WO2006106858A1 - プラズマドーピング方法及び装置 - Google Patents
プラズマドーピング方法及び装置 Download PDFInfo
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- WO2006106858A1 WO2006106858A1 PCT/JP2006/306721 JP2006306721W WO2006106858A1 WO 2006106858 A1 WO2006106858 A1 WO 2006106858A1 JP 2006306721 W JP2006306721 W JP 2006306721W WO 2006106858 A1 WO2006106858 A1 WO 2006106858A1
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- plasma
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- plasma doping
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- vacuum vessel
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Classifications
-
- H—ELECTRICITY
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/26—Bombardment with radiation
- H01L21/263—Bombardment with radiation with high-energy radiation
- H01L21/265—Bombardment with radiation with high-energy radiation producing ion implantation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32917—Plasma diagnostics
- H01J37/32935—Monitoring and controlling tubes by information coming from the object and/or discharge
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32009—Arrangements for generation of plasma specially adapted for examination or treatment of objects, e.g. plasma sources
- H01J37/32412—Plasma immersion ion implantation
-
- H—ELECTRICITY
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/22—Diffusion of impurity materials, e.g. doping materials, electrode materials, into or out of a semiconductor body, or between semiconductor regions; Interactions between two or more impurities; Redistribution of impurities
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L22/00—Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
- H01L22/20—Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps
- H01L22/26—Acting in response to an ongoing measurement without interruption of processing, e.g. endpoint detection, in-situ thickness measurement
-
- H—ELECTRICITY
- 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
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67098—Apparatus for thermal treatment
- H01L21/67115—Apparatus for thermal treatment mainly by radiation
Definitions
- the present invention relates to a plasma doping method and apparatus for implanting ions using a plasma on a sample surface that is a crystal.
- FIG. 19 shows a schematic configuration of a typical plasma processing apparatus used for conventional plasma doping.
- a sample electrode 6 for placing a sample 9 made of a silicon substrate is provided in a vacuum vessel 1.
- a gas supply device 2 for supplying a source gas containing a desired element such as helium gas in the vacuum vessel 1 and a pump 3 for reducing the pressure in the vacuum vessel 1 are provided. Can be kept in.
- Microwaves are radiated from the microwave waveguide 51 into the vacuum chamber 1 through the quartz plate 52 as a dielectric window.
- a magnetic field microwave plasma (electron cyclotron resonance plasma) 54 is formed in the vacuum chamber 1 by the interaction between the microwave and the DC magnetic field formed by the electromagnet 53.
- a high frequency power supply 10 is connected to the sample electrode 6 via a capacitor 55 so that the potential of the sample electrode 6 can be controlled.
- the gas supplied from the gas supply device 2 is introduced into the vacuum container 1 from the gas inlet 56 and exhausted from the exhaust port 11 to the pump 3.
- the raw material gas introduced from the gas introduction port 56 for example, helium gas
- a plasma generating means including a microwave waveguide 51 and an electromagnet 53.
- helium ions in the plasma 54 are introduced to the surface of the sample 9 by the high frequency power source 10.
- FIG. 20 is a schematic configuration of an apparatus showing an example.
- the silicon inside the vacuum vessel 1 A sample electrode 6 for mounting a sample 9 made of a substrate is provided.
- a gas supply device 2 for supplying a doping gas containing a desired element, for example, BH, into the vacuum vessel 1, true
- a pump 3 for depressurizing the inside of the empty container 1 is provided, and the inside of the vacuum container 1 can be maintained at a predetermined pressure.
- the inside of the vacuum container 1 can be maintained at a predetermined pressure.
- plasma is formed in the vacuum chamber 1, and boron ions in the plasma are introduced to the surface of the sample 9.
- the doped boron concentration can be controlled by measuring the high-frequency current during discharge with the ammeter 59 via the high-frequency current transformer 58.
- a counter electrode 57 is provided to face the sample electrode, and the counter electrode 57 is grounded.
- a desired impurity such as boron is introduced into the surface of the sample 9 thus amorphized by means such as ion implantation or plasma doping, and an activation process described later is performed. Further, after forming a metal wiring layer on the sample 9 into which impurities have been introduced, a thin oxide film is formed on the metal wiring layer in a predetermined oxidation atmosphere, and then a CVD apparatus or the like is formed. Thus, when a gate electrode is formed on the sample 9, for example, a MOS transistor is obtained. However, to form a transistor, it is necessary to carry out an active ion treatment after introducing impurity ions by plasma doping treatment.
- the activation process is a process in which an impurity-introduced layer is heated using a method such as RTA (Rapid Carothermal Annealing), Spike RTA (Spike Rapid Thermal Annealing), Laser Annealing, or Flash Lamp Annealing. Process to crystallize.
- RTA Rapid Carothermal Annealing
- Spike RTA Spike Rapid Thermal Annealing
- Laser Annealing or Flash Lamp Annealing. Process to crystallize.
- a shallow active layer can be obtained by effectively heating an extremely thin layer into which impurities are introduced.
- the absorption rate of the light source power, such as a laser or lamp, in the extremely thin layer to which the impurities are to be introduced is increased.
- a process to increase is performed. This process is called pre-amorphization.
- plasma such as the aforementioned He gas is generated, and ions such as generated He are generated by the bias voltage on the substrate. This is accelerated and collided to destroy the crystal structure on the surface of the substrate to make it amorphous, which has already been proposed by the present inventors.
- Non-Patent Document 1 Y. Sasaki et al., "B2H6 Plasma Doping with In -situ He Pre ⁇ amorphyzation ", 2004 Symposia on VLSI Technology and Circuits
- boron when boron is implanted into a silicon crystal by ion implantation, boron is implanted deeply due to the channeling effect.
- the channeling effect is a well-known phenomenon, in which boron is implanted deeply so as to pass through a tunnel in a crystal without colliding with silicon atoms. If this effect is reduced and boron is implanted shallowly, the pre-amorphization process is also used. That is, by disposing the silicon crystal in an amorphous state before boron implantation, the arrangement of silicon atoms is separated. As a result, boron atoms randomly collide with silicon atoms and can be implanted shallowly.
- the introduction of impurity ions and preamorphization can be performed simultaneously.
- This also uses a plasma processing apparatus having the same configuration as the plasma processing apparatus described above.
- a plasma such as a gas containing a very small amount of BH gas mixed with the above He gas is generated.
- Ions are accelerated and collided toward the substrate by a bias voltage, destroying the crystal structure on the surface of the substrate and making it amorphous.
- ions such as B are accelerated toward the substrate by a bias voltage and implanted into the substrate. To do.
- Figure 21 shows the results of measuring the depth of the amorphous layer formed on the silicon wafer surface.
- the vertical axis represents the depth of the amorphous layer, and the horizontal axis represents the number of samples. That is, there is a problem that the variation in the depth of the amorphous layer formed on the surface of the silicon wafer becomes large despite the plasma doping process being performed under the same conditions.
- the present inventors have proposed! This is a new problem that has occurred for the first time after amorphization by plasma irradiation. This is a problem that does not occur with the conventional technique of ion implantation of germanium or silicon ions, for example.
- the acceleration energy of ions can be obtained with good controllability and repeatability by the voltage applied to the acceleration electrode.
- the ion species irradiated to the silicon wafer can be obtained with a repeatability with a single desired ion species with an analysis electromagnet.
- the dose of the metal can also be obtained with good repeatability by using an electrical dose monitor using a Faraday cup and time control. Since the amorphous layer is determined by the ion species, acceleration energy, and dose, it is known that it is easy to form an amorphous layer with good repeatability.
- Plasma doping is a force that accelerates ions in the plasma by the potential difference generated in the plasma sheath between the plasma and the substrate.
- the plasma state is not as stable as the voltage applied to the acceleration electrode in ion implantation, and controllability is also good. Absent. This is because the plasma changes depending on the state of the process chamber. Therefore, when plasma doping is repeatedly performed for production, deposits containing boron and the like are attached to the process chamber.
- the present invention has been made in view of the above circumstances, and provides a plasma doping method and apparatus excellent in repeatability and controllability of the amorphous layer depth and impurity implantation depth formed on the sample surface. As a goal!
- the method of the present invention is a plasma doping method in which plasma is generated in a vacuum vessel, and ions in the plasma collide with the surface of the sample to modify the surface of the crystal sample to be amorphous.
- the conditions for processing the sample are controlled so that the optical characteristics obtained in the measurement process have desired values.
- the present invention proposes a method of improving repeatability by controlling the implantation depth of impurity ions by plasma doping.
- impurity ions are implanted by plasma doping.
- amorphization is performed simultaneously with implantation or prior to implantation.
- the present inventors have newly found that there is a strong proportional relationship between the implantation depth of impurity ions and the depth of the amorphous layer when the impurity ions are implanted by plasma doping and the silicon crystal is made amorphous. I found it.
- the depth of the amorphous layer is controlled, thereby implanting impurity ions. It was found that the depth of embedding can be controlled.
- the depth of an amorphous layer is measured using light in plasma doping, the plasma doping conditions are set so that the measured value becomes a desired value, and the depth of the amorphous layer is repeated. Improving the reproducibility, the impurity ion implantation depth is utilized in the plasma doping! /, Taking advantage of the strong proportional relationship between the impurity ion implantation depth and the amorphous layer depth. This is characterized by improved reproducibility.
- a sample is placed on a sample electrode in a vacuum vessel, and plasma is generated in the vacuum vessel, while ions in the plasma are used as a sample.
- the sample in the step of performing the amorphization treatment, is placed on the sample electrode in the vacuum vessel, and the vacuum vessel is evacuated while supplying the gas from the gas supply device into the vacuum vessel. Then, while controlling the inside of the vacuum vessel to a predetermined pressure and supplying power to the sample electrode to generate plasma in the vacuum vessel, the ions in the plasma are accelerated toward the sample surface and collide with each other. This includes the process of modifying the sample surface, which is crystalline, to amorphous.
- the sample is placed on the sample electrode in the vacuum vessel, and the gas is supplied from the gas supply device to the vacuum vessel and the vacuum vessel is evacuated. Then, while controlling the inside of the vacuum container to a predetermined pressure, plasma is generated in the vacuum container by supplying high-frequency power to the plasma source, and ions in the plasma are sampled by supplying power to the sample electrode. Accelerate and collide with the surface of the Including crystals.
- the surface of the dummy sample subjected to the plasma doping treatment is irradiated with light to detect a difference in the polarization state of the incident light and the reflected light.
- the modifying step includes a step of controlling the processing condition so as to change acceleration energy for accelerating ions in the plasma toward the surface of the sample. .
- the step of modifying the potential difference that can be adjusted by the magnitude of the power formed between the plasma and the sample electrode by changing the power supplied to the sample electrode Including a step of controlling the processing conditions so as to be performed.
- the modifying step includes a step of controlling the processing conditions so as to change a plasma irradiation time.
- the step of modifying includes a step of controlling the processing conditions so as to change a high-frequency power supplied to a plasma source.
- the modifying step includes a step of controlling the processing conditions so as to change the pressure in the vacuum vessel.
- the method of the present invention includes one in which the sample is a semiconductor substrate made of silicon.
- the method of the present invention includes a plasma force rare gas plasma generated in a vacuum vessel.
- the method of the present invention includes a plasma force generated in a vacuum vessel, helium, or a plasma of neon.
- the plasma generated in the vacuum vessel is a plasma containing impurities, and the sample surface that is a crystal is modified to be amorphous, and at the same time, the impurity is introduced into the sample surface. Including what is to do.
- the method of the present invention includes one in which the impurity is boron.
- the plasma is a plasma containing boron diluted with helium. Including some.
- the method of the present invention also includes a plasma force generated in a vacuum vessel that is a plasma containing diborane.
- the method of the present invention is a plasma containing arsenic, phosphorus, or antimony, which is generated in a vacuum vessel.
- the sample surface which is a crystal, is modified to be amorphous, arsenic, phosphorus, or Includes plasma doping that introduces antimony into the sample surface.
- the method of the present invention includes a method in which the dummy sample is a part of a sample provided in a portion that is not necessary as a sample device.
- the method of the present invention is a plasma doping method in which plasma is generated in a vacuum vessel, and ions in the plasma collide with the surface of the sample to modify the surface of the crystal sample to be amorphous. And the step of amorphizing the dummy sample by plasma irradiation, the step of measuring the depth of the amorphous layer formed on the surface of the dummy sample subjected to the plasma irradiation, and the measurement step It is characterized in that the conditions for processing the crystal sample are controlled so that the depth of the obtained amorphous layer becomes a desired value.
- the method of the present invention includes a method in which the depth of the introduced impurity ion is controlled by controlling the depth of the amorphous layer.
- the apparatus of the present invention also includes a plasma doping chamber comprising a vacuum vessel, a sample electrode, a plasma supply means for supplying plasma to the sample, and a power supply for the sample electrode for supplying power to the sample electrode. And a light irradiation unit for irradiating the sample with light, and a detection unit for detecting the polarization state of the incident light and the reflected light on the sample.
- the apparatus of the present invention controls a gas supply means for supplying a gas into the plasma doping chamber into the vacuum container, an exhaust means for exhausting the inside of the vacuum container, and a pressure in the vacuum container. Including those equipped with pressure control means.
- the apparatus of the present invention includes the detector provided in the plasma doping chamber.
- the detection unit is provided independently of the plasma doping chamber. Included in the inspection room.
- the optical characteristics indicate optical measurement results resulting from the depth of the amorphous layer formed by modification, the difference in the degree of amorphousness depending on the degree of modification, and the like.
- FIG. 1 is a cross-sectional view showing a configuration of a plasma doping chamber used in Embodiment 1 of the present invention.
- FIG. 2 is a plan view showing the overall configuration of the plasma doping apparatus in the first embodiment of the present invention.
- FIG. 3 is a cross-sectional view showing the configuration of a lamp annealing heating chamber according to Embodiment 1 of the present invention.
- FIG. 4 is a cross-sectional view showing a configuration of a laser chamber heating chamber according to Embodiment 1 of the present invention.
- FIG. 5 is a perspective view showing a schematic configuration of the sheet resistance measuring device according to the first embodiment of the present invention.
- FIG. 6 is a plan view of the silicon substrate according to the second embodiment of the present invention.
- FIG. 7 is a cross-sectional view showing the configuration of a lamp annealing heating chamber according to Embodiment 2 of the present invention.
- FIG. 8 is a plan view showing the overall configuration of the plasma doping apparatus in the third embodiment of the present invention.
- FIG. 9 is a cross-sectional view showing a configuration of an X-ray analysis chamber according to Embodiment 3 of the present invention.
- FIG. 10 is a cross-sectional view showing the configuration of the plasma doping chamber in the fourth embodiment of the present invention.
- FIG. 11 is a diagram showing the relationship between the depth and the bias voltage in the fifth embodiment of the present invention.
- FIG. 12 is a flowchart showing a method according to the fifth embodiment of the present invention.
- FIG. 13 is a diagram showing a measurement result of depth in the fifth embodiment of the present invention.
- FIG. 14 is a diagram showing the relationship between driving depth and power in the sixth embodiment of the present invention.
- FIG. 15 is a diagram showing the relationship between the depth of the amorphous layer and the power in the sixth embodiment of the present invention.
- FIG. 16 is a diagram showing the relationship between boron implantation depth and amorphous layer depth in Embodiment 6 of the present invention.
- FIG. 17 is a flowchart showing a method according to the sixth embodiment of the present invention.
- FIG. 18 is a diagram showing a measurement result of depth according to the sixth embodiment of the present invention.
- FIG. 19 is a cross-sectional view showing the configuration of the plasma doping apparatus used in the conventional example
- FIG. 20 is a cross-sectional view showing the configuration of the plasma doping apparatus used in the conventional example
- FIG. 21 is a diagram showing the measurement result of depth in the plasma doping apparatus used in the conventional example.
- FIG. 1 shows a cross-sectional view of the plasma irradiation chamber of the plasma doping apparatus used in Embodiment 1 of the present invention.
- FIG. 1 while introducing a predetermined gas from the gas supply device 2 into the vacuum vessel 1, exhaust is performed by the turbo molecular pump 3 as an exhaust device, and the inside of the vacuum vessel 1 is maintained at a predetermined pressure by the pressure regulating valve 4. be able to.
- the turbo molecular pump 3 as an exhaust device
- the inside of the vacuum vessel 1 is maintained at a predetermined pressure by the pressure regulating valve 4.
- a silicon substrate 9 as a sample is placed on the sample electrode 6.
- the sample electrode 6 A high-frequency power source 10 is provided to supply power, and this functions as a voltage source that controls the potential of the sample electrode 6 so that the substrate 9 as a sample has a negative potential with respect to the plasma. . In this way, ions in the plasma can be accelerated and collided against the surface of the sample to amorphize the surface of the sample or introduce impurities.
- the gas supplied from the gas supply device 2 is exhausted from the exhaust port 11 to the pump 3.
- the turbo molecular pump 3 and the exhaust port 11 are arranged immediately below the sample electrode 6, and the pressure regulating valve 4 is a lift valve located immediately below the sample electrode 6 and directly above the turbo molecular pump 3. It is.
- the sample electrode 6 is fixed to the vacuum vessel 1 by four columns 12.
- the vacuum container 1 After placing the substrate 9 on the sample electrode 6, the vacuum container 1 is evacuated from the gas supply device 2 while evacuating the vacuum container 1 from the exhaust port 11 while keeping the temperature of the sample electrode 6 at 25 ° C. Supply 50 SC cm of helium gas inside, and control the pressure regulating valve 4 to keep the pressure in the vacuum vessel 1 at lPa. Next, by supplying 800 W of high-frequency power to the coil 8 serving as a plasma source, plasma is generated in the vacuum chamber 1, and 200 W of high-frequency power is supplied to the base of the sample electrode 6.
- the surface crystal layer could be made amorphous.
- FIG. 2 is a plan view showing the overall configuration of the plasma doping apparatus.
- the loader chamber 13 is evacuated to a vacuum state.
- the gate 15 provided between the first transfer chamber 14a and the loader chamber 13 is opened, and the transfer arm A in the first transfer chamber 14a is operated to move the sample into the first transfer chamber 14a.
- the gate 15 is appropriately opened and closed, and the transfer arm A is operated to move the sample to the plasma irradiation chamber 16 to perform an amorphization process as described above.
- the sample is moved from the plasma irradiation chamber 16 to the second transfer chamber 14b, and the sample is further moved to the unloader chamber 19 to take out the sample.
- the optical characteristics and the depth of the amorphous layer were monitored using a dummy sample.
- the causes of changes in optical characteristics and depth under the same processing conditions include deposits on the inner wall of the vacuum vessel, temperature changes in the inner wall of the vacuum vessel, and changes in the characteristics of the high-frequency power supply, which cannot be easily identified.
- a dummy sample was introduced every time 25 samples were processed.
- a single crystal silicon substrate having the same size as the sample for forming a device was used.
- the dummy sample has a cash register The sample surface was not subjected to patterning, and the entire surface of the sample was subjected to an amorphization treatment.
- the loader chamber 13 is evacuated to a vacuum state.
- the gate 15 provided between the first transfer chamber 14a and the loader chamber 13 is opened, and the transfer arm A in the first transfer chamber 14a is operated to move the dummy sample into the first transfer chamber 14a.
- the gate 15 is appropriately opened and closed, and the transport arm A is operated to move the dummy sample to the plasma irradiation chamber 16 and perform the amorphization process under the condition that the sample is processed immediately before.
- the dummy sample is moved from the plasma irradiation chamber 16 to the second transfer chamber 14b, and further, the dummy sample is moved to the inspection chamber 17.
- the inspected dummy sample is moved again to the second transfer chamber 14b in FIG. Further, it is moved to the unloader chamber 19 and taken out.
- FIG. 3 is a cross-sectional view showing a configuration of a lamp annealing heating chamber.
- a dummy sample 21 is placed on a sample stage 20 provided in the heating chamber 17.
- Infrared light emitted from a lamp 22 as a sample heating device is applied to the surface of the dummy sample 21 through a window 21.
- a tungsten halogen lamp can be used as an example of the lamp 22. Lamp light irradiation conditions were set so that the temperature of sample 9 was 1100 ° C, and activation was performed under the condition of maintaining at 1100 ° C for 3 minutes.
- the heating chamber may be a laser annealing system as shown in FIG.
- a dummy sample 21 is placed on a sample stage 24 provided in the heating chamber 17.
- Laser light emitted from a laser light source 25 serving as a sample heating device is irradiated onto the surface of the dummy sample 21 through a window 27 while the direction of the beam is controlled by a mirror 26.
- the heating chamber may be a high-temperature furnace using a ceramic heater or the like.
- a lamp laser it is possible to heat only the very surface of the dummy sample to a high temperature by applying energy to the dummy sample.
- the entire dummy sample Is heated.
- the high temperature furnace has the advantage that it is inexpensive. The dummy sample that has been subjected to the active heat treatment by heating is moved again to the second transfer chamber 14b in FIG. 2, and then moved to the sheet resistance measuring chamber 18.
- FIG. 5 shows a schematic configuration of a sheet resistance measuring device provided in the sheet resistance measuring chamber 18. It is a perspective view.
- four probes 28 are arranged in a straight line on the surface of the dummy sample 21, and the outer two are connected to the constant current source 29.
- the voltmeter 30 measures the voltage between the two probes. More precisely, the applied current value I applied in the forward and reverse directions between the two outer probes pressed against the dummy sample 21 and the measured potential difference V between the two inner probes at this time V
- the sheet resistance R of the dummy sample is calculated using the following formula.
- the dummy sample is subjected to plasma doping treatment each time 25 samples are processed, and the amorphous sample of the dummy sample subjected to plasma doping processing is processed.
- the conditions under which the sample was processed were controlled so that the optical properties and depth of the layer were at the predetermined values. Specifically, if the depth of the amorphous layer of the dummy sample is smaller than the desired value, the power supplied to the sample electrode is increased under the conditions for processing the next 25 samples. Alternatively, the high frequency power supplied to the plasma source is reduced. Alternatively, the processing time is increased.
- the power supplied to the sample electrode is reduced under the conditions for processing the next 25 samples.
- the high frequency power supplied to the plasma source is increased. Or shorten the processing time.
- control parameters under standard amorphization conditions. It is sufficient to determine experimentally how much the depth of the amorphous layer will change if this is done. In order to change each of these control parameters, it is only necessary to construct software that is stored in the control system of the apparatus and that automatically rewrites the processing recipe as shown in the figure.
- the standard amorphization condition should be used. What is necessary is just to determine experimentally how much the optical characteristics of the surface change when each of these control parameters is changed. In order to change each of these control parameters, it is necessary to construct software that can be stored in the control system of the device and automatically rewrites the processing recipe as shown in the figure.
- Embodiment 2 of the present invention will be described with reference to FIGS.
- Embodiment 1 the case where a single crystal silicon substrate having the same size as that of a sample for forming a device is used as a dummy sample is illustrated.
- a dummy sample may be processed each time 100 samples are processed to reduce the frequency of dummy sample injection, but the controllability of the amorphous layer depth is impaired. Another disadvantage arises.
- the dummy sample is configured to be a part of the sample provided in a portion which is not necessary as a sample device.
- the controllability of the amorphous layer depth becomes extremely high. In other words, it becomes possible to finely adjust the processing conditions for each sheet.
- FIG. 6 shows a plan view of a silicon substrate as a sample and a dummy sample used in the second embodiment.
- the sample 9 is provided with a large number of chip portions 31 that are later divided into semiconductor elements, and the chip portions 31 are provided with openings for introducing impurities by resist or the like.
- the semiconductor substrate is circular, whereas the element is square. For this reason, there is a portion where the chip portion cannot be provided in the peripheral portion of the substrate. A part of this part can be used as a dummy sample 32.
- the dummy sample 32 has no resist pattern or the like, and the entire dummy sample 32 is amorphized and plasma-doped. One bing process is performed.
- a partial heat treatment is performed in a heating chamber 17 as shown in FIG.
- the sample 9 is placed on the sample stage 20 provided in the heating chamber 17.
- Infrared light emitted from a lamp 22 as a sample heating device is irradiated to a part of the surface of the sample 9 through the window 21.
- the sample 9 is covered with the mask 33 so that only the dummy sample is irradiated with the lamp light.
- a technique such as a flash lamp
- only the very surface of the dummy sample, which hardly heats the chip part can be heated to 1000 ° C or higher.
- the laser annealing method can also be used as a method for performing partial caloric heat treatment. In this case, it is only necessary to use the heating chamber configured as shown in FIG.
- the heating chamber be provided with a gas supply device that supplies an inert gas into the heating chamber. Or the same effect is acquired even if it heats in vacuum.
- Embodiment 3 of the present invention will be described with reference to FIGS.
- the plasma doping chamber of the plasma doping apparatus that performs amorphization and plasma doping is already in the first embodiment of the present invention! Since this is the same as FIG. 1 described above, the description is omitted here.
- FIG. 8 is a plan view showing the overall configuration of the plasma doping apparatus.
- the loader chamber 13 is evacuated to a vacuum state.
- the gate 15 provided between the first transfer chamber 14a and the loader chamber 13 is opened, and the transfer arm A in the first transfer chamber 14a is operated to move the sample into the first transfer chamber 14a.
- the gate 15 is appropriately opened and closed, and the transfer arm A is operated to move the sample to the plasma doping chamber 16 to perform an amorphization process and a plasma doping process.
- the sample is moved from the plasma doping chamber 16 to the second transfer chamber 14b.
- the sample is moved to the unloader chamber 19 and the sample is taken out.
- the difference between the polarization states of incident light and reflected light was monitored by ellipsometry using a dummy sample.
- the causes of changes in the depth and surface state of the amorphous layer under the same processing conditions include adhesion of gas and deposits to the inner wall of the vacuum vessel, and changes in the characteristics of the high-frequency power source, which cannot be easily identified.
- a dummy sample was introduced every time 25 samples were processed.
- a dummy sample a single crystal silicon substrate having the same size as the sample for forming a device was used. The dummy sample was not patterned such as resist, and the entire sample surface was amorphized and doped.
- the loader chamber 13 is evacuated to a vacuum state.
- the gate 15 provided between the first transfer chamber 14a and the loader chamber 13 is opened, and the transfer arm A in the first transfer chamber 14a is operated to move the dummy sample into the first transfer chamber 14a.
- the gate 15 is appropriately opened and closed, and the transfer arm A is operated to move the dummy sample to the plasma doping chamber 16, and the amorphous processing and plasma doping processing are performed immediately before the sample is processed. I do.
- the dummy sample is moved from the plasma doping chamber 16 to the second transfer chamber 14b, and the dummy sample is moved to the X-ray analysis chamber 34.
- FIG. 9 is a cross-sectional view showing the configuration of the examination room 34 for performing ellipsometry.
- the dummy sample 21 is placed on the sample stage 35 provided in the examination room 34.
- the light beam 37 irradiated with the light source 36 force hits the amorphous layer which has been made amorphous by the modification process at a depth of about 3 nm to 100 nm on the surface of the dummy sample 21.
- the reflected light becomes elliptically polarized light.
- the tangent obtained from the phase angle ⁇ of the elliptically polarized light and the amplitude intensity ratio of the ellipse is measured, and the film thickness and birefringence of the amorphous layer are measured.
- a detector comprising an analyzer 39 and a detector 40, the depth and surface state of the amorphous layer on the surface of the dummy sample can be known.
- the depth and surface state (optical characteristics) of the amorphous layer can be detected.
- the depth and surface state of the amorphous layer are detected, and the dose is adjusted as necessary.
- the measured dummy sample is moved again to the second transfer chamber 14b, then moved to the unloader chamber 19, and taken out from the apparatus.
- the measured value measured by ellipsometry is a desired value. Therefore, every time 25 samples are processed, the dummy sample is plasma doped, and the plasma-doped dummy sample is irradiated with linear polarization, and the reflected light emitted from the dummy sample is detected and detected. In addition, the conditions under which the sample was processed were controlled so that the depth and surface state of the amorphous layer had predetermined values.
- the power supplied to the sample electrode is reduced under the conditions for processing the next 25 samples. .
- the high frequency power supplied to the plasma source is increased. Or shorten the processing time.
- the power supplied to the sample electrode is increased under the conditions for processing the next 25 samples.
- the high frequency power supplied to the plasma source is reduced. Or increase the processing time.
- control parameters are set under standard amorphization conditions and doping conditions. What is necessary is just to experimentally obtain in advance the force by which the depth and polarization state of the amorphous layer change when it is changed. In order to change each of these control parameters, it is only necessary to construct software that automatically rewrites the processing recipe stored in the control system of the apparatus, as shown in the figure. With such a configuration, a plasma doping method excellent in controllability of the depth of the amorphous layer introduced into the sample surface could be realized.
- Embodiment 4 of the present invention will be described with reference to FIG.
- FIG. 10 is a cross-sectional view of the plasma doping chamber of the plasma doping apparatus used in Embodiment 4 of the present invention.
- a predetermined gas is introduced from the gas supply device 2 into the vacuum vessel 1 and exhausted by the turbo molecular pump 3 as an exhaust device.
- the inside of the vacuum vessel 1 can be kept at a predetermined pressure by the pressure regulating valve 4.
- a silicon substrate 9 as a sample is placed on the sample electrode 6.
- a high-frequency power source 10 for supplying high-frequency power to the sample electrode 6 is provided. This is because the substrate 9 as a sample has a negative potential with respect to the plasma. It functions as a voltage source that controls the potential. In this way, ions in the plasma can be accelerated and collide with the sample surface to amorphize the sample surface or introduce impurities.
- the turbo molecular pump 3 and the exhaust port 11 are arranged immediately below the sample electrode 6, and the pressure regulating valve 4 is a lift valve that is located directly below the sample electrode 6 and directly above the turbo molecular pump 3. .
- the sample electrode 6 is fixed to the vacuum vessel 1 by four columns 12.
- helium is introduced into the vacuum container 1 from the gas supply device 2.
- plasma is generated in the vacuum vessel 1 and 200 W of high-frequency power is supplied to the base 16 of the sample electrode 6 to thereby generate a silicon substrate.
- the crystal layer on the surface of 9 could be made amorphous.
- the plasma is generated in the vacuum vessel 1 by supplying 1000 W of high-frequency power to the coil 8 while maintaining a low temperature, and boron is introduced near the surface of the substrate 9 by supplying 250 W of high-frequency power to the sample electrode 6. We were able to.
- the plasma doping chamber is equipped with a detector comprising an analyzer 39 and a detector 40 for measuring the depth of the amorphous layer by ellipsometry. Since this operation has been described in Embodiment 3 of the present invention, description thereof is omitted here. Also Similarly, a detector consisting of an analyzer 39 and a detector 40 may be provided as a device for measuring X-rays emitted from the sample force in order to calculate the dose (impurity concentration).
- the polarization state force measured in this way The amorphous layer formed on the sample surface is controlled by controlling the conditions for amorphizing the sample so that the calculated depth of the amorphous layer becomes a predetermined value. Therefore, it is possible to realize a pre-amorphization treatment method with excellent controllability of the depth and, as a result, a plasma doping method with good controllability.
- the surface of the sample is amorphized and impurities are introduced by resist, etc., but it is widened so that the depth of the amorphous layer, X dose or X dose power can be measured easily.
- the opening is provided (the opening becomes a dummy sample).
- the power supplied to the sample electrode is reduced under the conditions for processing the next predetermined number of samples. Or, increase the high-frequency power supplied to the plasma source. Alternatively, the processing time is shortened.
- the power supplied to the sample electrode is increased under the conditions for processing the next predetermined number of samples.
- the high frequency power supplied to the plasma source is reduced.
- the processing time is increased.
- these control parameters were changed under standard amorphization conditions and doping conditions.
- the depth force S of the amorphous layer may be determined experimentally to determine how much it changes. In order to change each of these control parameters, it is only necessary to construct software that is stored in the control system of the apparatus and automatically rewrites the processing recipe as shown in the figure.
- the ellipsometry detector, the electron beam source, and the X-ray detector are configured to irradiate light onto the sample placed on the sample electrode in the vacuum vessel, so that the amorphous layer is formed. This eliminates the need for a special processing chamber for measuring the depth of the substrate, and increases productivity.
- the dummy sample is provided in a portion where the sample device is not required. It is the structure which is a part of prepared sample. With such a configuration, when processing an expensive sample such as a 300 mm silicon substrate, it is possible to minimize the cost imposed on the dummy sample. In addition, if a dummy sample is prepared for a part of all the samples, the impurity concentration controllability becomes extremely high. In other words, the processing conditions can be finely adjusted for each sheet.
- V may not be used even if a substrate is used as a dummy sample after forming a resist.
- the coil 8 may be planar, or a helicon wave plasma source, a magnetic neutral loop plasma source, or a magnetic field microwave plasma source (electron cyclotron resonance plasma source) may be used.
- a helicon wave plasma source a magnetic neutral loop plasma source
- a magnetic field microwave plasma source electron cyclotron resonance plasma source
- At least one of neon, argon, krypton, and xenon (zenon), which may be an inert gas other than helium, can be used.
- zenon which may be an inert gas other than helium.
- the present invention is also applied to a case where boron is doped simultaneously with amorphization using gas plasma in which diborane is mixed with helium. This is desirable because it reduces the number of processes from two to one and improves productivity.
- the present invention can be applied when processing samples of various other materials.
- the present invention is a particularly useful plasma doping method when the sample is a semiconductor substrate made of silicon. It is particularly useful when the impurity is arsenic, phosphorus, boron, aluminum or antimony. With such a configuration, an ultrafine silicon semiconductor device can be manufactured.
- the gas phase state may be monitored by performing an emission spectroscopic analysis of the plasma or performing a mass analysis during the doping process, and may be used to determine which parameter should be changed. . For example, if the sheet resistance changes even though there is no particular change in the gas phase, the power supplied to the sample electrode must be changed rather than changing the gas flow rate or the high-frequency power supplied to the plasma source. You can do it. Conversely, if a change in the gas phase is observed, the gas flow rate and the high-frequency power supplied to the plasma source may be changed rather than changing the power supplied to the sample electrode.
- a force exemplifying the case where the amorphization and the doping process are continuously processed in the same plasma processing chamber may be prepared and processed separately.
- the sheet resistance measuring device may be provided in the heating chamber.
- Plasma doping was performed on a 200 mm silicon substrate using helium gas plasma. Plasma doping was performed in the vacuum container 1 of the plasma irradiation chamber 16.
- the high-frequency power supplied to the plasma source was 1500 W
- the pressure in the vacuum vessel 1 was 0.9 Pa
- the processing time for plasma irradiation was 7 seconds.
- the power supplied to the sample electrode was changed in the range of 30W to 300W.
- the bias voltage generated between the plasma and the silicon substrate can be changed.
- the bias voltage increases when the power supplied to the sample electrode is large, and decreases when the power is small.
- the bias voltage was changed from 30V to 200V by changing the power supplied to the sample electrode in the range of 30W to 300W.
- the noise voltage and the depth of the amorphous layer are in a very good proportional relationship. It can be understood that the depth of the amorphous layer can be changed by about 0.1 nm by changing the bias voltage IV.
- the To change the bias voltage IV the power supplied to the sample electrode should be changed by about 1.5W. That is, it can be understood that the depth of the amorphous layer can be controlled with very high accuracy of 0.1 nm by changing the power supplied to the sample electrode.
- FIG. 12 shows the relationship between the relationship between the power supplied to the sample electrode and the depth of the amorphous layer, which has been experimentally determined as described above, and the inspection by ellipsometry. It is a flowchart which shows the method of improving the repeat reproducibility of the depth. If the depth of the amorphous layer is within the predetermined threshold range set by ellipsometry, the power supplied to the sample electrode remains unchanged. If it is deeper than the threshold, set the power supplied to the sample electrode to a smaller value. If it is shallower than the threshold, set the power supplied to the sample electrode to a larger value.
- Step 101 helium gas plasma irradiation is performed (Step 101, the wafer is taken out of the apparatus (Step 102), and the depth of the amorphous layer is measured by inspection by ellipsometry (Step 103). ).
- this measurement step 103 it is determined whether or not the depth of the amorphous layer measured is within a predetermined threshold range set (step 104), and if it is within the predetermined threshold range, it is supplied to the sample electrode. The power is left as is (step 105).
- step 106 If it is determined that it is not within the predetermined threshold range, it is determined whether or not it is larger than the threshold value (step 106). If it is determined in this determination step that the value is larger than the threshold value, the power supplied to the sample electrode is reset to a smaller value (step 107). On the other hand, if it is determined in the determination step 206 that the power is smaller than the threshold value, the power supplied to the sample electrode is set to a larger value (step 108).
- Fig. 13 shows the result of repeating the formation of an amorphous layer by plasma doping, the inspection by ellipsometry, and the feedback of the inspection result.
- 100 silicon substrates were plasma-doping processed, and one ellipsometry inspection and feedback of inspection results were performed for each plasma doping process.
- the bias voltage was changed twice, that is, the power supplied to the sample electrode. At one time, since the depth of the amorphous layer was deeper than the threshold, the bias voltage was reduced by 2V.
- the power supplied to the sample electrode was reduced by 3W.
- the amorphous layer Since the depth was shallower than the threshold, the bias voltage was increased by 2V. In other words, the power supplied to the sample electrode was increased by 3W.
- the average value was 9.6 nm, and the difference between the maximum value and the minimum value was 0.6 nm or less. The variation was less than 1% at 1 ⁇ . This is a very high reproducibility, indicating the effectiveness of the present invention.
- the method of feeding back the inspection result to the processing conditions is a force widely used in other general techniques.
- the power supplied to the sample electrode and the depth of the amorphous layer are very different. There is a strong proportional relationship, and even if the power supplied to the sample electrode is changed to 1.5 W, which is a sufficiently large value that can be practically used, the depth of the amorphous layer is as small as 0.1 nm.
- the main feature is that it is used in combination with variable control with accuracy.
- Embodiment 6 of the present invention will be described with reference to FIG. 14, FIG. 15, FIG. 16, FIG.
- the movement of the dummy sample is the same as in the first embodiment.
- Plasma driving was performed on a 200 mm silicon substrate using a mixed gas plasma of diborane and helium.
- the mixing ratio was such that the diborane gas concentration was 0.025% and the helium gas concentration was 99.975%.
- Plasma doping was performed in the vacuum container 1 of the plasma irradiation chamber 16.
- the high frequency power supplied to the plasma source was 1500 W, the pressure in the vacuum vessel 1 was 0.9 Pa, and the treatment time for plasma irradiation was 30 seconds.
- the power supplied to the sample electrode was changed in the range of 0W to 200W. Under this condition, it is possible to simultaneously implant boron into the silicon substrate by plasma doping and amorphize the silicon crystal on the silicon substrate surface. Even if the power supplied to the sample electrode is zero, ions in the plasma collide with and are driven into the silicon substrate by a potential difference that can be naturally generated between the silicon substrate and the plasma.
- the power supplied to the sample electrode was changed, and the dummy sample was subjected to plasma doping treatment, then moved to the inspection room 17 and the depth of the amorphous layer was measured by using an erythrometry. Thereafter, the boron depth profile in the silicon substrate was measured with a SIMS measurement device (not shown).
- the boron implantation depth was set to a depth at which the boron concentration was IX 10 18 cm 3 in the profile measured by SIMS. This is a method for determining the implantation depth of boron, which is generally widely used in the field of shallow junction formation in semiconductor processes.
- the boron implantation depth has a one-to-one correspondence with the power supplied to the sample electrode, and can be controlled by changing the power supplied to the sample electrode.
- the relationship between the power supplied to the sample electrode and the depth of the amorphous layer is shown in Fig. 15. The depth of the amorphous layer can also be controlled by changing the power supplied to the sample electrode.
- FIG. Figure 16 shows that the boron implantation depth can be determined by measuring the depth of the amorphous layer.
- the boron implantation depth must be measured using SIMS.
- SIMS takes several hours for a single measurement and is a destructive inspection.
- the inspection takes a long time, and many products are plasma-doping during the inspection. Since the depth of boron implantation in the product is insignificant until the inspection is completed, it is necessary to be able to inspect it in a shorter time.
- the boron implantation depth can be determined by measuring the depth of the amorphous layer, so that it can be detected by optical measurement using ellipsometry, which is not possible with SIMS. it can.
- Figure 17 shows a flowchart of how this approach is used to improve the repeatability of boron implantation depth.
- Step 201 helium gas plasma irradiation is performed (Step 201, the wafer is taken out of the apparatus (Step 202), and an amorphous state is obtained by inspection by ellipsometry. Measure layer depth (step 203).
- this measurement step 203 it is determined whether or not the depth of the amorphous layer measured is within a predetermined threshold range set (step 204), and if it is within the predetermined threshold range, it is supplied to the sample electrode. The power is left as is (step 205).
- step 206 If it is determined that it is not within the range of the predetermined threshold value, it is determined whether or not it is larger than the threshold value (step 206). If it is determined in this determination step that the value is larger than the threshold value, the power supplied to the sample electrode is set to a smaller value (step 207). On the other hand, if it is determined in the determination step 206 that the power is smaller than the threshold value, the power supplied to the sample electrode is set to a larger value (step 208).
- Fig. 18 shows the results of repeating the formation of an amorphous layer by plasma doping, the inspection by ellipsometry, and the feedback of the inspection results.
- 100 silicon substrates were plasma-doping processed, and one ellipsometry inspection and feedback of inspection results were performed for each plasma doping process.
- the bias voltage was changed twice, that is, the power supplied to the sample electrode was changed.
- the noise voltage was reduced by 2V. That is, the power supplied to the sample electrode was reduced by 3 W.
- the bias voltage was increased by 2V because the depth of the amorphous layer was shallower than the threshold.
- the power supplied to the sample electrode was increased by 3W.
- the average value of the boron implantation depth when the amorphous layer formation and boron implantation were simultaneously performed by repeating 100 sheets was 9.6 nm, and the difference between the maximum value and the minimum value was 0.6 nm or less. It was. The variation corresponds to 1% or less at 1 ⁇ . This is very high reproducibility and shows the effectiveness of the present invention.
- the method of feeding back the inspection result to the processing condition is a force widely used in other general techniques.
- the formation of an amorphous layer newly developed by the present inventors is used.
- plasma doping in which boron can be implanted at the same time, it has been found that there is a one-to-one relationship between the depth of the amorphous layer and the depth of boron implantation.
- this new discovery and the ability to control the depth of the amorphous layer and the depth of boron implantation with the power supplied to the sample electrode, such as ellipsometry It is characterized by a combination of the ability to measure the depth of an amorphous layer in a short time by optical measurement.
- the plasma doping method and apparatus of the present invention can provide a plasma doping method and apparatus excellent in controllability of the depth of implantation of impurities introduced into the sample surface or the depth of the amorphous layer. In addition to this impurity doping process, it can also be applied to the manufacture of thin film transistors used in liquid crystals and the like, and surface modification of various materials.
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US11/887,359 US20090035878A1 (en) | 2005-03-31 | 2006-03-30 | Plasma Doping Method and Apparatus |
JP2007512882A JPWO2006106858A1 (ja) | 2005-03-31 | 2006-03-30 | プラズマドーピング方法及び装置 |
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JP2008300687A (ja) * | 2007-05-31 | 2008-12-11 | Tokyo Electron Ltd | プラズマドーピング方法及びその装置 |
JP2014053452A (ja) * | 2012-09-07 | 2014-03-20 | Toshiba Corp | 半導体装置の製造方法 |
JP2019009368A (ja) * | 2017-06-28 | 2019-01-17 | 株式会社Screenホールディングス | 熱処理装置および熱処理方法 |
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EP1667212A4 (en) * | 2003-09-24 | 2009-03-04 | Panasonic Corp | IMPURITY INTRODUCTION METHOD, IMPRESS ENTRY APPARATUS, AND ELECTRONIC DEVICE PRODUCED THEREBY |
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JP5116463B2 (ja) * | 2005-02-23 | 2013-01-09 | パナソニック株式会社 | プラズマドーピング方法及び装置 |
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JP5237820B2 (ja) * | 2006-11-15 | 2013-07-17 | パナソニック株式会社 | プラズマドーピング方法 |
JP5237833B2 (ja) * | 2007-01-22 | 2013-07-17 | パナソニック株式会社 | 半導体装置の製造方法及び半導体製造装置 |
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US8030187B2 (en) * | 2007-12-28 | 2011-10-04 | Panasonic Corporation | Method for manufacturing semiconductor device |
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2006
- 2006-03-30 US US11/887,359 patent/US20090035878A1/en not_active Abandoned
- 2006-03-30 JP JP2007512882A patent/JPWO2006106858A1/ja not_active Withdrawn
- 2006-03-30 EP EP06730669A patent/EP1865544A4/en not_active Withdrawn
- 2006-03-30 CN CNA2006800103675A patent/CN101151711A/zh active Pending
- 2006-03-30 KR KR1020077019447A patent/KR20070115907A/ko not_active Application Discontinuation
- 2006-03-30 WO PCT/JP2006/306721 patent/WO2006106858A1/ja active Application Filing
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Cited By (3)
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JP2008300687A (ja) * | 2007-05-31 | 2008-12-11 | Tokyo Electron Ltd | プラズマドーピング方法及びその装置 |
JP2014053452A (ja) * | 2012-09-07 | 2014-03-20 | Toshiba Corp | 半導体装置の製造方法 |
JP2019009368A (ja) * | 2017-06-28 | 2019-01-17 | 株式会社Screenホールディングス | 熱処理装置および熱処理方法 |
Also Published As
Publication number | Publication date |
---|---|
KR20070115907A (ko) | 2007-12-06 |
EP1865544A4 (en) | 2010-12-22 |
CN101151711A (zh) | 2008-03-26 |
US20090035878A1 (en) | 2009-02-05 |
EP1865544A1 (en) | 2007-12-12 |
JPWO2006106858A1 (ja) | 2008-09-11 |
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