WO2020000602A1 - 一种半导体合成装置和合成方法 - Google Patents

一种半导体合成装置和合成方法 Download PDF

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Publication number
WO2020000602A1
WO2020000602A1 PCT/CN2018/101452 CN2018101452W WO2020000602A1 WO 2020000602 A1 WO2020000602 A1 WO 2020000602A1 CN 2018101452 W CN2018101452 W CN 2018101452W WO 2020000602 A1 WO2020000602 A1 WO 2020000602A1
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Prior art keywords
furnace body
horizontal boat
semiconductor
horizontal
container
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PCT/CN2018/101452
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English (en)
French (fr)
Inventor
雷仁贵
肖亚东
谈笑天
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汉能新材料科技有限公司
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Publication of WO2020000602A1 publication Critical patent/WO2020000602A1/zh

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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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/002—Crucibles or containers for supporting the melt
    • 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
    • C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C30B29/42—Gallium arsenide
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/006—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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
    • C30B28/06—Production of homogeneous polycrystalline material with defined structure from liquids by normal freezing or freezing under temperature gradient
    • 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
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
    • 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
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02538—Group 13/15 materials
    • H01L21/02546—Arsenides

Definitions

  • the present disclosure relates to improvements in a semiconductor fabrication apparatus and method (horizontal boat production method) employing a horizontal Bridgeman method.
  • the horizontal Bridgman method is a method developed by Bridgman to prepare large-area shaped flake crystals, also known as the horizontal boat method, or HB method for short.
  • the HB method is widely used, especially in the growth of compound semiconductor crystals, and it can also be used for doping semiconductor materials.
  • the HB method is to place the raw material for growing crystals or doped raw materials in a vessel, the vessel is placed in a round tube, and the mouth of the tube is closed after vacuum; the crystal is grown by directional solidification or directional melting or a suitable semiconductor doped
  • the doping method performs semiconductor doping.
  • CN 107268085A discloses a semi-insulating gallium arsenide polycrystalline carbon doped preparation device, which includes a cylindrical heating device, one end of the heating device is a source area, and the other end is a growth area. The temperature increases from the source region to the growth region; a quartz tube is fixedly arranged in the heating device, and a first PBN for containing graphite powder is disposed adjacent to a position corresponding to the source region in the quartz tube.
  • a first aspect of the present disclosure provides a semiconductor synthesis device applied to a horizontal Bridgeman method, including a closed reaction tube, a first furnace body, and a second furnace body, wherein the first furnace body and the first furnace body
  • the two furnace bodies are connected by an intermediate pipe, and the reaction tube is placed in a furnace cavity defined by the first furnace body, the intermediate pipe, and the second furnace body, corresponding to the first furnace body and the second furnace body.
  • the furnace body is separately provided with a temperature control device, wherein the reaction tube is provided with a plurality of horizontal boat containers, and the plurality of horizontal boat containers include a plurality of first ones arranged at different positions in the reaction tube in a horizontal direction.
  • a level boat container a bracket device is provided on at least one of the first layer horizontal boat container, and a second layer of horizontal boat container is stacked on the bracket device, wherein the bracket device is configured to support the A second-level horizontal boat container, and providing a gap between the first-level horizontal boat container and the second-level horizontal boat container.
  • a second aspect of the present disclosure provides a gallium arsenide polycrystal synthesis device, including the device described in the first aspect of the present disclosure, wherein the first furnace body is a low-temperature zone furnace body and the second furnace body is a high-temperature device.
  • the first furnace body is a low-temperature zone furnace body and the second furnace body is a high-temperature device.
  • a horizontal boat container filled with arsenic and a horizontal boat container filled with gallium are respectively placed in the low-temperature zone furnace body and the high-temperature zone furnace body.
  • Multiple gallium arsenide polycrystalline rods are provided during the preparation process.
  • a third aspect of the present disclosure provides a method for synthesizing gallium arsenide polycrystals, using the apparatus described in the second aspect of the present disclosure, wherein in a stacked horizontal boat, the loading weight of the upper horizontal boat container is less than the lower layer Loading weight of the horizontal boat container.
  • FIG. 1 is a schematic diagram of a reaction apparatus according to an embodiment of the present disclosure
  • FIG. 2 is a schematic diagram of a reaction apparatus according to an embodiment of the present disclosure
  • FIG. 3 is a schematic diagram of a reaction apparatus according to an embodiment of the present disclosure.
  • FIG. 4 is a schematic diagram of a reaction apparatus according to an embodiment of the present disclosure.
  • FIG. 5 is a schematic diagram of a reaction apparatus according to an embodiment of the present disclosure.
  • FIG. 6 is a schematic projection view of a horizontal boat container used in an embodiment of the present disclosure.
  • FIG. 7 is a schematic projection view of a horizontal boat container used in an embodiment of the present disclosure.
  • FIG. 8 is a schematic projection view of a horizontal boat container used in an embodiment of the present disclosure.
  • FIG. 9 is a schematic cross-sectional view of a horizontal boat container used in an embodiment of the present disclosure.
  • FIG. 10 is a schematic cross-sectional view of a horizontal boat container used in an embodiment of the present disclosure.
  • FIG. 11 is a plan view of a horizontal boat container used in an embodiment of the present disclosure.
  • FIG. 12 is a schematic structural diagram of a stent used in an embodiment of the present disclosure.
  • FIG. 13 is a schematic structural diagram of a stent used in an embodiment of the present disclosure.
  • the horizontal boat container is generally arranged horizontally at different positions of the closed reaction tube in the art. Due to the limited space inside the reaction tube, the arrangement of the horizontal boat container is further limited. In the art, there is no space arrangement scheme for stacking horizontal boats in the reaction tube. In particular, no design for stably stacking horizontal boats and a technical method for controlling the gap between the stacked horizontal boats are not proposed.
  • the inventor designed a structure that realizes the stacking of a plurality of horizontal boat containers, in order to effectively and stably control the gap between the stacked horizontal boat containers. Further, there is still room for improvement in the uniformity quality of a plurality of semiconductor ingots prepared by stacking a plurality of horizontal boat containers.
  • crystal rods are synthesized by the horizontal Bridgeman method, the temperature in the high and low temperature regions is difficult to control due to thermal radiation and other reasons. Polycrystalline oxide or arsenic leakage caused by quartz tube deformation and cracking often occurs, and polycrystalline materials Problems such as incomplete tail synthesis.
  • Embodiment 1 is a semiconductor synthesis device applied to a horizontal Bridgeman method.
  • the synthesis device includes a closed reaction tube 4, a first furnace body 1 and a second furnace body 2.
  • the first furnace body 1 and the second furnace body 2 are connected by an intermediate pipe 8, and the reaction tube 4 is placed in a furnace cavity defined by the first furnace body 1, the intermediate pipe 8, and the second furnace body 2, corresponding to the first furnace body 1 and
  • the second furnace body 2 is separately provided with temperature control devices 9-1 and 9-2.
  • the temperature control device 9-1 providing heating below 1000 ° C includes 2-4 temperature control units, and the temperature control device 9-2 providing heating above 1000 ° C includes 5-7 temperature control units.
  • the temperature control unit is used to control the temperature of the furnace body, and may include a heating unit and a temperature measuring unit.
  • the heating unit can be heated by a high-frequency induction coil or a resistance heating furnace, and the temperature measurement unit can be performed by a thermocouple.
  • a first-layer horizontal boat container 11 is placed on the left side of the sealed reaction tube 4.
  • a bracket device 13 is provided on the first-layer horizontal boat container 11, and a second-layer horizontal boat container 12 is stacked on the support device 13.
  • the bracket device 13 is configured to support the second-level horizontal boat container 12 and define a preset gap between the first-level horizontal boat container 11 and the second-level horizontal boat container 12 for the reactants from the stacked level Boat in and out.
  • another horizontal boat container 5 is arranged on the right side of the closed reaction tube 4. It can be understood that the horizontal boat container 5 can also adopt the structure of the first-level horizontal boat container 11 to facilitate the production of components.
  • the difference is that in the embodiment 2, a total of four horizontal boat containers are provided, which are divided into two groups, and the two horizontal boat containers are arranged in an overlapping manner.
  • two first-layer horizontal boat containers 11 are arranged at two ends in the horizontal direction in the sealed reaction tube 4.
  • a bracket device 13 is provided on the two first-layer horizontal boat containers 11, 13 is stacked on the second level horizontal boat container 12.
  • the bracket device 13 is provided to support the second-level horizontal boat container 12 and provide a gap between the first-level horizontal boat container 11 and the second-level horizontal boat container 12.
  • Embodiment 3 of the present disclosure three sets of horizontal boat containers are arranged in the horizontal direction of the reaction tube 4.
  • the first group is two horizontal boat stacks, and the first layer
  • the horizontal boat container 11 is provided with a support device 13, and a second layer of horizontal boat containers 12 is stacked on the support device 13.
  • the other two sets of horizontal boat containers 5 are separately arranged at the middle position and the right position in the horizontal direction. It can be understood that the horizontal boat container 5 can also adopt the structure of the first-level horizontal boat container 11 to facilitate the production of components.
  • the embodiment 4 provides three sets of double stacked horizontal boats. As shown in FIG. 4, in the closed reaction tube 4, three first-level horizontal boat containers 11 are arranged in the horizontal direction. The first-level horizontal boat containers 11 are respectively provided with a bracket device 13, and the bracket devices 13 are stacked on the bracket device 13 respectively. Three second-level horizontal boat containers 12 are placed, wherein the bracket device 13 is configured to support the second-level horizontal boat container 12 and provide a preset gap between the first-level horizontal boat container 11 and the second-level horizontal boat container 12. .
  • the device of Example 5 is applied to the preparation of a gallium arsenide semiconductor using a horizontal Bridgeman method.
  • the synthesis device includes a closed reaction tube 4, a first furnace body 1, and a second furnace body 2.
  • a furnace body 1 and a second furnace body 2 are connected by an intermediate pipe 8, and a reaction tube 4 is placed in a furnace cavity defined by the first furnace body 1, the intermediate pipe 8, and the second furnace body 2, corresponding to the first furnace.
  • the body 1 and the second furnace body 2 are respectively provided with temperature control devices 9-1 and 9-2.
  • the second furnace body 2 is composed of 6 sections of temperature control, and the first furnace body 1 is composed of 3 sections of temperature control.
  • the temperature control unit is used to control the temperature of the furnace body, and may include a heating unit and a temperature measuring unit.
  • the heating unit can be heated by a high-frequency induction coil or a resistance heating furnace, and the temperature measurement unit can be performed by a thermocouple.
  • An arsenic boat 5 and a gallium boat 11 and 12 sealed with a quartz closed reaction tube 4 are placed in the first furnace body 1 and the second furnace body 2, respectively.
  • the second layer of gallium boat 12 is stacked on the first layer of gallium boat 11 by setting a support device 13.
  • a certain gap is set between the first layer of gallium boat 11 and the second layer of gallium boat 12 so that the reactant arsenic can be removed from the substrate. Get in and out of stacked horizontal boat containers.
  • This arrangement enables two gallium arsenide crystal rods to be produced at a time by the device of this embodiment. It can be understood that although the arsenic boat 5 and the gallium boat 11 use different reference numbers, the arsenic boat 5 and the gallium boat 11 can adopt similar structures to facilitate the production of components.
  • reaction tube Through different settings and combinations, those skilled in the art can place more reaction products in the reaction tube according to the needs and different target products, or cooperate with a more reasonable arrangement and control heating method.
  • the device of the present disclosure can synthesize multiple ingots at the same time by stacking the horizontal boat containers at the same time, which improves the production efficiency and reduces the production cost.
  • the present disclosure further adopts a double heating method.
  • the heating structure of the furnace uses the furnace body for temperature control in the low temperature region and the high temperature region, respectively, so that the temperature is easy to control when synthesizing the semiconductor, and the precise control of the temperature of the furnace body is achieved. Therefore, multiple semiconductors such as polycrystalline The proportion of single crystal is uniform and the pass rate is high.
  • the outer periphery of the intermediate pipe 8 is covered with a heat insulating material 10. Due to proper heat preservation measures between the high temperature region and the low temperature region, the evaporated component can completely react with other components to obtain a semiconductor compound with uniform mixing ratio and good performance.
  • a spacer layer 3 is further provided on the inner side wall of at least one of the first furnace body 1 and the second furnace body 2 to define a uniformly heated furnace cavity within the space surrounded by the spacer layer 3.
  • This setting can be used to improve the uniformity of the internal thermal field, which is more conducive to the uniformity of the proportion of the synthesized semiconductor products and further improves the pass rate.
  • the spacer layer 3 is configured to be selected from the group consisting of a quartz tube, a silicon carbide tube, a mullite tube, and a combined casing thereof. It is preferably a silicon carbide tube, a mullite tube, or a combined casing.
  • the spacer layer of this structure is more durable, and at the same time, it can reduce the unevenness of the internal radial temperature more effectively.
  • the sealed reaction tube 4 when the sealed reaction tube 4 is placed in the first furnace body 1 and the second furnace body 2, the sealed reaction tube 4 is separated from the inner side wall by a spacer layer 3.
  • the uniformity of the internal thermal field can be further improved, which is more conducive to the uniformity of the proportion of the synthesized semiconductor products and further improves the qualification rate.
  • the distance between the first furnace body 1 and the second furnace body 2 is 15-20 cm.
  • the two furnace chambers are separated by a certain distance, which can avoid the difficult temperature control in the low temperature zone due to heat diffusion and heat radiation.
  • the distance is too long, such as greater than 20cm, the central part is likely to be too cold, and if it is too short, such as less than 15cm, the temperature control in the low temperature region and the high temperature region cannot be achieved.
  • the pitch in the above range can realize the temperature control in the low temperature region and the high temperature region, and at the same time, the temperature of the middle connection is always within a suitable range, which ensures that the reaction proceeds smoothly and obtains a semiconductor product with a uniform ratio.
  • the thermal insulation material 10 coated on the periphery of the intermediate pipe 8 is a low-density thermal insulation material, and the coating thickness thereof is 3 cm-5 cm.
  • the thickness of this material is too thin to effectively maintain heat, and it is too thick to waste raw materials. Therefore, choosing the above range can meet the requirements of heat insulation while minimizing costs.
  • the low-density thermal insulation material is a material made from a component containing silica and / or alumina. Insulation materials are also called thermal insulation materials, which refers to materials or material composites that have significant resistance to heat flow. The common characteristics of thermal insulation materials are light weight, loose, porous or fibrous, and they do not flow inside.
  • the air barrier insulation conducts inorganic materials such as non-combustible, wide operating temperature, good chemical resistance and so on.
  • the heat insulation material used in the present disclosure is, for example, a heat insulation material made of a silica component, a heat insulation material made of an alumina component, and a heat insulation material made of a silica and an alumina component. Specific preparation methods and products may refer to methods known in the art, such as products prepared by the methods disclosed in CN 101671158A, CN102795781A, and the like.
  • the preparation device further includes a heat-insulating sealing material plate 7 at both ends of the first furnace body 1 and the second furnace body 2.
  • the heat-preserving and sealing material plate 7 may be, for example, a heat-preserving cotton board, a silicate fiber board, or the like.
  • the insulation materials of the first furnace body and the second furnace body may use the same material or different materials.
  • the insulation materials of the first furnace room may be made of insulation materials suitable for providing a lower temperature furnace body.
  • a heat insulating material suitable for providing a higher temperature furnace body can be used.
  • the reaction tube used in the embodiment may be a quartz reaction tube, and the size may be a size generally used in the art, such as having an inner diameter of 80 mm.
  • the inner diameter of the horizontal boat container placed there is compatible with the reaction tube, which can be slightly smaller than the inner diameter of the reaction tube, and the depth can be set according to the number of layers placed. 35mm, specifically 24mm, 28mm, 31mm, 34mm, etc.
  • the raw material for growing a single crystal is placed in a vessel, the vessel is placed in a round tube, and the mouth of the vessel is closed after vacuuming.
  • This vessel is generally called a "boat”.
  • synthetic boats and crystal pull boats are used to synthesize polycrystals; those used to grow single crystals are called pulling crystal boats.
  • the open part of the synthesis boat can be rectangular, as shown in the projection diagram shown in Figure 5; or one end is semicircular, as shown in Figure 6; or both ends are semicircular, as shown in Figure 7 Schematic projection.
  • the semi-circular boat has been used for decades, and its biggest feature is that it is easy to process.
  • the circular tube can be broken in half, plus the boat head and / or the boat tail.
  • the main section of the synthetic boat or crystal boat is generally arched, as shown in Figure 8. Of course, it can also be rectangular, as shown in FIG. 9, or other shapes used in the art.
  • the upper left image in the projection diagram is a top view
  • the lower left image is the main view
  • the upper right image is the left view
  • the single crystal growth boat adds a seed region and a shoulder rest on the basis of a polycrystalline synthesis boat.
  • the structure is as follows: the front end is called a seed cavity, and the seed cavity has a variety of square, rectangular, and semicircular shapes; The part between the seed cavity and the seed cavity is called the shoulder, which is used to smoothly connect the seed cavity and the main body of the boat. In the middle is the main part of the single crystal growth boat, and finally at the tail of the boat.
  • z1-z4 are a seed crystal cavity part, a shoulder rest part, an equal diameter part (that is, a main body part), and a boat tail part in this order.
  • the bracket device 13 may be a separately provided component.
  • the stand device 13 is a separate component separate from the horizontal boat container.
  • the bracket device 13 may be assembled on the horizontal boat container to provide support for the horizontal boat container mounted thereon.
  • the bracket device 13 can be installed on the horizontal boat container after the loading operation is completed, and therefore, the stand device provided separately will not affect the loading operation of the horizontal boat container.
  • the bracket device 13 may be provided integrally with the horizontal boat container, for example, the bracket device 13 is provided integrally with an upper portion of the first layer of the horizontal boat 11 or a lower portion of the second layer of the horizontal boat 12.
  • the integrated setting is more convenient to use, is conducive to the realization of industrialized production, and is more conducive to the stability of the structure during use.
  • the horizontal boat container includes a main body portion provided at a substantially middle portion of the horizontal boat container, and the main body portion has a substantially U-shaped cross section.
  • the bracket device 13 is provided as a bridge-shaped member, and two ends of the bridge-shaped member are respectively snapped to two side walls of a horizontal boat container (for example, the first-level horizontal boat 11) arranged substantially parallel to the axial direction of the reaction tube 4 on.
  • the buckle joint can be used to conveniently assemble the horizontal boat container and the bracket device, simplifying the assembly steps.
  • a concave arc-shaped portion 20 is provided in the middle portion of the bracket device 13 to conform to the bottom shape of the second-layer horizontal boat container 12.
  • FIG. 12 shows a schematic structural diagram of a bracket.
  • a concave arc-shaped portion 20 is provided in the middle of the holder device 13.
  • the arc-shaped portion 20 of the bracket device 13 is in contact with the bottom of the horizontal boat container to provide stable support for the horizontal boat container.
  • the bracket device 13 further includes a horizontal portion 30, the thickness of the horizontal portion 30 is 2-3 mm, the thickness of the arc-shaped portion 20 is 2.5-3.5 mm, and the thickness of the arc-shaped portion 20 is slightly The thickness is larger than the horizontal portion.
  • the thickness of the arc-shaped portion 20 is 0.2-0.5 mm larger than the thickness of the horizontal portion 30.
  • the arc length of the arc-shaped portion 20 occupies 1 / 4-1 / 2, preferably 1/3, of the outer surface length of the horizontal boat container placed on the bracket.
  • the bracket device 13 further includes two grooves 10.
  • the grooves 10 are used for buckling the bracket 3 on the horizontal boat container 2.
  • the groove 10 may be provided at a position of the horizontal portion 30 near the end portion, as shown in FIGS. 11 and 12. Through the setting of the groove, the bracket device 13 can be stably joined with the lower horizontal boat container (for example, the first horizontal boat container 12), and the two form a stable assembly.
  • the depth of the groove 10 is 1-1.5 mm, more advantageously 1.2-1.4 mm, and most advantageously about 1.3 mm, making the buckle more stable. Both grooves have the same depth.
  • the width and thickness of the bracket 13 used in the present disclosure and the related dimensions of the groove 10 can be adjusted according to actual needs.
  • the length of the groove 10 can be set according to the wall thickness of the horizontal boat container, which can be just engaged or slightly larger than the wall thickness.
  • the length of the stent in the present disclosure may be determined according to the width of the lower horizontal boat container spanned by the stent, and is considered to facilitate the better movement of the laminated boat inside the quartz tube.
  • a specific form of the bracket is a bridge-type bracket.
  • the number of the bracket devices 13 provided on one horizontal boat is 1, 2, 3, 4, and the like, and may be two or more, especially three.
  • the reaction device of the embodiment is used for semiconductor synthesis or semiconductor doping reaction.
  • the reaction device is used for gallium arsenide polycrystal synthesis or gallium arsenide single crystal synthesis, and optionally, used for gallium arsenide polycrystal synthesis.
  • the stent device is made of PBN (pyrolyzed boron nitride) material, or a layer of PBN (pyrolyzed boron nitride) material is deposited on the surface of the graphite material.
  • PBN pyrolyzed boron nitride
  • a layer of PBN (pyrolyzed boron nitride) material is deposited on the surface of the graphite material.
  • the selection of the stent device material needs to consider not introducing impurities during the reaction.
  • An embodiment of the present disclosure also provides a gallium arsenide polycrystal synthesis device.
  • the first furnace body is a low temperature area furnace body and the second furnace body is a high temperature area furnace body.
  • a horizontal boat container containing arsenic and a gallium container The horizontal boat container is placed in the furnace in the low temperature region and the furnace in the high temperature region, and the horizontal boat container filled with gallium is set to be stacked (for example, the second horizontal boat container 12 is stacked on the first horizontal boat container 11) to Multiple gallium arsenide polycrystalline rods are provided in one fabrication process.
  • An aspect of the present disclosure also provides a method for synthesizing a gallium arsenide polycrystal using the present disclosure to provide a gallium arsenide polycrystal synthesizing device, wherein, in a stacked horizontal boat, the loading weight of the upper horizontal boat container Less than the loading weight of the lower horizontal boat container.
  • the sealed reaction tube is evacuated or filled with an inert gas for protection.
  • the loading weight of the lower horizontal boat container is 1-1.5 times the loading weight of the upper horizontal boat container, and more advantageously, it is about 1.3 times.
  • gallium arsenide is described as an example below.
  • control the temperature in the low temperature zone to about 620-650 ° C, the temperature of the furnace body in the high temperature zone is 1250-1255 ° C, and keep the temperature for 1-3h.
  • press the preset Cooling program to cool down to room temperature;
  • the polycrystalline rods synthesized in three times have surface gloss, dense, no holes, no gallium rich, and good synthesis ratio; each furnace can take 1 polycrystalline rod and take the head and tail pieces for testing.
  • the qualification rate and electrical properties of the polycrystals synthesized in three times The parameters are shown in Table 1 below.
  • a horizontal boat container is stacked, which allows multiple crystal rods to be manufactured at one time without increasing the volume of the reaction tube, which improves production efficiency and reduces costs.
  • the first furnace body and the second furnace body are separately provided with temperature control devices to achieve effective independent control of the temperature in the high temperature region and the low temperature region, reduce the influence of undesired heat radiation, and prevent deformation and cracking of the quartz tube.
  • the present disclosure proposes a bracket structure that facilitates placement of the upper boat. Based on this, the present disclosure proposes to stack the horizontal boat containers, which is particularly suitable for improving the synthesis device of the HB method.
  • the stacked structure of the multiple horizontal boat containers disclosed in the present disclosure is stable, which can make the reaction proceed smoothly, improve production efficiency, and reduce costs. More advantageously, the present disclosure can make multiple ingots at one time without increasing the volume of the reaction tube. In addition, applications with more chemical reaction components can be improved.
  • the device of the present disclosure separately sets a temperature control device through the first furnace body and the second furnace body, thereby effectively controlling the high temperature region and the low temperature region independently. Temperature, reducing the effects of undesired heat radiation, and preventing polycrystalline oxide or arsenic leakage caused by quartz tube deformation and cracking, etc., thereby obtaining a plurality of semiconductor compound crystal rods with uniform ratio and good performance.
  • the device provided by the present disclosure can further improve semiconductor synthesis and semiconductor doping processes.
  • the present disclosure provides a design in which horizontal boat containers are stacked in a closed reaction tube, and in particular, a unique design in which a bracket device is provided on a first layer of horizontal boat container, and a second layer of horizontal boat container is stacked on the bracket device, and With relatively high and low temperature control, the temperature is relatively independent. Compared with the traditional design, it is conducive to the development of new semiconductor manufacturing processes, new semiconductor synthesis methods, and new semiconductor products.
  • a semiconductor synthesis device applied to a horizontal Bridgeman method comprising a closed reaction tube, a first furnace body and a second furnace body,
  • the first furnace body and the second furnace body are connected by an intermediate pipe, and the reaction tube is placed in a furnace cavity defined by the first furnace body, the intermediate pipe, and the second furnace body.
  • a temperature control device is separately provided for each of the first furnace body and the second furnace body.
  • the reaction tube is provided with a plurality of horizontal boat containers, and the plurality of horizontal boat containers include a plurality of first-layer horizontal boat containers arranged at different positions in the reaction tube in a horizontal direction.
  • a support device is provided on at least one of the first-level horizontal boat containers, and a second-level horizontal boat container is stacked on the support device, wherein the support device is configured to support the second-level horizontal boat container, and A gap is provided between the first-layer horizontal boat container and the second-layer horizontal boat container.
  • the temperature control device includes a first temperature control device corresponding to the first furnace body, and has a 2-4 stage temperature control unit In order to provide heating below 1000 ° C, and a second temperature control device corresponding to the second furnace body, it has a 5-7 stage temperature control unit to provide heating above 1000 ° C.
  • bracket device is a bridge-shaped member, and two ends of the bridge-shaped member are respectively buckled to the horizontal boat container and the horizontal boat container.
  • the axial direction of the reaction tube is arranged on two side walls which are substantially parallel.
  • bracket device is made of a PBN material, or a layer of PBN material is deposited on a surface of a graphite material.
  • a synthesis device for gallium arsenide polycrystal comprising the semiconductor synthesis device according to any one of claims 1-20, the first furnace body is a low-temperature zone furnace body, and the second furnace The body is a high-temperature area furnace body, and a horizontal boat container filled with arsenic and a gallium container filled with gallium are respectively placed in the low-temperature area furnace and the high-temperature area furnace.
  • a horizontal boat container filled with arsenic and a gallium container filled with gallium are respectively placed in the low-temperature area furnace and the high-temperature area furnace.

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Abstract

一种半导体合成装置，包括密闭反应管（4）、第一炉体（1）和第二炉体（2），反应管（4）布置有多个水平舟容器，多个水平舟容器包括多个第一层水平舟容器（11），在第一层水平舟容器（11）的至少一个上设置有支架装置（13），在支架装置（13）上叠置一第二层水平舟容器（12），支架装置（13）设置为支撑所述第二层水平舟容器（12），并在第一层水平舟容器（11）和第二层水平舟容器（12）之间提供间隙。

Description

一种半导体合成装置和合成方法 技术领域
本公开涉及针对采用水平布里奇曼法的半导体制备装置和方法(水平舟生产法)的改进。
背景技术
水平布里奇曼法是由Bridgman研制成功的一种制备大面积定型薄片状晶体的方法，又称为水平舟法，简称为HB法。HB法应用相当广泛，在化合物半导体晶体的生长方面，尤其如此，另外还可以用于半导体材料的掺杂上。HB法是将生长晶体的原料或掺杂原料放在一种器皿中，器皿放入圆管中，抽真空后封闭管口；用定向凝固法或定向区熔法生长晶体或使用合适的半导体掺杂方法进行半导体的掺杂。
金敏等人介绍的水平定向凝固法合成砷化镓多晶(上海应用技术学院学报，2014年9月，187-190)，在一个由8段控单晶温组成的炉体中，分别有5段高温区、1段中温区，2段低温区。将砷和镓分别放置在石英舟中并安置于石英管的两端，石英管抽真空封焊后放入水平定向凝固炉中，并将镓的一端放在高温区，砷端处于低温区域。低温区温度控制在630℃左右，高温区温度控制在1250-1255℃，通过控制不同段的降温工艺，实现砷化镓多晶的定向凝固。
CN 107268085A公开了一种半绝缘砷化镓多晶掺碳的制备装置，包括一圆筒形的加热装置，所述加热装置的一端为源区，另一端为生长区，所述加热装置的控制温度从所述源区至所述生长区递增；所述加热装置内固定设置有一石英管，所述石英管内与所述源区相对应的位置相邻设置有用于盛放石墨粉的第一PBN舟和用于盛放第III-IV族氯化物、氟化物或氧化物的第二PBN舟，所述石英管内与所述生长区相对应的位置设有一用于盛放砷化镓多晶的第三PBN舟；所述石英管在反应时为真空密封状态。
公开内容
本公开的第一方面提供了一种应用于水平布里奇曼法的半导体合成装置，包括密闭反应管、第一炉体和第二炉体，其中，所述第一炉体和所述第二炉体由中间管道连接，所述反应管放置在由所述第一炉体、所述中间管道、所述第二炉体共同限定的炉腔中，对应所述第一炉体和第二炉体分别单独设置温度控制装置，其中，所述反应管布置有多个水平舟容器，所述多个水平舟容器包括在水平方向上布置于所述反应管内的不同位置处的多个第一层水平舟容器，在所述第一层水平舟容器的至少一个上设置有支架装置，在所述支架装置上叠置一第二层水平舟容器，其中，所述支架装置设置为支撑所述第二层水平舟容器，并在所述第一层水平舟容器和第二层水平舟容器之间提供间隙。
本公开的第二方面提供了一种砷化镓多晶的合成装置，包括本公开第一方面所述的装置，所述第一炉体为低温区炉体和所述第二炉体为高温区炉体，装有砷的水平舟容器和装有镓的水平舟容器分别放置在所述低温区炉体内和所述高温区炉体内，装有镓的水平舟容器设置为叠置，以在一次制备过程中提供多个砷化镓多晶棒。
本公开的第三方面提供了一种砷化镓多晶的合成方法，使用本公开第二方面所述的装置，其中，在叠置的水平舟中，上层水平舟容器的装料重量小于下层水平舟容器的装料重量。
附图说明
图1是本公开一实施例的反应装置示意图；
图2是本公开一实施例的反应装置示意图；
图3是本公开一实施例的反应装置示意图；
图4是本公开一实施例的反应装置示意图；
图5是本公开一实施例的反应装置示意图；
图6是本公开一实施例所用水平舟容器的投影示意图；
图7是本公开一实施例所用水平舟容器的投影示意图；
图8是本公开一实施例所用水平舟容器的投影示意图；
图9是本公开一实施例所用水平舟容器的横截面示意图；
图10是本公开一实施例所用水平舟容器的横截面示意图；
图11是本公开一实施例所用水平舟容器的俯视图；
图12是本公开一实施例所用支架的结构示意图；
图13是本公开一实施例所用支架的结构示意图。
具体实施方式
下文结合附图描述本公开的实施方式。通篇附图中采用相似的附图标记描述相似或相同的部件。这里披露的不同特征可以单独使用，或者彼此改变组合，没有规定将本公开限定于文中描述的特定组合。由此，所描述的实施方式不用于限定权利要求的范围。
说明中可能采用短语“在一实施方式中”、“在实施方式中”、“在一些实施方式中”，或者“在其他实施方式中”，分别可以各指根据本文披露的一个或多个相同或者不同的实施方式。
还需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种物品或者设备所固有的要素。在没有更多限制的情况下，由语句“包括一个……”限定的要素，并不排除在包括上述要素的物品或者设备中还存在另外的相同要素。
当前本领域普遍将水平舟容器水平方向布置于密闭反应管的不同位置，因反应管内部的空间有限，进一步限制了水平舟容器的布置方式。本领域未见在反应管中将水平舟叠置的空间布置方案，特别地，没有提出使水平舟稳定叠置的设计，以及控制叠置水平舟之间间隙的技术手段。
为了同时生产多个半导体晶棒，发明人设计了实现多个水平舟容 器叠置的构造，以期有效并稳定地控制叠置水平舟容器之间的空隙。进一步，多个水平舟容器叠置制得的多个半导体晶棒的均匀性品质仍有提高的空间。采用水平布里奇曼法合成晶棒时，由于热辐射等原因，高温区与低温区的温度不易控制，经常出现石英管变形和开裂等导致的多晶料氧化或砷泄露，以及多晶料尾部合成不完全等问题。
为了解决上述问题，本公开提出了不同技术方案。以下通过实施例的方式对不同技术方案进行详细描述。
[实施例1]
如图1所示，实施例1是应用于水平布里奇曼法的半导体合成装置，其中，该合成装置包括密闭反应管4、第一炉体1和第二炉体2，第一炉体1和第二炉体2由中间管道8连接，反应管4放置在由第一炉体1、中间管道8、第二炉体2共同限定的炉腔中，对应所述第一炉体1和第二炉体2分别单独设置温度控制装置9-1、9-2。
提供1000℃以下加热的温度控制装置9-1包括2-4段控温单元，提供高于1000℃加热的温度控制装置9-2包括5-7段控温单元。
控温单元用来控制炉体的温度，可包括加热单元和测温单元。加热单元可通过高频感应线圈或电阻加热炉加热，测温单元可通过热电偶进行。
密闭反应管4的左侧放置有第一层水平舟容器11，在第一层水平舟容器11上设置有支架装置13，在支架装置13上叠置第二层水平舟容器12。支架装置13设置为支撑第二层水平舟容器12，并在第一层水平舟容器11和第二层水平舟容器12之间限定出预设的间隙，以供反应物从被叠置的水平舟容器中进出。
密闭反应管4的右侧布置另外一个水平舟容器5。可以理解的是，水平舟容器5同样可以采用第一层水平舟容器11的构造，以便于部件的生产制造
在具体的应用中，水平舟中有反应物升华，以便与另外的水平舟中的反应物反应。
[实施例2]
类似于实施例1，不同之处在于，实施例2中共设置了4个水平舟容器，其中分为两组，两组水平舟容器都采取叠置的布置方式。
如图2所示，在密闭反应管4中的水平方向的两端布置两个第一层水平舟容器11，在两个第一层水平舟容器11上分别设置有支架装置13，在支架装置13上叠置第二层水平舟容器12。支架装置13设置为支撑第二层水平舟容器12，并在第一层水平舟容器11和第二层水平舟容器12之间提供间隙。
[实施例3]
类似于实施例1、2，如图3所示，在本公开实施例3中，在反应管4的水平方向布置三组水平舟容器，第一组为两个水平舟叠置，第一层水平舟容器11上设置有支架装置13，在支架装置13上叠置第二层水平舟容器12。另外两组水平舟容器5分别单独设置于水平方向的中间位置和右侧位置。可以理解的是，水平舟容器5同样可以采用第一层水平舟容器11的构造，以便于部件的生产制造。
[实施例4]
类似于实施例1、2、3，不同之处在于，实施例4提供了3组双层叠置的水平舟。如图4所示，在密闭反应管4中，于水平方向布置三个第一层水平舟容器11，在第一层水平舟容器11上分别设置有支架装置13，在支架装置13上分别叠置三个第二层水平舟容器12，其中，支架装置13设置为支撑第二层水平舟容器12，并在第一层水平舟容器11和第二层水平舟容器12之间提供预设间隙。
[实施例5]
如图5所示，实施例5装置应用于水平布里奇曼法砷化镓半导体制备，其中，该合成装置包括密闭反应管4、第一炉体1和第二炉体2，其中，第一炉体1和第二炉体2由中间管道8连接，反应管4放置在由第一炉体1、中间管道8、第二炉体2共同限定的炉腔中，对应所述 第一炉体1和第二炉体2分别单独设置温度控制装置9-1、9-2。
第二炉体2由6段控温组成，第一炉体1由3段控温组成。
控温单元用来控制炉体的温度，可包括加热单元和测温单元。加热单元可通过高频感应线圈或电阻加热炉加热，测温单元可通过热电偶进行。
用石英密闭反应管4密封的砷舟5和镓舟11、12分别放置在第一炉体1内和第二炉体2内。第二层镓舟12通过设置支架装置13叠置于第一层镓舟11上，第一层镓舟11与第二层镓舟12之间设定了一定间隙，以供反应物砷从被叠置的水平舟容器中进出。该设置可使得通过该实施例的装置一次制得两根砷化镓晶体棒。可以理解的是，虽然砷舟5和镓舟11采用不同的附图编号，但是，砷舟5和镓舟11可以采用相类似的结构，以便于部件的生产制造。
通过不同的设置和组合，本领域技术人员根据需要和目标产物的不同，可以反在应管中放置更多种反应产物，或者，配合更合理的布置方式和控制加热方式。
本公开的装置通过水平舟容器的叠置设置，可一次同时合成多个晶棒，提高了生产效率，降低了生产成本；为了提高所合成产品的品质，本公开进一步通过在加热方式上采用双炉的加热结构，将低温区和高温区分别用炉体进行温度控制，从而使得合成半导体时温度易于控制，实现了炉体温度的精确控制，籍此，一次合成的多个半导体如多晶或单晶的配比均匀，合格率高。
对于实施例1-5的进一步的变化实施方式如下。
[炉体]
可选地，在所述中间管道8的外周包覆有保温材料10。由于高温区与低温区之间设置适当的保温措施，使得蒸发的组分得以完全与其他组分反应，得到配比均匀、性能良好的半导体化合物。
可选地，第一炉体1和第二炉体2至少之一的内侧壁进一步设置间隔层3，以在间隔层3包围空间内限定均匀加热的炉腔。该设置可以 用来改善内部热场均匀性，以更有利于合成的半导体产品配比的均匀性和进一步提高合格率。
可选地，间隔层3构造为选自包括以下的组：石英管、碳化硅管、莫来石管以及其组合套管。优选为碳化硅管、莫来石管或其组合套管，该构造的间隔层更耐用，同时可更有效地降低内部径向温度的不均匀性。
可选地，密闭反应管4在第一炉体1和第二炉体2中放置时，与内侧壁之间由间隔层3隔开。由此，可以进一步改善内部热场均匀性，更有利于合成的半导体产品配比的均匀性和进一步提高合格率。
可选地，第一炉体1和第二炉体2之间的间距为15-20cm。
两个炉室之间隔开一定距离，可避免由于热扩散和热辐射等原因导致的难以进行低温区的温度控制。然而，该距离太长如大于20cm，易造成中部过冷，太短如小于15cm，达不到低温区和高温区的温度控制。通过研究发现，上述范围的间距可实现低温区和高温区的温度控制同时使得中部连接处温度始终在合适范围内，保证反应顺利进行，获得配比均匀的半导体产品。
可选地，在中间管道8的外周包覆的保温材料10为低密度保温材料，其包覆厚度为3cm-5cm。该材料的厚度太薄，不能有效保温，太厚浪费原料，因此选择上述范围即可满足保温要求同时使得成本最小化。
所述低密度保温材料为由包含二氧化硅和/或氧化铝的组分制得的材料。保温材料也称为保温隔热材料，是指对热流具有显著阻抗性的材料或材料复合体，保温隔热材料的共同特点是轻质、疏松，呈多孔状或纤维状，以其内部不流动的空气阻隔热的传导其中无机材料有不燃、使用温度宽、耐化学腐蚀性较好等。本公开使用的保温材料例如为包含二氧化硅组分制得的保温材料，包含氧化铝组分制得的保温材料，包含二氧化硅和氧化铝组分制得的保温材料。具体制备方法及产品可参照本领域已知的方法，如CN 101671158A、CN102795781A等公开的方法制备的产品。
可选地，制备装置还包括第一炉体1和第二炉体2两端的保温密 封材料板7。保温密封材料板7可例如为保温棉板、硅酸纤维板等。第一炉体和第二炉体的保温密封材料可以使用相同材料也可以使用不同材料，例如第一炉室的保温材料可使用适合于提供较低温度炉体的保温材料，第二炉室的保温材料可使用适合于提供较高温度炉体的保温材料。
[反应管]
实施方式中使用的反应管可为石英反应管，尺寸可为本领域一般使用的尺寸，如具有80mm的内径。其中放置的水平舟容器的内径与反应管相适应，可稍小于反应管的内径，深度可根据放置的层数设置，如设置两层，则水平舟容器的深度约为40mm以下，例如20-35mm，具体为24mm、28mm、31mm、34mm等。
[水平舟]
HB法是将生长单晶的原料放在一种器皿中，器皿放入圆管中，抽真空后封闭管口，这种器皿一般称之为“舟”。目前，从用途上分，有合成舟和拉晶舟。合成舟是用于合成多晶的；而用于生长单晶的称之为拉晶舟。
合成舟的敞口部可为长方形，可见图5所示的投影示意图；或一端为半圆形的，见图6所示的投影示意图；或者两端均为半圆形，见图7所示的投影示意图。半圆形舟应用了几十年，其最大特点是加工容易，圆形管一破两半，再加上舟头和/或舟尾即可。合成舟或拉晶舟的主体截面一般采用拱形，见图8所示。当然，也可为矩形，如图9所示，或本领域使用的其他形状。
投影示意图中左上图为俯视图，左下图为主视图，右上图为左视图。
单晶生长用舟在多晶合成舟的基础上增加籽晶区和放肩部，构成如下：最前端的叫籽晶腔，籽晶腔有方形、矩形、半圆形等多种；在主体和籽晶腔之间的部分叫放肩部，作用是平滑联接籽晶腔和舟的主体。中间是单晶生长舟的主体部分，最后是舟尾。具体可参见图10所示，图中z1-z4依次为籽晶腔部分、放肩部分、等径部分(也即主体部分)以及舟尾部分。
[支架装置]
可选地，支架装置13可以为单独设置的部件。换言之，支架装置13是与水平舟容器相分离的独立部件。支架装置13可以组装在水平舟容器上，以为安装于其上的水平舟容器提供支持。可以在装料操作结束后将支架装置13安装于水平舟容器，因此，单独设置的支架装置不会影响水平舟容器的装料操作。可选地，支架装置13可以与水平舟容器一体设置，例如，支架装置13与第一层水平舟11的上部或者第二层水平舟12的下部一体设置。一体设置更方便使用，有利于实现工业化生产，且使用时也更有利于结构的稳定。
可选地，水平舟容器包括主体部分，所述主体部分设置在水平舟容器大致中部，该主体部分的横截面为大致U形。
可选地，支架装置13设置为桥状部件，桥状部件两端分别搭扣于水平舟容器(例如第一层水平舟11)的与反应管4的轴向大致平行布置的两个侧壁上。采用搭扣接合，可以方便地组装水平舟容器与支架装置，简化装配步骤。
可选地，支架装置13的中部设置有下凹的弧状部20，以与第二层水平舟容器12的底部形状相符。具体地，如图12所示，其示出支架的结构示意图。在垂直于反应管4的轴向的平面内，支架装置13的中部设置有下凹的弧状部20。通过支架装置13的弧状部20与水平舟容器的底部相抵接，为水平舟容器提供稳定的支撑。可选地，如图11、图12中所示，支架装置13还包括水平部30，水平部30的厚度为2-3mm，弧状部20的厚度为2.5-3.5mm，弧状部20的厚度稍微大于水平部的厚度，例如，弧状部20的厚度较水平部30的厚度大0.2-0.5mm。此种设置方式更有利于稳定地支撑上层放置的舟，使支架装置更耐用，且有利于反应充分顺利进行。
可选地，弧状部20的弧长占放置于该支架上的水平舟容器外表面长度的1/4-1/2，优选为1/3。
可选地，支架装置13还包括两个凹槽10，凹槽10用于将支架3搭扣于水平舟容器2上。凹槽10可设置在水平部30靠近端部的位置，如图11、图12中所示。通过凹槽的设置，支架装置13可以稳定地与 下层水平舟容器(例如第一层水平舟容器12)相接合，二者形成稳定的组装体。
为了使得支架支撑的上层水平舟容器更稳固，可选地，凹槽10的深度为1-1.5mm，更有利地是1.2-1.4mm，最有利地是约1.3mm，使得搭扣更稳固，两个凹槽的深度相同。
本公开中使用的支架13的宽度、厚度及凹槽10相关尺寸可根据实际需要进行调整。凹槽10的长度可根据水平舟容器的壁厚设定，刚好卡合或者稍大于壁厚均可。
本公开中支架的长度可根据支架所跨越的下层水平舟容器的宽度而定，并且以方便叠层舟更好的在石英管内部的移动为考虑。支架的一种具体形式为桥梁式支架。
可选地，一个水平舟上设置支架装置13的数量为1、2、3、4个等，可选为2个以上，尤其为3个。
可选地，实施方式的反应装置用于半导体合成或半导体掺杂反应。
可选地，反应装置用于砷化镓多晶合成或砷化镓单晶合成，可选地，用于砷化镓多晶合成。
可选地，支架装置由PBN(热解氮化硼)材料制成，或者是在石墨材料的表面沉积一层PBN(热解氮化硼)材料。选用支架装置材料需要考虑不在反应过程中引进杂质。
本公开的一个实施例还提供了一种砷化镓多晶的合成装置，第一炉体为低温区炉体以及第二炉体为高温区炉体，装有砷的水平舟容器和装有镓的水平舟容器分别放置在低温区炉体内和高温区炉体内，装有镓的水平舟容器设置为叠置(例如在第一水平舟容器11上叠置第二水平舟容器12)，以在一次制备过程中提供多个砷化镓多晶棒。
本公开的一个方面还提供了一种砷化镓多晶的合成方法，使用本公开提供砷化镓多晶的合成装置，其中，在叠置的水平舟中，上层水平舟容器的装料重量小于下层水平舟容器的装料重量。反应时密闭反应管抽真空或者充惰性气体进行保护。
可选地，下层水平舟容器的装料重量为上层水平舟容器的装料重量的1-1.5倍，更有利地是1.3倍左右。
为了使本领域技术人员更好的理解本公开的技术方案，下面以砷化镓的多晶合成为例进行说明。
为了验证本公开为达成预订目的所采取的技术手段及功效，按下述实施方案重复生产实验3次，具体的实施过程详细如下：
(1)用氢氟酸、硝酸的混合酸及去离子水将石英安瓿、PBN舟及PBN桥等物料清洗干净，并用乙醇脱水风干备用；
(2)将清洗干净的PBN舟放入干净的石英烤炉内进行烘烤，烘烤温度为600-900℃左右，烘烤时间为2-4小时，然后自然冷却至室温待用；
(3)称取约2000g的6N镓放置在一个PBN舟中，并将其放入石英安瓿开口的端部，并在该舟上均匀的放置3根PBN桥，另外称取约1500g的6N镓放置在另外一个PBN舟中，并将其放在装有PBN桥的舟上，并同时一起推入石英安瓿底部；称取约3680g的6N砷放置在一个PBN舟中，并将该舟放入洗干净的石英安瓿端口，最后盖上石英帽；
(4)将安装好的石英安瓿移至烤炉上，抽真空，并加热至温度在150-300℃，保温3-4小时后关闭电源，并进行真空密封焊接，并自然冷却至室温；
(5)将装有砷和镓并密封好的石英安瓿装入HB水平炉体内，装砷的舟一端放在低温区炉内，装镓的舟的一端放在高温区炉内，两端用保温棉进行密封；
(6)按预设的加热程序加热，将低温区的温度控制在620-650℃左右，高温区炉体的温度在1250-1255℃，并保温1-3h，待反应完全后，按预设的降温程序进行降温至室温；
(7)从炉体内取出石英安瓿，从砷端将石英管切开，将合成好的半圆形多晶棒取出并进行检测。
三次合成出的多晶棒表面光泽，致密、无孔洞、无富镓、合成比例佳；每炉任取1条多晶棒取头尾部片进行测试，三次合成的多晶的合格率和电性能参数具体如下表1中所示。
表1
Figure PCTCN2018101452-appb-000001
本公开通过水平舟容器叠层放置的构造，在不增加反应管容积的情况下，可一次允许制作多根晶棒，提高了生产效率，降低了成本。同时配合通过第一炉体和第二炉体分别单独设置温度控制装置，实现了有效地独立控制高温区与低温区的温度，减少不期望的热辐射影响，以及，防止因石英管变形和开裂等导致的多晶料氧化或砷泄露；从表1所示数据可以看出，得到的砷化镓晶棒配比均匀、性能良好。
本公开提出有利于上层舟放置的支架构造。基于此，本公开提出将水平舟容器叠层放置，特别适合改进HB法的合成装置。本公开的多个水平舟容器叠层放置的构造稳定，可使反应正常地顺利进行，提高生产效率，降低成本。更为有利的是，在不增加反应管容积的情况下，本公开可一次制作多根晶棒。此外，也可以改善采用更多种化学反应组分的应用。
为了进一步优化利用多层水平舟容器制得的晶棒的品质，本公开的装置通过第一炉体和第二炉体分别单独设置温度控制装置，实现了有效地独立控制高温区与低温区的温度，减少不期望的热辐射影响，以及，防止因石英管变形和开裂等导致的多晶料氧化或砷泄露，从而得到配比均匀、性能良好的多个半导体化合物晶棒。
此外，本公开提供的装置，可进一步改善半导体的合成、半导体掺杂工艺。本公开提供了在密闭反应管中将水平舟容器叠置的设计，特别提供了在第一层水平舟容器上设置支架装置，在支架装置上叠置第二层水平舟容器的独特设计，并且配合高温区与低温区的温度相对 较为独立的控制。相比传统设计，有利于开发新的半导体制备工艺，新的半导体合成方法，以及新的半导体产品。
本公开至少包括如下的概念：
概念1.一种半导体合成装置，其应用于水平布里奇曼法，包括密闭反应管、第一炉体和第二炉体，
其中，所述第一炉体和所述第二炉体由中间管道连接，所述反应管放置在由所述第一炉体、所述中间管道、所述第二炉体共同限定的炉腔中，对应所述第一炉体和第二炉体分别单独设置温度控制装置，
其中，所述反应管布置有多个水平舟容器，所述多个水平舟容器包括在水平方向上布置于所述反应管内的不同位置处的多个第一层水平舟容器，在所述第一层水平舟容器的至少一个上设置有支架装置，在所述支架装置上叠置一第二层水平舟容器，其中，所述支架装置设置为支撑所述第二层水平舟容器，并在所述第一层水平舟容器和第二层水平舟容器之间提供间隙。
概念2.根据概念1所述的半导体合成装置，在所述中间管道的外周包覆有保温材料。
概念3.根据概念1或2所述的半导体合成装置，其中，第一炉体和所述第二炉体至少之一的内侧壁进一步设置间隔层，以在间隔层包围空间内限定均匀加热的炉腔。
概念4.根据概念3所述的半导体合成装置，其中，所述间隔层构造选自包括以下的组：石英管、碳化硅管、莫来石管以及其组合套管。
概念5.根据概念3所述的半导体合成装置，其中，所述密闭反应管在第一炉体和所述第二炉体中放置时，与所述内侧壁之间由所述间隔层隔开。
概念6.根据概念1-5中任一项所述的半导体合成装置，其中，所述温度控制装置包括对应所述第一炉体的第一温度控制装置，其具有2-4段控温单元以提供1000℃以下的加热，以及，对应所述第二炉体的第二温度控制装置，其具有5-7段控温单元以提供高于1000℃的 加热。
概念7.根据概念1-6中任一项所述的半导体合成装置，其中，所述第一炉体和所述第二炉体之间的间距为15-20cm。
概念8.根据概念2-7中任一项所述的半导体合成装置，其中，在所述中间管道的外周包覆的保温材料为低密度保温材料，其包覆厚度为3cm-5cm。
概念9.根据概念1-8中任一项所述的半导体合成装置，其中，所述支架装置为单独设置的部件。
概念10.根据概念1-8中任一项所述的半导体合成装置，其中，所述支架装置与水平舟容器一体设置。
概念11.根据概念10所述的半导体合成装置，其中，所述支架装置与第一层水平舟容器的上部或者第二层水平舟容器的下部一体设置。
概念12.根据概念1-11中任一项所述的半导体合成装置，其中，所述水平舟容器包括主体部分，所述主体部分设置在水平舟容器大致中部，该主体部分的横截面为大致U形。
概念13.根据概念1-12中任一项所述的半导体合成装置，其中，所述支架装置为桥状部件，所述桥状部件两端分别搭扣于所述水平舟容器的与所述反应管的轴向大致平行布置的两个侧壁上。
概念14.根据概念13所述的半导体合成装置，其中，所述支架装置的中部设置有下凹的弧状部，以与第二层水平舟容器的底部形状相符。
概念15.根据概念14所述的半导体合成装置，其中，所述弧状部的弧长占放置于该支架上的水平舟容器外表面长度的1/4-1/2，优选为1/3。
概念16.根据概念1-15中任一项所述的半导体合成装置，其中，所述支架还包括两个凹槽，所述凹槽用于将支架搭扣于水平舟容器上。
概念17.根据概念1-16中任一项所述的半导体合成装置，其中，所述支架装置的数量为2个以上。
概念18.根据概念1-17中任一项所述的半导体合成装置，其中， 所述支架装置由PBN材料制成，或者是在石墨材料的表面沉积一层PBN材料。
概念19.根据概念1-18中任一项所述的半导体合成装置，其中，所述装置用于半导体合成或半导体掺杂。
概念20.根据概念19所述的半导体合成装置，其中，所述反应装置用于砷化镓多晶合成或砷化镓单晶合成。
概念21.一种砷化镓多晶的合成装置，包括权利要求1-20中任一项所述的半导体合成装置，所述第一炉体为低温区炉体，以及，所述第二炉体为高温区炉体，装有砷的水平舟容器和装有镓的水平舟容器分别放置在所述低温区炉体内和所述高温区炉体内，装有镓的水平舟容器设置为叠置，以在一次制备过程中提供多个砷化镓多晶棒。
概念22.根据概念21所述的合成装置，其中，所述高温区炉体由6段控温组成，所述低温区炉体由3段控温组成。
概念23.一种砷化镓多晶的合成方法，使用权利要求21或22中任一项所述的装置，其中，在叠置的水平舟容器中，上层水平舟容器的装料重量小于下层水平舟容器的装料重量。
可以理解的是，以上实施例及其优选/可选的实例仅仅是为了说明本公开的原理而采用的示例性实施方式，然而本公开并不局限于此。对于本领域内的普通技术人员而言，在不脱离本公开的精神和实质的情况下，可以做出各种变型和改进，这些变型和改进也视为本公开的保护范围。

Claims (23)

  1. 一种半导体合成装置，其应用于水平布里奇曼法，包括密闭反应管、第一炉体和第二炉体，
    其中，所述第一炉体和所述第二炉体由中间管道连接，所述反应管放置在由所述第一炉体、所述中间管道、所述第二炉体共同限定的炉腔中，对应所述第一炉体和第二炉体分别单独设置温度控制装置，
    其中，所述反应管布置有多个水平舟容器，所述多个水平舟容器包括在水平方向上布置于所述反应管内的不同位置处的多个第一层水平舟容器，在所述第一层水平舟容器的至少一个上设置有支架装置，在所述支架装置上叠置一第二层水平舟容器，其中，所述支架装置设置为支撑所述第二层水平舟容器，并在所述第一层水平舟容器和第二层水平舟容器之间提供间隙。
  2. 根据权利要求1所述的半导体合成装置，在所述中间管道的外周包覆有保温材料。
  3. 根据权利要求1或2所述的半导体合成装置，其中，第一炉体和所述第二炉体至少之一的内侧壁进一步设置间隔层，以在间隔层包围空间内限定均匀加热的炉腔。
  4. 根据权利要求3所述的半导体合成装置，其中，所述间隔层构造选自包括以下的组：石英管、碳化硅管、莫来石管以及其组合套管。
  5. 根据权利要求3所述的半导体合成装置，其中，所述密闭反应管在第一炉体和所述第二炉体中放置时，与所述内侧壁之间由所述间隔层隔开。
  6. 根据权利要求1-5中任一项所述的半导体合成装置，其中，所述温度控制装置包括对应所述第一炉体的第一温度控制装置，其具有 2-4段控温单元以提供1000℃以下的加热，以及，对应所述第二炉体的第二温度控制装置，其具有5-7段控温单元以提供高于1000℃的加热。
  7. 根据权利要求1-6中任一项所述的半导体合成装置，其中，所述第一炉体和所述第二炉体之间的间距为15-20cm。
  8. 根据权利要求2-7中任一项所述的半导体合成装置，其中，在所述中间管道的外周包覆的保温材料为低密度保温材料，其包覆厚度为3cm-5cm。
  9. 根据权利要求1-8中任一项所述的半导体合成装置，其中，所述支架装置为单独设置的部件。
  10. 根据权利要求1-8中任一项所述的半导体合成装置，其中，所述支架装置与水平舟容器一体设置。
  11. 根据权利要求10所述的半导体合成装置，其中，所述支架装置与第一层水平舟容器的上部或者第二层水平舟容器的下部一体设置。
  12. 根据权利要求1-11中任一项所述的半导体合成装置，其中，所述水平舟容器包括主体部分，所述主体部分设置在水平舟容器大致中部，该主体部分的横截面为大致U形。
  13. 根据权利要求1-12中任一项所述的半导体合成装置，其中，所述支架装置为桥状部件，所述桥状部件两端分别搭扣于所述水平舟容器的与所述反应管的轴向大致平行布置的两个侧壁上。
  14. 根据权利要求13所述的半导体合成装置，其中，所述支架装置的中部设置有下凹的弧状部，以与第二层水平舟容器的底部形状相符。
  15. 根据权利要求14所述的半导体合成装置，其中，所述弧状部的弧长占放置于该支架上的水平舟容器外表面长度的1/4-1/2，优选为1/3。
  16. 根据权利要求1-15中任一项所述的半导体合成装置，其中，所述支架还包括两个凹槽，所述凹槽用于将支架搭扣于水平舟容器上。
  17. 根据权利要求1-16中任一项所述的半导体合成装置，其中，所述支架装置的数量为2个以上。
  18. 根据权利要求1-17中任一项所述的半导体合成装置，其中，所述支架装置由PBN材料制成，或者是在石墨材料的表面沉积一层PBN材料。
  19. 根据权利要求1-18中任一项所述的半导体合成装置，其中，所述装置用于半导体合成或半导体掺杂。
  20. 根据权利要求19所述的半导体合成装置，其中，所述反应装置用于砷化镓多晶合成或砷化镓单晶合成。
  21. 一种砷化镓多晶的合成装置，包括权利要求1-20中任一项所述的半导体合成装置，所述第一炉体为低温区炉体，以及，所述第二炉体为高温区炉体，装有砷的水平舟容器和装有镓的水平舟容器分别放置在所述低温区炉体内和所述高温区炉体内，装有镓的水平舟容器设置为叠置，以在一次制备过程中提供多个砷化镓多晶棒。
  22. 根据权利要求21所述的合成装置，其中，所述高温区炉体由6段控温组成，所述低温区炉体由3段控温组成。
  23. 一种砷化镓多晶的合成方法，使用权利要求21或22中任一项所述的装置，其中，在叠置的水平舟容器中，上层水平舟容器的装料重量小于下层水平舟容器的装料重量。
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