CN114105641A - Production process of photovoltaic graphite crucible - Google Patents
Production process of photovoltaic graphite crucible Download PDFInfo
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- CN114105641A CN114105641A CN202111288161.1A CN202111288161A CN114105641A CN 114105641 A CN114105641 A CN 114105641A CN 202111288161 A CN202111288161 A CN 202111288161A CN 114105641 A CN114105641 A CN 114105641A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000010439 graphite Substances 0.000 title claims abstract description 75
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 50
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000010426 asphalt Substances 0.000 claims abstract description 19
- 239000002006 petroleum coke Substances 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000006229 carbon black Substances 0.000 claims abstract description 14
- 238000007598 dipping method Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000000571 coke Substances 0.000 claims abstract description 8
- 239000006253 pitch coke Substances 0.000 claims abstract description 7
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- 230000004888 barrier function Effects 0.000 claims abstract description 4
- 238000000748 compression moulding Methods 0.000 claims abstract description 4
- 239000004615 ingredient Substances 0.000 claims abstract description 4
- 230000001965 increasing effect Effects 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 20
- 238000005470 impregnation Methods 0.000 claims description 11
- 230000004584 weight gain Effects 0.000 claims description 9
- 235000019786 weight gain Nutrition 0.000 claims description 9
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000011295 pitch Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 4
- 239000001087 glyceryl triacetate Substances 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 229960002622 triacetin Drugs 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 239000011294 coal tar pitch Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 description 11
- 238000001816 cooling Methods 0.000 description 5
- 238000010248 power generation Methods 0.000 description 5
- 238000001354 calcination Methods 0.000 description 3
- 239000011300 coal pitch Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 230000009172 bursting Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000002633 protecting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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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
- 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
- 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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- 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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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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Abstract
The invention relates to a production process of a graphite crucible for photovoltaic. The production process comprises the following steps: s1 providing pitch coke, petroleum coke and carbon black, providing moisture barrier material and pitch; s2, sequentially adding the asphalt coke, the petroleum coke, the carbon black and the moisture-proof material into a kneader for mixing to obtain a mixed raw material; s3, obtaining mixed ingredients; s4, rolling the mixed material to form a sheet, and grinding the sheet to obtain powder; s5, carrying out compression molding treatment on the powder by using a crucible mold to obtain a parison; s6, roasting and dipping to obtain a roasted blank; and S7 graphitizing the roasted blank to obtain the graphite crucible. The roasting treatment is carried out by raising and lowering the temperature based on a 576-hour roasting temperature curve. The resistivity of the graphite crucible is 12-13 mu omega m. The production process has the advantages of strong pertinence, high production specialization degree, high production efficiency and high product quality, is suitable for large-scale production, and produces the obtained graphite with good application safety.
Description
Technical Field
The invention relates to a production process, in particular to a production process of a graphite crucible for photovoltaic.
Background
Photovoltaic power generation refers to a solar panel made of semiconductor materials such as silicon, which generates direct current based on illumination, and single crystal silicon is drawn in a single crystal furnace using a graphite crucible as a thermal field and using high-purity polycrystalline silicon, and thus the graphite crucible is an important tool in photovoltaic power generation technology and needs to be produced specifically.
However, the existing production process has the problems of weak pertinence, low production specialization degree, low production efficiency, poor product quality, low production cost and short product service life, cannot meet the requirement of large-scale production, and has poor application safety of graphite products.
Disclosure of Invention
Therefore, it is necessary to provide a production process of a graphite crucible for photovoltaic use aiming at the problems that the existing production process is not strong in pertinence, low in production specialization degree, low in production efficiency, poor in product quality, low in production cost, short in product service life, incapable of meeting the requirement of large-scale production, and poor in safety of application of graphite products.
A production process of a graphite crucible for photovoltaic comprises the following steps:
s1 providing pitch coke, petroleum coke and carbon black, providing moisture barrier material and pitch;
s2, sequentially adding the asphalt coke, the petroleum coke, the carbon black and the moisture-proof material into a kneader for mixing to obtain a mixed raw material;
s3, stirring and mixing the asphalt and the mixed raw materials to obtain a mixed material;
s4, rolling the mixed material to form a sheet, and grinding the sheet to obtain powder;
s5, carrying out compression molding treatment on the powder by using a crucible mold to obtain a parison;
s6, roasting and dipping to obtain a roasted blank;
the roasting treatment is carried out on the basis of a 576-hour roasting temperature curve to carry out temperature rise and temperature reduction;
s7, graphitizing the roasted blank to obtain a graphite crucible;
the resistivity of the graphite crucible is 12-13 mu omega m.
The production process is specially directed at the graphite crucible for the photovoltaic power generation panel, has the advantages of strong pertinence, high production specialization degree, high production efficiency and high product quality, reduces the production cost, prolongs the service life of the product, and is suitable for large-scale production.
In one embodiment, modified asphalt is boiled at 160-165 ℃ and then is kept stand for 100-120 hours to prepare the asphalt; the moisture-proof material adopts triacetin.
In one embodiment, the mass ratio of the asphalt coke, the petroleum coke and the carbon black in the mixed raw material is 4:5.5: 0.5; the mass ratio of the mixed raw materials to the asphalt in the mixed ingredients is 41: 42.
in one embodiment, the thickness of the thin sheet is 2-2.5 mm; and (3) putting the slices into a 5R pendulum type grinding machine, grinding to obtain powder, and sieving the powder by using a 200-mesh sieve, wherein the balance of the sieve is 20-25%.
In one embodiment, the crucible moldA resisting block is welded inside; the abutting block is positioned at the center of the bottom of a crucible cavity of the crucible mold; the density of the pressing die is 1.45-1.46 g/cm3。
In one embodiment, the 576-hour roasting temperature curve is that the temperature is rapidly increased to 350 ℃, then uniformly increased to 520 ℃ at the temperature increasing speed of 5 ℃/8h and kept for 24h, then uniformly increased to 1250 ℃ at the temperature increasing speed of 27 ℃/8h and kept for 48h, and then the fire is shut off.
In one embodiment, the method of bake-dip treatment operates as follows:
s61, after primary roasting treatment is carried out on the parison, primary dipping treatment is continuously carried out on the roasted product, and a mixture A is obtained;
s62, after the mixture A is subjected to secondary roasting treatment, the roasted product is continuously subjected to secondary impregnation treatment to obtain a mixture B;
s63, after the mixture B is roasted for three times, the roasted product is continuously impregnated for three times to obtain a mixture C, namely a roasted blank.
Further, the weight gain rate of the primary impregnation is 18-19%; the weight gain rate of the secondary impregnation is 13-14%; the weight gain rate of the three times of dipping is 9-10%; the impregnation treatment is carried out in medium temperature coal tar pitch.
In one embodiment, the bottom of the graphite crucible is a concave structure, wherein the concave structure is matched with the abutting block.
In one embodiment, the roasted blank is put into an Acheson furnace, and the roasted blank is graphitized at the temperature of 2800-2900 ℃ to obtain the graphite crucible.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the roasting treatment is carried out by heating and cooling based on a 576-hour roasting temperature curve, wherein the 576-hour roasting temperature curve is that the temperature is rapidly increased to 350 ℃, then is uniformly increased to 520 ℃ at a heating rate of 5 ℃/8h and is kept for 24h, then is uniformly increased to 1250 ℃ at a heating rate of 27 ℃/8h and is kept for 48h, and then the fire is shut down. The 576-hour roasting temperature curve can improve the control precision of the roasting temperature, improve the roasting quality, improve the thermal efficiency of a blast furnace chamber, reduce the energy consumption of the roasting furnace and prolong the service life of the roasting furnace, and a graphite crucible product with low resistivity of 12-13 mu omega can be produced and obtained based on the 576-hour roasting temperature curve, and the low resistivity proves that the graphite product produced based on the production process has a compact internal structure and excellent quality.
According to the invention, by doping the moisture-proof material and based on the hydrophobic characteristic of the moisture-proof material, the produced graphite has moisture-proof performance, so that the quality damage caused by the wetting of the graphite is effectively prevented, and the bursting phenomenon of the wetted graphite in use is avoided, thereby ensuring the graphite quality and improving the application safety of the graphite.
According to the invention, the abutting block is welded in the crucible mold and is positioned at the central position of the bottom of the crucible cavity of the crucible mold, so that the improvement on the graphite crucible body is realized, the bottom of the finally prepared graphite crucible is provided with a space for positioning, and stable placement is realized, thereby effectively avoiding unnecessary loss of brittle fracture of the graphite crucible caused by errors caused by external force factors, and enhancing the protection effect of the graphite crucible.
In conclusion, the production process is specially directed at the graphite crucible for the photovoltaic power generation panel, has the advantages of strong pertinence, high production specialization degree, high production efficiency and high product quality, reduces the production cost, prolongs the service life of the product, and is suitable for large-scale production.
Drawings
Fig. 1 is a flow chart of a production process of a graphite crucible for photovoltaic provided by the invention.
FIG. 2 is a flow chart showing a method of the calcination-impregnation treatment in FIG. 1.
FIG. 3 is a graph showing the calcination temperature profile at 576 hours in accordance with the present invention.
Fig. 4 is a graph showing the resistivity of graphite products produced using a conventional firing profile and graphite products produced using a 576 hour firing temperature profile according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "mounted on" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. When an element is referred to as being "secured to" another element, it can be directly secured to the other element or intervening elements may also be present.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "or/and" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, this embodiment provides a production process of a graphite crucible for photovoltaic, which is used to produce a graphite crucible with good moisture resistance and high stability in use. The production process comprises the following steps:
s1 provides pitch coke, petroleum coke, and carbon black, and provides moisture barrier and pitch.
Modified asphalt is boiled at 160-165 ℃ and then is kept stand for 100-120 h to prepare the asphalt. The moisture-proof material adopts triacetin.
S2, sequentially adding the asphalt coke, the petroleum coke, the carbon black and the moisture-proof material into a kneader for mixing to obtain the mixed raw material.
Before mixing, sequentially crushing the asphalt coke, the petroleum coke and the carbon black, and then sequentially sieving the crushed asphalt coke, the petroleum coke and the carbon black by using a 325-mesh sieve, wherein the sieve residue is 2-7%; the crushing treatment was carried out in a 5R pendulum mill.
And sequentially adding the pitch coke, the petroleum coke and the carbon black into a kneader for uniform mixing, heating to 120-125 ℃, and continuously mixing for 50min to obtain the mixed raw material. The mass ratio of the asphalt coke, the petroleum coke and the carbon black in the mixed raw material is 4:5.5: 0.5.
This embodiment, through doping dampproofing material (triacetin), based on dampproofing material's hydrophobic nature characteristics for the graphite that the production obtained possesses the humidity resistance, effectively prevents the quality damage that the graphite led to weing and stops the phenomenon of bursting that the graphite that weirs appears when using, thereby ensures the graphite quality, improves the security that graphite used.
S3, stirring and mixing the asphalt and the mixed raw materials to obtain a mixed material.
And (3) putting the asphalt and the mixed raw materials into stirring equipment, and stirring and mixing for 60min at the temperature of 180-185 ℃ to obtain the mixed material. The mass ratio of the mixed raw materials to the asphalt in the mixed ingredients is 41: 42.
s4 rolling the mixed material to obtain thin slices, and grinding the thin slices to obtain powder.
And (3) putting the mixed materials into a plastic refining machine, rolling to obtain a sheet with the thickness of 2-2.5 mm, and standing the sheet at the temperature of 50-60 ℃ for 48 hours. Putting the slices into a 5R pendulum type grinding machine, grinding to obtain powder, and sieving the powder by using a 200-mesh sieve, wherein the balance of the sieve is 20-25%.
S5 press molding the powder using a crucible mold to obtain a parison.
And a resisting block is welded in the crucible mold and is positioned at the center of the bottom of a crucible cavity of the crucible mold.
Putting the powder into a crucible mold, and performing compression molding at the temperature of 25-30 ℃, wherein the compression mold density is 1.45-1.46 g/cm3And is placed in a room for not less than 48 h.
This embodiment, the welding has supported the piece in the crucible mould of adoption to support the piece and be located crucible die cavity bottom central point department of putting of crucible mould, thereby improvement on the graphite crucible body, make the graphite crucible who makes at last, its bottom has the space that is used for the location, realizes steady placing, thereby effectively avoid because of the error that external force factor leads to, and cause the graphite crucible to take place the unnecessary loss of brittle failure, reinforcing graphite crucible's protecting effect.
S6 roasting-dipping treatment to obtain the roasted green body.
The roasting treatment is carried out by heating and cooling based on a 576-hour roasting temperature curve. The 576-hour roasting temperature curve is that the temperature is rapidly increased to 350 ℃, then the temperature is uniformly increased to 520 ℃ at the temperature increasing speed of 5 ℃/8h and is kept for 24h, then the temperature is uniformly increased to 1250 ℃ at the temperature increasing speed of 27 ℃/8h and is kept for 48h, and then the fire is shut off.
In the embodiment, the roasting temperature curve of 576 hours is adopted for roasting, so that the control precision of the roasting temperature can be improved, the roasting quality can be improved, the thermal efficiency of a blast furnace chamber can be improved, the energy consumption of a roasting furnace can be reduced, the service life of the roasting furnace can be prolonged,
the product porosity is reduced and the product quality is improved by dipping treatment.
The roasting-dipping treatment method is operated as follows:
s61, after the parison is roasted for the first time, the roasted product is continuously soaked for the first time, and a mixture A is obtained.
And (3) loading the parison into a roasting furnace, carrying out primary roasting treatment by adopting a 576-hour roasting temperature curve, cooling for 240 hours until the temperature in the furnace is lower than 90 ℃, discharging, soaking the roasted product subjected to the primary roasting treatment in medium-temperature coal pitch, heating to 300-500 ℃ at a heating rate of 50-60 ℃/h, vacuumizing, and carrying out pressure maintaining treatment to obtain a mixture A. The weight gain rate of the primary impregnation is 18-19%.
S62, after the mixture A is subjected to secondary roasting treatment, the roasted product is continuously subjected to secondary impregnation treatment to obtain a mixture B.
And (3) loading the mixture A into a roasting furnace, carrying out secondary roasting treatment by adopting a 576-hour roasting temperature curve, cooling for 240 hours until the temperature in the furnace is lower than 90 ℃, discharging, soaking the roasted product after the secondary roasting treatment in medium-temperature coal pitch, heating to 300-500 ℃ at a heating rate of 50-60 ℃/h, vacuumizing, and carrying out pressure maintaining treatment to obtain a mixture B. The weight gain rate of the secondary impregnation is 13-14%.
S63, after the mixture B is roasted for three times, the roasted product is continuously impregnated for three times to obtain a mixture C, namely a roasted blank.
And (3) loading the mixture B into a roasting furnace, carrying out roasting treatment for three times by adopting a 576-hour roasting temperature curve, cooling for 240 hours until the temperature in the furnace is lower than 90 ℃, discharging, soaking the roasted product after the roasting treatment for three times into medium-temperature coal pitch, heating to 300-500 ℃ at a heating rate of 50-60 ℃/h, vacuumizing, and carrying out pressure maintaining treatment to obtain a mixture C (roasted material blank). The weight gain of the three times of dipping is 9-10%.
And S7 graphitizing the roasted blank to obtain the graphite crucible.
And (3) putting the roasted blank into an Acheson furnace, and graphitizing the roasted blank at the temperature of 2800-2900 ℃ to obtain the graphite crucible. The resistivity of the graphite crucible is 12-13 mu omega m. The bottom of the graphite crucible is of an inwards concave structure, wherein the inwards concave structure is matched with the abutting block.
In the embodiment, based on a 576-hour roasting temperature curve, a graphite crucible product with low resistivity of 12-13 mu omega can be produced, and the low resistivity proves that the graphite product produced based on the production process has a compact internal structure and excellent quality.
Referring to FIG. 3, FIG. 3 shows a graph of the calcination temperature at 576 hours. The temperature curve of 576 hours of roasting is that the temperature is rapidly increased to 350 ℃, then the temperature is uniformly increased to 520 ℃ at the temperature increasing speed of 5 ℃/8h and is kept for 24h, then the temperature is uniformly increased to 1250 ℃ at the temperature increasing speed of 27 ℃/8h and is kept for 48h, and then the fire is shut down. According to the 576-hour roasting temperature curve of the embodiment, the temperature rise balance is good, so that the pitch coke, the petroleum coke and the like are slowly and uniformly volatilized, uniform and compact-structure air holes are formed in a roasted product in the roasting process, and the physical and chemical properties of the roasted product are improved.
The resistivity of the graphite product produced by using the conventional roasting curve and the resistivity of the graphite product produced by using the 576-hour roasting temperature curve in this example were measured several times, and the results of the measurements are shown in fig. 4, in which the ordinate represents the resistivity/μ Ω m and the abscissa represents the number of times of the experiment. As can be seen from FIG. 4, the resistivity of the graphite crucible prepared in this example is 12-13 μ Ω m, which is significantly lower than that of the graphite product produced by the conventional calcination temperature profile. The test result proves that the production process can produce the graphite product with low resistivity, and the graphite product has the characteristic of internal structure densification and excellent quality.
In summary, the production process of the present embodiment has the following advantages compared to the current production process: the production process of this embodiment is directed against the graphite crucible that photovoltaic power generation board was used specially, with strong points, the production specialization degree is high, production efficiency is high and product quality is high, reduction in production cost improves product life, be applicable to large-scale production, the production process of this embodiment can produce the graphite that obtains possessing humidity resistance, the quality of graphite product has been ensured, improve the security that graphite was used, and, the production process of this embodiment, can produce and obtain the graphite crucible that the bottom has the space that is used for the location, realize steady placing, the protective effect is excellent.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The embodiments described above are more specific and detailed, but should not be construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.
Claims (10)
1. A production process of a photovoltaic graphite crucible is characterized by comprising the following steps:
s1 providing pitch coke, petroleum coke and carbon black, providing moisture barrier material and pitch;
s2, sequentially adding the asphalt coke, the petroleum coke, the carbon black and the moisture-proof material into a kneader for mixing to obtain a mixed raw material;
s3, stirring and mixing the asphalt and the mixed raw materials to obtain a mixed material;
s4, rolling the mixed material to form a sheet, and grinding the sheet to obtain powder;
s5, carrying out compression molding treatment on the powder by using a crucible mold to obtain a parison;
s6, roasting and dipping to obtain a roasted blank;
the roasting treatment is carried out on the basis of a 576-hour roasting temperature curve to carry out temperature rise and temperature reduction;
s7, graphitizing the roasted blank to obtain a graphite crucible;
the resistivity of the graphite crucible is 12-13 mu omega m.
2. The production process of the graphite crucible for the photovoltaic, as claimed in claim 1, is characterized in that the pitch is prepared by decocting modified pitch at 160-165 ℃ and then standing for 100-120 h;
the moisture-proof material adopts triacetin.
3. The production process of the graphite crucible for photovoltaic as claimed in claim 1, wherein the mass ratio of the pitch coke, the petroleum coke and the carbon black in the mixed raw material is 4:5.5: 0.5;
the mass ratio of the mixed raw materials to the asphalt in the mixed ingredients is 41: 42.
4. the production process of the graphite crucible for photovoltaic as claimed in claim 1, wherein the thickness of the thin sheet is 2-2.5 mm;
and (3) putting the slices into a 5R pendulum type grinding machine, grinding to obtain powder, and sieving the powder by using a 200-mesh sieve, wherein the balance of the sieve is 20-25%.
5. The production process of the graphite crucible for photovoltaic as claimed in claim 1, wherein a resisting block is welded in the crucible mold; the abutting block is positioned at the center of the bottom of a crucible cavity of the crucible mold;
the density of the pressing die is 1.45-1.46 g/cm3。
6. The production process of the graphite crucible for the photovoltaic as claimed in claim 1, wherein the 576 hour baking temperature curve is that the temperature is rapidly increased to 350 ℃, then uniformly increased to 520 ℃ at a temperature increasing rate of 5 ℃/8h and kept for 24h, then uniformly increased to 1250 ℃ at a temperature increasing rate of 27 ℃/8h and kept for 48h, and then the fire is shut down.
7. The process for producing a graphite crucible for photovoltaic use according to claim 1, wherein the firing-impregnating treatment is carried out by:
s61, after primary roasting treatment is carried out on the parison, primary dipping treatment is continuously carried out on the roasted product, and a mixture A is obtained;
s62, after the mixture A is subjected to secondary roasting treatment, the roasted product is continuously subjected to secondary impregnation treatment to obtain a mixture B;
s63, after the mixture B is roasted for three times, the roasted product is continuously impregnated for three times to obtain a mixture C, namely a roasted blank.
8. The production process of the graphite crucible for photovoltaic as claimed in claim 7, wherein the weight gain rate of the primary dipping is 18-19%; the weight gain rate of the secondary impregnation is 13-14%; the weight gain rate of the three times of dipping is 9-10%;
the impregnation treatment is carried out in medium temperature coal tar pitch.
9. The production process of the graphite crucible for the photovoltaic, as claimed in claim 1 or 5, wherein the bottom of the graphite crucible is a concave structure, wherein the concave structure is matched with the abutting block.
10. The process for producing a graphite crucible for photovoltaic use according to claim 1, wherein the fired green body is placed in an Acheson furnace and graphitized at 2800 to 2900 ℃ to obtain the graphite crucible.
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---|---|---|---|---|
CN116789453A (en) * | 2023-04-19 | 2023-09-22 | 湖北东南佳特碳新材料有限公司 | Graphite crucible and preparation method and application thereof |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1030367A (en) * | 1988-05-07 | 1989-01-18 | 天津市耐火器材厂 | Method for making graphite crucible |
JP2000185995A (en) * | 1998-12-22 | 2000-07-04 | Toyo Tanso Kk | Crucible for pulling up single crystal made of carbon- fiber reinforced carbon composite material |
CN102249237A (en) * | 2010-12-20 | 2011-11-23 | 龚炳生 | Graphite crucible |
CN202865333U (en) * | 2012-08-27 | 2013-04-10 | 北京博宇半导体工艺器皿技术有限公司 | Graphite mould for manufacturing pyrolytic boron nitride narrow-necked evaporator crucible |
CN106830938A (en) * | 2017-01-17 | 2017-06-13 | 韩俊培 | A kind of production technology of photovoltaic graphite crucible |
JP2018048041A (en) * | 2016-09-21 | 2018-03-29 | 株式会社Sumco | Crucible for single crystal production, and silicon single crystal production apparatus |
CN211866496U (en) * | 2019-11-28 | 2020-11-06 | 西南铝业(集团)有限责任公司 | Blank making die of 2014 aluminum alloy aviation precision hub die forging |
-
2021
- 2021-11-02 CN CN202111288161.1A patent/CN114105641A/en active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1030367A (en) * | 1988-05-07 | 1989-01-18 | 天津市耐火器材厂 | Method for making graphite crucible |
JP2000185995A (en) * | 1998-12-22 | 2000-07-04 | Toyo Tanso Kk | Crucible for pulling up single crystal made of carbon- fiber reinforced carbon composite material |
CN102249237A (en) * | 2010-12-20 | 2011-11-23 | 龚炳生 | Graphite crucible |
CN202865333U (en) * | 2012-08-27 | 2013-04-10 | 北京博宇半导体工艺器皿技术有限公司 | Graphite mould for manufacturing pyrolytic boron nitride narrow-necked evaporator crucible |
JP2018048041A (en) * | 2016-09-21 | 2018-03-29 | 株式会社Sumco | Crucible for single crystal production, and silicon single crystal production apparatus |
CN106830938A (en) * | 2017-01-17 | 2017-06-13 | 韩俊培 | A kind of production technology of photovoltaic graphite crucible |
CN211866496U (en) * | 2019-11-28 | 2020-11-06 | 西南铝业(集团)有限责任公司 | Blank making die of 2014 aluminum alloy aviation precision hub die forging |
Non-Patent Citations (1)
Title |
---|
汤长根: "《耐火材料生产工艺》", 28 February 1982 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116789453A (en) * | 2023-04-19 | 2023-09-22 | 湖北东南佳特碳新材料有限公司 | Graphite crucible and preparation method and application thereof |
CN116789453B (en) * | 2023-04-19 | 2024-03-19 | 湖北东南佳特碳新材料有限公司 | Graphite crucible and preparation method and application thereof |
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