CN112985330A - Preparation method of wafer-level film thickness standard sheet for online instrument calibration - Google Patents
Preparation method of wafer-level film thickness standard sheet for online instrument calibration Download PDFInfo
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
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Abstract
The invention provides a preparation method of a wafer-level film thickness standard wafer for instrument calibration, which comprises the following steps: cleaning a wafer substrate and removing a natural oxide layer to obtain a processed wafer substrate, and realizing non-crystallization high-quality film deposition on the wafer substrate by utilizing an atomic layer deposition method, so that the problems of large surface roughness and uneven thickness of a film caused by molecular clustering or crystallization in other traditional methods are solved, and a high-precision wafer-level film thickness standard sheet is obtained; the invention accurately controls the thickness of the film at the single atomic layer level, ensures that the growth of the film realizes 100 percent of uniformity, conformality and no pinhole; meanwhile, the preparation method provided by the invention has high repeatability, so that the thickness value repeatability of the standard sheets of the same batch and different batches is good.
Description
Technical Field
The invention relates to the field of semiconductor integrated circuits and instrument calibration, in particular to a method for preparing a wafer-level film thickness standard wafer for online instrument calibration.
Background
It is known that existing chips, large-scale integrated circuits and microelectronic devices are all manufactured based on processes of functional thin film preparation and subsequent etching packaging, but the progress of thin film preparation technology and the rapid development of micro-nano processing technologies such as photoetching bring us into the era of large-scale and super-large-scale integrated circuits. Nowadays, the integration degree of large-scale integrated circuits and microelectronic devices breaks through moore's law and enters the post-moore era, the key feature size of mainstream chips generally enters the magnitude below 100nm, so that the minimum thickness of a single-layer functional film serving as the most basic unit of the integrated circuits and the micro-nano devices reaches below 10nm, and the geometric feature parameter of the film thickness has greater and greater influence on the performance of the microelectronic devices such as the chips. The method can effectively measure and analyze the thickness of each layer of film of the integrated circuit such as the chip and the like, and is a key for controlling the quality of the large-scale integrated circuit and guarantee for the continuous and rapid development. Micro-nano analytical instruments such as an ellipsometer, an auger electron spectrometer, an X-ray photoelectric spectrometer, a secondary ion mass spectrometer and the like become main tools for measurement and analysis in the current nano technical field due to the characteristics of high resolution, high stability, measurement consistency and the like. In practical use, however, different standard sheets need to be used to accurately and effectively calibrate a nanometer measuring instrument by combining the structural characteristics of a device and a nanometer material, so that objective evaluation of the film thickness of key parameters of a micro-nano device in the microelectronic integrated circuit industry is realized, a unified standard is provided for large-scale manufacturing of various chips, the yield is improved, and the stability and the universality of a large-scale integrated circuit and a microelectronic device are improved. The traceability characteristic and the universality of the standard sheet can ensure that a quantity value transmission medium is established among different instruments, and the consistency and the reliability of the measured values among different instruments are ensured.
Nanometer measurement becomes the key of the foundation and quality control of the development of the nanometer industry at present, and a nanometer geometric characteristic parameter measurement standard device is used as a key carrier for realizing the transmission of nanometer quantity values from national measurement standards to the nanometer industry and is a crucial link in a nanometer quantity value transmission system. The development of the nanometer geometric characteristic parameter measurement standard device in China is still in the initial stage, and no series of nanometer geometric characteristic parameter measurement standard device products which are oriented to industrial requirements and perfect are available, so that the problems that the nanometer quantity value is not uniform in industrial practical application and the quantity value of a nanometer measuring instrument is traced to abroad are caused. Therefore, it is urgent to develop various nanometer standard sample wafers and trace and compare the measurement values so as to calibrate the nanometer measuring instrument, complete the accurate measurement and correction of each geometric parameter of the nanometer device, realize the controllable preparation of the nanometer device and improve the performance of the nanometer device.
Disclosure of Invention
The invention aims to provide a preparation method of a wafer-level film thickness standard wafer for instrument calibration, which solves the defects in the prior art.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of a wafer-level film thickness standard wafer for instrument calibration, which comprises the following steps:
and cleaning the wafer substrate, removing the natural oxide layer to obtain the processed wafer substrate, and depositing a film on the wafer substrate by using an atomic layer deposition method to obtain the wafer-level film thickness standard sheet.
Preferably, the wafer-level film thickness standard wafer is Si/Al2O3Film thickness standard wafer, Si/SiO2Film thickness standard wafer, Si/HfO2Film thickness standard wafer, Si/TiO2Film thickness standard wafer, Si/ZnO film thickness standard wafer, Si/ZrO film2A film thickness standard sheet or a Si/AlN film thickness standard sheet.
Preferably, Si/Al is prepared2O3The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is trimethyl aluminum, and the second precursor source is an oxygen source;
the pulse time of the first precursor source was 0.1 seconds, and the carrier gas flow rate was 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-0.2 seconds, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
Preferably, Si/SiO is prepared2Film thickness standardThe process parameters of the sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is bis (diethylamine) silane or tris (dimethylamino) silane; the second precursor source is O2And Ar2According to the flow ratio of 2: 1 mixed oxygen plasma; wherein, O2At a flow rate of 80sccm, Ar2The flow rate of (2) was 40 sccm.
The pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 4-6s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
Preferably, Si/HfO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is tetra (methylamino) hafnium or tetra (dimethylamino) hafnium, and the heating temperature of the first precursor source is 100-120 ℃;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-5s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
Preferably, Si/TiO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is tetra (dimethylamino) titanium, and the heating temperature of the first precursor source is 100-120 ℃;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-6s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
Preferably, Si/ZnO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 150-250 ℃;
the first precursor source is diethyl zinc;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-6s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
Preferably, Si/ZrO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 150-250 ℃;
the first precursor source is tetra (methylethylamino) zirconium or tetra (dimethylamino) zirconium and the heating temperature of the first precursor source is 111-170 ℃;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-5s, and the flow rate is 200 sccm; then, the nitrogen gas of 200sccm is used for purging for 6 to 10 seconds
Preferably, the technological parameters for preparing the Si/AlN film thickness standard piece are as follows:
the temperature in the ALD reaction chamber is 150-250 ℃;
the first precursor source is trimethylaluminum;
the second precursor source is a nitrogen source, which is NH3The plasma of (2);
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 2-16s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 3-5 seconds.
Preferably, the thickness of the obtained wafer-level film thickness standard sheet is 0-1000 nm.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a wafer-level film thickness standard sheet for instrument calibration, which is characterized in that films with different thicknesses are deposited on a single crystal substrate by utilizing film preparation technologies such as atomic layer deposition and the like to obtain high-precision wafer-level film thickness standard templates with different thicknesses; the invention accurately controls the thickness of the film at the single atomic layer level, ensures that the growth of the film realizes 100 percent of uniformity, conformality and no pinhole; meanwhile, the preparation method provided by the invention has high repeatability, so that the thickness value repeatability of the standard sheets of the same batch and different batches is good.
Further, by using the prepared Si/Al2O3Si/Al prepared by technological parameters of film thickness wafer standard wafer2O3The film thickness of the wafer standard wafer realizes Al2O3The non-crystallization growth of the film greatly reduces the conditions of film cracking, falling and the like caused by stress between the film and the substrate, and in addition, the problems of film surface roughness increase, uneven thickness and the like caused by molecular clusters and crystallization caused by surface energy are solved by utilizing a low-energy growth mode, and finally the film thickness standard wafer with the small substrate with the rough and ultra-high surface and the uniform large-area thickness is obtained.
Further, prepared Si/SiO2The wafer standard wafer has good environmental stability, small surface roughness and good thickness uniformity and has high repeatability. Because of the large SiO of this method2The film has very high compactness, and solves the problem of SiO prepared by other traditional methods2The film has pinholes and the compactness is poor to cause the prepared Si/SiO2The film thickness standard sheet is easy to be secondarily oxidized by oxygen and water vapor in the air in the atmospheric environment to cause the fatal problem of unstable thickness, self-limited low-temperature atomic layer is adopted for non-crystallizing growth layer by layer, the problem of increase of surface roughness caused by molecular clusters or crystal bloom caused by high temperature is avoided, and the smooth surface, uniformity and repeatability which cannot be obtained by other methods are obtained.
Drawings
FIG. 1 is atomic layer deposition of Al2O3Schematic diagram of the thin film;
FIG. 2 is a flow chart of a wafer level film thickness standard wafer fabrication for in-line instrument calibration.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
In order to overcome the defects of the existing wafer-level film thickness standard sheet preparation technology, the invention utilizes the film preparation technologies such as atomic layer deposition and the like to deposit films with different thicknesses on the single crystal substrate to obtain the high-precision wafer-level film thickness standard sample plates with different thicknesses.
The principle of ALD deposition of thin films is shown in fig. 1, each deposition cycle comprising the following four steps:
the first step is as follows: the first precursor source pulses into the reaction chamber to react with (or chemisorb) functional groups on the substrate surface and saturate and automatically terminate.
The second step is that: the first precursor source that has not reacted and the by-product purge produced by the reaction are purged away using an inert gas purge pulse.
The third step: and (3) a second precursor source is pulsed into the reaction cavity and reacts with an intermediate product generated in the first step reaction to generate a target film (the reaction is saturated and is automatically terminated at the same time).
The fourth step: the unreacted second precursor source and the by-product purge produced by the reaction are purged away using an inert gas purge pulse.
Repeating the above four steps continuously, atoms can be controlled to grow on the substrate layer by layer to form a film until the film thickness reaches the target thickness. This is because the ALD growth mode is a self-limiting surface chemical reaction between the chemical vapor precursor source and the surface of the solid substrate, and when the surface chemical adsorption is saturated, the amount of the surface reaction precursor does not increase with time, so ALD can accurately control the film thickness at the monoatomic level, and ensure that the film growth achieves 100% uniformity, conformality and no pinholes.
Specifically, the invention provides a preparation method of a wafer-level film thickness standard wafer for instrument calibration, which comprises the following steps:
step 1, cleaning a wafer substrate and removing a natural oxidation layer to obtain a processed wafer substrate;
and 2, depositing a film on the wafer substrate obtained in the step 1 by using an atomic layer deposition method to obtain a large-area uniform wafer-level film thickness standard sheet with accurately controllable thickness.
The standard sheet is Si/Al2O3Film thickness standard wafer, Si/SiO2Film thickness standard wafer, Si/HfO2Film thickness standard wafer, Si/TiO2Film thickness standard wafer, Si/ZnO film thickness standard wafer, Si/ZrO film2A film thickness standard sheet or a Si/AlN film thickness standard sheet.
The substrate selected is a 2 inch, 4 inch, 6 inch, 8 inch or 12 inch monocrystalline silicon wafer substrate.
The thickness of the obtained wafer-level film thickness standard sheet is 0-1000 nanometers.
Preparation of Si/Al2O3The film thickness standard sheet comprises the following steps:
step 1, cleaning a single crystal Si substrate with a selected size, and then soaking the single crystal Si substrate in a solution of 49% HF aqueous solution and 40% NH4F aqueous solution (volume ratio) for 3-10 seconds to remove SiO on the surface2After being fished out, the layer is washed by a large amount of deionized water and dried by dry nitrogen, and then is immediately put into an ALD reaction chamber to be heated to 200-300 ℃ to prepare for depositing a thin film material;
step 2, depositing Al with different periods on the surface of the single crystal Si wafer by using ALD technology on the basis of the step 12O3A film; the deposition process parameters are as follows: the first precursor source is trimethylaluminum; the second precursor source is an oxygen source, which is deionized water (H)2O) and hydrogen peroxide (H)2O2) Oxygen (O)2) Ozone (O)3) Or an oxygen plasma; the pulse time of the first precursor source was 0.1s, and the flow rate of the carrier gas (nitrogen) was 150 sccm; then, purging with 150sccm nitrogen gas for 6-10 seconds, and performing purging for 0.1-0.2 secondsThe second precursor with the flow rate of 200sccm is pulsed, and after the pulse is finished, nitrogen with the flow rate of 200sccm is used for purging for 6-10 seconds; repeating the above two pulses until Al with a set thickness is deposited on the single crystal Si substrate2O3And (4) preparing a thin film.
Step 3, utilizing a vacuum loading mechanical arm of the ALD system to completely grow Al in the step 22O3Transferring the wafer of the film to a sample chamber, cooling, taking out, putting into a special wafer box, and carrying out vacuum packaging to finally obtain 8-inch Si/Al2O3The film thickness of the wafer is standard.
Preparation of Si/SiO2The technological parameters of the film thickness standard wafer are the same as those of Si/Al2O3Film thickness standard sheet, except: the first precursor source is tris (dimethylamino) silicon or bis (diethylamine) silane and the second precursor source is O2And Ar2According to the flow ratio of 2: 10 as an O source precursor, wherein O is generated2Is set at 80sccm, Ar2The flow rate of (2) is controlled at 40 sccm; the pulse time of the oxygen plasma is 4-6 s.
Preparation of Si/HfO2The technological parameters of the film thickness standard wafer are the same as those of Si/Al2O3Film thickness standard sheet, except: the first precursor source is tetra (methylamino) hafnium or tetra (dimethylamino) hafnium, and the heating temperature of the first precursor source is 100-120 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of the first precursor source is 0.1s-0.2 s; the second precursor source is pulsed for a time of 0.1-5 s.
Preparation of Si/TiO2The technological parameters of the film thickness standard wafer are the same as those of Si/Al2O3Film thickness standard sheet, except: the first precursor source is tetra (dimethylamino) titanium, and the tetra (dimethylamino) titanium needs to be heated to 100-140 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of the first precursor source is 0.1s-0.2 s; the second precursor source is pulsed for a time of 0.1-6 seconds.
The technological parameters for preparing the Si/ZnO film thickness standard sheet are the same as those of Si/Al2O3Film thickness standard sheet, except: the first precursor source is diethyl zinc; deposition in a reaction chamberThe temperature is 150 ℃ and 250 ℃; the pulse time of the first precursor source is 0.1-0.2 seconds; the second precursor source is pulsed for a time of 0.1-6 seconds.
Preparation of Si/ZrO2The technological parameters of the film thickness standard wafer are the same as those of Si/Al2O3Film thickness standard sheet, except: the first precursor source is tetra (methylamino) zirconium or tetra (dimethylamino) zirconium, and the tetra (methylamino) zirconium or the tetra (dimethylamino) zirconium needs to be heated to 111-170 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of the first precursor source is 0.1-0.2 seconds; the second precursor source is pulsed for a time of 0.1-5 s.
The technological parameters for preparing the Si/AlN film thickness standard sheet are the same as those of Si/Al2O3Film thickness standard sheet, except: the first precursor source is trimethylaluminum, the second precursor source is a nitrogen source, and the nitrogen source is NH3The plasma of (2); the pulse time of the first precursor source is 0.1-0.2 seconds; NH (NH)3Plasma pulse time of 2-16s, NH3The cleaning time of the plasma is 3-5 s.
The invention has the following effects:
the invention adopts the ALD technology and other technologies to deposit the film, is convenient for accurately controlling the thickness of the film, has high repeatability, and ensures that the thickness value repeatability of standard sheets of the same batch and different batches is good.
The large area prepared by the ALD thin film technology has good uniformity of thickness, so that good in-chip uniformity of the prepared wafer-level film thickness standard sheet is guaranteed, and the precondition for guaranteeing the good uniformity is that the selection and matching of a precursor source, the precursor heating temperature, the pulse time, the purging time, the reaction temperature and the substrate can be realized only by selecting a specific combination of all elements in the arrangement, so that the result can not be obtained by limited tests.
Through the careful design of chemical reaction channel and process control, the SiO is solved2And Al2O3The formation of molecular clusters or crystal grains during the film formation process causes problems of film surface roughness and thickness non-uniformity, and SiO2And Al2O3Film atmospheric stability and temperature stabilityThe method is good, so that the prepared standard substance has better stability and uniformity. .
In addition, compared with other prior art, the ALD technology can prepare large-area uniform conformal films, and has the characteristics of high repeatability, controllable film thickness and single atomic layer magnitude, small surface roughness of deposited films, no pinholes, high quality and the like; meanwhile, the ALD technology is high in purity, pollution-free and quality, and the ALD technology is widely applied to the current semiconductor enterprise production line, so that the ALD technology is good in compatibility with the current semiconductor production line and the micro-nano manufacturing technology, and large-scale industrial production is facilitated. In particular the Si/Al produced2O3The standard film thickness can be stable for a long time under the atmospheric environment, can be stably used under the conditions of high temperature, high humidity and high oxygen, has no toxicity and pollution to the environment and human bodies, and effectively solves the problem of small Si/SiO value developed by the American VLSI and Chinese metrological science research institute2Film thickness standard wafers result in SiO oxidation due to exposure of Si wafers to air oxidation at room temperature and oxidation under conditions of high temperature and humidity or oxygen2The problem of film thickness value increase, still reach simultaneously and solved the difficult problem that current wafer film thickness standard piece can't use under extreme conditions such as high temperature, high humidity and high oxygen partial pressure.
When the nonstandard small-size film thickness standard wafer is needed, the wafer-level nanometer film thickness standard wafer can be cut into any required small size for use, the flexibility is high, and the application requirements of nonstandard small-size film thickness standard substances are met.
Example 1
For standard international and market requirements, 8 inch Si/Al of 200nm in series thickness was prepared2O3The preparation process of the film thickness standard sheet is shown in figure 1, and the specific steps are as follows:
step 1, cleaning an 8-inch single crystal Si substrate, and soaking the cleaned single crystal Si substrate in a solution of 49% HF aqueous solution and 40% NH4F aqueous solution (volume ratio) for 3 seconds to remove SiO on the surface2After being fished out, the layer is washed by a large amount of deionized water and dried by dry nitrogen, and then the layer is immediately put into an ALD reaction chamber to be heated to 200 ℃ to prepare for depositing thin film materials；
Step 2, adopting trimethylaluminum and deionized water (H) on the basis of the step 1 as shown in figure 22O) respectively serving as precursor sources of Al and O, and depositing Al with different periods on the surface of a single crystal Si wafer by using ALD (atomic layer deposition) technology2O3A film; the deposition process parameters are as follows: the pulse time of the trimethylaluminum is 0.1 second, and the flow rate of the carrier gas is 150 sccm; then, purging with 150sccm nitrogen for 6 seconds, performing deionized water pulse with the flow rate of 200sccm for 0.1 second after the purging is completed, and purging with 200sccm nitrogen for 6 seconds after the pulse is completed; repeating the above two pulses until Al with a set thickness is deposited on the single crystal Si substrate2O3Preparing a film;
step 3, utilizing a vacuum loading mechanical arm of the ALD system to completely grow Al in the step 22O3Transferring the wafer of the film to a sample chamber, cooling, taking out, putting into a special wafer box, and carrying out vacuum packaging to finally obtain 8-inch Si/Al2O3The film thickness of the wafer is standard.
Si/Al prepared by the scheme of the patent2O3Film thickness of wafer standard wafer, because Al is realized2O3The non-crystallization growth of the film greatly reduces the conditions of film cracking, falling and the like caused by stress between the film and the substrate, and in addition, the problems of film surface roughness increase, uneven thickness and the like caused by molecular clusters and crystallization caused by surface energy are solved by utilizing a low-energy growth mode, and finally the film thickness standard wafer with the small substrate with the rough and ultra-high surface and the uniform large-area thickness is obtained.
Example 2
The difference from the embodiment 1 is that: the temperature of the ALD reaction chamber is 250 ℃; the second precursor source is H2O2；H2O2Pulse time of (2) was 0.15 second, and 2nm of 8-inch Si/Al was obtained2O3The film thickness of the wafer is standard.
Example 3
The difference from the embodiment 1 is that: the temperature of the ALD reaction chamber is 300 ℃; the second precursor source is O3；O3Pulse time of (3) was 0.2 seconds, and a 50nm Si/Al pulse of 8 inches was obtained2O3The film thickness of the wafer is standard.
Example 4
Preparation of Si/SiO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
tris (dimethylamino) silane is used as a precursor source of Si; the second precursor source is O2And Ar2According to the flow ratio of 2: 10 as an O source precursor, wherein O is2Is set at 80sccm, Ar2The flow rate of (2) was controlled at 40sccm and the pulse time of the oxygen plasma was 4s, to obtain 2-inch 10nm Si/SiO2The film thickness of the wafer is standard.
Si/SiO prepared by the solution2The wafer standard wafer has good environmental stability, small surface roughness and good thickness uniformity and has high repeatability. Because of the large SiO of this method2The film has very high compactness, and solves the problem of SiO prepared by other traditional methods2The film has pinholes and the compactness is poor to cause the prepared Si/SiO2The film thickness standard sheet is easy to be secondarily oxidized by oxygen and water vapor in the air in the atmospheric environment, so that the fatal problem of unstable thickness is caused. The self-limited low-temperature atomic layer non-crystallizing growth is adopted, the problem of surface roughness and excess increase caused by molecular clusters or crystal bloom caused by high temperature is avoided, and smooth surface, uniformity and repeatability which cannot be obtained by other methods are obtained.
Example 5
Preparation of Si/SiO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
the temperature of the ALD reaction chamber is 250 ℃; bis (diethylamine) silane was used as a precursor source for Si, with a pulse time of 0.15 s; the second precursor source is O2And Ar2According to the flow ratio of 2: 10 as an O source precursor, wherein O is2Is set at 80sccm, Ar2The flow rate of (2) was controlled at 40sccm, the pulse time of the oxygen plasma was 5s, and 8-inch 20nm Si/SiO film was obtained2The film thickness of the wafer is standard.
Example 6
Preparation of Si/SiO2Film thicknessThe specific steps of the standard tablet are different from those of example 1 in that:
the temperature of the ALD reaction chamber is 300 ℃; bis (diethylamine) silane was used as a precursor source for Si, with a pulse time of 0.2 s; the second precursor source is O2And Ar2According to the flow ratio of 2: 10 as an O source precursor, wherein O is2Is set at 80sccm, Ar2The flow rate of (2) was controlled at 40sccm and the pulse time of the oxygen plasma was 6s, to obtain 4-inch 50nm Si/SiO2The film thickness of the wafer is standard.
Example 7
Preparation of Si/HfO2The film thickness standard sheet differs from example 1 in that:
mixing tetra (methylethylamino) hafnium and deionized water (H)2O) are respectively used as precursor sources of Hf and O, and simultaneously, the tetra (methylethylamino) hafnium is heated to 100 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; finally obtaining 8-inch 10nm Si/HfO2The film thickness of the wafer is standard.
Example 8
Preparation of Si/HfO2The film thickness standard sheet differs from example 1 in that:
the temperature of the ALD reaction chamber is 250 ℃; the first precursor source is tetrakis (dimethylamino) hafnium; the second precursor source is O3(ii) a Meanwhile, heating the tetra (methylethylamino) hafnium to 110 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of tetrakis (dimethylamino) hafnium was 0.15 seconds; o is3The pulse time of (3) was 3 seconds, and finally 6 inches of 50nm of Si/HfO was obtained2The film thickness of the wafer is standard.
Example 9
Preparation of Si/HfO2The film thickness standard sheet differs from example 1 in that:
the temperature of the ALD reaction chamber is 300 ℃; the first precursor source is tetrakis (dimethylamino) hafnium; the second precursor source is O2(ii) a Meanwhile, heating the tetra (methylethylamino) hafnium to 120 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of tetrakis (dimethylamino) hafnium was 0.2 seconds; o is2Pulse time of (3) was 5 seconds, and Si/Al of 8 inches and 100nm was obtained2O3The film thickness of the wafer is standard.
Example 10
Preparation of Si/TiO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
mixing tetra (dimethylamino) titanium and deionized water (H)2O) are respectively used as precursor sources of Ti and O, and simultaneously, the tetra (methyl ethylamine) hafnium is heated to 100 ℃ to ensure that the titanium source has sufficient output vapor pressure value, and 8 inches of Si/TiO with the thickness of 20nm is obtained2The film thickness of the wafer is standard.
Example 11
Preparation of Si/TiO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
the temperature of the ALD reaction chamber is 250 ℃; reacting tetra (dimethylamino) titanium with O2Respectively serving as precursor sources of Ti and O, and simultaneously heating tetra (dimethylamino) titanium to 120 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of the (dimethylamino) titanium was 0.15 seconds; o is2Pulse time of 3 seconds to obtain 8 inches of 50nm Si/TiO2The film thickness of the wafer is standard.
Example 12
Preparation of Si/TiO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
the temperature of the ALD reaction chamber is 300 ℃; the second precursor source is O2(ii) a Reacting tetra (dimethylamino) titanium with O2Respectively serving as precursor sources of Ti and O, and simultaneously heating tetra (dimethylamino) titanium to 140 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of the (dimethylamino) titanium was 0.2 seconds; o is2Pulse time of 6 seconds, 12 inches of 50nm Si/TiO2The film thickness of the wafer is standard.
Example 13
The specific steps for preparing the Si/ZnO film thickness standard sheet are different from those in the example 1:
the temperature of the ALD reaction chamber is 150 ℃; diethyl zinc and deionized water (H)2O) as precursor sources for Zn and O, respectively; obtaining 8-inch 50nm Si/ZnO2The film thickness of the wafer is standard.
Example 14
The specific steps for preparing the Si/ZnO film thickness standard sheet are different from those in the example 1:
the temperature of the ALD reaction chamber is 250 ℃; reacting diethyl zinc and O2As precursor sources for Zn and O, respectively; the pulse time of diethyl zinc was 0.15 s; o is2The pulse time of (3) seconds; obtaining 8-inch 50nm Si/ZnO2The film thickness of the wafer is standard.
Example 15
The specific steps for preparing the Si/ZnO film thickness standard sheet are different from those in the example 1:
the temperature of the ALD reaction chamber is 200 ℃; reacting diethyl zinc and O2As precursor sources for Zn and O, respectively; the pulse time of diethyl zinc was 0.2 s; o is2The pulse time of (2) was 6 seconds; obtaining 8-inch 50nm Si/ZnO2The film thickness of the wafer is standard.
Example 16
Preparation of Si/ZrO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
tetrakis (methylethylamino) zirconium and deionized water (H)2O) are respectively used as precursor sources of Zr and O, and simultaneously, the tetra (methylethylamino) zirconium is heated to 111 ℃ to ensure that the titanium source has sufficient output vapor pressure value, and 8 inches of Si/ZrO with the thickness of 100nm is obtained2The film thickness of the wafer is standard.
Example 17
Preparation of Si/ZrO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
the temperature of the ALD reaction chamber is 250 ℃; tetrakis (methylethylamino) zirconium and deionized water (H)2O) are respectively used as precursor sources of Zr and O, and simultaneously, the tetra (methylethylamino) zirconium is heated to 140 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of tetrakis (methylethylamino) zirconium was 0.15 s; o is2The pulse time of (3) seconds; obtaining 8-inch 200nm Si/ZrO2The film thickness of the wafer is standard.
Example 18
Preparation of Si/ZrO2The specific steps of the film thickness standard sheet are different from those of the example 1 in that:
ALD reactionThe temperature of the cavity is 300 ℃; tetrakis (methylethylamino) zirconium and deionized water (H)2O) are respectively used as precursor sources of Zr and O, and simultaneously, the tetra (methylethylamino) zirconium is heated to 170 ℃ to ensure that the titanium source has a sufficient output vapor pressure value; the pulse time of tetrakis (methylethylamino) zirconium was 0.2 s; o is2The pulse time of (2) is 5 seconds; obtaining 8 inch 500nm Si/ZrO2The film thickness of the wafer is standard.
Example 19
The specific steps for preparing the Si/AlN film thickness standard sheet are different from those in example 1 in that:
the first precursor source is trimethylaluminum;
the second precursor source is a nitrogen source, which is NH3The plasma of (2); NH (NH)3The plasma pulse time of (2) was 6 s; after the second precursor source pulse was completed, the wafer standard wafer of 8 inches Si/AlN film thickness was obtained with a thickness of 5nm by purging with 200sccm of nitrogen gas for 3 seconds.
The problem of poor adhesion between an AlN thin film deposited by the traditional PVD method and a substrate is solved by reacting chemical bonds or functional groups on the surfaces of a precursor source and a substrate in the AlN film forming process to form chemical bond combination; by adopting self-limited atomic layer-by-layer growth and non-crystallization growth, smooth surface, uniformity and repeatability which cannot be obtained by other methods are obtained; the growth temperature of the AlN thin film is greatly reduced by means of the plasma, and the problems of surface roughness increase caused by crystallization of the AlN thin film and uneven thickness of the thin film caused by CVD reaction caused by high temperature are avoided.
Example 20
The specific steps for preparing the Si/AlN film thickness standard sheet are different from those in example 1 in that:
the temperature of the ALD reaction chamber is 250 ℃;
the first precursor source was trimethylaluminum with a pulse time of 0.15 s;
the second precursor source is a nitrogen source, which is NH3Plasma of (2), NH3The plasma pulse time of (2) s; after the second precursor source pulse is completed, the wafer is purged with 200sccm of nitrogen for 4s to obtain a 5nm thick wafer standard of 8 inches Si/AlN film thicknessAnd (3) slicing.
Example 21
The specific steps for preparing the Si/AlN film thickness standard sheet are different from those in example 1 in that:
the temperature of the ALD reaction chamber is 300 ℃; the first precursor source was trimethylaluminum with a pulse time of 0.15 s;
the second precursor source is a nitrogen source, which is NH3Plasma of (2), NH3Plasma pulse time of 16 s; after the second precursor source pulse is finished, the wafer standard wafer with the thickness of 8 inches Si/AlN film and the thickness of 5nm is obtained by cleaning the wafer for 5s by using nitrogen of 200sccm
In conclusion, the method successfully prepares the wafer-level film thickness standard wafer for on-line instrument calibration and process quality control on the 2-12 inch wafer by using the film thickness accurate controllable and large-area uniform film preparation technology, namely breaks through the defects of extremely small film thickness (1nm) and small film thickness Si/SiO which cannot be realized by the traditional PVD, CVD, thermal oxidation and other methods2The unstable amount of the wafer sample is exposed to the oxygen and the moisture environment. The method has simple and easy preparation process, is compatible with the existing industrialized semiconductor preparation process flow, and can prepare the span-level multi-scale line width sample plate with low cost and simple equipment.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all equivalent changes and modifications made within the scope of the present invention should be considered as the technical scope of the present invention.
Claims (10)
1. A preparation method of a wafer-level film thickness standard wafer for instrument calibration is characterized by comprising the following steps:
and cleaning the wafer substrate, removing the natural oxide layer to obtain the processed wafer substrate, and depositing a film on the wafer substrate by using an atomic layer deposition method to obtain the wafer-level film thickness standard sheet.
2. The method for preparing wafer-level film thickness standard wafer for instrument calibration as claimed in claim 1, wherein the wafer-level film thickness standard wafer is prepared by a method comprising a step of preparing a wafer-level film thickness standard wafer for instrument calibrationThe wafer-level film thickness standard wafer is Si/Al2O3Film thickness standard wafer, Si/SiO2Film thickness standard wafer, Si/HfO2Film thickness standard wafer, Si/TiO2Film thickness standard wafer, Si/ZnO film thickness standard wafer, Si/ZrO film2A film thickness standard sheet or a Si/AlN film thickness standard sheet.
3. The method for preparing wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein Si/Al is prepared2O3The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is trimethyl aluminum, and the second precursor source is an oxygen source;
the pulse time of the first precursor source was 0.1 seconds, and the carrier gas flow rate was 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-0.2 seconds, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
4. The method for preparing wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein Si/SiO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is bis (diethylamine) silane or tris (dimethylamino) silane; the second precursor source is O2And Ar2According to the flow ratio of 2: 1 mixed oxygen plasma; wherein, O2At a flow rate of 80sccm, Ar2The flow rate of (2) was 40 sccm.
The pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 4-6s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
5. According to the rightThe method for preparing a wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein the Si/HfO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is tetra (methylamino) hafnium or tetra (dimethylamino) hafnium, and the heating temperature of the first precursor source is 100-120 ℃;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-5s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
6. The method for preparing wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein Si/TiO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 200-300 ℃;
the first precursor source is tetra (dimethylamino) titanium, and the heating temperature of the first precursor source is 100-120 ℃;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-6s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
7. The method for preparing the wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein Si/ZnO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 150-250 ℃;
the first precursor source is diethyl zinc;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-6s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
8. The method for preparing a wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein the Si/ZrO is prepared2The technological parameters of the film thickness standard sheet are as follows:
the temperature in the ALD reaction chamber is 150-250 ℃;
the first precursor source is tetra (methylethylamino) zirconium or tetra (dimethylamino) zirconium and the heating temperature of the first precursor source is 111-170 ℃;
the second precursor source is an oxygen source;
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 0.1-5s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 6-10 seconds.
9. The method for preparing the wafer-level film thickness standard wafer for instrument calibration as claimed in claim 2, wherein the process parameters for preparing the Si/AlN film thickness standard wafer are as follows:
the temperature in the ALD reaction chamber is 150-250 ℃;
the first precursor source is trimethylaluminum;
the second precursor source is a nitrogen source, which is NH3The plasma of (2);
the pulse time of the first precursor source is 0.1-0.2 seconds, and the carrier gas flow is 150 sccm; then flushing with nitrogen of 150sccm for 6-10 seconds;
the pulse time of the second precursor source is 2-16s, and the flow rate is 200 sccm; followed by a nitrogen purge of 200sccm for 3-5 seconds.
10. The method for preparing a wafer-level film thickness standard wafer for instrument calibration as claimed in claim 1, wherein the thickness of the obtained wafer-level film thickness standard wafer is 0-1000 nm.
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