United States Patent [19]
`Narita et al.
`
`[11] Patent Number:
`[45] Date of Patent:
`
`4,913,790
`Apr. 3, 1990
`
`[54] TREATING METHOD
`
`[73] Assignee:
`
`_
`_
`_
`_
`[751 Inventors= Tomonol'i Narlta, Tokyo; Klmlhll'?
`Matsuse, Yokohama, both of Japan
`Tokyo Electron Limited, Tokyo,
`Japan
`[21] Appl. No.: 326,689
`[22] Filed:
`Mar. 21, 1989
`[30]
`Foreign Application Priority Data
`Mar. 25, 1988 [JP]
`....... .. 63-72995
`
`Japan ................... ..
`
`[51] Int. Cl.4 .................... .. C23C 145/34; C23C 16/00;
`C03C 15/00
`[52] US. Cl. ........................ .. 204/ 192.13; 204/ 192.33;
`204/298.03; 204/298.09; 204/298.32; 156/626;
`‘
`_
`156/643; 427/8; 427/248.1
`[58] Field of Search ..................... .. 156/ 626, 643, 646;
`427/8, 248.1; 118/666, 712, 725; 204/298 MT,
`298 CS, 298 ET, 192.13, 192.12, 192.32, 192.33
`References Cited
`U.S. PATENT DOCUMENTS
`
`[56]
`
`204/298 MT
`3,573,190 3/1971 Bloom ......... ..
`204/298 MT
`4,172,020 10/1979 Tisone et al. .
`4,324,631 4/ 1982 Meckel et al. ............. .. 204/298 MT
`4,396,478 8/1983 Aizenshtein et al.
`204/298 ET
`
`4,407,708 10/1983 Landau ...................... .. 204/298 MT
`4,565,601 l/1986 Kakehietal. ..
`204/298 ET
`4,648,952 3/1987 Savov et a1.
`204/298 MT
`4,687,544 8/1987 Bersin ......................
`204/298 ET
`
`FOREIGN PATENT DOCUMENTS
`60-022635 2/1985 Japan.
`63-65901 3/1988 Japan.
`Primary Examiner--Nam X. Nguyen
`Attorney, Agent, or Firm-Oblon, Spivak, McClelland,
`Maier & Neustadt
`ABS I RACI‘
`1571
`A workpiece treating method includes a temperature
`rise step in which ?rst temperature control is performed
`and a treatment step in which second temperature con
`trol is performed and is adapted to treat a workpiece
`whose emissivity of infrared rays in the temperature rise
`step is different from that in the treatment step. In the
`temperature rise step, the temperature of the workpiece
`is detected by a non-contact type temperature detecting
`means so as to perform the ?rst temperature control. In
`the treatment step, the temperature of the workpiece is
`detected by a contact type temperature detecting means
`so asito perform the second temperature control.
`
`7 Claims, 4 Drawing Sheets
`
`10
`VACUUM
`PUMP
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`LAM Exh 1004-pg 1
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`U.Sf Patent Apr; 3, 1990
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`Shegt 0f4
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`4,913,790 '
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`Patgnt Apr. 3, 1990
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`Sheet 2 of 4
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`4,913,790
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`Apr. 3, 1990
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`U.S. Patent’
`
`Apr. 3, 1990
`
`Sheet 4 of 4
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`4,913,790
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`VACUUM
`PUMP
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`

`
`1
`
`TREATING METHOD
`
`4,913,790
`
`10
`
`BACKGROUND OF THE INVENTION
`1. Field of the Invention
`The present invention relates to a treating method of
`a workpiece and, more particularly, to temperature
`control in deposition of a metal on a surface of a semi
`conductor substrate.
`2. Description of the Related Art
`In a conventional manufacturing process of semicon
`ductor integrated circuits, physical vapor deposition
`(PVD), such as evaporation and sputtering deposition,
`is used as a technique for depositing a metal on a surface
`of a substrate. However, with advances in integration,
`speed, and density of an integrated circuit as in an ultra
`large scaled integrated circuit (ultra LSI), a great deal
`of attention has been paid to a technique for depositing
`a refractory metal, e.g., W (tungsten), having a resis
`tance which is 1/10 or less that of polycrystalline sili
`con, in order to form a gate electrode and perform
`selective deposition of a metal in contact holes and
`through holes.
`For such a purpose, chemical vapor deposition,
`which is excellent in deposition selectivity, is widely
`utilized. When a W thin ?lm is to be selectively depos
`ited on a substrate, e. g., a substrate having an aluminum
`film formed on its surface, by chemical vapor deposi
`tion, the substrate must be quickly heated, and its tem
`perature must be controlled to a desired temperature
`afterward in order to improve deposition selectivity. In
`this case, the temperature of the substrate must be accu
`rately detected for its temperature control. The follow
`ing two methods are available for detection of the tem
`perature: a method of detecting the temperature of a
`substrate by bringing a thermocouple as a contact type
`temperature detecting device into ' contact with the
`substrate; and a method of detecting the temperature of
`a substrate by.detecting the radiation energy of infrared
`rays from the substrate using a pyrometer as a non-con
`tact type temperature detecting device.
`If, however, a thermocouple is used for temperature
`detection in order to perform such temperature control
`of a substrate, high reliability can be expected with
`respect to stable temperatures, but reliability is de
`creased with respect to quickly rising temperatures"
`because it takes a considerably long period of time to
`increase the temperature of the thermocouple itself.
`Therefore, when the substrate is quickly heated, the
`thermocouple cannot follow the temperature rise. As a
`result, the difference between a temperature detected
`by the thermocouple and an actual temperature be
`comes large, and a set value to be kept constant after
`quick rise is greatly overshot. If such overshoot occurs,
`‘when a surface of the substrate consists of aluminum,
`the surface is melted. Hence, a CVD process cannot be
`performed. In addition, if CVD is to be applied onto a
`diffusion region of a silicon substrate, the reaction ad
`vances into the substrate, i.e., a phenomenon called '
`“encroachment” occurs.
`60
`In contrast to this, if a pyrometer is used for tempera
`ture control of a substrate, the pyrometer can properly
`respond to quick heating because it has good response
`characteristics. However, when deposition of a metal
`on a surface of the substrate is started, since the emissiv
`ity of infrared rays radiated from the surface of the
`substrate prior to deposition is different from that of a
`deposited ?lm material, emissivity of infrared rays radi
`
`65
`
`40
`
`2
`ated from the surface of the substrate is changed as
`deposition progresses. The pyrometer cannot follow
`this change. Therefore, temperature detection cannot
`be properly performed.
`
`SUMMARY OF THE INVENTION
`It is an object of the present invention to provide a
`workpiece treating method accompanied with heating,
`which can treat a surface of a workpiece while accu
`rately controlling the temperature of the workpiece.
`According to the present invention, there is provided
`a workpiece treating method comprising a temperature
`rise step in which ?rst temperature control is performed
`and a treatment step in which second temperature con
`trol is performed and adapted to treat a workpiece
`whose emissivity of infrared rays in the temperature rise
`step is different from that in the treatment step, wherein
`a temperature of a workpiece is detected by non-contact
`type temperature detecting means in the temperature
`rise step so as to perform the ?rst temperature control,
`and the temperature of the workpiece is detected by
`contact type temperature detecting means in the treat
`ment step so as to perform the second temperature con
`trol.
`
`BRIEF DESCRIPTION OF THE DRAWINGS
`FIG. 1 shows a CVD apparatus used for a CVD
`process according to an embodiment of the present
`invention;
`FIG. 2 is a graph showing temperatures detected by
`a thermocouple and a pyrometer when temperature
`control of a wafer is performed by using only the ther
`mocouple in a process using the apparatus shown in
`FIG. 1;
`-
`’
`FIG. 3 is a block diagram showing an arrangement
`for temperature control of a wafer; and
`FIG. 4 shows‘a CVD apparatus wherein the position
`of the pyrometer is changed from that shown in FIG. 1.
`
`DETAILED DESCRIPTION OF THE
`PREFERRED EMBODIMENTS
`According to a method of present invention, a work
`piece is heated from a room temperature to a predeter
`mined treatment temperature, and the workpiece is then
`treated at this treatment temperature. In either of these
`heating and treating steps, the temperature of the work
`piece is accurately controlled. In this case, the emissiv
`ity of infrared ray of the workpiece in the temperature
`rise step is different from that in the treating step. In
`accordance with this difference, the temperature of the
`workpiece in the temperature rise step is detected by a
`non-contact type temperature detecting means, whereas
`the temperature of the workpiece in the treating step is
`detected by a contact type temperature detecting
`means.
`In the present invention, the temperature rise speed in
`the temperature rise step is preferably set to be 5° C./ sec
`or more.'At such a temperature rise speed, temperature
`detection cannot be properly performed by a contact
`type temperature detecting means. Therefore, the pres
`ent invention can be effectively applied to such a case.
`Heating of the workpiece can be performed by utiliz
`ing radiation of an infrared ray lamp, halogen lamp or a
`normal heater.
`A pyrometer and a thermocouple can be respectively
`used as non-contact and contact type temperature de
`tecting means used in the method of the present inven
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`4,913,790
`3
`tion. However, the present invention is not limited to
`them.
`The present invention can be applied to various treat
`ing methods, namely, evaporation, sputtering, thermal
`CVD, plasma etching, ozone ashing, and plasma ashing.
`Especially, the present invention can be suitably applied
`to a treatment which is not accompanied with genera
`tion of a plasma. Note that since a voltage is applied to
`a workpiece to be treated in plasma CVD and reactive
`ion etching, a thermocouple is dif?cult to use, and
`hence application of the present invention is difficult in
`these cases.
`An embodiment wherein the method of the present
`invention is applied to formation of a thin ?lm consist
`ing of a refractory metal by a single wafer treatment in
`a thin ?lm forming step by chemical vapor deposition in
`a semiconductor manufacturing process will be de
`scribed below with reference to the accompanying
`drawings.
`A mount base 3 is arranged at an upper portion of a
`hermetic, cylindrical Al (aluminum) reaction chamber 1
`on which a jacket is arranged so as to cool its wall
`surfaces with cooling water or the like. A substrate to
`be treated, e.g., a semiconductor wafer 2, can be
`mounted on the mount base 3 vsuch that a surface to be
`treated faces down. A support member 5 having a lift
`ing mechanism 4 such as an air cylinder is arranged near
`the mount base 3. The support member 5 supports, e. g.,
`the periphery of the semiconductor wafer 2 and ?xes it
`to the mount base 3. A groove is formed at a predeter
`mined position of the support member 5, and a contact
`type temperature detecting mechanism, e.g., a thermo
`couple 6 is arranged therein. More speci?cally, when
`the semiconductor wafer 2 is supported by the support
`member 5 on the mount base 3, the thermocouple 6
`arranged on the support member 5 is brought into
`contact with the wafer 2. The thermocouple 6 is prefer
`ably constituted by an alumel-chromel thermocouple of
`the K type which can properly respond to temperatures
`from a room temperature to 600° C. An IR lamp (infra
`red ray lamp) or halogen lamp 8 is arranged above the
`mount base 3. The lamp 8 can heat the mount base 3 up
`to, e.g., 300° C. to 1,00Q" C. through a quartz glass
`window 7. Two exhaust ports 9 are formed in the upper
`wall of the reaction chamber 1 near the mount base 3. A
`45
`vacuum pump 10, e. g., a turbo molecular pump, capable
`of evacuating the reaction chamber 1 to a desired pres
`sure and exhausting a reactive gas and the like is con
`nected to the exhaust ports 9.
`An annular oxidation gas inlet port 11 having a large
`number of small holes is formed at a lower portion of
`the reaction chamber 1 so as to supply a ?lm forming
`gas, e.g., WF6 (tungsten hexa?uoride), as an oxidation
`gas. Similarly, an annular reduction or carrier gas inlet
`port 12 having a large number of small holes is arranged
`to supply H2 (hydrogen) as a reduction gas or Ar (ar
`gon) as a carrier gas. These gas inlet ports 11 and 12 are
`connected to gas supply sources through a ?ow rate
`control mechanism 13, e.g., a mass flow controller. In
`addition, a disk-like ?ow control plate 14 comprising a
`moving mechanism (not shown) utilizing linear move
`ment by, e.g., a stepping motor is arranged between the
`mount base 3 and the gas inlet ports 11 and 12 so as to
`control gas flows.
`A cylindrical space 15 having a diameter of 5 cm
`65
`axially extends from the center of the disk-like flow
`control plate 14 toward the center of the semiconductor
`wafer 2 mounted on the mount base 3. The bottom
`
`35
`
`4
`portion of the space 15 is connected through a lens 17 to
`a non-contact type temperature detecting mechanism,
`e.g., a pyrometer 16 capable of detecting a temperature
`from radiation energy of infrared rays. The pyrometer
`16 is arranged outside the bottom of the reaction cham~
`ber 1. More speci?cally, the pyrometer 16 is located to
`oppose the semiconductor wafer 2 mounted on the
`mount base 3 through the lens 17 and the space 15, and
`is designed to detect a temperature by detecting radia
`tion energy of infrared rays of a portion of the wafer 2,
`e.g., a circular portion having a diameter of 2 to 3 cm
`and the center coinciding with substantially the center
`of the wafer 2.
`A hermetic transfer preliminary chamber 22 is ar
`ranged on one side of the reaction chamber 1 through a
`gate valve 18 which can be opened/closed upon verti
`cal movement. By opening/closing the gate valve 18,
`the semiconductor wafer 2 can be transferred in and out
`of the reaction chamber 1. The chamber 22 houses a
`hand arm 19, designed to freely expand/contract and
`rotate, for holding/transferring the wafer 2, and a base
`21 which can be vertically moved while a cassette 20
`storing, e.g., about 25 wafers 2, is mounted on the base
`
`A control section 23 performs temperature control
`based on detection results obtained by the above
`described thermocouple and pyrometer respectively
`serving as temperature detecting mechanisms, and also
`performs operation and setting control of the ?lm form
`ing apparatus.
`A method of selectively forming ?lms on the semi
`conductor wafer 2 by using the above-described ?lm
`forming apparatus will be described below.
`The cassette 20 in which, e.g., about 25 semiconduc
`tor wafers 2 to be treated are stacked/stored at prede
`termined intervals is mounted on the base 21, which can
`be vertically moved, through an opening/closing port
`(not shown) of the preliminary chamber 22 by a robot
`hand or a manual operation. At this time, the gate valve
`18 is closed, and the reaction chamber 1 has already
`been evacuated by the vacuum pump 10 to a desired
`pressure. After the cassette 20 is set in this manner, the
`opening/closing port (not shown) of the chamber 22 is
`airtightly closed, and the chamber 22 is then evacuated
`by a vacuum pump (not shown) to a pressure equivalent
`to that of the reaction chamber 1.
`The gate valve 18 is then opened, and the height of
`the base 21 is adjusted while the desired pressure is
`maintained. Upon this operation, a desired one of the
`wafers 2 is picked up from the cassette 20 and is trans
`ferred into the reaction chamber 1 by using the hand
`arm 19 which can freely expand/contact. At this time,
`the support member 5 is lowered by the lifting mecha
`nism 4, and the wafer 2 is mounted on the support mem
`ber 5 while its surface to be treated faces down. Subse
`quently, the support member 5 is raised by the lifting
`mechanism 4, so that the wafer 2 is placed to be
`clamped between the mount base 3 and the support
`member 5 and be brought into contact with the thermo
`couple 6. The mount base 3 has already been heated by
`the lamp 8 by this time. In this case, if the contact sur
`face of the support member 5 with the wafer 2 is consti»
`tuted by a ceramic material or the like having a low heat
`conductivity, the temperature distribution of the wafer
`2 becomes uniform. Hence, variations in treatment can
`be prevented. When mounting of the semiconductor
`wafer 2 on the mount base 3 is completed, the hand arm
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`4,913,790
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`6
`19 is returned into the preliminary chamber 22, and the
`are supplied in step 7. Upon supply of the WF6 and H2
`gate valve 18 is closed.
`gases, the reaction progresses in accordance with the
`A treatment of depositing a W ?lm on the surface to
`following reaction formula, and hence chemical vapor
`be treated of the semiconductor wafer 2, e.g., on an
`deposition is performed on the surface of the semicon
`aluminum layer occupying several to several tens per
`ductor wafer 2.
`cent of the upper surface area is started. During the
`process, evacuation control of the reaction chamber 1 is
`always performed by the vacuum pump 10 so as to keep
`the chamber 1 at a desired reduced pressure, e.g., 100 to
`200 mm Torr.
`The surface to be treated of the semiconductor wafer
`2 is quickly heated by the lamp 8 to a desired tempera
`ture range, e.g., about 370° C. At this time, the tempera
`ture of the wafer 2 is detected in a non-contact manner
`by detecting radiation energy of infrared rays radiated
`from the wafer 2 using the pyrometer 16, thus control
`ling an output to the lamp 8 by the control section 23.
`When the temperature of the wafer 2 is stabilized at the
`desired temperature, e.g., 370° C. after this quick heat
`ing, and a temperature detected by the thermocouple 6
`arranged in contact with the wafer 2 is stabilized, a
`temperature detecting operation of the wafer 2 is manu
`ally or automatically switched from the pyrometer 16 to
`the thermocouple 6. As a result, temperature adjust
`ment is performed by the control section 23 on the basis
`of temperatures detected by the thermocouple 6.
`Temperature control of the semiconductor wafer 2
`by the control section 23 is performed in accordance
`with, e.g., the block diagram shown in FIG. 3.
`When heating of the wafer 2 is started by the lamp 8,
`its temperature is detected by the pyrometer 16. Heat
`ing is performed in accordance with a predetermined
`temperature rise speed. The detection value obtained by
`the pyrometer 16 is compared with a reference value by
`a comparator. In this case, the detection value is com
`pared with a value corresponding to 370° C., and the
`resultant output signal is supplied to the lamp 8 through
`a lamp current controller. The temperature of the wafer
`2 is maintained at 370° C. in this manner. Thereafter, a
`temperature detecting operation is switched to the ther
`mocouple 6, and temperature control is performed in
`the same manner as described above.
`Subsequently, a ?lm forming gas such as WF6, a
`reducing gas such as H2, and a carrier gas such as Ar are
`fed through the gas inlet ports 11 and 12 at a predeter
`mined ?ow rate by using the flow rate control mecha
`nism 13, thereby performing chemical vapor deposition.
`If the gas flow rates and the temperature of the semicon
`ductor wafer 2 as a substrate to be treated are controlled
`as in the following table, a W ?lm can be selectively
`deposited on a surface to be treated, e.g., an aluminum
`layer.
`
`35
`
`TABLE
`Ar flow H1 flow WF6 ?ow
`Substrate
`rate
`rate
`rate
`temperature Time
`(°C.)
`(sec) (00/ min) (cc/min)
`(cc/min)
`0
`60
`70
`500
`0
`370
`60
`70
`500
`0
`370
`30
`70
`500
`0
`370
`30
`70
`500
`0
`370
`30
`70
`500
`0
`370
`30
`10
`500
`0
`370
`120
`10
`500
`3
`0
`60
`100
`0
`0
`
`55
`
`STEP 1
`STEP 2
`STEP 3
`STEP 4
`STEP 5
`STEP 6
`STEP 7
`STEP 8
`
`Steps 1 to 8 in the above table will be described be
`low. In step 1, supply of an Ar gas is started. In step 2,
`heating is started. After the substrate temperature be
`comes constant through steps 3 to 6, WF6 and H2 gases
`
`65
`
`5
`
`10
`
`20
`
`25
`
`The treatment by the reaction between WF6 and H2
`based on the above formula is executed. In this case, a
`switching operation of a temperature detecting means
`of the semiconductor wafer 2 from the pyrometer 16 to
`the thermocouple 6 in each step may be performed prior
`to the chemical vapor deposition in step 7. However,
`the switching operation may be performed in step 6, or
`may be performed at the time when the temperature
`detected by the thermocouple 6 is stabilized.
`FIG. 2 shows changes in temperature when the treat
`ment shown in the above table is performed by tempera
`ture control using only the thermocouple 6. In FIG. 2,
`time is plotted along the axis of abscissa, and tempera
`tures are plotted along the axis of ordinate. In this
`graph, a solid curve represents the temperatures de
`tected by the thermocouple 6; and a dotted curve, the
`temperatures detected by the pyrometer 16. As is appar
`ent from this graph, when the wafer 2 is quickly heated
`by the lamp 8, the thermocouple 6 having a slow re
`sponse speed indicates near 370° C., but the pyrometer
`16 having a high response speed indicates 600° C. or
`more. Thus, the actual temperature considerably over
`shoots the set temperature. In contrast to this, during
`the chemical vapor deposition in step 7, in spite of the
`fact that the thermocouple 6 exhibiting high reliability
`when a temperature is stabilized indicates near 370° C.,
`the temperatures detected by the pyrometer 16 vary
`because the emissivity of the surface to be treated is
`different from that of the deposited substance and the
`pyrometer cannot follow changes in emissivity.
`As is apparent from the above description, it is advan
`tageous that temperature control is executed on the
`basis of results obtained by detecting temperatures using
`the pyrometer 16 during a time period of quick heating
`to which the thermocouple 6 cannot respond, and tem
`perature control is executed on the basis of results ob
`tained by detecting temperatures using the thermo
`couple 6 during a time period in which a treatment
`accompanied with changes in emissivity to which the
`pyrometer 16 cannot respond is performed.
`Note that unnecessary ?lms such as natural oxide
`?lms formed on the surface of the semiconductor wafer
`2 are removed by plasma etching in the chamber 1 prior
`to execution of the above-described treatment.
`The flow of a reactive gas can be controlled so as to
`bring the reactive gas into contact with the surface to be
`treated of the set semiconductor wafer 2 more uni
`formly by adjusting the position of the disk-like flow
`control plate 14 arranged between the mount base 3 and
`the gas inlet ports 11 and 12 by using the moving mech
`anism.
`When the formation of the desired ?lm is completed,
`supply of the reactive gas is stopped, and the support
`member 5 is lowered by the lifting mechanism 4 with
`the wafer 2 supported by the support member 5. The
`gate valve 18 is then opened. The wafer 2 is transferred '
`out of the reaction chamber 1 by using the hand arm 19
`which can freely expand/ contract and rotate. At the
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`4,913,790
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`same time, the gate valve 18 is closed, and hence the
`treatment is completed.
`In the above-described embodiment, the W ?lm is
`deposited on a surface to be treated by H2 reduction
`using WF6 as a ?lm forming gas. However, a W ?lm
`may be deposited on the surface by using an SiH4 gas as
`a reducing gas and reducing WF6 in accordance with
`the following formula.
`
`15
`
`20
`
`The treatment of the present invention is not limited to
`a chemical vapor deposition treatment. Any treatment
`can be employed as long as it is accompanied with
`changes in emissivity of infrared rays of a surface to be
`treated after a substrate to be treated is quickly heated.
`For example, the present invention can be properly
`applied to an etching treatment. In addition, a device
`for quickly heating a substrate to be treated is not lim
`ited to an IR lamp or halogen lamp. For example, an
`electric heater may be employed. Furthermore, temper
`ature detecting mechanisms are not limited to a thermo
`couple and a pyrometer.
`Moreover, in the above embodiment, a single wafer
`treatment is performed. However, the present invention
`is not limited to this, but can be applied to a batch treat
`ment in which a large number of semiconductor wafers
`are simultaneously treated. In this case, it is difficult to
`detect the temperatures of all the wafers.
`However, temperature detection of wafers on both
`the sides and the center, i.e., three wafers in total, will
`be suf?cient.
`As has been described above, according to the pres
`ent invention, either in a temperature rise step accompa
`nied by quick heating or in a constant temperature step
`accompanied by changes in emissivity, the temperature
`of an objected to be treated can be accurately detected,
`
`8
`and hence a treatment can be performed while tempera
`ture control is performed with high precision.
`What is claimed is:
`1. A workpiece treating method comprising a temper
`ature rise step in which ?rst temperature control is
`performed and a treatment step in which second tem
`perature control is performed and adapted to treat a
`workpiece whose emissivity of infrared rays in the tem
`perature rise step is different from that in the treatment
`step, wherein a temperature of the workpiece is de
`tected by non-contact type temperature detecting
`means in the temperature rise step so as to perform the
`?rst temperature control, and the temperature of the
`workpiece is detected by contact type temperature
`detecting means in the treatment step so as to perform
`the second temperature control.
`2. A method according to claim 1, wherein said
`workpiece is a semiconductor substrate.
`3. A method according to claim 1, wherein a temper
`ature rise speed in the temperature rise step is not less
`than 5° C./sec.
`.
`4. A method according to claim 1, wherein the work
`piece is heated by radiation of an infrared ray lamp,
`halogen lamp or an electric heater.
`5. A method according to claim 1, wherein said non
`contact type temperature detecting means comprises a
`pyrometer.
`6. A method according to claim 1, wherein said
`contact type temperature detecting means comprises a
`thermocouple.
`7. A method according to claim 1, wherein said
`method comprises a method selected from the group
`consisting of evaporation, sputtering, thermal CVD,
`plasma etching, sputter etching, ozone ashing, and
`plasma ashing.
`
`*
`
`1!
`
`1k
`
`* *
`
`25
`
`30
`
`35
`
`45
`
`55
`
`60
`
`65
`
`LAM Exh 1004-pg 9