value on the particle sheet, and judging the adhesiveness of the film.
Example 4
This example differs from example 1 only in that the pressure of the nitrogen gas introduced is 1torr, and other conditions and parameters are exactly the same as example 1.
Example 5
This example differs from example 1 only in that the pressure of the nitrogen gas introduced was 6torr, and other conditions and parameters were exactly the same as example 1.
Example 6
The present example differs from example 1 only in that the high frequency power of the bombardment treatment was 1200W, and other conditions and parameters were identical to those of example 1.
Example 7
This example differs from example 1 only in that the high frequency power of the bombardment treatment is 500W, and other conditions and parameters are exactly the same as those of example 1.
Comparative example 1
The comparative example uses a new clean wafer film to measure particle size.
Comparative example 2
This comparative example differs from example 1 only in that the film was bombarded with silane in place of nitrogen, and the other conditions and parameters were exactly the same as in example 1.
Performance test:
the particle increment obtained in examples and comparative examples was calculated and the actual pull-off strength of the film was measured using a pull-off tester, and the test results are shown in table 1:
TABLE 1
From table 1, it can be seen that, according to examples 1 to 7, the method of the present invention can accurately and rapidly determine the adhesion and pull-off strength of different types of films deposited on the PECVD chamber wall according to the particle increment, without damaging the films, and can rapidly evaluate the macroscopic adhesion stability of the PECVD chamber wall film by monitoring the amount of particles generated by film peeling, especially suitable for preventive maintenance in a mass production environment, and avoid the problem of too low film formation quality due to poor film adhesion.
As can be seen from comparison of examples 1 and 4-5, in the method for detecting adhesion of a deposited film on a PECVD chamber wall according to the present invention, the pressure of the introduced nitrogen gas affects the detection accuracy, the pressure of the introduced nitrogen gas is controlled to be 2-5 torr, the detection accuracy is high, if the pressure of the introduced nitrogen gas is too low, the mean free path of ions is long, the ion energy is high, the bombardment intensity is high, the film may be damaged unexpectedly due to excessive bombardment, the detection accuracy is reduced, and if the pressure of the introduced nitrogen gas is too high, the generated plasma energy is low, the density of the plasma is high, the bombardment effect is poor, the sensitivity is reduced, and the adhesion of the film cannot be accurately determined.
As can be seen from comparison of examples 1 and examples 6-7, in the method for detecting adhesion of a deposited film on a PECVD chamber wall according to the present invention, the power of bombardment treatment affects the detection accuracy, the power of bombardment treatment is controlled to 600 w-1000 w, the detection accuracy is higher, if the power of bombardment treatment is too low, the ion density is low, the bombardment energy is weak, the detection accuracy is reduced, and if the power of bombardment treatment is too high, the ion density is high, the energy is strong, sputtering and secondary deposition may be initiated, the film or substrate material sputtering may pollute the chamber, and the subsequent detection analysis is interfered.
By comparing the embodiment 1 with the comparative example 1, under the condition that the amount of the added particles is controlled to be in a proper range, the added particles are coated on the surface of the wafer instead of being coated under the film, so that the shape can be easily seen, the detection accuracy is higher, the detection accuracy is equivalent to that of a film grown on the wafer, but the wafer can be recycled, and the cost is greatly reduced.
By comparing the embodiment 1 with the comparative example 2, the invention bombards the film by using nitrogen plasma, only bombards or nitriding the surface of the film, no new sediment is introduced, the peeled particles come from the film itself, pretreatment is not needed before the bombardment, the detection speed is high, the loss of equipment is avoided, the detection precision is also high, the problem that the bombardment intensity is too high or too low is caused by using other gas sources for bombardment, and the accurate detection is difficult.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and it should be apparent to those skilled in the art that any changes or substitutions that fall within the technical scope of the present invention disclosed herein are within the scope of the present invention.