CN114507900B - Reaction cavity inner surface protection device, epitaxial reaction monitoring device and method - Google Patents

Reaction cavity inner surface protection device, epitaxial reaction monitoring device and method Download PDF

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CN114507900B
CN114507900B CN202210205878.3A CN202210205878A CN114507900B CN 114507900 B CN114507900 B CN 114507900B CN 202210205878 A CN202210205878 A CN 202210205878A CN 114507900 B CN114507900 B CN 114507900B
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graphite paper
pivot
reaction
reaction chamber
epitaxial
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CN114507900A (en
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刘欣然
黄吉裕
王慧勇
刘自然
王鑫
徐俊
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/08—Reaction chambers; Selection of materials therefor
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/16—Controlling or regulating
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/36—Carbides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
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Abstract

The application relates to the field of semiconductor manufacturing, in particular to a reaction cavity inner surface protection device, an epitaxial reaction monitoring device and a method, which are used for protecting the inner surface of a reaction cavity of epitaxial equipment, wherein the reaction cavity inner surface protection device comprises: graphite paper, first pivot and second pivot, first pivot with the second pivot is installed respectively the inlet end of reaction chamber with give vent to anger the end, the graphite paper both ends cup joint respectively first pivot with in the second pivot, the graphite paper is in the interior top of reaction chamber has the horizontal segment, and can first pivot and the rotation of second pivot is in down the horizontal transport of single direction is followed at the interior top of reaction chamber, through setting up protection device at the reaction intracavity surface, and the crystallization on the graphite paper is taken away in the continuous work of graphite paper, prevents that the crystallization from dropping on the substrate, and need not to frequently wash reaction intracavity surface.

Description

Reaction cavity inner surface protection device, epitaxial reaction monitoring device and method
Technical Field
The application relates to the field of semiconductor manufacturing, in particular to a reaction cavity inner surface protection device, an epitaxial reaction monitoring device and a method.
Background
In the epitaxial process, because the SiC is grown in a continuous multi-piece manner, in the epitaxial reaction process, reaction gas is continuously introduced into a reaction chamber of the epitaxial equipment, in the reaction process under the reaction condition of 1700 ℃, because the reaction gas may form Si drops on the inner surface in the reaction chamber or form SiC particles on the surface, crystals fall on the substrate, defects are generated on the surface of the substrate, and the yield of the substrate is greatly affected, so that the inner surface of the reaction chamber needs to be protected to prevent the crystals from falling on the substrate.
The existing method for protecting the inner surface of the reaction cavity mainly comprises the step of plating a TaC protective layer on the inner surface of the reaction cavity, so that reaction gas is prevented from crystallizing on the inner surface of the reaction cavity and falling on a substrate, and in the long-time reaction process, the inner surface of the reaction cavity still reacts to generate crystals and falls on the substrate, and the inner surface of the reaction cavity needs to be frequently cleaned.
In view of the above problems, no effective technical solution exists at present.
Disclosure of Invention
The application aims to provide a reaction cavity inner surface protection device, an epitaxial reaction monitoring device and a method, and aims to solve the problem that in an epitaxial process, reaction gas introduced into a reaction cavity can generate crystals on the inner surface of the reaction cavity and fall on a substrate, so that the yield of the substrate is influenced.
In a first aspect, the present application provides a reaction chamber inner surface protection device for protecting a reaction chamber inner surface of an epitaxial apparatus, the reaction chamber inner surface protection device includes: graphite paper, first pivot and second pivot, first pivot with the second pivot is installed respectively the inlet end of reaction chamber with give vent to anger the end, the graphite paper both ends are cup jointed respectively first pivot with in the second pivot, the graphite paper is in the interior top of reaction chamber has the horizontal segment, and can first pivot and the rotation of second pivot is in down the horizontal transport of interior top along the single direction of reaction chamber.
The application provides a reaction intracavity surface protection device can follow the graphite paper of unidirectional horizontal transport through setting up at reaction intracavity surface, make the substrate in carrying out epitaxial reaction in-process, reduce reaction gas at graphite intracavity surface crystallization and drop on the substrate, and simultaneously, for further preventing reaction gas at reaction intracavity surface crystallization, in substrate reaction process, graphite paper continuously carries, carry the impurity crystallization of reaction gas on graphite paper outside the reaction chamber, carry the impurity crystallization outside the reaction chamber through the graphite paper that lasts along same direction conveying, prevent that the crystallization from dropping the yield that influences the substrate on the substrate, simultaneously because the impurity crystallization can continuously transport out the reaction chamber, consequently, need not frequently to clean the reaction chamber.
Optionally, in the device for protecting the inner surface of the reaction chamber described in the present application, the graphite paper is plated with a TaC plating layer.
This application can effectively reduce reaction gas and generate the crystallization on graphite paper through plating the TaC layer on graphite paper to further avoid the crystallization to drop, in addition, owing to the crystallization reduces on the TaC cladding material, consequently can reduce the transport speed of graphite paper, thereby reduce the use amount of graphite paper, improve the utilization ratio of graphite paper.
Optionally, this application reaction intracavity surface protection device, graphite paper gets into one of reaction chamber is served and is provided with heating device, is used for heating graphite paper.
This application sets up heating device through the one end that gets into the reaction chamber at graphite paper, and heating graphite paper makes graphite paper less with the difference in temperature in reaction chamber when getting into the reaction chamber, prevents because graphite paper is great with the difference in temperature in the reaction chamber when graphite paper gets into the reaction chamber, influences the temperature field in the reaction chamber to influence the epitaxial growth quality of substrate.
Optionally, this application reaction intracavity surface protection device, the reaction chamber inlet end is provided with first sealed chamber, first pivot sets up in the first sealed chamber, the reaction chamber is given vent to anger the end and is provided with the second sealed chamber, the second pivot sets up in the second sealed chamber.
This application sets up first pivot and second pivot in sealed intracavity, keeps apart reaction chamber and external world, prevents that reaction gas from taking place to leak.
Optionally, in the device for protecting the inner surface of the reaction chamber, the width of the graphite paper is greater than or equal to the diameter of a substrate tray used for supporting the substrate in the reaction chamber.
The application designs the width more than or equal to diameter of substrate tray of graphite paper, makes the graphite paper cover the substrate tray at least to prevent that reaction gas from crystallizing above the substrate tray.
Optionally, in the device for protecting the inner surface of the reaction chamber described in the present application, a distance between the horizontal section of the graphite paper and the inner surface of the reaction chamber is 2 to 5mm.
Optionally, this application reaction intracavity surface protection device, graphite paper's direction of delivery is for following the inlet end of reaction chamber is towards the end transport of giving vent to anger of reaction chamber.
In a second aspect, the present application further provides an epitaxial reaction monitoring apparatus for monitoring a crystallization condition of an inner surface of a reaction chamber in an epitaxial reaction, where the epitaxial reaction monitoring apparatus is applied to an epitaxial device having a reaction chamber inner surface protection apparatus, the reaction chamber inner surface protection apparatus includes: graphite paper, first pivot and second pivot, first pivot with the second pivot is installed respectively the inlet end of reaction chamber with give vent to anger the end, graphite paper cup joints first pivot with in the second pivot, graphite paper is in the interior top of reaction chamber has the horizontal segment, and can first pivot and the rotation of second pivot is in down the interior top court of reaction chamber give vent to anger the end horizontal transport, epitaxial reaction monitoring device includes: the observation lamp is arranged at the air outlet end of the reaction cavity and used for providing illumination so that a user can observe the impurity amount on the graphite paper plated with the TaC layer at the second rotating shaft; the optical detection device comprises an X-ray emitting device and an X-ray absorbing device, is positioned at the gas outlet end of the reaction cavity and is used for detecting the composition of doped elements on the graphite paper positioned at the second rotating shaft.
The application provides an epitaxial reaction monitoring device sets up the observation lamp through giving vent to anger the end at the reaction chamber, thereby obtain the impurity amount on the graphite paper through the colour of observing the impurity crystallization in the TaC layer under the observation lamp, through giving vent to anger the end department at the reaction chamber and setting up optical detection device, through X ray emitter and X ray absorbing device, it constitutes to obtain the doping element on the graphite paper, thereby can constitute according to the doping element on the graphite paper, adjust the doping source proportion that lets in, through above-mentioned epitaxial reaction monitoring device, the content of impurity crystallization on the real time monitoring graphite paper, thereby in time adjust each reaction parameter in the epitaxial reaction, improve the growth yield of substrate.
In a third aspect, the present application further provides an epitaxial reaction monitoring method, configured to monitor a crystallization condition of an inner surface of a reaction chamber through an epitaxial reaction monitoring apparatus, where the epitaxial reaction monitoring apparatus is applied to an epitaxial device having a reaction chamber inner surface protection apparatus, where the reaction chamber inner surface protection apparatus includes: graphite paper, first pivot and second pivot, first pivot with the second pivot is installed respectively the inlet end of reaction chamber with give vent to anger the end, graphite paper cup joints first pivot with in the second pivot, graphite paper is in the interior top of reaction chamber has the horizontal segment, and can first pivot and the rotation of second pivot is in down the interior top court of reaction chamber give vent to anger the end horizontal transport, epitaxial reaction monitoring device includes:
the optical detection device comprises an X-ray emission device and an X-ray absorption device, is positioned at the gas outlet end of the reaction cavity and is used for detecting the composition of doped elements of the graphite paper positioned at the second rotating shaft,
the epitaxial reaction monitoring method comprises the following steps:
s1, obtaining composition information of doped elements of the graphite paper at the second rotating shaft based on the optical detection device;
s2, adjusting the proportion of doping sources introduced into the reaction cavity according to the composition information of the doping elements of the graphite paper at the second rotating shaft.
The application provides an epitaxial reaction monitoring method, thereby obtain the impurity amount on the graphite paper through the colour of observing the impurity crystallization in the TaC layer under the observation lamp, end department of giving vent to anger through at the reaction chamber sets up optical detection device, through X ray emitter to graphite paper transmission X ray and through the X ray absorption device with the X ray absorption that passes the graphite paper, thereby obtain the doping element composition on the graphite paper, and can constitute according to the doping element on the graphite paper, adjust the doping source proportion that lets in, through above-mentioned epitaxial reaction monitoring device, the content of impurity crystallization on the real time monitoring graphite paper, thereby in time adjust each reaction parameter in the epitaxial reaction, improve the growth yield of substrate.
Optionally, in the epitaxial reaction monitoring method described in the present application, step S1 includes:
s11, emitting X rays to the graphite paper positioned at the second rotating shaft through the X ray emitting device;
s12, absorbing the X-ray passing through the graphite paper at the second rotating shaft by the X-ray absorption device to obtain a fluorescence spectrum;
and S13, obtaining the composition information of the doped elements of the graphite paper at the second rotating shaft according to the fluorescence spectrum.
According to the above, the present application provides a device for protecting the inner surface of a reaction chamber, a device for monitoring an epitaxial reaction, and a method thereof, wherein graphite paper capable of being horizontally conveyed along a single direction is disposed on the inner surface of the reaction chamber, so that a substrate is subjected to an epitaxial reaction process, the crystallization of reaction gas on the inner surface of the graphite chamber is reduced and the reaction gas falls on the substrate, and meanwhile, in order to further prevent the crystallization of reaction gas on the inner surface of the reaction chamber, the graphite paper is continuously conveyed, the impurity crystals of the reaction gas on the graphite paper are conveyed to the outside of the reaction chamber, so that the impurity crystals are further prevented from falling on the substrate, an epitaxial reaction monitoring device is disposed at the gas outlet end of the reaction chamber, an observation lamp is disposed at the gas outlet end of the reaction chamber, the impurity amount on the graphite paper is obtained by observing the color of the impurity crystals in a TaC layer under the observation lamp, an optical detection device is disposed at the gas outlet end of the reaction chamber, a graphite element composition on the graphite paper is obtained by an X-ray emission device and an X-ray absorption device, so that the graphite paper is adjusted according to the composition of the doping elements on the graphite paper, and the epitaxial reaction parameters of the epitaxial reaction of the graphite paper are timely increased, and the reaction parameters of the epitaxial reaction parameters of the crystal growth rate are increased.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. The objectives and other advantages of the application may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
Fig. 1 is a schematic structural diagram of a device for protecting an inner surface of a reaction chamber according to an embodiment of the present disclosure.
Fig. 2 is a schematic structural diagram of an epitaxial reaction monitoring apparatus according to an embodiment of the present disclosure.
Fig. 3 is a flowchart illustrating steps of a method for monitoring an epitaxial reaction according to an embodiment of the present disclosure.
Description of reference numerals: 1. a reaction chamber; 2. a substrate; 3. graphite paper; 41. a first rotating shaft; 411. a heating device; 42. a second rotating shaft; 421. a cooling device; 51. a first sealed chamber; 52. a second sealed chamber; 521. a transparent quartz plate; 61. an observation lamp; 62. an optical detection device; 71. a front side door; 72. a rear side door.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present application without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures. Meanwhile, in the description of the present application, the terms "first", "second", and the like are used only for distinguishing the description, and are not to be construed as indicating or implying relative importance.
During the epitaxial process, the reaction gas may generate impurity crystals on the inner surface of the reaction chamber 1, and the crystal falling on the substrate 2 may affect the growth yield of the substrate 2.
Specifically, the epitaxial reaction is an epitaxial reaction of a SiC substrate, the reaction chamber 1 is a graphite chamber, and a reaction gas is introduced into the graphite chamber during the epitaxial reaction, specifically, a certain proportion of C is introduced into the reaction chamber 1 during the epitaxial reaction 2 H 4 、TCS、H 2 HCl, etc. are used as reaction gas, which may crystallize on the inner surface of the reaction chamber 1 during the reaction process, specifically, the crystals are SiC, si, etc. and may fall on the substrate 2 after a long time reaction, which may affect the growth yield of the substrate 2.
In a first aspect, referring to fig. 1, fig. 1 is a schematic structural diagram of a reactor inner surface protection device provided in the present application, and the reactor inner surface protection device shown in fig. 1 is used for protecting an inner surface of a reactor 1 of an epitaxial apparatus, and the reactor inner surface protection device includes: graphite paper 3, first pivot 41 and second pivot 42, the inlet end of reaction chamber 1 is installed respectively at first pivot 41 and second pivot 42 and the end of giving vent to anger is held to first pivot 41 and second, 3 both ends of graphite paper cup joint respectively on first pivot 41 and second pivot 42, graphite paper 3 has the horizontal segment at the interior top of reaction chamber 1, and can be at the interior top of reaction chamber 1 along single direction horizontal transport under the rotation effect of first pivot 41 and second pivot 42.
Specifically, the inlet end of reaction chamber 1 is the one end that lets in reactant gas, first pivot 41 sets up the inlet end at reaction chamber 1, the one end of the end of giving vent to anger of reaction chamber 1 is exhaust reactant gas, second pivot 42 sets up the exhaust end at reaction chamber 1, in this embodiment, graphite paper 3 is flexible graphite scroll, graphite paper 3 cup joints on first pivot 41 and second pivot 42, when first pivot 41 and/or second pivot 42 rotate, drive graphite paper 3 and rotate on first pivot 41 and second pivot 42, thereby make the horizontal segment of graphite paper 3 remove along the horizontal direction.
Specifically, when the epitaxial reaction does not start, the flexible graphite paper roll is sleeved on the first rotating shaft 41 or the second rotating shaft 42, in this embodiment, the flexible graphite paper roll is sleeved on the first rotating shaft 41, one end of the graphite paper roll passes through the reaction chamber 1 and is connected with the second rotating shaft 42, when the epitaxial reaction starts, the first rotating shaft 41 feeds the graphite paper 3 into the reaction chamber 1, and the second rotating shaft 42 pulls the graphite paper 3 to roll up and recover the graphite paper 3 at the second rotating shaft 42, so that the graphite paper 3 is conveyed at the inner top of the reaction chamber 1.
Specifically, in order to make the graphite paper 3 in the reaction chamber 1 have a horizontal section, it is necessary to ensure that the position where the graphite paper 3 enters the reaction chamber 1 and the position where the graphite paper 3 moves out of the reaction chamber 1 are at the same horizontal plane.
Specifically, a front side door 71 and a rear side door 72 are arranged at the air inlet end and the air outlet end of the reaction chamber 1, the front side door 71 is arranged at the air inlet end of the reaction chamber 1, the rear side door 72 is arranged at the air outlet end of the reaction chamber 1, in order to enable the graphite paper 3 to pass through the front side door 71 to enter the reaction chamber 1 and pass through the rear side door 72 to move out of the reaction chamber 1, openings are required to be formed in the front side door 71 and the rear side door 72 for enabling the graphite paper 3 to pass through the reaction chamber 1, specifically, the openings of the front side door 71 and the rear side door 72 are located on the same horizontal plane, and the horizontal section of the graphite paper 3 is parallel to the inner surface of the reaction chamber 1.
After the epitaxial reaction starts, the graphite paper drives the graphite paper 3 to be continuously and horizontally conveyed along a single direction under the rotation of the first rotating shaft 41 and/or the second rotating shaft 42, the impurity crystals are attached to the horizontal section of the graphite paper 3 positioned at the top in the reaction chamber 1, and the impurity crystals are conveyed out of the reaction chamber 1 by the graphite paper 3 when the size of the crystals is not enough to drop, so that the impurity crystals are prevented from dropping on the substrate 2, and the yield of the substrate 2 is prevented from being influenced.
Reaction intracavity surface protection device in the embodiment of the application, through the graphite paper 3 that can follow the unilateral horizontal transport at 1 internal surface setting of reaction chamber, make substrate 2 in carrying out epitaxial reaction in-process, reduce reaction gas at 1 internal surface crystallization of reaction chamber and drop on substrate 2, and simultaneously, for further preventing reaction gas at 1 internal surface crystallization of reaction chamber, in 2 reaction process of substrate, graphite paper 3 continuously carries, carry the impurity crystal that reaction gas produced on graphite paper 3 outside reaction chamber 1, carry impurity crystal to reaction chamber 1 through graphite paper 3 that lasts along the same direction conveying, prevent that the crystal from dropping the yield that influences substrate 2 on substrate 2, simultaneously because impurity crystal can continuously transport out reaction chamber 1, consequently, need not frequently to clean reaction chamber 1.
In some preferred embodiments, the graphite paper 3 is plated with a TaC coating.
Specifically, can plate the TaC cladding material through the mode of electroplating on graphite paper 3, the TaC cladding material can effectively reduce reaction gas and generate the crystallization on graphite paper 3 to further avoid the crystallization to drop, in addition, because the crystallization reduces on the TaC cladding material, consequently can reduce the conveying speed of graphite paper 3, thereby reduce the use amount of graphite paper 3, improve graphite paper 3's utilization ratio. Specifically, in this embodiment, only the TaC plating layer needs to be plated on the surface of the whole graphite paper 3 facing the substrate 2, and in the electroplating process, the TaC plating layer is generated on each surface of the graphite paper 3, therefore, in order to realize that the TaC plating layer is generated on the surface of the graphite paper 3 facing the substrate 2, before electroplating, firstly, an insulating layer or a non-reaction layer is wrapped on the surface which does not need to be plated with the TaC plating layer, and after the electroplating is finished, the insulating layer or the non-reaction layer is torn off, so that the graphite paper 3 with the TaC plating layer plated on the surface of the graphite paper 3 facing the substrate 2 can be obtained.
In some preferred embodiments, the graphite paper 3 is transported in a direction from the gas inlet end of the reaction chamber 1 toward the gas outlet end of the reaction chamber 1.
Optionally, the conveying direction of the graphite paper 3 may be conveying from the gas inlet end of the reaction chamber 1 to the gas outlet end of the reaction chamber 1, or conveying from the gas outlet end of the reaction chamber 1 to the gas inlet end of the reaction chamber 1, in this embodiment, the conveying direction of the graphite paper 3 is the same as the flowing direction of the reaction gas, and conveying from the gas inlet end of the reaction chamber 1 to the gas outlet end of the reaction chamber 1.
Specifically, in order to drive the conveying movement of the graphite paper 3, a driving motor needs to be arranged on the first rotating shaft 41 and/or the second rotating shaft 42, because the first rotating shaft 41 is connected with the second rotating shaft 42 through the graphite paper 3, and in this embodiment, the conveying direction of the graphite paper 3 is from the air inlet end of the reaction chamber 1 to the air outlet end of the reaction chamber 1, in this embodiment, in order to ensure that the graphite paper 3 is conveyed at a uniform speed, the driving motors are arranged on the first rotating shaft 41 and the second rotating shaft 42, and are used for driving the first rotating shaft 41 and the second rotating shaft 42 to rotate, so as to drive the graphite paper 3 to convey at a uniform speed.
In some preferred embodiments, a heating device 411 is disposed at one end of the graphite paper 3 entering the reaction chamber 1 for heating the graphite paper 3.
Specifically, in the epitaxial reaction, epitaxial growth needs to be carried out under 1700 ℃, if graphite paper 3 gets into reaction chamber 1 from the room temperature, because the difference in temperature in graphite paper 3 and reaction chamber 1 is great, microthermal graphite paper 3 can influence the temperature field in reaction chamber 1, thereby influence epitaxial growth's quality, for avoid influencing the temperature field in reaction chamber 2, thereby reduce the crystallization, need heat graphite paper 3 when graphite paper 3 gets into reaction chamber 1, be used for heating graphite paper 3, in this embodiment, because graphite paper 3's transmission direction is for carrying towards the end of giving vent to anger of reaction chamber 1 from the inlet end of reaction chamber 1, consequently, heating device 411 sets up on first pivot 41, heating device 411 chooses to use the thermal resistance to heat, through going to circular telegram in the thermal resistance, make graphite paper 3 heat up before getting into reaction chamber 1.
Alternatively, the heating device 411 may be disposed outside the first rotating shaft 41 to directly heat the graphite paper 3 for warming up, and preferably, in this embodiment, in order to prevent the high temperature from directly acting on the graphite paper 3 and affecting the protective effect of the TaC layer on the graphite paper 3, the heating device 411 is disposed inside the first rotating shaft 41, and the first rotating shaft 41 is heated by supplying electricity into the heat resistor, so as to warm up the graphite paper 3 at the first rotating shaft 41.
Preferably, a temperature monitoring device is arranged at the first rotating shaft 41 to monitor the temperature of the graphite paper 3 at the first rotating shaft 41 in real time, so as to ensure that the temperature of the graphite paper 3 conveyed into the reaction chamber 1 does not influence the temperature in the reaction chamber 1.
Preferably, in this embodiment, in order to prevent the graphite paper 3 entering the reaction chamber 1 from influencing the temperature field in the reaction chamber 1 due to low temperature, the graphite paper 3 needs to be heated to 500 ℃ by the heating device 411 before entering the reaction chamber 1.
Preferably, in this embodiment, because the temperature in the reaction chamber 1 is too high, when the graphite paper 3 moves out of the reaction chamber 1, the temperature of the graphite paper 3 is close to the temperature in the reaction chamber 1, in order to prevent the occurrence of dangerous accidents such as the life of other parts being affected by the too high temperature or the occurrence of scalding, the cooling device 421 is disposed at the second rotating shaft 42, and in this embodiment, the graphite paper 3 at the second rotating shaft 42 is rapidly cooled by introducing cooling water into the second rotating shaft 42.
In some preferred embodiments, the inlet end of the reaction chamber 1 is provided with a first sealed cavity 51, the first rotating shaft 41 is arranged in the first sealed cavity 51, the outlet end of the reaction chamber 1 is provided with a second sealed cavity 52, and the second rotating shaft 42 is arranged in the second sealed cavity 52.
Specifically, in order to prevent gas leakage, a first sealed cavity 51 needs to be arranged at the position where the graphite paper 3 enters the reaction cavity 1, a second sealed cavity 52 needs to be arranged at the position where the graphite paper 3 leaves the reaction cavity 1, the first rotating shaft 41 is arranged in the first sealed cavity 51, and the second rotating shaft 42 is arranged in the second sealed cavity 52, so that the inner surface protection device of the reaction cavity is isolated from the outside.
In some preferred embodiments, the graphite paper 3 has a width equal to or greater than the diameter of the substrate tray holding the substrate 2 in the reaction chamber 1.
Specifically, since the reaction gas generates crystals on the inner surface of the reaction chamber 1 above the substrate 2 during the reaction of the substrate 2, in order to prevent the crystals from falling onto the substrate 2, it is only necessary to cover the graphite paper 3 on the substrate tray for supporting the substrate 2, and it is not necessary to completely cover the inner surface of the reaction chamber 1 with the graphite paper 3, thereby reducing the processing cost of the graphite paper 3.
In some preferred embodiments, the horizontal segment of graphite paper 3 is spaced from the inner surface of reaction chamber 1 by a distance of 2 to 5mm.
Alternatively, the horizontal section of the graphite paper 3 in the reaction chamber 1 may be attached to the inner surface of the reaction chamber 1, or may have a certain distance from the inner surface of the reaction chamber 1, since the graphite paper 3 needs to continuously move in the reaction process of the substrate 2, if the graphite paper 3 is attached to the inner surface of the reaction chamber 1, there is frictional resistance between the graphite paper 3 and the reaction chamber 1, a larger driving force is required at the same moving speed, and if there is an unsmooth portion on the inner surface of the reaction chamber 1, the graphite paper 3 is easily damaged in the continuous movement, and the service life of the graphite paper 3 is reduced, therefore, in this embodiment, it is preferable that a certain distance exists between the horizontal section of the graphite paper 3 and the inner surface of the reaction chamber 1, and specifically, the distance between the horizontal section of the graphite paper 3 and the inner surface of the reaction chamber 1 is 2-5mm.
The reaction intracavity surface protection device that this embodiment provided can follow the graphite paper 3 of unidirectional direction horizontal transport through the internal surface setting at reaction chamber 1, makes substrate 2 in carrying out epitaxial reaction in-process, reduces reaction gas at the crystallization of graphite intracavity surface and drops on substrate 2, simultaneously, for further preventing reaction gas at the crystallization of reaction chamber 1 internal surface, in 2 reaction processes of substrate, graphite paper 3 continuously carries, carries reaction gas impurity crystallization on graphite paper 3 outside reaction chamber 1.
In a second aspect, referring to fig. 2, fig. 2 is a schematic structural diagram of an epitaxial reaction monitoring apparatus provided in the present application, and fig. 2 is an epitaxial reaction monitoring apparatus for monitoring crystallization of an inner surface of a reaction chamber 1 in an epitaxial reaction, where the epitaxial reaction monitoring apparatus is applied to an epitaxial device having a reaction chamber inner surface protection apparatus, and the reaction chamber inner surface protection apparatus includes: graphite paper 3, first pivot 41 and second pivot 42, the inlet end and the end of giving vent to anger at reaction chamber 1 are installed respectively to first pivot 41 and second pivot 42, graphite paper 3 cup joints on first pivot 41 and second pivot 42, graphite paper 3 has the horizontal segment at reaction chamber 1's interior top, and can give vent to anger at reaction chamber 1's interior top towards reaction chamber 1 and hold horizontal transport under the rotation effect of first pivot 41 and second pivot 42, epitaxial reaction monitoring device includes: an observation lamp 61 and/or an optical detection device 62, wherein the graphite paper 3 is plated with a TaC layer, the observation lamp 61 is arranged at the gas outlet end of the reaction chamber 1 and is used for providing illumination so that a user can observe the impurity amount on the graphite paper 3 plated with the TaC layer at the second rotating shaft 42; the optical detection device 62 comprises an X-ray emitting device and an X-ray absorbing device, and the optical detection device 62 is located at the gas outlet end of the reaction chamber 1 and is used for detecting the composition of the doped elements on the graphite paper 3 located at the second rotating shaft 42.
Specifically, in this embodiment, when the epitaxial reaction monitoring apparatus is provided with the observation lamp 61 and the optical detection device 62, the specific steps of the epitaxial reaction monitoring apparatus for monitoring the epitaxial reaction are as follows:
a1, placing a first batch of substrates 2 which need to undergo epitaxial reaction into a reaction chamber 1, and introducing reaction gas for growth;
a2, observing the impurity crystallization condition on the graphite paper 3 corresponding to each substrate 2 through an observation lamp 61 to obtain one substrate 2 with the best growth state in the first batch of substrates 2;
a3, carrying out epitaxial growth again on one substrate 2 with the best growth state, and observing the state of impurity crystals on the graphite paper 3 after the substrate 2 grows again through an observation lamp 61;
a4, if impurity crystals on the graphite paper 3 are obviously increased, the crystallization phenomenon is proved to be serious, the introduction proportion of HCl needs to be increased, and the introduction amount of silicon source gas needs to be reduced; if there is no or less crystallization on the graphite paper 3, it is proved that the reaction gas flow rate is low or the carrier gas content is too high, and H needs to be reduced 2 Introducing the ratio and increasing the ratio of Si source gas;
and A5, emitting X rays to the graphite paper 3 through the optical detection device 62 and absorbing the X rays to obtain a fluorescence spectrum, analyzing the fluorescence spectrum to obtain the element composition on the graphite paper 3, monitoring the doping elements on the graphite paper 3 in real time, and changing the concentration of the doping elements in the reaction gas by controlling a doping source.
Specifically, in order to observe the impurity crystals generated during the growth of each substrate 2 on the continuously moving graphite paper 3 at the same time in the case where a plurality of substrates 2 are epitaxially grown, in the present embodiment, the substrates 2 are arranged in an array, 1 substrate is arranged in each row in the row direction, a plurality of substrates 2 are arranged in the column direction, and the substrates 2 do not interfere with each other, wherein the row direction is the moving direction of the graphite paper 3, and the column direction is perpendicular to the row direction, and the substrate 2 is mounted in this manner, and the growth condition of the corresponding substrate 2 can be determined by observing the impurity crystals generated on each row on the graphite paper 3 when observing the graphite paper 3.
Specifically, in the present embodiment, the observation lamp 61 is a white light lamp, the TaC plated layer is gold, the impurity crystal is black, and the graphite paper 3 is also black, and if the impurity crystal is crystallized on the graphite paper 3, it is difficult to observe the state of the impurity crystal and the amount of the impurity on the graphite paper 3, whereas under the irradiation of the white light lamp, the black impurity crystal on the gold TaC plated layer has a significant color difference from the TaC plated layer, and it is easy to observe the state of the impurity crystal and the amount of the impurity, and in the present embodiment, the observation lamp 61 is disposed in the second sealed cavity 52, so that the light of the observation lamp 61 is irradiated on the graphite paper 3.
Alternatively, if the epitaxial reaction monitoring apparatus includes only the observation lamp 61, the worker may judge the growth state of the substrate 2 by observing the form of impurity crystals in the TaC coating layer, and control the proportion, flow rate, and flow rate of the introduced gas source.
Alternatively, if the epitaxial reaction monitoring device only includes the optical detection device 62, the operator obtains the doping element composition on the graphite paper 3 through the X-ray emission device and the X-ray absorption device, so that the proportion of the introduced doping source can be adjusted according to the doping element composition on the graphite paper 3.
Specifically, since the temperature in the reaction chamber 1 is high during the epitaxial reaction, in order to prevent the high temperature from affecting the detection accuracy of the optical detection device 62 or the lifetime of the device, in the present embodiment, the optical detection device 62 is disposed outside the second sealed chamber 52, and in order to enable the X-rays emitted by the optical detection device 62 to irradiate the graphite paper 3, it is preferable that the side wall portion of the second sealed chamber 52 between the optical detection device 62 and the graphite paper 3 is a transparent quartz plate 521, and the X-rays are irradiated onto the graphite paper 3 through the second sealed chamber 52.
Preferably, an optical microscope may be further disposed under the transparent quartz plate 521, and the surface morphology of the graphite paper 3 surface crystals is observed through the optical microscope, and the crystal surface morphology information is transmitted to the outside for observation.
Preferably, in this embodiment, the epitaxial reaction monitoring device includes an observation lamp 61 and an optical detection device 62, the observation lamp 61 is used to observe the crystal form on the graphite paper 3, the proportion, flow rate and flow rate of the introduced reaction gas are primarily adjusted, when the growth state of the substrate 2 is difficult to be determined by observation, the optical detection device 62 is used to monitor the growth state of the substrate 2, the composition of the doping elements on the graphite paper 3 is obtained by the X-ray emission device and the X-ray absorption device, and the proportion of the introduced doping source is adjusted according to the composition of the doping elements on the graphite paper 3.
The epitaxial reaction monitoring device that this application embodiment provided is through giving vent to anger at reaction chamber 1 and holding observation lamp 61, thereby obtain the impurity volume on the graphite paper 3 through the colour of observing the impurity crystallization in the TaC layer under observation lamp 61, through holding optical detection device 62 at reaction chamber 1 department of giving vent to anger, through X ray emitter and X ray absorbing device, it constitutes to obtain the doping element on the graphite paper 3, thereby can constitute according to the doping element on the graphite paper 3, adjust the doping source proportion that lets in, through above-mentioned epitaxial reaction monitoring device, the content of impurity crystallization on the real time monitoring graphite paper 3, thereby each reaction parameter in the epitaxial reaction of in time adjusting, improve the growth yield of substrate 2.
In a third aspect, referring to fig. 3, fig. 3 is a method for monitoring an epitaxial reaction provided by the present application, for monitoring crystallization of an inner surface of a reaction chamber 1 by an epitaxial reaction monitoring device, where the epitaxial reaction monitoring device is applied to an epitaxial apparatus having a reaction chamber inner surface protection device, where the reaction chamber inner surface protection device includes: graphite paper 3, first pivot 41 and second pivot 42, the inlet end and the end of giving vent to anger at reaction chamber 1 are installed respectively to first pivot 41 and second pivot 42, graphite paper 3 cup joints on first pivot 41 and second pivot 42, graphite paper 3 has the horizontal segment at reaction chamber 1's interior top, and can give vent to anger at reaction chamber 1's interior top towards reaction chamber 1 and hold horizontal transport under the rotation effect of first pivot 41 and second pivot 42, epitaxial reaction monitoring device includes:
the optical detection device 62, the optical detection device 62 includes an X-ray emission device and an X-ray absorption device, the optical detection device 62 is located at the gas outlet end of the reaction chamber 1, and is used for detecting the composition of doped elements at the second rotating shaft 42 of the graphite paper 3,
the epitaxial reaction monitoring method comprises the following steps:
s1, obtaining the composition information of doping elements of the graphite paper 3 at the second rotating shaft 42 based on the optical detection device 62;
s2, adjusting the proportion of doping sources introduced into the reaction cavity 1 according to the composition information of the doping elements of the graphite paper 3 at the second rotating shaft 42.
Specifically, the doping elements include a heavy doping element and a light doping element, wherein the heavy doping element is an element having an atomic number greater than or equal to 11, and the light doping element is an element having an atomic number less than 11.
Specifically, after the composition information of the doping elements is obtained, the proportion of the doping source is controlled within a preset range, the preset proportion range is within the content range of the doping elements, the proportion can be manually set by a craftsman according to experience values, and when the proportion of the doping elements exceeds the preset range, the proportion of the doping source is automatically controlled, so that the content of the doping elements is stabilized within the preset range, and the automatic adjustment of the proportion of the doping source is realized.
In some preferred embodiments, step S1 comprises:
s11, emitting X rays to the graphite paper 3 positioned at the second rotating shaft 42 through an X ray emitting device;
s12, absorbing the X-rays passing through the graphite paper 3 at the second rotating shaft 42 by an X-ray absorption device to obtain a fluorescence spectrum;
and S13, obtaining the composition information of the doping elements of the graphite paper 3 at the second rotating shaft 42 according to the fluorescence spectrum.
Preferably, an electron microscope may be further provided in this embodiment, and is configured to perform scanning analysis on the graphite paper 3 taken out after the reaction is completed, so as to obtain element distribution on the graphite paper 3 to study the proportion of the light element, thereby controlling the C/Si ratio by changing the gas source proportion.
According to the epitaxial reaction monitoring method in the embodiment of the application, the amount of impurities on the graphite paper 3 is obtained by observing the color of the impurity crystals in the TaC layer under the observation lamp 61, the optical detection device 62 is arranged at the gas outlet end of the reaction cavity 1, the X-ray is transmitted to the graphite paper 3 through the X-ray transmitting device, and the X-ray which passes through the graphite paper 3 is absorbed through the X-ray absorbing device, so that the doped element composition on the graphite paper 3 is obtained, the proportion of the introduced doped source can be adjusted according to the doped element composition on the graphite paper 3, and by the epitaxial reaction monitoring method, the content of the impurity crystals on the graphite paper 3 is monitored in real time, so that each reaction parameter in the epitaxial reaction is adjusted in time, and the growth yield of the substrate 2 is improved.
In the embodiments provided in the present application, it should be understood that the disclosed apparatus and method may be implemented in other ways. The above-described embodiments of the apparatus are merely illustrative, and for example, the division of the units is only one logical division, and there may be other divisions when actually implemented, and for example, a plurality of units or components may be combined or integrated into another system, or some features may be omitted, or not executed. In addition, the shown or discussed coupling or direct coupling or communication connection between each other may be through some communication interfaces, indirect coupling or communication connection between devices or units, and may be in an electrical, mechanical or other form.
In addition, units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
Furthermore, the functional modules in the embodiments of the present application may be integrated together to form an independent part, or each module may exist separately, or two or more modules may be integrated to form an independent part.
In this document, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions.
The above description is only an example of the present application and is not intended to limit the scope of the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (9)

1. A reactor chamber inner surface protection device for protecting the inner surface of a reactor chamber (1) of an epitaxial apparatus, characterized in that it comprises: graphite paper (3), first pivot (41) and second pivot (42), first pivot (41) with second pivot (42) are installed respectively the inlet end of reaction chamber (1) with give vent to anger the end, reaction chamber (1) inlet end is provided with first sealed chamber (51), first pivot (41) set up in first sealed chamber (51), reaction chamber (1) give vent to anger the end and be provided with second sealed chamber (52), second pivot (42) set up in second sealed chamber (52), graphite paper (3) both ends are cup jointed respectively first pivot (41) with on second pivot (42), graphite paper (3) are in the interior top of reaction chamber (1) has the horizontal segment, and can be in first pivot (41) and the rotation of second pivot (42) is in the interior top of reaction chamber (1) is along single direction horizontal transport.
2. The reactor cavity inner surface protection device according to claim 1, wherein the graphite paper (3) is plated with TaC plating.
3. The reaction chamber inner surface protection device according to claim 1, characterized in that a heating device (411) is arranged on one end of the graphite paper (3) entering the reaction chamber (1) for heating the graphite paper (3).
4. The reaction chamber inner surface protection device according to claim 1, characterized in that the graphite paper (3) has a width equal to or larger than the diameter of a substrate tray for holding a substrate (2) in the reaction chamber (1).
5. A reactor chamber inner surface protection device according to claim 1, characterized in that the distance between the horizontal section of the graphite paper (3) and the inner surface of the reactor chamber (1) is 2-5mm.
6. The reaction chamber inner surface protection device according to claim 1, wherein the graphite paper (3) is transported in a direction from an inlet end of the reaction chamber (1) toward an outlet end of the reaction chamber (1).
7. An epitaxial reaction monitoring apparatus for monitoring crystallization of an inner surface of a reaction chamber (1) in an epitaxial reaction, the epitaxial reaction monitoring apparatus being applied to an epitaxial device having a reaction chamber inner surface protection apparatus, the reaction chamber inner surface protection apparatus comprising: graphite paper (3), first pivot (41) and second pivot (42), first pivot (41) with second pivot (42) are installed respectively the inlet end of reaction chamber (1) with give vent to anger the end, reaction chamber (1) inlet end is provided with first sealed chamber (51), first pivot (41) set up in first sealed chamber (51), reaction chamber (1) give vent to anger the end and be provided with second sealed chamber (52), second pivot (42) set up in second sealed chamber (52), graphite paper (3) cup joint first pivot (41) with on second pivot (42), graphite paper (3) are in the interior top of reaction chamber (1) has the horizontal segment, and can be in first pivot (41) and the rotation of second pivot (42) is in the interior top of reaction chamber (1) is towards reaction chamber (1) end horizontal transport of giving vent to anger, epitaxial reaction monitoring device includes: an observation lamp (61) and/or an optical detection device (62), wherein the graphite paper (3) is plated with a TaC layer, the observation lamp (61) is arranged at the gas outlet end of the reaction chamber (1) and used for providing illumination so that a user can observe the impurity amount on the graphite paper (3) which is plated with the TaC layer and is positioned at the second rotating shaft (42); the optical detection device (62) comprises an X-ray emitting device and an X-ray absorbing device, and the optical detection device (62) is located at the gas outlet end of the reaction cavity (1) and used for detecting the composition of doped elements on the graphite paper (3) located at the second rotating shaft (42).
8. An epitaxial reaction monitoring method is characterized by being used for monitoring the crystallization condition of the inner surface of a reaction cavity (1) through an epitaxial reaction monitoring device, wherein the epitaxial reaction monitoring device is applied to epitaxial equipment with a reaction cavity inner surface protection device, and the reaction cavity inner surface protection device comprises: graphite paper (3), first pivot (41) and second pivot (42), first pivot (41) with second pivot (42) are installed respectively the inlet end of reaction chamber (1) with give vent to anger the end, graphite paper (3) cup joint first pivot (41) with on second pivot (42), graphite paper (3) are in the interior top of reaction chamber (1) has the horizontal segment, and can first pivot (41) and the rotation of second pivot (42) is in down the interior top court of reaction chamber (1) give vent to anger the end horizontal transport, epitaxial reaction monitoring device includes:
the optical detection device (62) comprises an X-ray emission device and an X-ray absorption device, the optical detection device (62) is positioned at the gas outlet end of the reaction cavity (1) and is used for detecting the composition of doped elements of the graphite paper (3) positioned at the second rotating shaft (42),
the epitaxial reaction monitoring method comprises the following steps:
s1, obtaining composition information of doping elements of the graphite paper (3) at the second rotating shaft (42) based on the optical detection device (62);
s2, adjusting the proportion of doping sources introduced into the reaction cavity (1) according to the composition information of doping elements of the graphite paper (3) at the second rotating shaft (42).
9. The epitaxial reaction monitoring method of claim 8, wherein step S1 comprises:
s11, emitting X-rays to the graphite paper (3) at the second rotating shaft (42) through the X-ray emitting device;
s12, absorbing the X-rays passing through the graphite paper (3) at the second rotating shaft (42) through the X-ray absorption device to obtain a fluorescence spectrum;
and S13, obtaining the composition information of the doped elements of the graphite paper (3) at the second rotating shaft (42) according to the fluorescence spectrum.
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JPH11240796A (en) * 1998-02-27 1999-09-07 Super Silicon Kenkyusho:Kk Epitaxial growth apparatus
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