CN102206080A - Graphite material for monocrystalline silicon growth thermal field in solar photovoltaic industry and production method thereof - Google Patents
Graphite material for monocrystalline silicon growth thermal field in solar photovoltaic industry and production method thereof Download PDFInfo
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Abstract
The invention relates to a graphite material for a monocrystalline silicon growth thermal field in a solar photovoltaic industry. In the graphite material, an aggregate is calcined petroleum coke, wherein the true density of the calcined petroleum coke is more than or equal to 2.1g/cm <3>, and the ash content of the calcined petroleum coke is less than or equal to 0.3%; a binder is medium temperature pitch, wherein the softening point of the medium temperature pitch is 83-86 DEG C, and the coking value of the medium temperature pitch is more than or equal to 49%; and the volume density of the graphite material is larger than or equal to 1.80g/cm<3>, the resistivity of the graphite material is less than or equal to 7.0 mu omega m, the compression strength of the graphite material is larger than or equal to 38Mpa, the rupture strength of the graphite material is more than or equal to 18Mpa, the porosity of the graphite material is less than or equal to 14%, the ash content of the graphite material is less than or equal to 0.2%, and the thermal expansion coefficient of the graphite material is less than or equal to 2*10<-6>/DEG C. The preparation method of the graphite material comprises the following steps: smashing raw materials, sieving, burdening, kneading, molding, primarily roasting, secondarily roasting, secondarily dipping, and thirdly roasting; and graphitizing, thus obtaining a finished product.
Description
Technical field
The present invention relates to a kind of graphite material, particularly a kind of photovoltaic industry monocrystalline silicon growing thermal field graphite material and manufacture method thereof.
Background technology
Sun power is a kind of cleaning, the safe and reliable energy, and the best mode that utilizes sun power is the photovoltaic conversion, utilizes photovoltaic effect exactly, sunlight is mapped to produces the electric current direct generation of electricity on the silicon materials.Photovoltaic industry is with the industry chain (supply chain) of the application and development formation of silicon materials, comprises the manufacturing of high-purity silicon single crystal, the production of polysilicon starting material, manufacture of solar cells, solar module production, related production equipment etc.
The monocrystalline silicon growing thermal field mainly contains parts such as quartz crucible, plumbago crucible (three lobe pots), well heater, guide shell, interior thermal insulator (lining), thermal insulator, insulation cover, insulation base plate, crucible pallet and swivel bearing and forms.This thermal field is except that quartz crucible, and remaining part is that graphite product is formed all.
Because of silicon materials to purity require high, so the graphite material of using as thermal field is wanted the purity height, is wanted that resistance of oxidation is strong, void content is low.If graphite purity is not high, a little less than the resistance of oxidation, the void content height, impurity is too much, and crystal silicon draws environment and is polluted, and the quality of wafer just can not get guaranteeing.By way of example, the distance of graphite thermal field and polysilicon founding is very near, and the single crystal rod quality of pulling out is had a direct impact, and its influence degree is only second to polysilicon itself.In pulling monocrystal silicon rod process, the graphite thermal field is pasting quartzy pot, and quartzy pot will be scrapped renewal after each monocrystalline pulls, and the graphite thermal field has certain access times repeatedly.Use repeatedly, this just need have higher requirement to its performance.If the graphite thermal field is pure inadequately, material is good inadequately, and graphite thermal field body has that impurity is general to send under the pyritous situation, and in the single crystal growth process, in case impurity mixes with it, this process is irreversible, and the crystal bar quality is had a greatly reduced quality certainly.The monocrystalline silicon growing thermal field requires with the graphite material quality technology: volume density is big, purity is high, high temperature resistant, corrosion-resistant, characteristics such as oxidation-resistance is strong, void content is low, thermal expansivity is low.
Chinese patent 201010263217.3 discloses a kind of graphite material that is used for solar energy thermal-power-generating heat build-up accumulation of energy, its volume density 〉=1.75g/cm
3, resistivity≤7.5 μ Ω m, ash≤0.2% folding strength 〉=18.5Mpa, Young's modulus≤8.8Gpa, thermal expansivity≤2.0 * 10
-6/ ℃
-1, its physicochemical property can't satisfy the performance requriements of monocrystalline silicon growing thermal field with graphite material.
Chinese patent 200710090789 disclosed graphite materials with after-smithing petroleum coke, graphite is broken and mid-temperature pitch is a raw material, its purity 〉=99%; Volume density 〉=1.68g/cm
3, its physicochemical property also can't satisfy the performance requriements of monocrystalline silicon growing thermal field with graphite material.
The graphite material that Chinese patent 200910179699.1 provides is siccative with the after-smithing petroleum coke, mid-temperature pitch or modified pitch are tackiness agent, though this patent does not disclose volume density, the maximum particle diameter of after-smithing petroleum coke is 1mm, belong to the macrobead prescription, its volume density is inevitable less.
Because crystalline silicon is high especially to the physicochemical property requirement of graphite material, common graphite can't satisfy its practical requirement.At present, be the isostatic pressing formed graphite goods with the most akin implementation of the present invention on the market.
The isostatic pressing formed graphite piece is to have isotropy, high-density, and a kind of very widely high-tech graphite products of high added value, industrial use of high strength and very uniform material structure belongs to high-end product in graphite products.It can be widely used in fields such as metallurgy, non-ferrous metal, electrochemical applications, energy technology and management, semiconductor material preparation, space flight, nuclear power.
The isostatic pressing formed graphite goods be with heat treated refinery coke behind broken, abrasive dust, mix with ature of coal pitch and to pinch, and carry out the hot sheet that rolls; To roll sheet again and wear in the bag of packing into behind the powder, and be put into etc. in the static pressure jar and carry out moulding.Since etc. the applying of quiet jar internal pressure by liquid transfer, this pressure that has guaranteed all directions that raw material is subjected in the bag equates, so the isostatic pressing product that obtain are isotropy.The equal pressing forming technology applied pressure is bigger, generally all is P 〉=160mpa, and along with the increase of product specification, its pressure requires also big; Its composition of raw materials granularity little (0.0425mm) on the other hand, operations such as its follow-up roasting, dipping, greying, processing parameter also is difficult for grasping, therefore, wait the static pressure product technology content higher, technique means is very complicated, accordingly, the price of isostatic pressing formed graphite is also very high, be 150,000 yuan per ton.At present, countries such as industrially developed country Japan, Germany, the U.S. are ripe and promote the use of abroad Deng the static pressure product technology, and the producer of China's capable production isostatic pressing formed graphite is very limited, and mostly be and produce some low side small-size products, be in particular in that size is less, intensity, volume density is not enough, and the high performance product of high-end large size is still being groped experimental stage.Because isostatic pressing formed graphite import volume deficiency, market has openings is very big at home to cause this product.
In view of this, the special the technical program that proposes.
Summary of the invention
First purpose of the present invention provides a kind of photovoltaic industry monocrystalline silicon growing thermal field graphite material, this graphite material has that volume density is big, purity is high, high temperature resistant, corrosion-resistant, characteristics such as oxidation-resistance is strong, void content is low, thermal expansivity is low, can replace isostatic pressing formed graphite.
Second purpose of the present invention provides the manufacture method of a kind of photovoltaic industry monocrystalline silicon growing thermal field with graphite material.
For realizing first purpose of the present invention, adopt following technical scheme:
A kind of photovoltaic industry monocrystalline silicon growing thermal field graphite material, the volume density 〉=1.80g/cm of described graphite material
3, resistivity≤7.0 μ Ω m, ultimate compression strength 〉=38Mpa, folding strength 〉=18Mpa, void content≤14%, ash content≤0.2%, thermal expansivity≤2*10
-6/ ℃; Described graphite material is preferably volume density 〉=1.82g/cm
3, resistivity≤6.8 μ Ω m, ultimate compression strength 〉=39Mpa, folding strength 〉=19Mpa, void content≤13%, ash content≤0.17%, thermal expansivity≤2*10
-6/ ℃.
In the raw material of described graphite material, aggregate is an after-smithing petroleum coke, and binding agent is a mid-temperature pitch, and soaker is impregnating pitch, the true density 〉=2.1g/cm3 of described after-smithing petroleum coke, ash content≤0.3%; The softening temperature of described mid-temperature pitch is 83～86 ℃, coking value 〉=49%; Described impregnating pitch is: quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃.
The weight ratio of described after-smithing petroleum coke and mid-temperature pitch is 70: 30～75: 25, be preferably 70: 29～and 30.
Percentage composition meter by weight, the particle size range of described after-smithing petroleum coke and content are:
0.5mm＜particle diameter≤0.335mm 10%-25%,
0.335mm＜particle diameter≤0.15mm 20%-25%,
0.15mm＜particle diameter≤0.075mm 15%-20%,
Particle diameter＜0.075mm 40%-45%;
The particle size range and the content of described after-smithing petroleum coke are preferably:
0.5mm＜particle diameter≤0.335mm 25%,
0.335mm＜particle diameter≤0.15mm 20%,
0.15mm＜particle diameter≤0.075mm 15%,
Particle diameter＜0.075mm 40%.
For realizing second purpose of the present invention, a kind of photovoltaic industry monocrystalline silicon growing thermal field preparation method with graphite material is provided, and described preparation method may further comprise the steps: the fragmentation of raw material, screening, batching, mix pinch, moulding, roasting, single-steeping, re-baking, double-steeping, three roastings and greying obtain finished product; Described bakes to burn the article is: in the time of 150-400 ℃, temperature rise rate is 1.1-1.5 ℃/h; In the time of 400-600 ℃, temperature rise rate is 0.7-0.9 ℃/h; In the time of 600-900 ℃, temperature rise rate is 1.1-1.5 ℃/h; In the time of 900-1200 ℃, temperature rise rate is 2.3-3 ℃/h.
Described mixed pinching is divided into the dry blend wet mixing, and the described dried time of mixing is 40-45 minute, and doing the temperature of mixing is 120～130 ℃; Described wet mixing is mid-temperature pitch to be joined to mix in the aggregate of doing after mixing at twice pinch, the temperature of wet mixing is 135～145 ℃, for the first time the weight of the mid-temperature pitch that adds is the 70-80% of total mid-temperature pitch, the time of wet mixing for the first time is 15～20 minutes, for the second time the weight of the mid-temperature pitch that adds is the 20-30% of total mid-temperature pitch, and the time of wet mixing for the second time is 15～20 minutes.
Describedly be shaped to vibratory compaction, the volume density of green compact reaches 1.74g/cm after the moulding
3More than.
When described single-steeping and double-steeping, impregnating pitch is carried out pre-treatment, impregnating pitch is heated to 210～300 ℃, preferably be heated to 210～250 ℃, be incubated 1～2 hour, impregnating pitch is risen again 180～200 ℃ again, flood; The preheating temperature of pickled product is 360-380 ℃ during single-steeping, and rate of body weight gain is more than 13%; The preheating temperature of pickled product is 360-380 ℃ during double-steeping, and rate of body weight gain is more than 7%.
The time of described re-baking is 300-320h, and the top temperature of re-baking reaches 750 ℃.
The time of described three roastings is 300-320h, and top temperature reaches 750 ℃.
The described graphited time is 130-140h, and graphited top temperature is 2800-3000 ℃.
Below be detailed description of the present invention:
Monocrystalline silicon growing thermal field graphite material is a kind of high-end graphite products, has extraordinary physical and chemical index, though the isostatic pressing formed graphite product properties can satisfy the monocrystalline silicon production processing requirement fully, but its price is very expensive, and the high performance isostatic pressing formed graphite goods of domestic large size still are in the stage of fumbling, and the common graphite material can't reach the physical and chemical index of isostatic pressing formed graphite material.The present invention has prepared a kind of photovoltaic industry monocrystalline silicon growing thermal field graphite material, its volume density 〉=1.80g/cm by raw material, prescription and preparation technology are studied in great detail
3, resistivity≤7.0 μ Ω m, ultimate compression strength 〉=38Mpa, folding strength 〉=18Mpa, void content≤14%, ash content≤0.2%, thermal expansivity≤2*10
-6/ ℃, graphite material of the present invention can substitute isostatic pressing formed graphite at the monocrystalline silicon growing thermal field fully aspect graphite material.
The contriver aspect material choice, finally determines with the after-smithing petroleum coke to be that aggregate, mid-temperature pitch are binding agent, the true density 〉=2.1g/cm of after-smithing petroleum coke through repeatedly testing, research and analyse and the product trial production
3, ash content≤0.3%, the softening temperature of mid-temperature pitch is 83～86 ℃, coking value 〉=49% o'clock, and impregnating pitch satisfies: when quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃, help obtaining the higher roasting product of volume density, help improving yield rate, and mid-temperature pitch is in the easy greying of graphitization process, and the physical and chemical index of its finished product could satisfy the needs of monocrystalline silicon growing thermal field with graphite material.
Among the preparation technology of graphite product, prescription is bigger to the influence of the performance perameter of graphite product, particularly to the influence of volume density, void content and thermal expansivity.In general, employing is big than the volume density that the vibratory compaction of fine particle prescription obtains product, void content is less, ultimate compression strength is high, and the present invention adopts super fine powder, small-particle prescription when batching, and the maximum particle diameter of aggregate is less than 0.5mm.In this particle size range, the distribution of grain diameter directly influences the particulate accumulation mode, and particle packing is tight more, the volume density of graphite product is big more, void content is more little, in addition, and in this particle size range, as keep granularity constant, and mean particle size doubles, and coefficient of thermal expansion descends about 6%; Increase by 10 times, it is about 12% to descend, but mean particle size is when increasing, and graphite intensity but descends to some extent.The present invention is through studying repeatedly and testing, the following aggregate prescription of final use, after-smithing petroleum coke is pressed: the weight of the after-smithing petroleum coke of 0.5mm＜particle diameter≤0.335mm accounts for the 10%-25% of total after-smithing petroleum coke, 0.335mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.15mm accounts for the 20%-25% of total after-smithing petroleum coke, 0.15mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.075mm accounts for the 15%-20% of total after-smithing petroleum coke, the 40%-45% that the weight of the after-smithing petroleum coke of particle diameter＜0.075mm accounts for total after-smithing petroleum coke prepares burden, at this moment, the particles of aggregates of different-grain diameter is piled up comparatively tight, the volume density of graphite product, void content, ultimate compression strength and thermal expansivity can reach an extraordinary balance, and the volume density of prepared graphite product is big, void content is little, thermal expansivity is less.
What the present invention adopted is the vibratory compaction mode, therefore the consumption to binder pitch has strict ratio requirement, the consumption of binding agent and the surface-area of aggregate have direct relation, the particle diameter of aggregate is more little, and surface-area is big more, and the binding agent consumption is then many more, but the binding agent consumption is too much, be difficult for jolt ramming during moulding, thereby the volume density of product is less, and product easy deformation after the demoulding.Binding agent of the present invention and aggregate proportioning are 70: 30～75: 25, aggregate and binding agent are after mixed pinching, and the thickener that obtains is not agglomerate basically, are poured on cold and expect that great majority are the shot shape on the platform, or a little less little agglomerate, obtain the higher moulding product of volume density after the moulding.
In general, the particle of aggregate is tiny more, and surface-area is big more, difficult more mixing in the time of wet mixing, and the time that wet mixing is used is just long more, and power consumption also increases thereupon.The present invention is in the process of wet mixing, binding agent joined to mix in the aggregate after do mixing at twice pinch, binding agent and the aggregate that adds the 70%-80% that accounts for total binding agent quality coheres for the first time, because the amount that adds is few, the stickiness of mixture is lower, under the whipping force effect of equal conditions, can mix at short notice and pinch evenly, after the wet mixing for the first time, make the feed particles particle diameter ratio become big more uniformly, its specific surface area is diminished, more remaining binding agent is added, can be at short notice with aggregate and tackiness agent uniform mixing.Add binder modification pitch at twice, both can reduce the time of wet mixing, cut down the consumption of energy, thickener is mixed pinch evenly, obtain the good thickener of plasticity, help improving the yield rate and the physicals of green compact after the moulding.
The purpose of roasting is to make the binder pitch charing, forms the coke grid between particles of aggregates, and varigrained aggregate is bonded to an integral body securely.The small-particle prescription is when the preparation graphite material, the chance that occurs crackle in follow-up roasting and graphitizing process is many, yield rate may be on the low side, factors such as the heating curve when the present invention passes through optimization and improves roasting, the duration of heat, improved the coking rate of binding agent, overcome the low problem of appearance crackle, yield rate that small-particle brings, to guarantee product overall target and yield rate.
In the bakes to burn the article process of the present invention, in the time of 150-400 ℃, temperature rise rate is 11-1.5 ℃/h, lightweight fugitive constituent in the roasting product is discharged with slower speed volatilization, the suffered pressure of roasting product inside is less, balance comparatively, avoided the generation of crackle in the temperature-rise period, and light component there is adequate time to discharge roasting product; In the time of 400-600 ℃, polycondensation strengthens in the roasting product, and coke begins to form, and heats up with 0.7-0.9 ℃/h, helps improving the coking rate of binding agent, and carbonization at low temperature changes coking into; In the time of 600-900 ℃, polycondensation continue to take place, and the further coking of goods heats up with the slower temperature rise rate of 1.1-1.5 ℃/h, help improving the volume density and the intensity of roasting product, and avoid that roasting product cracks in the process of polycondensation when shrinking; In the time of 900-1200 ℃, heat up the further densification of the weave construction of roasting product with the very fast temperature rise rate of 2.3-3 ℃/h.
The characteristic of impregnating pitch has significant effects to dipping effect, mainly shows on bituminous viscosity, quinoline insolubles content, the coking value.Coking value is high more, the volume density of product and physical strength are big more after the roasting, and coking value increases with the softening temperature rising, therefore adopt the higher coal-tar pitch of softening temperature as cakingagent, help improving the volume density and the physical strength of graphite material, but the impregnating pitch softening temperature is high more, and relative viscosity is just big more, is difficult to be penetrated in the hole of pickled product go.Asphalt viscosity both had been subjected to property effect own, just was inversely proportional to Heating temperature again.Be to improve dipping effect, the present invention one is that to select softening temperature for use be 83-86 ℃, coking value and is 〉=48% pitch, the 2nd, impregnating pitch is heated, to reduce the viscosity of impregnating pitch.In general, after surpassing 200 ℃, light component in the pitch begins volatilization, 200～400 ℃ is the volatilization stage of the light component in the impregnating pitch, and rising along with temperature, the molecular weight of evaporable light component increases gradually in the impregnating pitch, evaporable gas enters in the pore of pickled product, hindered the bituminous infiltration, so in the prior art, begin dipping after impregnating pitch is heated to 160～180 ℃, the temperature of impregnating pitch heating can be above 200 ℃, but, because the preheating temperature of the carbon element product that need flood is generally all between 300～400 ℃, so in the process of dipping, still have the impregnating pitch of light component in the carbon element product of dipping to evaporate, not only hinder the infiltration of impregnating pitch, also in pickled product, formed the aperture of many gases.The present invention is before dipping, earlier impregnating pitch is heated to 210～300 ℃, preferably be heated to 210～250 ℃, make the part light component in the impregnating pitch volatilize away, the volatile small molecules of part is volatilized away, making impregnating pitch cool to 180～200 ℃ afterwards again floods, at this moment, impregnating pitch still has lower viscosity, and than being easier to penetrate in the pickled product, the preheating temperature of pickled product is 360-380 ℃ during single-steeping of the present invention, the preheating temperature of pickled product is 360-380 ℃ during double-steeping, when dipping,, not only improved the coking value of impregnating pitch because the part light component volatilizees away in the impregnating pitch, also accelerated the infiltration of impregnating pitch, and reduced the void content in the pickled product, dipping effective helps improving the physical and chemical index of graphite product.When dipping, carbon element product to the need dipping vacuumize earlier earlier, the purpose that vacuumizes is the gas of discharging in the carbon element product open pores that needs dipping, be beneficial to the infiltration of impregnating pitch, after adding impregnating pitch, under the effect of pressure, impregnating pitch is than going in the hole that is easier to be penetrated into the carbon element product that need dipping, thus the assurance rate of body weight gain; Quinoline in the coal-tar pitch not fusant is a kind of small particle, during dipping quinoline not fusant form thin film at porous material surface, hinder the infiltration of soaker to porous material, therefore, the present invention selects the not impregnating pitch of fusant≤0.2% of quinoline for use.
The present invention has greatly improved the volume density of graphite material by carrying out greying after double-steeping and three roastings.
Compared with prior art, the preparation method's of graphite material provided by the invention beneficial effect is:
The present invention is with true density 〉=2.1g/cm
3The after-smithing petroleum coke of ash content≤0.3% is an aggregate, softening temperature is 83～86 ℃, the mid-temperature pitch of coking value 〉=49% is a binding agent, adopt super fine powder, the small-particle prescription, by optimizing and improvement preparation technology, heating curve during particularly by optimization and improvement roasting, the duration of heat, and to the heating of impregnating pitch, the processing of rising again, the physical and chemical index of graphite material of the preparation isostatic pressing formed graphite material that can match in excellence or beauty, alternative isostatic pressing formed graphite material, be used for photovoltaic industry monocrystalline silicon growing thermal field, but raw material sources are wide, price is low, and preparation technology is simple relatively, and technical difficulty is low, production cost is low, so price is low, its price is less than 1/5 of isostatic pressing formed graphite, obtained great success commercial.
Description of drawings
Fig. 1 is the preparation method's of graphite material of the present invention process flow sheet
Embodiment
Specific embodiments of the invention only make further explanation content of the present invention, content of the present invention are not construed as limiting.Raw material of the present invention is marketable material, and the mechanical means that is adopted also is the equipment that this area is known altogether.
Embodiment 1
With true density 〉=2.1g/cm
3The after-smithing petroleum coke of ash content≤0.3% is made 0.5mm＜particle diameter≤0.335mm, 0.335mm＜particle diameter≤0.15mm, 0.15mm＜particle diameter≤0.075mm and particle diameter four other pellets of level less than 0.075mm after fragmentation, screening, place respectively in four feed bins.Prepare burden then, aggregate and tackiness agent are prepared burden according to weight ratio at 70: 30, tackiness agent is that softening temperature is 83～86 ℃, the mid-temperature pitch of coking value 〉=49%, wherein aggregate is pressed: the weight of the after-smithing petroleum coke of 0.5mm＜particle diameter≤0.335mm accounts for 25% of total after-smithing petroleum coke, 0.335mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.15mm accounts for 20% of total after-smithing petroleum coke, 0.15mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.075mm accounts for 15% of total after-smithing petroleum coke, the weight of the after-smithing petroleum coke of particle diameter＜0.075mm accounts for 40% of total after-smithing petroleum coke and prepares burden.
The above-mentioned aggregate for preparing put into to mix to pinch to do in the pot mix, dried doing time is 40 minutes, and doing mixed temperature is 120 ℃.After dried the mixing, add mid-temperature pitch and carry out wet mixing, the temperature of wet mixing is 135 ℃, for the first time the weight of the mid-temperature pitch that adds is 70% of total mid-temperature pitch, the time of wet mixing for the first time is 15 minutes, for the second time the weight of the mid-temperature pitch that adds is 30% of total mid-temperature pitch, and the time of wet mixing for the second time is 20 minutes.
Thickener after the wet mixing is put into dry in the air material operation of the material machine that dries in the air, when treating that the thickener temperature is reduced to 110 ℃, thickener is put into the vibrating forming machine grinding tool carry out vibratory compaction, die mould product flawless, volume density is 1.75g/cm
3
The moulding product are put into ring-form calcining furnace carry out bakes to burn the article, in the time of 150-400 ℃, temperature rise rate is 1.3 ℃/h; In the time of 400-600 ℃, temperature rise rate is 0.8 ℃/h; In the time of 600-900 ℃, temperature rise rate is 1.3 ℃/h; In the time of 900-1200 ℃, temperature rise rate is 2.5 ℃/h, and whole temperature-rise period is controlled with the temperature alarming instrument, the temperature range that guarantees the temperature alarming instrument in 5 ℃, the roasting product flawless.
Behind the bakes to burn the article, carry out single-steeping, re-baking, double-steeping and three roastings successively, soaker is the impregnating pitch that quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃, during dipping, impregnating pitch is heated to 250 ℃, be incubated 1.5 hours, impregnating pitch risen again 190 ℃ again, flood.During single-steeping pickled product is preheating between 360 ℃, rate of body weight gain is 13.3% behind the single-steeping.Re-baking carries out at tunnel furnace, re-baking time spent 300h, and the top temperature of re-baking is 750 ℃.During double-steeping pickled product is preheating between 360 ℃, rate of body weight gain is 7% behind the double-steeping.Three roastings are carried out at tunnel furnace, and the time of three roastings is 320h, and top temperature is 750 ℃.
Three roasting products are put into the greying circuit carry out greying, electric power feeding time is 140h, and the greying top temperature is 3000 ℃.Come out of the stove after the machining cutting obtains graphite material.Graphite finished product flawless, small product size density are 1.82g/cm
3, resistivity is 6.8 μ Ω m, and ultimate compression strength is 39Mpa, and folding strength is 18.5Mpa, and void content is 13%, and ash content is 0.17%, and thermal expansivity is 2*10
-6/ ℃.
Embodiment 2
With true density 〉=2.1g/cm
3The after-smithing petroleum coke of ash content≤0.3% is made 0.5mm＜particle diameter≤0.335mm, 0.335mm＜particle diameter≤0.15mm, 0.15mm＜particle diameter≤0.075mm and particle diameter four other pellets of level less than 0.075mm after fragmentation, screening, place respectively in four feed bins.Prepare burden then, aggregate and tackiness agent are prepared burden according to weight ratio at 70: 30, tackiness agent is that softening temperature is 83～86 ℃, the mid-temperature pitch of coking value 〉=49%, wherein aggregate is pressed: the weight of the after-smithing petroleum coke of 0.5mm＜particle diameter≤0.335mm accounts for 15% of total after-smithing petroleum coke, 0.335mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.15mm accounts for 22% of total after-smithing petroleum coke, 0.15mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.075mm accounts for 18% of total after-smithing petroleum coke, the weight of the after-smithing petroleum coke of particle diameter＜0.075mm accounts for 45% of total after-smithing petroleum coke and prepares burden.
The above-mentioned aggregate for preparing put into to mix to pinch to do in the pot mix, dried doing time is 45 minutes, and doing mixed temperature is 130 ℃.After dried the mixing, add mid-temperature pitch and carry out wet mixing, the temperature of wet mixing is 145 ℃, for the first time the weight of the mid-temperature pitch that adds is 80% of total mid-temperature pitch, the time of wet mixing for the first time is 20 minutes, for the second time the weight of the mid-temperature pitch that adds is 20% of total mid-temperature pitch, and the time of wet mixing for the second time is 20 minutes.
Thickener after the wet mixing is put into dry in the air material operation of the material machine that dries in the air, when treating that the thickener temperature is reduced to 110 ℃, thickener is put into the vibrating forming machine grinding tool carry out vibratory compaction, die mould product flawless, volume density is 1.75g/cm
3
The moulding product are put into ring-form calcining furnace carry out bakes to burn the article, in the time of 150-400 ℃, temperature rise rate is 1.5 ℃/h; In the time of 400-600 ℃, temperature rise rate is 0.7 ℃/h; In the time of 600-900 ℃, temperature rise rate is 1.5 ℃/h; In the time of 900-1200 ℃, temperature rise rate is 2.3 ℃/h, and whole temperature-rise period is controlled with the temperature alarming instrument, the temperature range that guarantees the temperature alarming instrument in 5 ℃, the roasting product flawless.
Behind the bakes to burn the article, carry out single-steeping, re-baking, double-steeping and three roastings successively, soaker is the impregnating pitch that quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃, during dipping, impregnating pitch is heated to 210 ℃, be incubated 1 hour, impregnating pitch risen again 180 ℃ again, flood.During single-steeping pickled product is preheating between 380 ℃, rate of body weight gain is 13% behind the single-steeping.Re-baking carries out at tunnel furnace, re-baking time spent 320h, and the top temperature of re-baking is 750 ℃.During double-steeping pickled product is preheating between 380 ℃, rate of body weight gain is 7.2% behind the double-steeping.Three roastings are carried out at tunnel furnace, and the time of three roastings is 300h, and top temperature is 750 ℃.
Three roasting products are put into the greying circuit carry out greying, electric power feeding time is 135h, and the greying top temperature is 2900 ℃.Come out of the stove after the machining cutting obtains graphite material.Graphite finished product flawless, small product size density are 1.83g/cm
3, resistivity is 6.9 μ Ω m, and ultimate compression strength is 38Mpa, and folding strength is 19Mpa, and void content is 14%, and ash content is 0.2%, and thermal expansivity is 2*10
-6/ ℃.
Embodiment 3
With true density 〉=2.1g/cm
3The after-smithing petroleum coke of ash content≤0.3% is made 0.5mm＜particle diameter≤0.335mm, 0.335mm＜particle diameter≤0.15mm, 0.15mm＜particle diameter≤0.075mm and particle diameter four other pellets of level less than 0.075mm after fragmentation, screening, place respectively in four feed bins.Prepare burden then, aggregate and tackiness agent are prepared burden according to weight ratio at 75: 25, tackiness agent is that softening temperature is 83～86 ℃, the mid-temperature pitch of coking value 〉=49%, wherein aggregate is pressed: the weight of the after-smithing petroleum coke of 0.5mm＜particle diameter≤0.335mm accounts for 10% of total after-smithing petroleum coke, 0.335mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.15mm accounts for 25% of total after-smithing petroleum coke, 0.15mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.075mm accounts for 20% of total after-smithing petroleum coke, the weight of the after-smithing petroleum coke of particle diameter＜0.075mm accounts for 45% of total after-smithing petroleum coke and prepares burden.
The above-mentioned aggregate for preparing put into to mix to pinch to do in the pot mix, dried doing time is 40 minutes, and doing mixed temperature is 120 ℃.After dried the mixing, add mid-temperature pitch and carry out wet mixing, the temperature of wet mixing is 145 ℃, for the first time the weight of the mid-temperature pitch that adds is 75% of total mid-temperature pitch, the time of wet mixing for the first time is 20 minutes, for the second time the weight of the mid-temperature pitch that adds is 25% of total mid-temperature pitch, and the time of wet mixing for the second time is 15 minutes.
Thickener after the wet mixing is put into dry in the air material operation of the material machine that dries in the air, when treating that the thickener temperature is reduced to 110 ℃, thickener is put into the vibrating forming machine grinding tool carry out vibratory compaction, die mould product flawless, volume density is 1.74g/cm
3
The moulding product are put into ring-form calcining furnace carry out bakes to burn the article, in the time of 150-400 ℃, temperature rise rate is 11 ℃/h; In the time of 400-600 ℃, temperature rise rate is 0.9 ℃/h; In the time of 600-900 ℃, temperature rise rate is 1.1 ℃/h; In the time of 900-1200 ℃, temperature rise rate is 3 ℃/h, and whole temperature-rise period is controlled with the temperature alarming instrument, the temperature range that guarantees the temperature alarming instrument in 5 ℃, the roasting product flawless.
Behind the bakes to burn the article, carry out single-steeping, re-baking, double-steeping and three roastings successively, soaker is the impregnating pitch that quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃, during dipping, impregnating pitch is heated to 300 ℃, be incubated 1 hour, impregnating pitch risen again 200 ℃ again, flood.During single-steeping pickled product is preheating to 370 ℃, rate of body weight gain is 13% behind the single-steeping.Re-baking carries out at tunnel furnace, re-baking time spent 310h, and the top temperature of re-baking is 750 ℃.During double-steeping pickled product is preheating between 370 ℃, rate of body weight gain is 7% behind the double-steeping.Three roastings are carried out at tunnel furnace, and the time of three roastings is 310h, and top temperature is 750 ℃.
Three roasting products are put into the greying circuit carry out greying, electric power feeding time is 130h, and the greying top temperature is 2800 ℃.Come out of the stove after the machining cutting obtains graphite material.Graphite finished product flawless, small product size density are 1.80g/cm
3, resistivity is 7.0 μ Ω m, and ultimate compression strength is 38Mpa, and folding strength is 19Mpa, and void content is 12%, and ash content is 0.2%, and thermal expansivity is 2*10
-6/ ℃.
Embodiment 4
With true density 〉=2.1g/cm
3The after-smithing petroleum coke of ash content≤0.3% is made 0.5mm＜particle diameter≤0.335mm, 0.335mm＜particle diameter≤0.15mm, 0.15mm＜particle diameter≤0.075mm and particle diameter four other pellets of level less than 0.075mm after fragmentation, screening, place respectively in four feed bins.Prepare burden then, aggregate and tackiness agent are prepared burden according to weight ratio at 72: 28, tackiness agent is that softening temperature is 83～86 ℃, the mid-temperature pitch of coking value 〉=49%, wherein aggregate is pressed: the weight of the after-smithing petroleum coke of 0.5mm＜particle diameter≤0.335mm accounts for 20% of total after-smithing petroleum coke, 0.335mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.15mm accounts for 20% of total after-smithing petroleum coke, 0.15mm the weight of the after-smithing petroleum coke of＜particle diameter≤0.075mm accounts for 18% of total after-smithing petroleum coke, the weight of the after-smithing petroleum coke of particle diameter＜0.075mm accounts for 42% of total after-smithing petroleum coke and prepares burden.
The above-mentioned aggregate for preparing put into to mix to pinch to do in the pot mix, dried doing time is 40 minutes, and doing mixed temperature is 120 ℃.After dried the mixing, add mid-temperature pitch and carry out wet mixing, the temperature of wet mixing is 135 ℃, for the first time the weight of the mid-temperature pitch that adds is 70% of total mid-temperature pitch, the time of wet mixing for the first time is 15 minutes, for the second time the weight of the mid-temperature pitch that adds is 30% of total mid-temperature pitch, and the time of wet mixing for the second time is 15 minutes.
Thickener after the wet mixing is put into dry in the air material operation of the material machine that dries in the air, when treating that the thickener temperature is reduced to 110 ℃, thickener is put into the vibrating forming machine grinding tool carry out vibratory compaction, die mould product flawless, volume density is 1.74g/cm
3
The moulding product are put into ring-form calcining furnace carry out bakes to burn the article, in the time of 150-400 ℃, temperature rise rate is 1.4 ℃/h; In the time of 400-600 ℃, temperature rise rate is 0.8 ℃/h; In the time of 600-900 ℃, temperature rise rate is 1.4 ℃/h; In the time of 900-1200 ℃, temperature rise rate is 2.5 ℃/h, and whole temperature-rise period is controlled with the temperature alarming instrument, the temperature range that guarantees the temperature alarming instrument in 5 ℃, the roasting product flawless.
Behind the bakes to burn the article, carry out single-steeping, re-baking, double-steeping and three roastings successively, soaker is the impregnating pitch that quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃, during dipping, impregnating pitch is heated to 280 ℃, be incubated 1 hour, impregnating pitch risen again 200 ℃ again, flood.During single-steeping pickled product is preheating to 375 ℃, rate of body weight gain is 13.2% behind the single-steeping.Re-baking carries out at tunnel furnace, re-baking time spent 315h, and the top temperature of re-baking is 750 ℃.During double-steeping pickled product is preheating between 375 ℃, rate of body weight gain is 7.1% behind the double-steeping.Three roastings are carried out at tunnel furnace, and the time of three roastings is 315h, and top temperature is 750 ℃.
Three roasting products are put into the greying circuit carry out greying, electric power feeding time is 138h, and the greying top temperature is 2950 ℃.Come out of the stove after the machining cutting obtains graphite material.Graphite finished product flawless, small product size density are 1.81g/cm
3, resistivity is 6.9 μ Ω m, and ultimate compression strength is 39Mpa, and folding strength is 18Mpa, and void content is 14%, and ash content is 0.16%, and thermal expansivity is 2*10
-6/ ℃.
Experimental example 1
This experimental example is the comparative experiments that the raw material of graphite material of the present invention is chosen.First group is adopted the marketable material defined in the present invention, selects common marketable material for use for second group, and presses preparation method and the processing parameter preparation of embodiment 1, and measures its volume density, resistivity and ash content, the results are shown in Table 1.
Table 1
Conclusion: compare with common marketable material, select true density 〉=2.1g/cm for use
3The after-smithing petroleum coke of ash content≤0.3%, softening temperature are 83～86 ℃, the impregnating pitch that the mid-temperature pitch of coking value 〉=49%, quinoline do not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃ is a raw material, improve the volume density of graphite material, and reduced the ash content and the resistivity of graphite material.
Experimental example 2
This experimental example is the comparative experiments to the batching of aggregate in the raw material of the present invention, wherein, first group is the embodiment of the invention 1, second group of particle diameter and content with reference to Chinese patent 201010263217.3 is prepared burden, the 3rd group of particle diameter and the content with reference to Chinese patent 200710090789.4 is prepared burden, all preparation method and the processing parameter according to the embodiment of the invention 1 prepares, and measures its volume density, void content, ultimate compression strength and thermal expansivity, the results are shown in Table 2.
Table 2
Conclusion: the particle diameter of aggregate is less than 0.5mm in first group, the particle diameter of aggregate is less than 0.8mm in second group and the 3rd group, first group is the batching of small-particle more, first group volume density and ultimate compression strength are apparently higher than second group and the 3rd group, void content is starkly lower than second group and the 3rd group, the thermal expansivity of first group and second group is all lower, and the 3rd group thermal expansivity is higher relatively, and this may be higher the causing of quality percentage composition of the particles of aggregates of particle diameter＜0.075mm in the 3rd group.In general, when adopting the particle diameter of aggregate among the present invention and quality percentage composition, pile up comparatively closely, improved the over-all properties of graphite material.
Experimental example 3
This experimental example by three groups of experiment comparative analyses the different pretreatments of impregnating pitch to the graphite material Effect on Performance, the method of the embodiment of the invention 1 is all adopted in three groups of experiments of this experimental example, and adopts all processing parameters except that the impregnating pitch pre-treatment among the embodiment 1.
First group of pretreating scheme that is prior art to impregnating pitch is heated to 170 ℃ with impregnating pitch, adds impregnating autoclave then, floods; Second group and the 3rd group are heated to 210 ℃ and 300 ℃ for the pretreating scheme of the present invention to impregnating pitch respectively with impregnating pitch, make the volatilization of part light component, rise again respectively after 180 ℃ and 200 ℃ again, and the adding impregnating autoclave floods.The results are shown in Table 3.
Table 3
Conclusion: by impregnating pitch being heated to 210～300 ℃, make the volatilization of part light component, rise again respectively again after 180 ℃ and 200 ℃, though the viscosity of impregnating pitch slightly rises, its viscosity numerical value is still more satisfactory, and the impregnating pitch ratio is easier to penetrate in the pickled product, but the surface as a result of dipping, rate of body weight gain behind the dipping obviously increases, and makes the volume density of final finished graphite material also obviously improve, and void content obviously reduces.
Claims (11)
1. a photovoltaic industry monocrystalline silicon growing thermal field graphite material is characterized in that the volume density 〉=1.80g/cm of described graphite material
3, resistivity≤7.0 μ Ω m, ultimate compression strength 〉=38Mpa, folding strength 〉=18Mpa, void content≤14%, ash content≤0.2%, thermal expansivity≤2*10
-6/ ℃; Described graphite material is preferably volume density 〉=1.82g/cm
3, resistivity≤6.8 μ Ω m, ultimate compression strength 〉=39Mpa, folding strength 〉=19Mpa, void content≤13%, ash content≤0.17%, thermal expansivity≤2*10
-6/ ℃.
2. graphite material according to claim 1 is characterized in that, in the raw material of described graphite material, aggregate is an after-smithing petroleum coke, and binding agent is a mid-temperature pitch, and soaker is impregnating pitch; True density 〉=the 2.1g/cm of described after-smithing petroleum coke
3, ash content≤0.3%; The softening temperature of described mid-temperature pitch is 83～86 ℃, coking value 〉=49%; Described impregnating pitch is: quinoline does not melt thing≤0.2%, coking value 〉=48%, softening temperature 83-86 ℃.
3. graphite material according to claim 1 is characterized in that the weight ratio of described after-smithing petroleum coke and mid-temperature pitch is 70: 30～75: 25, be preferably 70: 29～and 30.
4. graphite material according to claim 1 is characterized in that, percentage composition meter by weight, and the particle size range of described after-smithing petroleum coke and content are:
0.5mm＜particle diameter≤0.335mm 10%-25%,
0.335mm＜particle diameter≤0.15mm 20%-25%,
0.15mm＜particle diameter≤0.075mm 15%-20%,
Particle diameter＜0.075mm 40%-45%;
The particle size range and the content of described after-smithing petroleum coke are preferably:
0.5mm＜particle diameter≤0.335mm 25%,
0.335mm＜particle diameter≤0.15mm 20%,
0.15mm＜particle diameter≤0.075mm 15%,
Particle diameter＜0.075mm 40%.
5. the preparation method of the described graphite material of claim 1, described preparation method may further comprise the steps: the fragmentation of raw material, screening, batching, mix pinch, moulding, bakes to burn the article, single-steeping, re-baking, double-steeping, three roastings and greying obtain finished product, it is characterized in that
Described bakes to burn the article is: in the time of 150-400 ℃, temperature rise rate is 1.1-1.5 ℃/h; In the time of 400-600 ℃, temperature rise rate is 0.7-0.9 ℃/h; In the time of 600-900 ℃, temperature rise rate is 1.1-1.5 ℃/h; In the time of 900-1200 ℃, temperature rise rate is 2.3-3 ℃/h.
6. preparation method according to claim 4, it is characterized in that, described mixed pinching is divided into the dry blend wet mixing, described wet mixing is mid-temperature pitch to be joined to mix in the aggregate of doing after mixing at twice pinch, for the first time the weight of the mid-temperature pitch that adds is the 70-80% of total mid-temperature pitch, and the weight of the mid-temperature pitch that adds is the 20-30% of total mid-temperature pitch for the second time.
7. preparation method according to claim 4 is characterized in that, describedly is shaped to vibratory compaction, and the volume density of green compact reaches 1.74g/cm after the moulding
3More than.
8. preparation method according to claim 4 is characterized in that, during dipping, impregnating pitch is heated to 210～300 ℃, preferably is heated to 210～250 ℃, is incubated 1～2 hour, impregnating pitch is risen again 180～200 ℃ again, floods;
The preheating temperature of pickled product is 360-380 ℃ during single-steeping, and rate of body weight gain is more than 13%;
The preheating temperature of pickled product is 360-380 ℃ during double-steeping, and rate of body weight gain is more than 7%.
9. preparation method according to claim 4 is characterized in that, the time of described re-baking is 300-320h, and the top temperature of re-baking reaches 750 ℃.
10. preparation method according to claim 4 is characterized in that, the time of described three roastings is 300-320h, and top temperature reaches 750 ℃.
11. preparation method according to claim 4 is characterized in that, the described graphited time is 130-140h, and graphited top temperature is 2800-3000 ℃.
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| CN109503168A (en) * | 2018-10-08 | 2019-03-22 | 湖北捷地安电气有限公司 | A kind of efficient discharge earthing module |
| CN109852081A (en) * | 2018-12-20 | 2019-06-07 | 淄博大陆石墨科技有限公司 | The preparation method that vibration-compression molding special graphite is homogenized with thickener |
| CN109852081B (en) * | 2018-12-20 | 2021-07-30 | 淄博大陆石墨科技有限公司 | Preparation method of paste homogenization for special graphite by vibration-compression molding |
| CN111138207A (en) * | 2020-01-14 | 2020-05-12 | 大同新成新材料股份有限公司 | Preparation method of graphite thermal field material for Czochralski silicon furnace |
| CN115259870A (en) * | 2022-07-29 | 2022-11-01 | 宝丰县洁石碳素材料有限公司 | Preparation process of graphite for single crystal thermal field |
| CN116082041A (en) * | 2023-02-20 | 2023-05-09 | 平顶山东方碳素股份有限公司 | Graphite material with low thermal expansion coefficient and production method thereof |
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