CN114506828A - Low-cost aluminum nitride powder preparation process - Google Patents
Low-cost aluminum nitride powder preparation process Download PDFInfo
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- CN114506828A CN114506828A CN202210060313.0A CN202210060313A CN114506828A CN 114506828 A CN114506828 A CN 114506828A CN 202210060313 A CN202210060313 A CN 202210060313A CN 114506828 A CN114506828 A CN 114506828A
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000009826 distribution Methods 0.000 claims abstract description 214
- 239000007789 gas Substances 0.000 claims abstract description 141
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 75
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 12
- 239000010439 graphite Substances 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 239000008187 granular material Substances 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- 230000006835 compression Effects 0.000 claims description 32
- 238000007906 compression Methods 0.000 claims description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 239000006229 carbon black Substances 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 9
- 238000007789 sealing Methods 0.000 description 11
- 239000000919 ceramic Substances 0.000 description 4
- 239000007770 graphite material Substances 0.000 description 4
- 239000000945 filler Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007833 carbon precursor Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 229910004261 CaF 2 Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 229910003443 lutetium oxide Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0726—Preparation by carboreductive nitridation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention relates to a low-cost preparation process of aluminum nitride powder, which is prepared by utilizing a graphite furnace, wherein the graphite furnace comprises a gas distribution system and a reaction device; sieving the mixed powder to obtain granules; introducing nitrogen into a gas distribution system, wherein the gas distribution system is provided with a gas distribution power part and two linked gas distribution devices, each gas distribution device comprises a gas distribution air inlet and a gas distribution air outlet, each gas distribution air inlet is communicated with an air inlet fan, the air inlet fan blows the nitrogen into each gas distribution air inlet, each gas distribution air outlet is communicated with a corresponding reaction device, the nitrogen blown by the air inlet fan enters the corresponding reaction device through the gas distribution air outlet, and the gas distribution power part controls each gas distribution device to output the same quality of nitrogen; placing the granulated material in each reaction device for sintering, and introducing flowing nitrogen all the time in the sintering process; each reaction device is communicated with an exhaust fan so as to extract reaction products; cooling along with the furnace; excessive nitrogen gas introduction is not needed, and the cost is greatly saved.
Description
Technical Field
The invention relates to the technical field of aluminum nitride powder manufacturing, in particular to a low-cost aluminum nitride powder preparation process.
Background
The direct nitriding method is to produce porous aluminum nitride ceramic by using aluminum powder as main material, first producing porous formed body, and then putting it into nitrogen gas to make direct reaction and nitridation. The reaction formula of the aluminum metal nitridation is Al + N → AlN. Direct nitrogenization method needs to let in nitrogen gas in succession, and nitrogen gas per liter price is about seven yuan, for accelerating production speed, often lets in a plurality of reaction unit with nitrogen gas simultaneously, and the nitrogen gas volume that each nitrogen gas reaction unit lets in is difficult to guarantee the same, leads to like this in order to guarantee that the nitridation in every reaction unit is thorough, needs to let in excessive nitrogen gas, greatly increased the cost.
Disclosure of Invention
In order to overcome the technical defects in the prior art, the invention provides a low-cost aluminum nitride powder preparation process, excessive nitrogen gas is not required to be introduced, and the cost is greatly saved.
The technical solution adopted by the invention is as follows:
the low-cost aluminum nitride powder preparation process is characterized by utilizing a graphite furnace to prepare the aluminum nitride powder, wherein the graphite furnace comprises a gas distribution system and a reaction device, and the process comprises the following steps:
s1, preparing mixed powder;
s2, sieving the mixed powder prepared in the step S1 to prepare granules;
s3: introducing nitrogen into a gas distribution system, wherein the gas distribution system is provided with a gas distribution power part and two linked gas distribution devices, each gas distribution device comprises a gas distribution gas inlet and a gas distribution gas outlet, each gas distribution gas inlet is communicated with a gas inlet fan, the gas inlet fan blows the nitrogen into each gas distribution gas inlet, each gas distribution gas outlet is communicated with a corresponding reaction device, the nitrogen blown by the gas inlet fan enters the corresponding reaction device through the gas distribution gas outlet, and the gas distribution power part controls each gas distribution device to output the same quality of nitrogen;
s4, placing the granulated material in each reaction device, heating the reaction devices to 1700 ℃ in the nitrogen atmosphere fed from the gas distribution gas outlet, and preserving heat for 3 hours, wherein flowing nitrogen is always introduced in the sintering process;
s5: each reaction device is communicated with an exhaust fan so as to extract reaction products;
s6: and (5) cooling along with the furnace.
Preferably, the mixed powder comprises the following components in percentage by weight: 65% of alumina, 5% of sintering aid, 20% of carbon black and 10% of aluminum nitride seed crystal are respectively weighed, and the aluminum oxide powder is prepared after wet ball milling and drying.
Preferably, each of the air distribution devices in step S3 includes an air distribution box, a driving air distribution piston, and an air inlet and outlet control assembly, the air distribution box has an air compression cavity, the air distribution power part pushes the driving air distribution piston on two adjacent air distribution devices to slide along the air compression cavity, the air inlet and outlet control rod is located in the air compression cavity, and the air inlet and outlet control rod slides along the air distribution air inlet and the air distribution air outlet, and step S3 includes the following steps:
s31: the air inlet step, the air inlet and outlet control component opens the air distribution air inlet and seals the air distribution air outlet when the active air distribution piston slides along the air compression cavity to make the volume of the air compression cavity maximum;
s32: and in the exhaust step, the active air distribution piston slides along the air compression cavity to ensure that the volume of the air compression cavity is gradually reduced from the maximum, and the air inlet and exhaust control assembly seals the air distribution air inlet and opens the air distribution air outlet.
Preferably, the air intake and exhaust control assembly comprises an air intake and exhaust control rod and an air intake and exhaust control gear, the air intake and exhaust control gear is in transmission connection with the active air distribution piston, the air intake and exhaust control gear is provided with a lifting thread in threaded connection with the exhaust control rod, the active air distribution piston is provided with an active air distribution rack meshed with the air intake and exhaust control gear, the air intake and exhaust control gear is provided with a limit baffle matched with the active air distribution rack, and the limit baffle limits the axial movement of the air intake and exhaust control gear.
Preferably, the alumina has an Al2O3 content of > 95% by weight.
Preferably, the alumina has an average particle size of 1 μm.
Preferably, the aluminum nitride seed crystal has an AlN content of > 95% by weight.
Preferably, the carbon black has a C content of > 95% by weight.
The invention has the beneficial effects that:
the nitrogen is introduced into a gas distribution system, the gas distribution system is provided with a gas distribution power part and two linked gas distribution devices, each gas distribution device comprises a gas distribution air inlet and a gas distribution air outlet, each gas distribution air inlet is communicated with a gas inlet fan, the gas inlet fan blows the nitrogen into each gas distribution air inlet, each gas distribution air outlet is communicated with a corresponding reaction device, the nitrogen blown by the gas inlet fan enters the corresponding reaction device through the gas distribution air outlet, the gas distribution power part controls each gas distribution device to output the same quality of nitrogen, the nitrogen introduction amount in each reaction device is ensured to be equal, the reaction process in each reaction device is ensured to be the same, excessive nitrogen introduction is not needed, and the cost is greatly saved.
Drawings
FIG. 1 is a schematic view of the overall structure of a graphite furnace used in the present invention.
Fig. 2 is a schematic structural diagram of the gas distribution system.
Fig. 3 is a schematic structural diagram of the air distribution device.
Fig. 4 is a schematic structural view of the active air distribution rack and the air intake and exhaust control gear.
Fig. 5 is a schematic view of the exhaust control lever.
Description of reference numerals:
1. an air intake fan;
2. an exhaust fan;
3. a gas distribution system; 31. a gas distribution device; 311. a gas distribution air inlet; 312. an air distribution air outlet; 313. a gas distribution box body; 3131. a gas distribution cylinder; 3132. a sealing cover; 314. an active gas distribution piston; 3141. an active gas distribution rack; 315. an intake and exhaust control assembly; 3151. an exhaust control lever; 31511. a rod body; 31512. an air intake strut group; 31513. an air inlet sealing plug; 31514. an air outlet sealing plug; 31515. an air outlet support rod group; 3152. an intake and exhaust control gear; 31521. a limit baffle; 32. a gas distribution power part; 33. a compressed air cavity;
4. a graphite bin;
5. a filler;
6. a passive displacer.
Detailed Description
The invention will be further described with reference to the accompanying drawings in which:
as shown in fig. 1 to 5, this example provides a low-cost aluminum nitride powder production process, which is carried out using a graphite furnace, the graphite furnace including a gas distribution system 3 and a reaction apparatus, and the process includes the following steps:
s1, preparing mixed powder;
s2, sieving the mixed powder prepared in the step S1 to prepare granules;
s3: introducing nitrogen into a gas distribution system 3, wherein the gas distribution system 3 is provided with a gas distribution power part 32 and two linked gas distribution devices 31, each gas distribution device 31 comprises a gas distribution air inlet 311 and a gas distribution air outlet 312, each gas distribution air inlet 311 is communicated with an air inlet fan 1, the air inlet fan 1 blows the nitrogen into each gas distribution air inlet 311, each gas distribution air outlet 312 is communicated with a corresponding reaction device, the nitrogen blown in by the air inlet fan 1 enters the corresponding reaction device through the gas distribution air outlet 312, the gas distribution power part 32 controls each gas distribution device 31 to output the same quality of nitrogen, the nitrogen introduced into each reaction device is equal, the reaction processes in each reaction device are same, excessive nitrogen introduction is not needed, and the cost is greatly saved;
each air distribution device 31 in the step S3 includes an air distribution box 313, a driving air distribution piston 314, and an air inlet and outlet control assembly 315, the air distribution box 313 has an air compression cavity 33, the air distribution power assembly 32 pushes the driving air distribution piston 314 on two adjacent air distribution devices 31 to slide along the air compression cavity 33, the air inlet and outlet control rod 3151 is located in the air compression cavity 33, and the air inlet and outlet control rod 3151 slides along the air distribution air inlet 311 and the air distribution air outlet 312, and the step S3 includes the following steps:
s31: an air inlet step, in which the air inlet and outlet control component 315 opens the air distribution air inlet 311 and seals the air distribution air outlet 312 when the active air distribution piston 314 slides along the air pressure chamber 33 to enable the volume of the air pressure chamber 33 to be maximum;
s32: in the exhaust step, the intake and exhaust control assembly 315 seals the air distribution inlet 311 and opens the air distribution outlet 312 in the process that the active air distribution piston 314 slides along the air compression chamber 33 to reduce the volume of the air compression chamber 33 from the maximum to the minimum.
S4, placing the granulated material in each reaction device, heating the reaction device to 1700 ℃ in the nitrogen atmosphere fed from the gas distribution air outlet 312, and preserving heat for 3 hours, wherein flowing nitrogen is always introduced in the sintering process;
s5: each reaction device is communicated with the exhaust fan 2, and then reaction products are extracted;
s6: and (5) cooling along with the furnace.
The mixed powder comprises the following components in percentage by weight: 65% of alumina, 5% of sintering aid, 20% of carbon black and 10% of aluminum nitride seed crystal are respectively weighed, and the aluminum oxide is prepared after wet ball milling and drying, wherein the content of Al2O3 in the alumina is more than 95% by weight, the content of the sintering aid is more than 10%, the shrinkage rate of the porous ceramic is increased, and the porosity is reduced and a large amount of intercrystalline glass phase is caused. A content of less than 1% results in a low degree of densification by sintering and a decrease in mechanical properties. The sintering aid herein mainly refers to a metal oxide which changes into glass in the high temperature field of sintering, and also includes a mixture in which oxides of one or more components can change into a glass phase by reaction, and some fluorides. Such a sintering aid is selected from any one of group Ia oxides Li2O, group IIa oxides MgO, group IIIa oxides B2O3, rare earth element oxides Yb2O3, Lu2O3, La2O3, Y2O3, fluorides YF3, CaF 2.
The average particle size of alumina is 1 μm, and if the average particle size is less than 0.2 μm, the powder is easy to agglomerate, which is not beneficial to carbothermic reduction reaction, and the porosity of the aluminum nitride porous ceramic formed by more than 2 μm is too high, the crystal grain is coarse, and the mechanical property is reduced.
The porosity of the porous ceramic is reduced when the aluminum nitride seed crystal exceeds 10%, and the cost of raw materials is increased. If less than 1%, the carbothermic reduction reaction may be incomplete, and the AlN content may be more than 95% by weight.
Carbon black, having a C content of > 95% by weight, can be any form of carbon, for example charcoal, carbon black, also including carbon precursors, such as various resins, and mixtures of carbon black and carbon precursors can also be used.
Specifically, the graphite furnace comprises an air inlet fan 1, an air outlet fan 2, an air control and distribution system 3 and two reaction devices, wherein the air distribution system 3 is provided with an air distribution power part 32 and two linkage air distribution devices 31, each air distribution device 31 comprises an air distribution air inlet 311 and an air distribution air outlet 312, each air distribution air inlet 311 is communicated with the air inlet fan 1, the air inlet fan 1 blows nitrogen into each air distribution air inlet 311, each air distribution air outlet 312 is communicated with the corresponding reaction device, the nitrogen blown in by the air inlet fan 1 enters the corresponding reaction device through the air distribution air outlet 312, and each reaction device is communicated with the air outlet fan 2 so as to draw out a reaction product.
Each air distribution device 31 comprises an air distribution box body 313, an active air distribution piston 314 and an air inlet and exhaust control assembly 315, the air distribution box body 313 is provided with an air pressure cavity 33, the air distribution power part 32 pushes the active air distribution pistons 314 on two adjacent air distribution devices 31 to slide along the air pressure cavity 33, the air distribution power part 32 is a double-acting air cylinder, two output ends of the air distribution power part 32 respectively extend into the air pressure cavities 33 of the corresponding air distribution box bodies 313 to be in transmission connection with the corresponding active air distribution pistons 314, so that the volume in the air pressure cavities 33 is changed, the air inlet and exhaust control assembly 315 is used for controlling the communication and the sealing of the air distribution air inlet 311 and the air distribution air outlet 312, the air inlet and exhaust control assembly 315 is in transmission connection with the active air distribution pistons 314, namely, the action of the active air distribution pistons 314 drives the air inlet and exhaust control assembly 315 to move.
When the air compression chamber 33 is used for air intake, the air intake and exhaust control assembly 315 opens the air distribution air inlet 311 and the air distribution air outlet 312 to be synchronously closed, the air distribution power part 32 drives the active air distribution piston 314 to slide along the air compression chamber 33 so as to increase the volume of the air compression chamber 33, the air intake fan 1 sends nitrogen into the air compression chamber 33, when the air compression chamber 33 is used for air exhaust, the air intake and exhaust control assembly 315 closes the air distribution air inlet 311 and the air distribution air outlet 312 to be synchronously opened, the air distribution power part 32 drives the active air distribution piston 314 to slide along the air compression chamber 33 so as to reduce the volume of the air compression chamber 33, and the air intake fan 1 pumps the nitrogen out of the air distribution air outlet 312 from the air compression chamber 33 so as to send the nitrogen to each reaction device.
The method for controlling the opening and closing states of the air distribution inlet 311 and the air distribution outlet 312 by the air inlet and outlet control component 315 driven by the movement of the active air distribution piston 314 is as follows: the air intake and exhaust control assembly 315 comprises an air intake and exhaust control rod 3151 and an air intake and exhaust control gear 3152, the air intake and exhaust control rod 3151 is positioned in the air compression chamber 33, the air intake and exhaust control rod 3151 slides along the air distribution air inlet 311 and the air distribution air outlet 312, the air intake and exhaust control gear 3152 is in transmission connection with the active air distribution piston 314, the air intake and exhaust control gear 3152 is provided with a lifting thread in threaded connection with the exhaust control rod 3151, the active air distribution piston 314 is provided with an active air distribution rack 3141 engaged with the air intake and exhaust control gear 3152, the air intake and exhaust control gear 3152 is provided with a limit baffle 31521 matched with the active air distribution rack 3141, the limit baffle 31521 limits the axial movement of the air intake and exhaust control gear 3152, the active air distribution piston 314 drives the air intake and exhaust control gear 3152 to rotate when moving, the air intake and exhaust control gear 3152 and the lifting thread on the air intake and exhaust control gear 3152 rotate to drive the exhaust control rod 3151 to lift, it should be noted that the air distribution inlet 311 and the air distribution outlet 312 are provided with elongated slots (not shown in the figure) for limiting the rotation of the exhaust control rod 3151, the air distribution inlet 311 is opened by the air distribution control rod 3151 to seal the air distribution outlet 312 when the active air distribution piston 314 slides along the air compression chamber 33 to make the volume of the air compression chamber 33 maximum, the air distribution inlet 311 is sealed by the air distribution control rod 3151 to open the air distribution outlet 312 when the active air distribution piston 314 slides along the air compression chamber 33 to make the volume of the air compression chamber 33 gradually decrease from maximum, and the volumes of the air compression chambers 33 are the same, so that the air supply amount of the air compression chambers 33 is kept equal, the same air supply amount of each reaction device is ensured, and the same product quality is ensured.
In order to increase the reaction speed, the reaction device is provided with a plurality of graphite material boxes 4, the graphite material boxes 4 are connected in series to form a row through connecting pipelines, the air inlet of each row of graphite material boxes 4 is communicated with the air distribution air outlet 312 of the corresponding air distribution device 31, the air outlet of each row of graphite material boxes 4 is communicated with the exhaust fan 2, each graphite box can be filled with reaction raw materials, and the reaction speed is increased.
The gas distribution device 31 further comprises a passive gas distribution piston 6, a gas distribution box body 313 is composed of a gas distribution cylinder 3131 and sealing covers 3132 for sealing two ends of the gas distribution cylinder 3131, the sealing covers 3132 are arranged to facilitate installation of the passive gas distribution piston 6 and the active gas distribution piston 314, the passive gas distribution piston 6 slides along the gas pressing cavity 33, a passive gas distribution rack meshed with the gas inlet and outlet control gear 3152 is arranged on the passive gas distribution piston 6, a plurality of fillers 5 are arranged in an area where the active gas distribution piston 314 cannot reach in the gas pressing cavity 33, the passive gas distribution rack and the active gas distribution rack 3141 have certain lengths to prevent the passive gas distribution piston 6 and the active gas distribution piston 314 from approaching each other, and when the passive gas distribution piston 6 and the active gas distribution piston 314 approach each other to the nearest position, the fillers 5 can ensure that gas in the gas pressing cavity 33 is exhausted completely, and the exhaust amount is accurate.
The air inlet and exhaust control rod 3151 comprises a rod body 31511, an air inlet support rod group 31512, an air inlet sealing plug 31513, an air outlet sealing plug 31514 and an air outlet support rod group 31515, which are sequentially arranged on the rod body 31511, wherein the air inlet support rod group 31512 slides along a long groove in the air distribution air inlet 311 to prevent axial rotation, the air outlet support rod group 31515 slides along the air distribution air outlet 312, the air inlet support rod group 31512 and the air outlet support rod group 31515 are respectively provided with three support rods which are distributed at equal angles to ensure the integral stability of the rod body 31511, the distance between the air inlet sealing plug 31513 and the farthest end of the air outlet sealing plug 31514 is larger than the inner diameter of the air compression chamber 33, and the air distribution air inlet 311 and the air distribution air outlet 312 are simultaneously communicated to avoid inaccurate air supply amount.
While there have been shown and described what are at present considered the fundamental principles and essential features of the invention and its advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (8)
1. The preparation process of low-cost aluminum nitride powder is characterized by utilizing a graphite furnace for preparation, wherein the graphite furnace comprises a gas distribution system and a reaction device, and the process comprises the following steps:
s1, preparing mixed powder;
s2, sieving the mixed powder prepared in the step S1 to prepare granules;
s3: introducing nitrogen into a gas distribution system, wherein the gas distribution system is provided with a gas distribution power part and two linked gas distribution devices, each gas distribution device comprises a gas distribution gas inlet and a gas distribution gas outlet, each gas distribution gas inlet is communicated with a gas inlet fan, the gas inlet fan blows the nitrogen into each gas distribution gas inlet, each gas distribution gas outlet is communicated with a corresponding reaction device, the nitrogen blown by the gas inlet fan enters the corresponding reaction device through the gas distribution gas outlet, and the gas distribution power part controls each gas distribution device to output the same quality of nitrogen;
s4, placing the granulated material in each reaction device, heating the reaction devices to 1700 ℃ in the nitrogen atmosphere fed from the gas distribution gas outlet, and preserving heat for 3 hours, wherein flowing nitrogen is always introduced in the sintering process;
s5: each reaction device is communicated with an exhaust fan so as to extract reaction products;
s6: and (5) cooling along with the furnace.
2. The process for preparing the low-cost aluminum nitride powder according to claim 1, wherein the mixed powder comprises, in weight percent: 65% of alumina, 5% of sintering aid, 20% of carbon black and 10% of aluminum nitride seed crystal are respectively weighed, and the aluminum oxide powder is prepared after wet ball milling and drying.
3. The process for preparing low-cost aluminum nitride powder according to claim 1, wherein each of the gas distribution devices in step S3 comprises a gas distribution box, a driving gas distribution piston and a gas inlet and outlet control assembly, the gas distribution box has a gas pressure chamber, the gas distribution power assembly pushes the driving gas distribution piston on two adjacent gas distribution devices to slide along the gas pressure chamber, the gas inlet and outlet control rod is located in the gas pressure chamber and the gas inlet and outlet control rod slides along the gas distribution gas inlet and outlet, and step S3 comprises the following steps:
s31: the air inlet step, the air inlet and outlet control component opens the air distribution air inlet and seals the air distribution air outlet when the active air distribution piston slides along the air compression cavity to make the volume of the air compression cavity maximum;
s32: and in the exhaust step, the active air distribution piston slides along the air compression cavity to ensure that the volume of the air compression cavity is gradually reduced from the maximum, and the air inlet and exhaust control assembly seals the air distribution air inlet and opens the air distribution air outlet.
4. The process for preparing low-cost aluminum nitride powder according to claim 3, wherein the air intake and exhaust control assembly comprises an air intake and exhaust control rod and an air intake and exhaust control gear, the air intake and exhaust control gear is in transmission connection with a driving air distribution piston, the air intake and exhaust control gear is provided with a lifting thread in threaded connection with the exhaust control rod, the driving air distribution piston is provided with a driving air distribution rack engaged with the air intake and exhaust control gear, the air intake and exhaust control gear is provided with a limit baffle matched with the driving air distribution rack, and the limit baffle limits the axial movement of the air intake and exhaust control gear.
5. The process for producing low-cost aluminum nitride powder as claimed in claim 1, wherein the alumina has an Al2O3 content of > 95% by weight.
6. The process for producing the low-cost aluminum nitride powder as claimed in claim 1, wherein the average particle size of the aluminum oxide is 1 μm.
7. The process for producing a low-cost aluminum nitride powder as claimed in claim 1, wherein the aluminum nitride seed crystal has an AlN content of > 95% by weight.
8. The process for producing the aluminum nitride powder according to claim 1, wherein the carbon black has a C content of > 95% by weight.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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