CN113005426A - Preparation method and equipment of pyrolytic boron nitride - Google Patents
Preparation method and equipment of pyrolytic boron nitride Download PDFInfo
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- CN113005426A CN113005426A CN202110190423.4A CN202110190423A CN113005426A CN 113005426 A CN113005426 A CN 113005426A CN 202110190423 A CN202110190423 A CN 202110190423A CN 113005426 A CN113005426 A CN 113005426A
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000007740 vapor deposition Methods 0.000 claims abstract description 116
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 28
- 239000010439 graphite Substances 0.000 claims abstract description 28
- 230000001681 protective effect Effects 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 23
- 238000004321 preservation Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 68
- 238000005086 pumping Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000000151 deposition Methods 0.000 claims description 10
- 230000008021 deposition Effects 0.000 claims description 10
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 claims description 10
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 5
- 238000000605 extraction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000000463 material Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 229910052582 BN Inorganic materials 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 229910015844 BCl3 Inorganic materials 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001451 molecular beam epitaxy Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C23C16/303—Nitrides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/458—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber
- C23C16/4581—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for supporting substrates in the reaction chamber characterised by material of construction or surface finish of the means for supporting the substrate
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/54—Apparatus specially adapted for continuous coating
Abstract
The invention provides a pyrolytic boron nitride preparation device, which comprises: vapor deposition stove and set up the graphite jig in the vapor deposition stove still includes: the heating system and the driving system are used for driving the graphite mould to rotate; an air extraction system, an air intake system; a cooling jacket disposed on an outer surface of the vapor deposition furnace. A preparation method of pyrolytic boron nitride comprises the following steps: putting the mould into a reaction chamber in a vapor deposition furnace, vacuumizing, heating; carrying out heat preservation operation when the vacuum degree and the temperature in the reaction chamber respectively reach preset values, and introducing raw material gas and protective gas; rotating the mold to react for a period of time; only introducing protective gas for a period of time; introducing raw material gas in proportion to react for a period of time. The preparation process of the pyrolytic boron nitride product with high quality, environmental protection and low cost can be achieved, and the effect of producing the pyrolytic boron nitride product with stability and high quality is achieved.
Description
Technical Field
The invention relates to a preparation method and equipment of boron nitride, in particular to a preparation method and equipment of pyrolytic boron nitride.
Background
Since the 70 s of the 20 th century, novel inorganic nonmetallic material Pyrolytic Boron Nitride (PBN) materials have been widely applied in various fields such as metallurgical manufacturing, aerospace, electronic devices, chemical production, medical appliances and the like. Pyrolytic Boron Nitride (PBN) is used as a special ceramic material and has the excellent properties of high thermal conductivity, high mechanical strength, good electrical insulation, strong chemical inertness, no toxicity and the like. This makes the boron nitride material very suitable for use as crucibles, high temperature fixtures, substrates for electronic components, dielectrics, electrical vacuums, and the like.
Pyrolytic boron nitride is an ideal container for elemental purification, compound and compound semiconductor crystal growth. The pyrolytic boron nitride crucible prepared by the chemical vapor deposition method is widely applied to crucibles for OLED manufacturing, molecular beam epitaxy crucibles, compound semiconductor single crystal growth crucibles, polycrystal synthesis reaction vessels, MOCVD heaters, satellite communication traveling-wave tubes and the like because the pyrolytic boron nitride crucible has compact surface, good air tightness, high temperature resistance, acid resistance, alkali resistance, salt resistance and organic reagents, and is non-wetting and non-reacting with most materials such as molten metal, semiconductors and the like at high temperature. With the rapid development of the semiconductor industry in recent years, a large number of normalized, multi-variety and high-quality pyrolysis PBN crucibles are urgently required by the technologies such as GaAs single crystal, MBE, OLED and the like. Currently, pyrolytic PBN has been widely used in fields related to element purification, compound and compound semiconductor crystal growth and demand is increasing.
In the prior art, in the production of pyrolytic boron nitride, the PBN is prepared by chemical vapor deposition using BCl3 and NH3 as raw materials. The deposition temperature is high (above 1900 ℃), the flow and proportion of BCl3 and NH3 need to be strictly controlled, the requirement on process stability is high, the process control difficulty is high, a large amount of NH4Cl powder byproducts and HCl tail gas with strong corrosiveness are generated in the production process, and the damage to production equipment, personnel and environment is serious. In addition, the change of the process parameters such as temperature, pressure, gas flow, raw material gas concentration and the like has great influence on the deposition of the pyrolytic boron nitride, and the tiny fluctuation can cause the final pyrolytic boron nitride material to have the defects of cracking, layering and the like.
Disclosure of Invention
In view of the above disadvantages of the existing boron nitride preparation method and equipment, the invention provides a pyrolytic boron nitride preparation method and equipment, which can meet the requirements of high-quality, environment-friendly and low-cost pyrolytic boron nitride product preparation process, thereby realizing the effect of stable and high-quality pyrolytic boron nitride product production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production apparatus for pyrolytic boron nitride, comprising: vapor deposition stove and set up the graphite jig in the vapor deposition stove still includes:
the heating system is used for heating the vapor deposition furnace to a vapor deposition temperature;
the driving system is used for driving the graphite mould to rotate;
the air pumping system is used for vacuumizing the vapor deposition furnace and maintaining the vacuum degree;
the gas inlet system is used for mixing raw material gases and feeding the vapor deposition furnace;
a cooling jacket disposed on an outer surface of the vapor deposition furnace for cooling the outer surface of the vapor deposition furnace.
According to one aspect of the invention, the equipment for preparing pyrolytic boron nitride further comprises a filtering and cooling system, wherein the filtering and cooling system is used for cooling the gas pumped out by the gas pumping system.
According to one aspect of the present invention, the heating system includes a power source, an electrode disposed at a bottom of the vapor deposition furnace, and a heater disposed within the vapor deposition furnace, the electrode being electrically connected to the power source and the heater, respectively.
According to one aspect of the invention, the driving system comprises a motor, a speed reducer arranged on the vapor deposition furnace and a rotating shaft arranged in the vapor deposition furnace, the graphite mold is arranged on the rotating shaft, a power output shaft of the motor is arranged in a power input end of the speed reducer, and the rotating shaft is arranged in a power output end of the speed reducer.
According to one aspect of the invention, the air pumping system comprises a rough pumping device and a fine pumping device which are respectively used for vacuumizing the vapor deposition furnace before the reaction is started and stabilizing the vacuum degree in the vapor deposition furnace during the reaction.
According to one aspect of the invention, the vapor deposition furnace is provided with a thermocouple, an optical infrared thermometer and a vacuum gauge.
According to one aspect of the invention, the equipment for preparing pyrolytic boron nitride further comprises an air inlet system, wherein the air inlet system comprises an air inlet cabinet, an air inlet control module arranged in the air inlet cabinet and a mixing tank connected with the air inlet control module, and an outlet of the mixing tank is communicated with an air inlet of the vapor deposition furnace.
A preparation method of pyrolytic boron nitride comprises the following steps:
putting the mould into a reaction chamber in the vapor deposition furnace, and vacuumizing and heating the reaction chamber in the vapor deposition furnace;
carrying out heat preservation operation when the vacuum degree and the temperature in the reaction chamber respectively reach preset values, and introducing raw material gas and protective gas according to a preset proportion;
maintaining a certain vacuum degree and temperature, rotating the mold to react for a period of time to generate a precoating layer on the mold;
only introducing protective gas for a period of time;
keeping a certain vacuum degree and temperature, and proportionally introducing raw material gas to react for a period of time to obtain the pyrolytic boron nitride with the precoat.
According to one aspect of the invention, the steps of placing the mold into a reaction chamber in the vapor deposition furnace, vacuumizing the reaction chamber in the vapor deposition furnace and heating the reaction chamber by raising the temperature are as follows: the graphite mold is arranged in the center of a reaction chamber of a vapor deposition furnace, the vapor deposition furnace is vacuumized to the vacuum degree of more than 10Pa through rough pumping equipment in an air pumping system, the deposition furnace is continuously heated to the temperature of 1800-1900 ℃ through a heating system, and meanwhile, the surface of the vapor deposition furnace is cooled.
According to one aspect of the invention, the step of performing heat preservation operation when the vacuum degree and the temperature in the reaction chamber respectively reach preset values, and introducing the raw material gas and the protective gas according to a preset proportion specifically comprises the following steps: when the temperature reaches 1800-1900 ℃, the vacuum degree reaches 10Pa and the temperature is stabilized for 1hr, introducing protective gas into the vapor deposition furnace, and simultaneously introducing raw material gases of ammonia and boron chloride into the vapor deposition furnace according to the volume ratio of 2: 1.
According to one aspect of the invention, the maintaining of the vacuum and the temperature, and the rotating mold reacting for a period of time to form the precoat layer on the mold are specifically: keeping the temperature in the reaction chamber at 1800-1900 ℃ and the vacuum degree at 10-100 Pa, and driving the graphite mold to rotate through a driving system to enable the gas in the reaction chamber to react for 1-2hr so as to generate a pyrolytic boron nitride precoat on the graphite mold.
According to one aspect of the invention, the period of time for which only the protective gas is introduced is specifically: the temperature in the vapor deposition furnace is kept between 1800 ℃ and 2000 ℃ through a heating system, and nitrogen is introduced as a protective gas and a carrier gas within 1 hr.
According to one aspect of the invention, the pyrolytic boron nitride with the precoat layer is obtained by maintaining a certain vacuum degree and temperature and introducing raw material gas in proportion for reaction for a period of time, and the pyrolytic boron nitride with the precoat layer is specifically: keeping 1800-2000 ℃ in the vapor deposition furnace through a heating system, keeping the vacuum degree of 50-100 Pa in the vapor deposition furnace through fine pumping equipment in a pumping system, and introducing boron chloride into the vapor deposition furnace according to the volume ratio of 2: 1.
According to one aspect of the invention, the method for preparing pyrolytic boron nitride further comprises the following steps: and closing the heating system to stop heating the vapor deposition furnace, gradually reducing the temperature in the vapor deposition furnace through the water-cooling jacket, and taking out the product when the temperature of the product reaches the room temperature.
The implementation of the invention has the advantages that:
the invention provides a pyrolytic boron nitride preparation device, which comprises: vapor deposition stove and set up the graphite jig in the vapor deposition stove still includes: the heating system is used for heating the vapor deposition furnace to a vapor deposition temperature; the driving system is used for driving the graphite mould to rotate; the air pumping system is used for vacuumizing the vapor deposition furnace and maintaining the vacuum degree; the gas inlet system is used for mixing raw material gases and feeding the vapor deposition furnace; a cooling jacket disposed on an outer surface of the vapor deposition furnace for cooling the outer surface of the vapor deposition furnace. A preparation method of pyrolytic boron nitride comprises the following steps: putting the mould into a reaction chamber in the vapor deposition furnace, and vacuumizing and heating the reaction chamber in the vapor deposition furnace; carrying out heat preservation operation when the vacuum degree and the temperature in the reaction chamber respectively reach preset values, and introducing raw material gas and protective gas according to a preset proportion; maintaining a certain vacuum degree and temperature, rotating the mold to react for a period of time to generate a precoating layer on the mold; only introducing protective gas for a period of time; keeping a certain vacuum degree and temperature, and proportionally introducing raw material gas to react for a period of time to obtain the pyrolytic boron nitride with the precoat. The preparation process of the pyrolytic boron nitride product with high quality, environmental protection and low cost can be achieved, and the effect of producing the pyrolytic boron nitride product with stability and high quality is achieved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a pyrolytic boron nitride preparation method according to the present invention;
fig. 2 is a schematic structural diagram of a pyrolytic boron nitride preparation apparatus according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
as shown in fig. 1, a method for preparing pyrolytic boron nitride, the method for preparing pyrolytic boron nitride comprises the following steps:
s1, placing the mould into a reaction chamber in the vapor deposition furnace, and vacuumizing and heating the reaction chamber in the vapor deposition furnace;
in the specific implementation, the graphite mold is arranged in the center of a reaction chamber of the vapor deposition furnace, the vapor deposition furnace is vacuumized to the vacuum degree of more than 10Pa by rough pumping equipment in an air pumping system, the deposition furnace is continuously heated by a heating system to the temperature of 1800-1900 ℃, and the outer surface of the vapor deposition furnace is cooled by a water cooling system.
S2, performing heat preservation operation when the vacuum degree and the temperature in the reaction chamber reach preset values respectively, and introducing raw material gas and protective gas according to a preset proportion;
in the specific implementation, when the temperature reaches 1800-1900 ℃, the vacuum degree reaches 10Pa and the temperature is stabilized for 1hr, nitrogen is used as protective gas and carrier gas to be introduced into the vapor deposition furnace, and simultaneously, raw material gases of ammonia and boron chloride are introduced into the vapor deposition furnace according to the volume ratio of 2: 1.
S3: maintaining a certain vacuum degree and temperature, rotating the mold to react for a period of time to generate a precoating layer on the mold;
in specific implementation, the temperature in the reaction chamber is kept at 1800-1900 ℃ and the vacuum degree is kept at 10-100 Pa, the graphite mold is driven to rotate by the driving system, so that the gas in the reaction chamber reacts for 1-2hr, and the pyrolytic boron nitride precoat is generated on the graphite mold.
S4, only introducing protective gas for a period of time;
in the specific implementation, the heating system is used for keeping the temperature in the vapor deposition furnace at 1800-2000 ℃, the fine pumping equipment in the pumping system is used for keeping the vacuum degree in the vapor deposition furnace at 50Pa-100Pa, and nitrogen is introduced.
And S5, keeping a certain vacuum degree and temperature, and proportionally introducing raw material gas to react for a period of time to obtain the pyrolytic boron nitride with the precoat.
In the specific implementation, the heating system is used for keeping the temperature in the vapor deposition furnace at 1800-2000 ℃, the fine pumping equipment in the pumping system is used for keeping the vacuum degree in the vapor deposition furnace at 50Pa-100Pa, and after 1hr of nitrogen is introduced, the raw material gases of ammonia and boron chloride are introduced into the vapor deposition furnace according to the volume ratio of 2: 1.
And S6, stopping heating the vapor deposition furnace and raising the temperature to cool the product to room temperature and discharging the product.
In specific implementation, the heating system is closed to stop heating and temperature rise in the vapor deposition furnace, the temperature in the vapor deposition furnace is gradually reduced through the water cooling jacket, and the product is taken out when the temperature of the product reaches the room temperature.
The implementation of the invention has the advantages that:
the invention provides a preparation method of pyrolytic boron nitride, which comprises the following steps: installing a graphite mold in the vapor deposition furnace and sealing the vapor deposition furnace; vacuumizing the vapor deposition furnace, heating the vapor deposition furnace to raise the temperature and cooling the outer surface of the vapor deposition furnace; introducing protective gas and raw material gas in a fixed proportion into a vapor deposition furnace to enable a graphite mold to rotate; introducing protective gas under the condition of keeping a certain vacuum degree and temperature in the vapor deposition furnace; under the condition of keeping a certain vacuum degree and temperature in the vapor deposition furnace, raw material gas is introduced according to a fixed proportion. The preparation process of the pyrolytic boron nitride product with high quality, environmental protection and low cost can be achieved, and the effect of producing the pyrolytic boron nitride product with stability and high quality is achieved.
Example two:
as shown in fig. 2: a production apparatus for pyrolytic boron nitride, comprising:
a vapor deposition furnace 1 as a reaction site for the raw material gas;
a graphite mold disposed in the vapor deposition furnace 1 as a substrate for vapor deposition of the raw material gas;
a heating system including a power supply, an electrode and a heater for heating in the vapor deposition furnace 1;
the driving system 4 is arranged on the vapor deposition furnace 1 and comprises a motor, a speed reducer and a rotating shaft and is used for driving the graphite mold to rotate;
the air extraction system 5 is communicated with the interior of the vapor deposition furnace 1 and comprises rough extraction equipment and fine extraction equipment which are respectively used for vacuumizing the vapor deposition furnace 1 before the reaction starts and stabilizing the vacuum degree in the vapor deposition furnace 1 during the reaction;
the gas outlet end of the material mixing tank is communicated with the interior of the vapor deposition furnace 1 and is used for mixing protective gas and raw material gas;
a cooling jacket attached to the outer surface of the vapor deposition furnace 1 for cooling the outer surface of the vapor deposition furnace 1;
and the filtering and cooling system is used for cooling the gas pumped out by the gas pumping system. The cooler is arranged behind the outlet of the deposition furnace, adopts a baffle type filtering structure and has cooling and filtering functions.
The boron nitride vapor deposition furnace adopts a graphite tubular squirrel-cage structure form inside, and adopts a hard and soft felt combined graphite felt for heat preservation. After the flow of the nitrogen, the boron chloride and the ammonia is regulated by the air inlet cabinet of the 2 air inlet control module, the nitrogen, the boron chloride and the ammonia are firstly mixed in the air mixing tank and then enter the deposition furnace for chemical vapor deposition reaction.
In this embodiment, the rough pumping device and the fine pumping device are respectively a vane pump and a roots screw pump set.
In this embodiment, the vapor deposition furnace 1 is provided with a thermocouple, an optical infrared thermometer, and a vacuum gauge.
In this embodiment, the equipment for preparing pyrolytic boron nitride further comprises an air inlet system, wherein the air inlet system comprises an air inlet cabinet, an air inlet control module 2 arranged in the air inlet cabinet and a mixing tank connected with the air inlet control module 2, and an outlet of the mixing tank is communicated with an air inlet of the vapor deposition furnace 1.
The using process flow comprises the following steps: hanging the treated graphite mold in a furnace, starting an air extraction system to enable the furnace to reach a vacuum state (the vacuum degree is 10Pa), electrifying, heating to 1800-2000 ℃, keeping the temperature, and introducing ammonia gas and boron chloride according to the volume ratio of 2:1 by taking nitrogen as carrier gas and protective gas; after ventilation, the pressure in the furnace is kept at 50Pa, the furnace temperature is 1800-2000 ℃, and the temperature is kept for 15-30 h. And then the power is cut off, the product is cooled to room temperature along with the furnace and taken out of the furnace, the white hard shell deposited on the die is taken down to form a complete PBN crucible blank, and the PBN crucible blank is machined into a qualified size, so that a qualified PBN product can be obtained.
The implementation of the invention has the advantages that:
the invention provides a pyrolytic boron nitride preparation device, which comprises: a vapor deposition furnace as a reaction site for the raw material gas; a graphite mold disposed in the vapor deposition furnace as a substrate for vapor deposition of the raw material gas; the heating system is used for heating the vapor deposition furnace to a vapor deposition temperature; the driving system is arranged on the vapor deposition furnace and is used for driving the graphite mold to rotate; the gas extraction system is communicated with the interior of the vapor deposition furnace, and the material mixing tank is used for mixing protective gas and raw material gas, and the gas outlet end of the material mixing tank is communicated with the interior of the vapor deposition furnace; a cooling jacket attached to an outer surface of the vapor deposition furnace, for cooling the outer surface of the vapor deposition furnace; and the filtering and cooling system is used for cooling the gas pumped out by the gas pumping system. The preparation process of the pyrolytic boron nitride product with high quality, environmental protection and low cost can be achieved, and the effect of producing the pyrolytic boron nitride product with stability and high quality is achieved. Successfully solve BCl3And NH3The raw material proportion is difficult to control, so that the technical problem of influencing the preparation process and the product performance is solved, the single-gas-path transportation of reaction gas can be realized, and the process controllability and the stability are improved. The method can realize accurate and stable control on the process parameters such as temperature, pressure, gas flow, feed gas concentration and the like during operation, fully ensure the low-pressure and high-temperature deposition environment required by pyrolysis of the boron nitride material, realize the production of the boron nitride material with good lamellar crystallization, and avoid the generation of defects such as cracking, layering and the like.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein are intended to be covered by the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A production apparatus for pyrolytic boron nitride, comprising: vapour deposition stove and setting up the graphite jig in vapour deposition stove, its characterized in that still includes:
the heating system is used for heating the vapor deposition furnace to a vapor deposition temperature;
the graphite mould is arranged on the driving system and used for driving the graphite mould to rotate;
the air pumping system is communicated with the inside of the vapor deposition furnace and is used for vacuumizing the inside of the vapor deposition furnace and maintaining the vacuum degree;
the gas inlet system is communicated with the inside of the vapor deposition furnace and is used for mixing raw material gas and feeding the vapor deposition furnace;
and the cooling system is used for cooling the outer surface of the vapor deposition furnace.
2. The apparatus for preparing pyrolytic boron nitride according to claim 2, wherein: the heating system comprises a power supply, an electrode arranged at the bottom of the vapor deposition furnace and a heater arranged in the vapor deposition furnace, wherein the electrode is respectively connected with the power supply and the heater circuit.
3. The apparatus for preparing pyrolytic boron nitride according to claim 4, wherein: the air pumping system comprises rough pumping equipment and fine pumping equipment which are respectively used for vacuumizing the vapor deposition furnace before reaction and maintaining the vacuum degree in the vapor deposition furnace during reaction.
4. The apparatus for producing pyrolytic boron nitride according to any one of claims 1 to 3, wherein: the air inlet system comprises an air inlet cabinet, an air inlet control module arranged in the air inlet cabinet and a mixing tank connected with the air inlet control module, wherein an outlet of the mixing tank is communicated with an air inlet of the vapor deposition furnace.
5. A preparation method of pyrolytic boron nitride is characterized by comprising the following steps: the preparation method of the pyrolytic boron nitride comprises the following steps:
putting the mould into a reaction chamber in the vapor deposition furnace, and vacuumizing and heating the reaction chamber in the vapor deposition furnace;
carrying out heat preservation operation when the vacuum degree and the temperature in the reaction chamber respectively reach preset values, and introducing raw material gas and protective gas according to a preset proportion;
maintaining a certain vacuum degree and temperature, rotating the mold to react for a period of time to generate a precoating layer on the mold;
only introducing protective gas for a period of time;
keeping a certain vacuum degree and temperature, and proportionally introducing raw material gas to react for a period of time to obtain the pyrolytic boron nitride with the precoat.
6. The method of claim 5, wherein the method comprises the following steps: the method comprises the following steps of putting a mould into a reaction chamber in a vapor deposition furnace, vacuumizing the reaction chamber in the vapor deposition furnace, and heating the reaction chamber by heating: the graphite mold is arranged in the center of a reaction chamber of a vapor deposition furnace, the vapor deposition furnace is vacuumized to the vacuum degree of more than 10Pa by rough pumping equipment, the deposition furnace is continuously heated to the temperature of 1800-1900 ℃, and simultaneously the surface of the vapor deposition furnace is cooled.
7. The method of claim 5, wherein the method comprises the following steps: the method is characterized in that the heat preservation operation is carried out when the vacuum degree and the temperature in the reaction chamber respectively reach preset values, and the steps of introducing raw material gas and protective gas according to a preset proportion are as follows: when the temperature reaches 1800-1900 ℃, the vacuum degree reaches 10Pa and the temperature is stabilized for 1hr, introducing protective gas and carrier gas into the vapor deposition furnace, and simultaneously introducing raw material gases of ammonia and boron chloride into the vapor deposition furnace according to the volume ratio of 2: 1.
8. The method of claim 5, wherein the method comprises the following steps: keeping a certain vacuum degree and temperature, rotating the mold to react for a period of time to enable the precoating layer generated on the mold to be specifically as follows: keeping the temperature in the reaction chamber at 1800-1900 ℃ and the vacuum degree at 10-100 Pa, driving the graphite mold to rotate, and enabling the gas in the reaction chamber to react for 1-2hr to generate a pyrolytic boron nitride precoat on the graphite mold.
9. The method of claim 5, wherein the method comprises the following steps: the step of only introducing the protective gas for a period of time specifically comprises the following steps: the temperature in the vapor deposition furnace is kept between 1800 and 2000 ℃ through a heating system, and protective gas and carrier gas are introduced within 1 hr.
10. The method for producing pyrolytic boron nitride according to any one of claims 5 to 9, wherein: the preparation method of the pyrolytic boron nitride further comprises the following steps: stopping heating and raising the temperature in the vapor deposition furnace, gradually reducing the temperature in the vapor deposition furnace, and taking out the product after the product is cooled.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090169781A1 (en) * | 2007-12-31 | 2009-07-02 | Marc Schaepkens | Low thermal conductivity low density pyrolytic boron nitride material, method of making, and articles made therefrom |
| CN201890928U (en) * | 2010-11-22 | 2011-07-06 | 赵凤鸣 | Vapor phase deposition furnace |
| CN102330068A (en) * | 2011-10-21 | 2012-01-25 | 苏州明林光电科技有限公司 | Pyrolysis boron nitride plate preparing method and vapor phase deposition furnace used in same |
| CN102586754A (en) * | 2012-03-06 | 2012-07-18 | 山东国晶新材料有限公司 | Method for preparing pyrolytic boron nitride crucible easy to demould |
| CN206624946U (en) * | 2017-02-14 | 2017-11-10 | 台山市华兴光电科技有限公司 | A kind of pressure furnace for being used to prepare indium phosphide single crystal |
-
2021
- 2021-02-18 CN CN202110190423.4A patent/CN113005426A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090169781A1 (en) * | 2007-12-31 | 2009-07-02 | Marc Schaepkens | Low thermal conductivity low density pyrolytic boron nitride material, method of making, and articles made therefrom |
| CN201890928U (en) * | 2010-11-22 | 2011-07-06 | 赵凤鸣 | Vapor phase deposition furnace |
| CN102330068A (en) * | 2011-10-21 | 2012-01-25 | 苏州明林光电科技有限公司 | Pyrolysis boron nitride plate preparing method and vapor phase deposition furnace used in same |
| CN102586754A (en) * | 2012-03-06 | 2012-07-18 | 山东国晶新材料有限公司 | Method for preparing pyrolytic boron nitride crucible easy to demould |
| CN206624946U (en) * | 2017-02-14 | 2017-11-10 | 台山市华兴光电科技有限公司 | A kind of pressure furnace for being used to prepare indium phosphide single crystal |
Non-Patent Citations (1)
| Title |
|---|
| 黄锐 * |
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