CN102330068B - Pyrolysis boron nitride plate preparing method and vapor phase deposition furnace used in same - Google Patents
Pyrolysis boron nitride plate preparing method and vapor phase deposition furnace used in same Download PDFInfo
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- CN102330068B CN102330068B CN201110323008A CN201110323008A CN102330068B CN 102330068 B CN102330068 B CN 102330068B CN 201110323008 A CN201110323008 A CN 201110323008A CN 201110323008 A CN201110323008 A CN 201110323008A CN 102330068 B CN102330068 B CN 102330068B
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- 238000000034 method Methods 0.000 title claims abstract description 34
- 229910052582 BN Inorganic materials 0.000 title claims abstract description 33
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000001947 vapour-phase growth Methods 0.000 title abstract 6
- 238000000197 pyrolysis Methods 0.000 title abstract 4
- 230000008021 deposition Effects 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 230000007246 mechanism Effects 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000007792 gaseous phase Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 6
- 230000000284 resting effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 4
- 125000006850 spacer group Chemical group 0.000 claims description 4
- 239000011449 brick Substances 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 3
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 229910015844 BCl3 Inorganic materials 0.000 abstract 1
- 230000006872 improvement Effects 0.000 abstract 1
- 230000009467 reduction Effects 0.000 abstract 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 description 18
- 238000000151 deposition Methods 0.000 description 12
- 239000004567 concrete Substances 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- 229910005540 GaP Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- HZXMRANICFIONG-UHFFFAOYSA-N gallium phosphide Chemical compound [Ga]#P HZXMRANICFIONG-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical compound C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Images
Abstract
The invention discloses a pyrolysis boron nitride plate preparing method and a vapor phase deposition furnace used in the same, and belongs to the technical field of preparation of special ceramic materials. In the method, an air inlet mechanism and the vapor phase deposition furnace in which a rotating mold is arranged are utilized; raw material gas is mixed gas of N2, NH3 and BCl3 in the molar ratio of (30-10):(10-1):(8-0.5); the vapor phase deposition furnace has the temperature of between 1,700 and 2,000 DEG C and the heat insulation time of 14 to 26 hours; and the rotating mold is obliquely arranged in the vapor phase deposition furnace. The invention has the advantages that: the rotating mold is obliquely arranged in the vapor phase deposition furnace, so that the raw material gas obliquely flows upwards along an oblique angle and fully fills a groove in the flowing process, a pyrolysis boron nitride plate has a smooth surface, and obvious reduction in residual stress and improvement on yield are facilitated; and the deposition furnace provided by the invention has a simple structure, and the condition that the technical effect of the pyrolysis boron nitride plate is comprehensively reflected can be guaranteed.
Description
Technical field
The invention belongs to the special ceramic material preparing technical field, be specifically related to a kind of pyrolitic boron nitride preparation of plates method, and relate to the used gaseous phase deposition stove of this method
Background technology
pyrolitic boron nitride (being called for short PBN), because it has the following strong point that is not limited to: purity is high, nontoxic, easy processes and higher high temperature purity; Acidproof, alkaline-resisting, salt tolerant and organic solvent-resistant; At high temperature nonwetting with most molten metals, semiconductor material, do not react; Inclusion-free volatilization under the good and high temperature of electrical insulation capability; Heat-shock resistance is excellent, heat conductance is good and thermal expansivity is low; Resistance is high, dielectric strength is high, specific inductivity is little, the magnetic loss tangent is low and have good microwave and infrared rays performance thoroughly, or the like.Therefore the crucible, the pedestal that are used as the synthetic usefulness of semiconductor monocrystal and III-V group compound; Original position is synthesized GaAs (gallium arsenide); LEC (LEC) genealogy of law row crucible of InP (indium phosphide), GaP (gallium phosphide) monocrystalline; The serial crucible of molecular beam epitaxy (MBE) usefulness; VGF (VGF), VB (vertical Bu Shi) genealogy of law row crucible; The compound well heater coating of PBN/PG (pyrolitic boron nitride/pyrolytic graphite); The high-temperature insulation fluid tip; The graphite heater insulating coating; MOCVD (metal organic chemical vapor deposition) system insulation plate; Special-shaped crucible and special-shaped graphite piece coating; The wafer annealing process is used compound well heater, or the like.
Be seen in that disclosed Chinese patent document is existing about the technical intelligence of pyrolitic boron nitride and preparation thereof
; Typical case's application for a patent for invention publication No. CN102021533A (chemical vapor deposition method and gaseous phase deposition stove that preparation pyrolitic boron nitride goods are used), the SP 1 goods that this patented claim scheme obtains are crucible.
The development of
pyrolitic boron nitride crucible and sheet material has inseparable relation with employed technology, because the crucible size at initial stage is less, therefore required cover plate and dead ring are also smaller.Along with the development of LEC method, crucible size enlarges markedly, and the inlet mouth of gaseous phase deposition stove also changes thereupon, becomes two inlet mouths or many inlet mouths by single inlet mouth.The outward appearance of the pyrolitic boron nitride sheet material that the various inlet situation is prepared is different.Because single inlet mouth is the center air inlet, if therefore mould does not rotate, peripheral approaching thick middle (center is thick) can appear and in sheet material so, and the thickness of periphery also is uneven.If mould rotates, so also only can improve the homogeneity of the periphery of sheet material, middle thickness difference with periphery can not effectively be improved; Promptly; Overall appearance can not effectively be promoted, and unrelieved stress is big, easy of crack (cracking in the middle of mostly showing as); Sometimes do not ftractureing during the demoulding as yet, sometimes just cracking after breaking away from mould.Two inlet mouths have two kinds of situations usually, and the one, the center inlet mouth of stationkeeping (also claiming primary air inlet) adds side-inlet (or claiming auxilairy air intake); The 2nd, can change two inlet mouths of position as required; Two kinds of situations appear in sheet material under this pair inlet mouth situation: the former; The material material of producing is just as lapidation caused ripple apperance in water, and the great circle that the center that shows is thick then is recessed ring; And be protruding ring, so circulation is until periphery; The sheet material that the latter produces shows central dip, has corrugated to intersect again, and convexity is recessed again thereupon.Although the unrelieved stress of two inlet mouths is more far better than single inlet mouth, the surface of resulting sheet material all is irregular.Seek out the pyrolitic boron nitride sheet material of ideal flatness, then must carry out follow-up and complicated mechanical processing, for example carry out comparatively loaded down with trivial details turning and grinding.Yet, in pyrolitic boron nitride sheet material being made the process of planeness processing,, both influenced the yield rate of product because of the release of unrelieved stress causes the probability that bursts higher, improved preparation cost again.
Perhaps based on said circumstances; At present China is for such as the still main dependence on import of the pyrolitic boron nitride sheet material of the used big specification of MOCVD (organometallics chemical vapour deposition) equipment; Therefore be necessary from the autonomous angle of industry; Innovate, the applicant has done positive and useful exploration for this reason, and the technical scheme that will introduce below produces under this background
Summary of the invention
task of the present invention is to provide a kind of and helps to ensure surface finish, helps significantly reducing unrelieved stress and be of value to the pyrolitic boron nitride preparation of plates method that improves qualification rate.
another task of the present invention is to provide a kind of pyrolitic boron nitride preparation of plates method used gaseous phase deposition stove, and this gaseous phase deposition stove can ensure comprehensive embodiment of the technique effect of said pyrolitic boron nitride sheet material.
Task of the present invention is accomplished like this, a kind of pyrolitic boron nitride preparation of plates method, and this method adopts the gaseous phase deposition stove that has admission gear and in stove, be provided with the mould of rotation, and unstripped gas is N
2
, NH
3
And BCl
3
Mixed gas, wherein: N
2
, NH
3
And BCl
3
The mol of gas is than being 30-10: 10-1: 8-0.5, and the furnace temperature of gaseous phase deposition stove is 1700～2000 ℃, and soaking time is 14-26h, and described rotating mold is inclined to set in described gaseous phase deposition stove.
in a concrete embodiment of the present invention, the said angle of inclination that is obliquely installed is for to become 10-20 ° with level.
another task of the present invention is accomplished like this; The used gaseous phase deposition stove of a kind of pyrolitic boron nitride preparation of plates method; Comprise a body of heater; This body of heater is supported on one group of leg with airborne, and body of heater has one first watercooling jacket, on this first watercooling jacket, has connected one first water inlet interface and one first water outlet interface; One bell, this bell have one second watercooling jacket, on this second watercooling jacket, have connected one second water inlet interface and one second water outlet interface, and have received an aiutage in the central authorities of bell, on this aiutage, are connected with a vapor pipe; One has the graphite cylindrical shell of mold cavity; This graphite cylindrical shell is arranged in the body of heater chamber of body of heater; And the top of this graphite cylindrical shell is furnished with a graphite cylinder cover; The central authorities of this graphite cylinder cover and be extended with the gas that fixes with bell towards the direction of said bell and draw cover; The gas that this gas is drawn cover is drawn mantle cavity and is communicated with the aiutage chamber of aiutage and communicate with described mold cavity, and the outer wall of graphite cylindrical shell is provided with electromagnetic heating coil, and is evenly distributed with three to eight inlet mouths in the bottom of the mold cavity of graphite cylindrical shell; One mould rotating mechanism, this mould rotating mechanism is arranged on the described bell; One main shaft, the upper end of this main shaft are drawn mantle cavity by way of described gas successively and are connected with described mould rotating mechanism with the aiutage chamber, and the lower end is stretched in the said mold cavity and be fixed with a rotating disk; One mould, this mould are connected and are connected with rotating disk through joint pin with said main shaft inclination corresponding to the below of said rotating disk; The one group of admission gear that is used in said mold cavity, introducing unstripped gas that quantity equates with the quantity of said inlet mouth, each admission gear and said body of heater are fixed, and corresponding with inlet mouth.
In another concrete embodiment of the present invention, on the inwall of described first watercooling jacket and be positioned at that the below of inwall is spaced apart to be provided with one group of transitional pore, transitional pore communicates with the cooling spacer chamber of the bottom that is formed in said body of heater
.
are in another concrete embodiment of the present invention; Described first water inlet interface and the described first water outlet interface are the diagonal angle setting each other; Wherein, the first water inlet interface is positioned at the lower side of said body of heater, and the first water outlet interface is positioned at the upper lateral part of body of heater.
are provided with the furnace lining layer at the inwall of described body of heater in another concrete embodiment of the present invention, the inwall of described bell is provided with the bell air retaining wall, and furnace lining layer and bell air retaining wall are refractory mortar or refractory brick.
also have among the concrete embodiment of the present invention, and described bell matches with said body of heater through one group of clamping piece that is provided with at interval.
are more of the present invention and among concrete embodiment; Described mould rotating mechanism comprises motor, step-down gear, first conical gear and second conical gear; Motor and step-down gear are matched and be fixed on the step-down gear resting support together with motor by step-down gear, and the step-down gear resting support is fixed on the described bell, and first conical gear is fixed on the step-down gear final stage PTO of step-down gear; And be meshed with second conical gear; And second conical gear is fixed on the upper end of said main shaft, and the upper end of main shaft is bearing on the chock rotationally, and chock is fixed on the described aiutage.
in of the present invention and then concrete embodiment, said mould is 10-25 ° with the obliquity that said main shaft tilts to be connected, and mould is a graphite jig.
are of the present invention again more and among concrete embodiment; Said one group of admission gear respectively comprises the escape pipe with three concentric(al) circles air outlets and connects the virgin gas inlet tube that the quantity on escape pipe equates with the concentric(al) circles air outlet; Escape pipe and said body of heater are fixed, and the concentric(al) circles air outlet is corresponding with said inlet mouth.
technical scheme provided by the invention is owing to be oblique setting with the mould that rotates in the gas cvd furnace; Thereby can make the unstripped gas bias current that makes progress along the angle of inclination; In flow process, groove is filled and led up; Make the pyrolitic boron nitride plate surface that obtains smooth, help significantly reducing unrelieved stress and improve qualification rate; The cvd furnace that provides is simple in structure, can ensure comprehensive embodiment of the said technique effect of pyrolitic boron nitride sheet material.
Description of drawings
Fig. 1 is the example structure figure of the used gaseous phase deposition stove of the inventive method.
Fig. 2 is the sectional view of Fig. 1.
Embodiment
can be expressly understood technical spirit of the present invention and beneficial effect more for the inspector that the makes Patent Office especially public; The applicant general elaborates with the mode of embodiment below; But the description to embodiment all is not the restriction to the present invention program, any according to the present invention design done only for pro forma but not substantial equivalent transformation all should be regarded as technical scheme category of the present invention.
Embodiment 1:
Fig. 1 and Fig. 2 are asked for an interview in
; The inventive method used and comprise by gaseous phase deposition stove illustrated in figures 1 and 2: a body of heater 1 is fixed on one group of leg 14 with airborne; Constitute one first watercooling jacket 11 on the perisporium of this body of heater 1; And constitute a cooling spacer chamber 12 in the bottom of body of heater 1, be provided with furnace lining layer 13 at the inwall of body of heater 1, the material of furnace lining layer 13 is a carbon-carbon composite.On first watercooling jacket 11, be connected with one first water inlet interface 111 and one first water outlet interface 112; The first water inlet interface 111 and the first water outlet interface 112 are the diagonal angle setting each other; Wherein: water inlet interface 111 is positioned on the sidewall of bottom of body of heater 1, and the first water outlet interface 112 is positioned on the sidewall on top of body of heater 1.Spaced apartly in the bottom of the inwall of first watercooling jacket 11 be provided with one group of transitional pore 113, transitional pore 113 communicates with cooling spacer chamber 12.
graphite cylindrical shell 3 is arranged in the body of heater chamber (also can claim burner hearth) of body of heater 1; This graphite cylindrical shell 3 has mold cavity 31 (this mold cavity 31 also can be claimed the sediment chamber); Outer wall at graphite cylindrical shell 3 is provided with electromagnetic heating coil 33; The bottom of mold cavity 31 is evenly equipped with three to eight inlet mouths 311; Be furnished with a graphite cylinder cover 32 on the top of graphite cylindrical shell 3, towards a side of aforesaid bell 2 and occupy middle position and be extended with a gas and draw cover 321, the gas that this gas is drawn cover 321 is drawn mantle cavity 3211 and is communicated with the aiutage chamber 222 of aforementioned aiutage 22 at graphite cylinder cover 32; The gas that comes from the mold cavity 31 is drawn mantle cavity 3211 and aiutage chamber 222 through gas successively, until being drawn by aforesaid vapor pipe 221.
mould rotating mechanism 4 comprises motor 41, step-down gear 42, first conical gear 43 and second conical gear 44; Motor 41 connects with step-down gear 42 transmissions; And be installed on the step-down gear resting support 422 together with motor 41 by step-down gear 42, and step-down gear resting support 422 is fixed on the aforesaid bell 2, first conical gear 43 is fixed on the step-down gear final stage PTO 421 of step-down gear 42; And be meshed with second conical gear 44; And second conical gear 44 is fixed on the upper end of main shaft 5, and the upper end of main shaft 5 is bearing on the chock 52 rotationally, and chock 52 is fixed on the nozzle position of aiutage 22.The lower end of main shaft 5 222 is drawn mantle cavity 3211 with gas and is stretched in the mold cavity 31 and is fixed with a rotating disk 51 by way of the aiutage chamber.
one group of admission gear 7 that equates with the quantity of aforesaid inlet mouth 311 is arranged on the bottom of body of heater 1, because the quantity of inlet mouth 311 is three to eight, so the quantity of admission gear 7 is similarly three to eight.Each admission gear 7 comprises the escape pipe 71 with three concentric(al) circles air outlets 711 and connects the virgin gas inlet tube 72 that the quantity on escape pipe 71 equates with concentric(al) circles air outlet 711; Escape pipe 71 is fixed with the bottom of body of heater 1, and concentric(al) circles air outlet 711 is corresponding with inlet mouth 311.In Fig. 1; Though the applicant has illustrated two concentric(al) circles air outlets 711 and on escape pipe 71, connected a pair of virgin gas skirt 72 on each escape pipe 71; Yet this only is in order to make diagram be tending towards clear; And in fact as structure shown in the CN102021533A, concentric(al) circles air outlet 711 is three, and virgin gas inlet tube 72 also is three.
Under the work of the motor 41 of mould rotating mechanism 4, slow down through step-down gear 42, drive second conical gear 44 by first conical gear 43, because second conical gear 44 is fixed on the main shaft 5, so main shaft 5 rotations, by main shaft 5 driven rotary dishes 51 and mould 6 rotations, simultaneously, N
2
, NH
3
And BCl
3
Gas is introduced from admission gear 7, both can make 7 air inlets simultaneously of three to eight admission gears as required, that is to say to make 311 air inlets simultaneously of three to eight inlet mouths, also can optionally make inlet mouth 311 air inlets.Also simultaneously, first, second watercooling jacket 11,21 circulates simultaneously and introduces water coolant, by electromagnetic heating coil 33 energisings graphite cylindrical shell 3 is heated.
Adopting said structure to prepare diameter is that the process of pyrolitic boron nitride sheet material of 290 ㎜ is following:
Mould diameter is 293 ㎜, starts vacuum extractor, makes in the mold cavity 31 to be in vacuum state, and vacuum tightness is 100Pa, and electromagnetic heating coil 33 energising heating start 4 work of mould rotating mechanism when temperature reaches 1780 ℃, and gas is introduced in molar ratio, N
2
: NH
3
: BCl
3
=24: 8: 5; Pressure remains on 399Pa in the stove; Furnace temperature is kept 1780 ℃, and mould 6 becomes in the mold cavity 31 of graphite cylindrical shell 3 and horizontal 10-20 ° angle of inclination and rotation, the about 3n/min of speed of rotation; Behind the 22h that holds time under 1780 ℃, cut off the power supply, promptly cut off the power supply of electromagnetic heating coil 33.Open bell 2 after cooling to room temperature with the furnace; The preferred handling apparatus that uses hangs body of heater 1 with bell 2; The white duricrust that is deposited on the mould 6 is taken off, obtain the pyrolitic boron nitride that diameter is 293 ㎜ (PBN) blank, obtain the PBN finished product that diameter is 290 ㎜ with grinding through mechanical workout.
In the present embodiment, inlet mouth 311 is launched three, promptly by 7 air inlets simultaneously of three admission gears, wherein: N
2
6L/min, NH
3
1L/min and BCl
3
0.6L/min.
Because mould 6 becomes inclination 10-20 ° angular turn with level, the awave rotation of its movement locus around the center, making unstripped gas is N
2
, NH
3
And BCl
3
Mixed gas (also being reactant gases) is had an opportunity along the bias current that makes progress of this angle, and this liquid form helps filling and leading up groove, makes PBN sheet material more smooth, and unrelieved stress is less, improves product percent of pass and production efficiency, helps reducing cost.
Embodiment 2:
Only with N
2
, NH
3
And BCl
3
The mol ratio of gas changes 12: 4.2: 1.4 into, that is to say N
2
, NH
3
And BCl
3
The flow of gas is respectively N
2
12L/min, NH
3
4.2L/min and BCl
3
1.4L/min pressure changes 270Pa in the stove, temperature is 1800 ℃, and soaking time is 26h, wherein:, inlet mouth 311 is launched two and be provided with shunting nozzle, and all the other are all with the description to embodiment 1.
Embodiment 3:
Only with N
2
, NH
3
And BCl
3
The mol ratio of gas changes 10: 4: 3.2 into, that is to say N
2
, NH
3
And BCl
3
The flow of gas is respectively N
2
10L/min, NH
3
4L/min and BCl
3
3.2L/min pressure changes 260Pa in the stove, temperature changes 2000 ℃ into, and soaking time changes 16h into, and inlet mouth 311 is launched five, and all the other are all with the description to embodiment 1
Claims (9)
1.
A kind of pyrolitic boron nitride preparation of plates method, this method adopts the gaseous phase deposition stove that has admission gear and in stove, be provided with the mould of rotation, and unstripped gas is N 2 , NH 3 And BCl 3 Mixed gas, wherein: N 2 , NH 3 And BCl 3 The mol of gas is than being 30-10: 10-1: 8-0.5; The furnace temperature of gaseous phase deposition stove is 1700～2000 ℃; Soaking time is 14-26h, it is characterized in that described rotating mold is inclined to set in described gaseous phase deposition stove, and the angle of inclination that is obliquely installed is for to become 10-20 ° with level.
2. the used gaseous phase deposition stove of
a kind of pyrolitic boron nitride preparation of plates method as claimed in claim 1; It is characterized in that comprising a body of heater (1); This body of heater (1) is supported on one group of leg (14) with airborne; And body of heater (1) has one first watercooling jacket (11), on this first watercooling jacket (11), has connected one first water inlet interface (111) and one first water outlet interface (112); One bell (2); This bell (2) has one second watercooling jacket (21); On this second watercooling jacket (21), connected one second water inlet interface (211) and one second water outlet interface (212); And received an aiutage (22) in the central authorities of bell (2), on this aiutage (22), be connected with a vapor pipe (221); One has the graphite cylindrical shell (3) of mold cavity (31); This graphite cylindrical shell (3) is arranged in the body of heater chamber of body of heater (1); And the top of this graphite cylindrical shell (3) is furnished with a graphite cylinder cover (32); The central authorities of this graphite cylinder cover (32) and be extended with the gas that fixes with bell (2) towards the direction of said bell (2) and draw cover (321); The gas that this gas is drawn cover (321) is drawn mantle cavity (3211) and is communicated with the aiutage chamber (222) of aiutage (22) and communicate with described mold cavity (31); The outer wall of graphite cylindrical shell (3) is provided with electromagnetic heating coil (33), and is evenly distributed with three to eight inlet mouths (311) in the bottom of the mold cavity (31) of graphite cylindrical shell (3); One mould rotating mechanism (4), this mould rotating mechanism (4) is arranged on the described bell (2); One main shaft (5), the upper end of this main shaft (5) are drawn mantle cavity (3211) by way of described gas successively and are connected with described mould rotating mechanism (4) with aiutage chamber (222), and the lower end is stretched in the said mold cavity (31) and be fixed with a rotating disk (51); One mould (6), this mould (6) are corresponding to the below of said rotating disk (51), and this mould (6) becomes 10-20 ° angle of inclination to be connected and to be connected with rotating disk (51) through joint pin (61) with said main shaft (5) inclination with level; The one group of admission gear (7) that is used in said mold cavity (31), introducing unstripped gas that quantity equates with the quantity of said inlet mouth (311), each admission gear (7) is fixing with said body of heater (1), and corresponding with inlet mouth (311).
3. the used gaseous phase deposition stove of
pyrolitic boron nitride preparation of plates method according to claim 2; It is characterized in that on the inwall of described first watercooling jacket (11) and be positioned at the spaced apart one group of transitional pore (113) that is provided with in below of inwall that transitional pore (113) communicates with the cooling spacer chamber (12) of the bottom that is formed in said body of heater (1).
4. the used gaseous phase deposition stove of
pyrolitic boron nitride preparation of plates method according to claim 2; It is characterized in that described first water inlet interface (111) and the described first water outlet interface (112) are the diagonal angle setting each other; Wherein, The first water inlet interface (111) is positioned at the lower side of said body of heater (1), and the first water outlet interface (112) is positioned at the upper lateral part of body of heater (1).
5. the used gaseous phase deposition stove of
pyrolitic boron nitride preparation of plates method according to claim 2; It is characterized in that being provided with furnace lining layer (13) at the inwall of described body of heater (1); The inwall of described bell (2) is provided with bell air retaining wall (23), and furnace lining layer (13) and bell air retaining wall (23) are refractory mortar or refractory brick.
6. the used gaseous phase deposition stove of
pyrolitic boron nitride preparation of plates method according to claim 2, (10 match with said body of heater through one group of clamping piece that is provided with at interval (24) to it is characterized in that described bell (2).
7. the used gaseous phase deposition stove of
pyrolitic boron nitride preparation of plates method according to claim 2; It is characterized in that described mould rotating mechanism (4) comprises motor (41), step-down gear (42), first conical gear (43) and second conical gear (44); Motor (41) and step-down gear (42) are matched and be fixed on the step-down gear resting support (422) together with motor (41) by step-down gear (42); And step-down gear resting support (422) is fixed on the described bell (2); First conical gear (43) is fixed on the step-down gear final stage PTO (421) of step-down gear (42), and is meshed with second conical gear (44), and second conical gear (44) is fixed on the upper end of said main shaft (5); The upper end of main shaft (5) is bearing on the chock (52) rotationally, and chock (52) is fixed on the described aiutage (22).
8. the used gaseous phase deposition stove of
pyrolitic boron nitride preparation of plates method according to claim 2; It is characterized in that said mould (6) is 10-25 ° with the obliquity that said main shaft (5) tilts to be connected, and mould (6) is a graphite jig.
9.
The used gaseous phase deposition stove of pyrolitic boron nitride preparation of plates method according to claim 2; It is characterized in that said one group of admission gear (7) respectively comprises the escape pipe (71) with three concentric(al) circles air outlets (711) and connects the virgin gas inlet tube (72) that the quantity on escape pipe (71) equates with concentric(al) circles air outlet (711); Escape pipe (71) is fixing with said body of heater (1), and concentric(al) circles air outlet (711) are corresponding with said inlet mouth (311)
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| CN102796995B (en) * | 2012-08-27 | 2015-01-28 | 北京博宇半导体工艺器皿技术有限公司 | Vapor deposition furnace and method for preparing pyrolytic boron nitride product |
| CN103541000B (en) * | 2013-11-06 | 2016-09-07 | 中国科学院苏州纳米技术与纳米仿生研究所 | A kind of device and method preparing boron nitride monocrystal |
| CN105603388B (en) * | 2016-01-22 | 2018-05-15 | 山东国晶新材料有限公司 | A kind of preparation method of long-life pyrolytic boron nitride crucible |
| CN105970186B (en) * | 2016-07-04 | 2018-05-15 | 山东国晶新材料有限公司 | A kind of method of efficiently production pyrolytic boron nitride product |
| CN107460447A (en) * | 2017-09-25 | 2017-12-12 | 何军舫 | A kind of production method of the boron nitride plectane with high-flatness |
| CN113005426A (en) * | 2021-02-18 | 2021-06-22 | 上海韵申新能源科技有限公司 | Preparation method and equipment of pyrolytic boron nitride |
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| CN2218916Y (en) * | 1994-12-28 | 1996-01-31 | 中国科学院金属研究所 | Intermediate frequency induction furnace for preparing crucible product for pyrolyzing boron nitride |
| CN102021533A (en) * | 2010-11-22 | 2011-04-20 | 赵凤鸣 | Chemical vapor deposition technology and vapor deposition furnace for preparing pyrolytic boron nitride (PBN) products |
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| RU94032296A (en) * | 1994-09-07 | 1996-07-20 | Обнинское научно-производственное предприятие "Технология" | Method for manufacturing ceramic article based on boron nitride |
| US6670025B2 (en) * | 2001-05-24 | 2003-12-30 | General Electric Company | Pyrolytic boron nitride crucible and method |
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| CN2218916Y (en) * | 1994-12-28 | 1996-01-31 | 中国科学院金属研究所 | Intermediate frequency induction furnace for preparing crucible product for pyrolyzing boron nitride |
| CN102021533A (en) * | 2010-11-22 | 2011-04-20 | 赵凤鸣 | Chemical vapor deposition technology and vapor deposition furnace for preparing pyrolytic boron nitride (PBN) products |
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