CN108997019A - graphite crucible and its manufacturing method - Google Patents
graphite crucible and its manufacturing method Download PDFInfo
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- CN108997019A CN108997019A CN201710406654.8A CN201710406654A CN108997019A CN 108997019 A CN108997019 A CN 108997019A CN 201710406654 A CN201710406654 A CN 201710406654A CN 108997019 A CN108997019 A CN 108997019A
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/10—Crucibles or containers for supporting the melt
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
- C30B29/06—Silicon
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
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- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/52—Constituents or additives characterised by their shapes
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Abstract
The present invention provides a kind of graphite crucible and its manufacturing method, comprising: 1) provides a crucible die；2) Perhydropolysilazane fiber is provided, cross lapping is carried out after shredding processing and needle thorn consolidation produces Perhydropolysilazane fibrofelt, obtains silicon nitride fiber felt after ammonia pyrolysis and sintering；3) in the binder for coating graphitiferous raw material in the crucible die, the silicon nitride fiber felt is bedded on the binder；4) repeat step 3)；5) mold separation is carried out after solidifying obtains crucible template；6) carbonization and graphitization processing are carried out, graphite crucible is obtained.The present invention prepares continuous silicon nitride fiber felt by dry spinning and needle thorn consolidation, has many advantages, such as that the coefficient of expansion is low, thermal conductivity is good, mechanical performance is superior；By the way that continuous silicon nitride fiber felt is arranged in graphite crucible wall, graphite crucible can be substantially reduced due to the deformation extent in thermal expansion and cooling procedure, avoid the generation of graphite crucible crackle.
Description
Technical field
The present invention relates to a kind of semiconductor manufacturing facility and manufacturing methods, more particularly to a kind of graphite crucible and its manufacture
Method.
Background technique
Czochralski method is a kind of method of synthetic crystal by Czochralski (Czochralski) invention in 1917, so
Also referred to as " Czoncharlski method " is a kind of method from the raw material of molten condition growth crystal.The principle of czochralski method is to utilize temperature
Field control comes so that the raw material of melting grows into crystal.Raw material for crystal growth, which is placed in crucible, is heated as melt, control
Temperature Distribution (thermal field) in growth furnace processed, so that melt and seed crystal/crystal temperature have certain temperature gradient, at this moment, seed
Seed crystal on crystalline style is melted with melt contacts rear surface, lifts and rotate seed rod, the melt in supercooled state will
It crystallizes on seed crystal, and with lifting and rotary course, the weight of atom or molecule is constantly carried out on the interface of seed crystal and melt
New arrangement, gradually solidifies and grows monocrystal.
Silica crucible is a kind of general equipment for carrying frit reaction material.However, silica crucible is at high temperature
Softening transform can be generated.Therefore, it is extremely important for selecting a kind of material of shape that silica crucible can be supported to keep its original
's.
Since graphite has good heat resistance and thermal shock resistance, especially there is good chemical stability, graphite quilt
It is widely used in crucible field.Silica crucible 201 and graphite crucible 202 are used for device structure such as Fig. 1 institute of pulling silicon single crystal
Show, the raw material for monocrystalline silicon growing, which is placed in silica crucible, is heated as melt 204 by heater 205, controls growth furnace
Interior Temperature Distribution (thermal field), so that the temperature of melt 204 and seed crystal/crystal 205 has certain temperature gradient, at this moment, seed crystal
Seed crystal 203 on bar contacts rear surface with melt 204 and melts, and lifts and rotate seed rod, the melt in supercooled state
It will crystallize on seed crystal, and with lifting and rotary course, constantly carry out atom or molecule on the interface of seed crystal and melt
Rearrange, gradually solidify and grow monocrystal silicon.
But since the diameter of the silicon wafer of required stretching is bigger, the thermal expansion of silica crucible and graphite crucible mismatches effect
Should be more serious, this mismatch effect, which makes it obtain the supporting role of graphite crucible, can not fully meet application requirement.
Based on the above, it one kind is provided can be effectively improved graphite crucible and cause larger change since the coefficient of expansion is larger
The method and structure of shape is necessary.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of graphite crucible and its manufacturers
Method causes it to spend Gao Errong with silica crucible mismatch since the graphite crucible coefficient of expansion is high in the prior art for solving
Easily there is the problems such as crack.
In order to achieve the above objects and other related objects, the present invention provides a kind of manufacturing method of graphite crucible, the system
The method of making includes: 1) to provide a crucible die；2) Perhydropolysilazane fiber is provided, to the Perhydropolysilazane fiber opening
Cross lapping is carried out after processing, and consolidation technique is pierced by needle and produces Perhydropolysilazane fibrofelt, the poly- silicon nitrogen of perhydro
Alkane fibrofelt obtains silicon nitride fiber felt after ammonia is pyrolyzed and is sintered；3) in coating graphitiferous raw material in the crucible die
Binder, the silicon nitride fiber felt is bedded on the binder；4) repeat step 3), number of repetition N,
In, N > 0；5) it after carrying out curing process to the binder, carries out mold separation and obtains crucible template；6) to the crucible template
Carbonization and graphitization processing are carried out, graphite crucible is obtained.
Preferably, it includes: a) by SiH that step 2), which provides Perhydropolysilazane fiber,2Cl2And pyridine mix in proportion it is laggard
Row polymerization reaction and ammonolysis reaction obtain Perhydropolysilazane resin (PHS)；B) by the Perhydropolysilazane resin (PHS)
It is dissolved in organic solvent dimethylbenzene, obtains spinning solution；C) spinning solution is filtered, is obtained after dry spinning complete
Hydrogen polysilazane fiber.
Preferably, in step a), the SiH2Cl2And the mass ratio of the material of pyridine is between 1:1~1:3.
Preferably, in step a), the temperature range of the polymerization reaction is 80~220 DEG C, the atmosphere of the ammonolysis reaction
For ammonia atmosphere, temperature is room temperature.
Preferably, in step 2), the needle thorn consolidation technique is real by puncturing by Perhydropolysilazane fiber crossovers position
Fluffy Perhydropolysilazane fiber is fabricated to the Perhydropolysilazane of some strength and thickness fibre by now mutually winding
Tie up felt.
Preferably, the crucible die includes die main body and mold bottom, and step 3) includes: 3-1) the first nitrogen is provided
SiClx fibrofelt, in the binder for coating graphitiferous raw material in the die main body, by the first silicon nitride fiber felt bedding
In on the binder；The second silicon nitride fiber felt 3-2) is provided, in the bonding for coating graphitiferous raw material in the mold bottom
The second silicon nitride fiber felt is bedded on the binder by agent；Wherein, the nitridation in the second silicon nitride fiber felt
The length of silica fibre is less than the length of the silicon nitride fiber in the first silicon nitride fiber felt.
Preferably, the binder of the graphitiferous raw material is the mixture of powdered graphite and resin material.
Preferably, the diameter range of the silicon nitride fiber in the silicon nitride fiber felt is 4~20 μm.
Preferably, the silicon nitride fiber felt includes multiple first direction silicon nitride fiber arranged in parallel along first direction
And multiple second direction silicon nitride fibers arranged in parallel in a second direction, the folder between the first direction and second direction
Angle θ is 180 ° of 90 °≤θ <.
Preferably, the size of mesh opening range of the silicon nitride fiber felt is 0.1~2mm.
Preferably, it is 4~10 times that step 4), which repeats the number of step 3), and the silicon nitride fiber felt is parallel arrangement.
The present invention also provides a kind of graphite crucible, at least one layer of silicon nitride fiber felt, institute are provided in the graphite crucible
It states silicon nitride fiber felt and entire graphite crucible range, and the graphite of the silicon nitride fiber felt and the graphite crucible is completely covered
Material tight combines, and in the silicon nitride fiber felt, the crossover location of silicon nitride fiber is be combined with each other by needle thorn consolidation.
Preferably, the graphite crucible includes crucible body portion and crucible bottom, and the silicon nitride fiber felt includes setting
In the first silicon nitride fiber felt in crucible body portion and the second silicon nitride fiber felt being set in the crucible bottom,
In, the length of the silicon nitride fiber in the second silicon nitride fiber felt is less than the silicon nitride in the first silicon nitride fiber felt
The length of fiber.
Preferably, the diameter range of the silicon nitride fiber in the silicon nitride fiber felt is 4~20 μm.
Preferably, the silicon nitride fiber felt includes multiple first direction silicon nitride fiber arranged in parallel along first direction
And multiple second direction silicon nitride fibers arranged in parallel in a second direction, the folder between the first direction and second direction
Angle θ is 180 ° of 90 °≤θ <.
Preferably, the size of mesh opening range of the silicon nitride fiber felt is 0.1~2mm.
Preferably, the number of plies of the silicon nitride fiber felt is 4~10 layers, and the silicon nitride fiber felt is parallel arrangement.
As described above, graphite crucible and its manufacturing method of the invention, have the advantages that the present invention passes through dry method
Spinning technique prepares continuous silicon nitride fiber, and the silicon nitride fiber is with the coefficient of expansion is low, thermal conductivity is good, mechanical performance
The advantages that superior；Silicon nitride fiber felt is prepared by needle thorn consolidation, further improves mechanical strength；By in graphite crucible
The continuous silicon nitride fiber felt of one or more parallel arrangements is set in wall, forms continuous fiber-reinforced layer, it can be significantly
It reduces graphite crucible and the generation of graphite crucible crackle is avoided due to the deformation extent in thermal expansion and cooling procedure, and improve it
With the fitness of silica crucible.The present invention can effectively improve the quality of graphite crucible, have in semiconductor equipment and manufacturing field
Broad application prospect.
Detailed description of the invention
Fig. 1 is shown as graphite crucible and silica crucible in the prior art and illustrates applied to the device structure of pulling silicon single crystal
Figure.
Fig. 2 is shown as the step flow diagram of the manufacturing method of graphite crucible of the invention.
Fig. 3 is shown as in the manufacturing method of graphite crucible of the invention, silicon nitride fiber schematic diagram.
Fig. 4 a is shown as in the manufacturing method of graphite crucible of the invention, the device structure schematic diagram of dry spinning.
Fig. 4 b is shown as in the manufacturing method of graphite crucible of the invention, the device structure schematic diagram of needle thorn consolidation
Fig. 5~Fig. 6 is shown as in the manufacturing method of graphite crucible of the invention, the structural schematic diagram of silicon nitride fiber felt.
Fig. 7 is shown as the structural schematic diagram of the invention for reinforcing graphite crucible using silicon nitride fiber felt.
Component label instructions
10 silicon nitride fiber felts
101 silicon nitride fibers
301 head tanks
302 gear wheel metering pumps
303 spinning heads
304 spinning shafts
305 hot-airs
306 infeed disks
307 lead hook
308 twisting and winding mechanisms
309 air outlet slits
40 graphite crucibles
401 crucible body portions
402 crucible bottoms
501 first silicon nitride fiber felts
502 second silicon nitride fiber felts
601 main transmissions
602 needle plates
603 prickers
604 support halftones
605 stripping web plates
606 are fed for curtain
607 outlet rollers
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Please refer to Fig. 2~Fig. 7.It should be noted that diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, only shown in diagram then with related component in the present invention rather than package count when according to actual implementation
Mesh, shape and size are drawn, when actual implementation kenel, quantity and the ratio of each component can arbitrarily change for one kind, and its
Assembly layout kenel may also be increasingly complex.
As shown in Figure 2 to 7, the present embodiment provides a kind of manufacturing method of graphite crucible 40, the manufacturing method includes:
As shown in Fig. 2, carrying out step 1) S11 first, a crucible die is provided.
As an example, the crucible die is with certain rigid and material resistant to high temperature is formed, material can be with
It is separated for metal, such as stainless steel with smooth inner wall so that subsequent crucible template carries out grinding tool with crucible die,
Improve the quality of crucible template.
The crucible die includes die main body and mold bottom, and the die main body has cylindrical side wall, institute
Mold bottom is stated with cambered surface bottom, to cooperate with the shape of subsequent silica crucible.
As shown in Fig. 2~Fig. 6, step 2) S12 is then carried out, Perhydropolysilazane fiber is provided, to the poly- silicon of the perhydro
Cross lapping is carried out after the processing of azane fiber opening, and consolidation technique is pierced by needle and produces Perhydropolysilazane fibrofelt, institute
It states Perhydropolysilazane fibrofelt and obtains silicon nitride fiber felt after ammonia is pyrolyzed and is sintered.
As an example, the diameter range of the silicon nitride fiber 101 in the silicon nitride fiber felt 10 is 4~20 μm, this is straight
The silicon nitride fiber 101 of diameter range can be realized by dry-spinning process, and can guarantee the intensity of silicon nitride fiber 101.?
In the present embodiment, the diameter of the silicon nitride fiber 101 is 10 μm.
As shown in Figures 5 and 6, as an example, the silicon nitride fiber felt 10 includes multiple arranged in parallel along first direction
First direction silicon nitride fiber 101 and multiple second direction silicon nitride fibers 101 arranged in parallel in a second direction, it is described
Angle theta between first direction and second direction is 180 ° of 90 °≤θ <.Angle between the first direction and second direction
Preferably 90 °≤θ≤120 °, the size of mesh opening range of the silicon nitride fiber felt 10 are 0.1~2mm, can get higher-strength
Silicon nitride fiber felt 10.Fig. 5 is shown as the structural schematic diagram of the silicon nitride fiber felt 10 of θ=90 °, mesh parameter d1And d2
Range be 0.1~2mm.Fig. 6 is shown as the structural schematic diagram of the silicon nitride fiber felt 10 of θ=120 °, mesh parameter d3And d4
Range be 0.1~2mm.
There is provided Perhydropolysilazane fiber as shown in Fig. 3~Fig. 4 a, in step 2) includes:
Step a) S21 is carried out first, by SiH2Cl2And pyridine mix in proportion after carry out polymerization reaction and ammonolysis reaction, obtain
It obtains Perhydropolysilazane resin (PHS)；
As an example, in step a), the SiH2Cl2And amount (mole) ratio of the substance of pyridine is between 1:1~1:3.?
In the present embodiment, the SiH2Cl2And the mass ratio of the material of pyridine is 1:2.
As an example, using mechanical agitation methods by the SiH2Cl2And pyridine is mixed, and uniform mixture is obtained.
As an example, in step a), the temperature range of the polymerization reaction is 80~220 DEG C, be specifically as follows 100 DEG C,
150 DEG C etc., the atmosphere of the ammonolysis reaction is ammonia atmosphere, and temperature is room temperature.
Then step b) S22 is carried out, the Perhydropolysilazane resin (PHS) is dissolved in organic solvent, is spun
Silk stock solution.
As an example, it is dimethylbenzene that the organic solvent, which is selected, by stirring the Perhydropolysilazane resin (PHS)
And dimethylbenzene is uniformly mixed.
Then step c) S23 is carried out, the spinning solution is filtered, it is fine that Perhydropolysilazane is obtained after dry spinning
Dimension.
As an example, method used in the filtering is physical filtering, that is, use by nylon fabric protective layer and by filtering
Paper forms intermediate filter material matrix and is filtered to the spinning solution.
The present embodiment forms Perhydropolysilazane fiber using dry spinning, and the dry spinning equipment that the present embodiment uses is such as
Shown in Fig. 4 a comprising head tank 301, spinning head 303, spinning shaft 304, infeed disk 306, leads hook at gear wheel metering pump 302
307 and twisting and winding mechanism 308.After spinning solution is sent to head tank 301, gear wheel metering pump 302 is first passed around, it is described
Gear wheel metering pump 302 is by a pair of of pitch wheel, one of them is driving gear, another is driven gear,
Engagement is driven to rotate by driving gear, directly there are lesser gaps for the shell of gear and pump.When gear rotation when, the gear teeth by
In the imbibition chamber being gradually disengaged from, between cog sealed volume increases, and forms parital vacuum, and the spinning solution in head tank 301 is being pressed
Difference effect is lower to suck imbibition chamber, and as gear rotates, spinning solution divides two-way to be advanced between gear and shell by gear promotion,
It is sent to exhaust chamber, two gears are progressively engaged in exhaust chamber, volume reducing, and the liquid between gear is extruded into spinning head 303, lead to
Cross the revolving speed of measuring and calculating gear wheel metering pump, the flow of available gear wheel metering pump.Then, spinning head 303 is to the spinning shaft
304 carry out spinneret, and hot-air 305 enters the spinning shaft 304, by the organic solvent evaporation in spinning solution and carry to sky
309 discharge of gas outlet, the spinning that spinning head 303 sprays, which passes through infeed disk 306 and leads hook 307, is sent to twisting and winding mechanism 308,
Twisting and operating winding are carried out, Perhydropolysilazane fiber is obtained.
Then, cross lapping is carried out after handling the Perhydropolysilazane fiber opening of above-mentioned acquisition, and is pierced admittedly by needle
Knot technique produces Perhydropolysilazane fibrofelt, and the Perhydropolysilazane fibrofelt obtains after ammonia is pyrolyzed and is sintered
Silicon nitride fiber felt.
The present embodiment use needle thorn consolidation device it is as shown in Figure 4 b comprising main transmission 601, needle plate 602, pricker 603,
Stripping web plate 605, is fed for curtain 606 and outlet roller 607 at support halftone 604.The curtain 606 that is fed for is for after feeding cross lapping
Perhydropolysilazane fiber is simultaneously sent to the support halftone 604, and the pricker 603 is embedded on the needle plate 602, with main transmission
601 rotation and move up and down, by Perhydropolysilazane fiber crossovers position by puncture realize mutually winding, will be fluffy
Perhydropolysilazane fiber is fabricated to the Perhydropolysilazane fibrofelt with some strength and thickness, and the stripping web plate 605 is used
In in pricker 603 and when Perhydropolysilazane fiber separation, stop Perhydropolysilazane fiber, so that the pricker 603 and complete
Hydrogen polysilazane fiber is kept completely separate.
Finally, obtaining silicon nitride fiber felt, institute after carrying out ammonia pyrolysis and sintering to the Perhydropolysilazane fibrofelt
The atmosphere for stating ammonia pyrolysis is ammonia atmosphere, and temperature range is 1100 DEG C~1300 DEG C, is specifically as follows 1200 DEG C.The sintering
Atmosphere be high pure nitrogen atmosphere, temperature range be 1400 DEG C~1600 DEG C, be specifically as follows 1500 DEG C.
As shown in fig. 7, step 3) S13 is then carried out, it, will in the binder for coating graphitiferous raw material in the crucible die
The silicon nitride fiber felt 10 is bedded on the binder.
As an example, the crucible die includes die main body and mold bottom, step 3) includes:
First silicon nitride fiber felt 501 3-1) is provided, it, will in the binder for coating graphitiferous raw material in the die main body
The first silicon nitride fiber felt 501 is bedded on the binder；
Second silicon nitride fiber felt 502 3-2) is provided, it, will in the binder for coating graphitiferous raw material in the mold bottom
The second silicon nitride fiber felt 502 is bedded on the binder；Wherein, the nitrogen in the second silicon nitride fiber felt 502
The length of SiClx fiber 101 is less than the length of the silicon nitride fiber 101 in the first silicon nitride fiber felt 501.
Since die main body is usually cylinder design, and mold bottom is usually cambered surface design, by designing two parts
The silicon nitride fiber felt 10 of different length, can be more complete, and more continuously covers entire crucible die, can greatly enhance stone
The mechanical strength of black crucible 40 inhibits its deformation degree.
As an example, the binder of the graphitiferous raw material is the mixture of powdered graphite and resin material.The mixture
It is subsequent be carbonized and be graphitized after formed graphite crucible 40 main body.
As shown in Fig. 2, then carrying out step 4) S14, repeat step 3), number of repetition N, wherein N > 0；
As an example, the number that step 4) repeats step 3) is 4~10 times, and the silicon nitride fiber felt 10 is parallel
Cloth.Repetition is arranged the silicon nitride fiber felts 10 of multiple parallel arrangements, and the graphite crucible 40 of more high mechanical strength can be obtained.
As shown in Fig. 2, then carrying out step 5) S15, after carrying out curing process to the binder, carries out mold separation and obtain
Obtain crucible template.
As shown in Fig. 2 and Fig. 7, step 6) S16 is finally carried out, carbonization and graphitization processing are carried out to the crucible template,
Obtain graphite crucible 40.
As shown in fig. 7, the present embodiment also provides a kind of graphite crucible 40, at least one layer is provided in the graphite crucible 40
Entire 40 range of graphite crucible, and the silicon nitride fiber is completely covered in silicon nitride fiber felt 10, the silicon nitride fiber felt 10
Felt 10 and the graphite material of the graphite crucible 40 are combined closely, in the silicon nitride fiber felt 10, the intersection of silicon nitride fiber
Position is be combined with each other by needle thorn consolidation.Wherein, Fig. 7 shows only the setting form of silicon nitride fiber felt 10, graphite material
It does not provide, but its shape is corresponding with the shape of silicon nitride fiber felt 10 in Fig. 7.
As an example, the graphite crucible 40 includes crucible body portion 401 and crucible bottom 402, the silicon nitride fiber
Felt 10 includes the first silicon nitride fiber felt 501 being set in crucible body portion 401 and is set in the crucible bottom 402
The second silicon nitride fiber felt 502, wherein the length of the silicon nitride fiber 101 in the second silicon nitride fiber felt 502 is less than
The length of silicon nitride fiber 101 in the first silicon nitride fiber felt 501.
As an example, the diameter range of the silicon nitride fiber 101 in the silicon nitride fiber felt 10 is 4~20 μm.
As an example, the silicon nitride fiber felt 10 includes multiple first direction silicon nitrides arranged in parallel along first direction
Fiber 101 and multiple second direction silicon nitride fibers 101 arranged in parallel in a second direction, the first direction and second party
Angle theta between is 180 ° of 90 °≤θ <.
As an example, the size of mesh opening range of the silicon nitride fiber felt 10 is 0.1~2mm.
As an example, the number of plies of the silicon nitride fiber felt 10 is 4~10 layers, and the silicon nitride fiber felt 10 is parallel
Arrangement.
As described above, graphite crucible 40 of the invention and its manufacturing method, it is dry to have the advantages that the present invention passes through
Method spinning technique prepares continuous silicon nitride fiber 101, the silicon nitride fiber 101 have the coefficient of expansion is low, thermal conductivity is good,
The advantages that mechanical performance is superior；Silicon nitride fiber felt 10 is prepared by needle thorn consolidation, further improves mechanical strength；Pass through
The continuous silicon nitride fiber felt 10 of one or more parallel arrangements is set in 40 wall of graphite crucible, forms continuous fiber and increases
Strong layer can substantially reduce graphite crucible 40 due to the deformation extent in thermal expansion and cooling procedure, graphite crucible 40 is avoided to split
The generation of line, and improve its fitness with silica crucible.The present invention can effectively improve the quality of graphite crucible 40, in semiconductor
Equipment and manufacturing field are with a wide range of applications.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (17)
1. a kind of manufacturing method of graphite crucible, which is characterized in that the manufacturing method includes:
1) crucible die is provided；
2) Perhydropolysilazane fiber is provided, carries out cross lapping after handling the Perhydropolysilazane fiber opening, and lead to
It crosses needle thorn consolidation technique and produces Perhydropolysilazane fibrofelt, the Perhydropolysilazane fibrofelt is pyrolyzed and burns by ammonia
Silicon nitride fiber felt is obtained after knot；
3) in the binder for coating graphitiferous raw material in the crucible die, the silicon nitride fiber felt is bedded in the bonding
In agent；
4) repeat step 3), number of repetition N, wherein N > 0；
5) it after carrying out curing process to the binder, carries out mold separation and obtains crucible template；
6) carbonization and graphitization processing are carried out to the crucible template, obtains graphite crucible.
2. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: step 2) provides Perhydropolysilazane
Fiber includes:
A) by SiH2Cl2And pyridine mix in proportion after carry out polymerization reaction and ammonolysis reaction, obtain Perhydropolysilazane resin
(PHS)；
B) the Perhydropolysilazane resin (PHS) is dissolved in organic solvent dimethylbenzene, obtains spinning solution；
C) spinning solution is filtered, Perhydropolysilazane fiber is obtained after dry spinning.
3. the manufacturing method of graphite crucible according to claim 2, it is characterised in that: in step a), the SiH2Cl2And
The mass ratio of the material of pyridine is between 1:1~1:3.
4. the manufacturing method of graphite crucible according to claim 2, it is characterised in that: in step a), the polymerization reaction
Temperature range be 80~220 DEG C, the atmosphere of the ammonolysis reaction is ammonia atmosphere, and temperature is room temperature.
5. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: in step 2), the needle thorn consolidation
Mutually winding is realized by puncturing in Perhydropolysilazane fiber crossovers position by technique, by fluffy Perhydropolysilazane fiber
It is fabricated to the Perhydropolysilazane fibrofelt with some strength and thickness.
6. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: the crucible die includes mold
Portion and mold bottom, step 3) include:
The first silicon nitride fiber felt 3-1) is provided, in the binder for coating graphitiferous raw material in the die main body, by described the
One silicon nitride fiber felt is bedded on the binder；
The second silicon nitride fiber felt 3-2) is provided, in the binder for coating graphitiferous raw material in the mold bottom, by described the
Nitride silica fibre felt is bedded on the binder；
Wherein, the length of the silicon nitride fiber in the second silicon nitride fiber felt is less than in the first silicon nitride fiber felt
The length of silicon nitride fiber.
7. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: the binder of the graphitiferous raw material
For the mixture of powdered graphite and resin material.
8. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: the nitrogen in the silicon nitride fiber felt
The diameter range of SiClx fiber is 4~20 μm.
9. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: the silicon nitride fiber felt includes more
A first direction silicon nitride fiber arranged in parallel along first direction and multiple second directions arranged in parallel in a second direction
Silicon nitride fiber, the angle theta between the first direction and second direction are 180 ° of 90 °≤θ <.
10. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: the net of the silicon nitride fiber felt
Lattice size range is 0.1~2mm.
11. the manufacturing method of graphite crucible according to claim 1, it is characterised in that: step 4) repeats time of step 3)
Number is 4~10 times, and the silicon nitride fiber felt is parallel arrangement.
12. a kind of graphite crucible, which is characterized in that at least one layer of silicon nitride fiber felt is provided in the graphite crucible, it is described
Entire graphite crucible range, and the graphite material of the silicon nitride fiber felt and the graphite crucible is completely covered in silicon nitride fiber felt
Material is combined closely, and in the silicon nitride fiber felt, the crossover location of silicon nitride fiber is be combined with each other by needle thorn consolidation.
13. graphite crucible according to claim 12, it is characterised in that: the graphite crucible includes crucible body portion and earthenware
Crucible bottom, the silicon nitride fiber felt include the first silicon nitride fiber felt being set in crucible body portion and are set to described
The second silicon nitride fiber felt in crucible bottom, wherein the length of the silicon nitride fiber in the second silicon nitride fiber felt is small
The length of silicon nitride fiber in the first silicon nitride fiber felt.
14. graphite crucible according to claim 12, it is characterised in that: the silicon nitride fiber in the silicon nitride fiber felt
Diameter range be 4~20 μm.
15. graphite crucible according to claim 12, it is characterised in that: the silicon nitride fiber felt includes multiple along first
Direction first direction silicon nitride fiber arranged in parallel and multiple second direction silicon nitrides arranged in parallel in a second direction are fine
Dimension, the angle theta between the first direction and second direction are 180 ° of 90 °≤θ <.
16. graphite crucible according to claim 12, it is characterised in that: the size of mesh opening range of the silicon nitride fiber felt
For 0.1~2mm.
17. graphite crucible according to claim 12, it is characterised in that: the number of plies of the silicon nitride fiber felt is 4~10
Layer, and the silicon nitride fiber felt is parallel arrangement.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113370591A (en) * | 2021-07-12 | 2021-09-10 | 成都东骏激光股份有限公司 | High-temperature volatilization inhibition device and method and application of device |
| CN114315399A (en) * | 2021-12-23 | 2022-04-12 | 湖南金博碳素股份有限公司 | Carbon/carbon composite die and preparation method and application thereof |
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| JPS61256993A (en) * | 1985-05-09 | 1986-11-14 | Toyo Tanso Kk | Graphite crucible and heater for silicon single crystal pulling device |
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| CN113370591B (en) * | 2021-07-12 | 2022-12-23 | 成都东骏激光股份有限公司 | High-temperature volatilization inhibition device and method and application of device |
| CN114315399A (en) * | 2021-12-23 | 2022-04-12 | 湖南金博碳素股份有限公司 | Carbon/carbon composite die and preparation method and application thereof |
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