CN1562830A - Manufacturing technique for preparing microcrystalline glass of imitating biologic clast through crystallization method of crack glass - Google Patents

Manufacturing technique for preparing microcrystalline glass of imitating biologic clast through crystallization method of crack glass Download PDF

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CN1562830A
CN1562830A CN 200410012997 CN200410012997A CN1562830A CN 1562830 A CN1562830 A CN 1562830A CN 200410012997 CN200410012997 CN 200410012997 CN 200410012997 A CN200410012997 A CN 200410012997A CN 1562830 A CN1562830 A CN 1562830A
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glass
crackle
crystallization
sintering
particle
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CN1251982C (en
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周俊
王焰新
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Wuhan In Big Asset Management Co ltd
Zhejiang China Science And Technology Co ltd
Zhou Jun
China University of Geosciences
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China University of Geosciences
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/08Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce crackled effects
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/076Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C03C3/093Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
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Abstract

The prodn. processing steps are: (1) prepn. of glass fusant; (2) prepn. of crackle glass, the glass fusant is formed to required shape by regular rolling and teeming forming technology, then it is punching broken to be cracked but non-separated crackle glass by shrending braking or cold airflow airflow braking or press machine; (3) heating process, the crackle glass is put into refractory model which is send into electric furnace or turnnel kiln or roller kiln or shuttle kiln to do burning and crystallizing heating process for crackle glass; (4) to produce imitated biological clastic microcrystal glass product by grinding and polishing. The product has low-porosity compact texture in and at surface of the crackle glass.

Description

Crackle glass crystallization method prepares the production technique of bionical thing chip devitrified glass
Technical field
The present invention relates to a kind of production technique of devitrified glass, particularly relate to a kind of production technique with creature dross grain emulated, that void content is low devitrified glass.
Background technology
Devitrified glass also is microlite, beautiful spar, be with parent glass through Overheating Treatment, on glass matrix, generate a kind of crystal and the glassy phase compound material of microcrystal.Devitrified glass has compact structure, physical strength height, wear-resisting, corrosion-resistant, advantageous property such as the weathering resistance ability is strong, has been widely used in each field such as building, chemical industry, electronics, biomedicine, mechanical engineering, military affairs.
At present, the processing method of production devitrified glass mainly contains three kinds: sintering process, rolling process and casting.Wherein sintering process is most widely used, and the rolling process application is less, and casting mass-producing is not yet used.
The technical process of sintering process is: batching, mixing, glass smelting, shrend become glass particle, dry, sieve, classification, dress mould, sintering, crystallization, grinding and polishing, finished product.The advantage of this technology is: there is texture on the surface of (1) product; (2) crystallization is fast, controls the crystallization process easily; (3) thickness of product and specification are easy to adjust; (4) though technical process is numerous, production process is easy to control.The weak point of this technology is: the intergranular space of (1) parent glass is difficult to get rid of fully in sintering process, inevitably gas hole defect can occur; (2) the surface compact layer depth is shallow, usually less than 2mm; (3) stone is difficult to fully evenly, needs to force the surface molten flat with very high firing temperature the energy consumption height; (4) the shrend glass particle oven dry, broken, sieve, store, adorn in the operation process such as mould, polluted easily, make product the fault defective occur; (5) exhaust the formula production technique between belonging to, production efficiency is not high; (6) texture is generally granular.
The technical process of rolling process is: batching, mixing, glass smelting, calendering formation, crystallization, grinding and polishing, finished product.The advantage of rolling process is: product density height, pore-free, and folding strength is big; Manufacturing process is continuous, automatic production completely; Be easy to moulding.Its deficiency shows: (1) superficial makings is not obvious; (2) crystallization is wayward, and the whole crystallization time is long, and production efficiency is low; (3) burst in the heat treatment process seriously, yield rate is low.
The technical process of casting is: batching, mixing, glass smelting, casting, crystallization, grinding and polishing, finished product.The advantage of casting shows: pourable one-tenth sketch plate; Product density height, pore-free, folding strength is big.Its deficiency shows: (1) requires high to die quality, the mould loss is big; (2) produce the large-sized plates material because of difficulty; (3) superficial makings is not obvious; (4) crystallization is wayward, and the whole crystallization time is long, and production efficiency is low.
For overcoming the deficiency that a glass material sintering process is easy to generate gas hole defect, Chinese patent publication number CN1438192A has proposed a kind of layering technology of preparing, promptly on the sheet glass base material of single or multiple lift, evenly spread cloth glass particle material, sintering, crystallization under 900 ℃~1230 ℃ conditions then, and glass particle is melted on the sheet glass base material, make the devitrified glass of low porosity.Wherein, one of treatment process of sheet glass base material is that it is carried out cold quenching under 400 ℃~900 ℃ conditions, makes it crackle occur; Again with the crackle sheet glass as base material, spread cloth glass particle material in the above, the more related glass baseplate of glass particle material is promptly produced the devitrified glass of low porosity in 1000 ℃~1230 ℃ sintering, crystallizatioies in kiln.The weak point of this patent is, with sheet glass (comprising the crackle sheet glass) as base material, must spread cloth glass particle material in the above, glass particle according to aforesaid sintering process preparating mechanism through oversintering, crystallization, and be fused on lower floor's sheet glass base material, just can be prepared into the devitrified glass panel products.Wherein, upper strata glass particle material found, dry, spread operations such as cloth and sintering, the crystallization process is consistent with conventional sintering method technology.Final object that grinds, polishes and the appearance surfaces that shows also are the glass-ceramic layer that glass particle generates, and therefore, this patent can not overcome the deficiency of sintering process fully, and the active effect that can rise is to reduce the void content of microcrystal glass plate lower floor.In addition, as surface decoration sheet material, the exterior appearance of the patented product is the pattern that is generated by upper strata glass particle sintering, crystallization, shows as the particulate state texture; And the crack morphology that lower floor's crackle glass baseplate generates can't show, and does not play decoration function.As seen, major function that the crackle sheet glass that this patent is mentioned is play and effect are the carryings to the upper strata glass particle bed of material, and the lower floor that constitutes final devitrified glass product, to reduce the void content of product lower floor.
Summary of the invention
At existing deficiency in the currently used devitrified glass production technique, the object of the present invention is to provide a kind of production technique with creature dross grain emulated, that void content is extremely low bionical thing chip devitrified glass.
" bionical thing chip devitrified glass " of the present invention means that the devitrified glass product has the irregular dendroid of the residual body of similar extinct plants and animal and the texture of particulate state pattern.
To achieve these goals, technical scheme of the present invention is: crackle glass crystallization method prepares the production technique of bionical thing chip devitrified glass, it is characterized in that production craft step is as follows:
(1) preparation of glass melt: the weighing desired raw material mixes; Utilize conventional glass smelting technology, be dosed in the glass melter, at 1400~1550 ℃ of following melting 1~2.5h; Glass melt is clarified, is all changed in cooling again;
(2) preparation of crackle glass: adopt conventional calendering or cast or horizontal drawing or float glass process or briquetting process that glass melt is made desired shape, split in that 700~1000 ℃ of following shrends are frightened, or cold air flow is frightened splits, or in cooling back pressing machine punching press fragmentation fully, pressure is 5~20MPa, makes the crackle glass of " split and do not loose ";
(3) thermal treatment: the crackle glass that makes is transferred in the fireproof die, enter electric furnace or tunnel furnace or roller kiln or shuttle kiln, carry out sintering, crystallization and thermal treatment, its temperature schedule can be with two kinds of systems, be respectively: 1. the temperature rise rate with 2~15 ℃/min rises to 1000~1180 ℃, insulation 50~120min makes crackle glass sintering, crystallization become devitrified glass; 2. the temperature rise rate with 10~15 ℃/min rises to 710~890 ℃, and insulation 30~90min makes the healing of glass crack sintering; Temperature rise rate with 1~10 ℃/min rises to 950~1180 ℃ again, and insulation 30~120min makes glass crystallization;
(4) the devitrified glass blank is ground, polishes, make bionical thing chip devitrified glass finished product.
In described step (2) and the step (3), shrend is frightened to be split or frightened temperature or the stamping press that splits of cold air flow controlled crack number, glass cullet granular size by regulating, and then the devitrified glass surface topography after control sintering, the crystallization and thermal treatment, promptly, cold quenching temperature height or stamping press are big, can make the crackle glass that crackle is many, particle is little, after the thermal treatment, creature dross grain emulated intensive, the floating turbid glass particle of complete crystallization is not little; Otherwise, can make the crackle glass that crackle is few, particle is big, creature dross grain emulated loose after the thermal treatment, floating turbid glass particle is big.
The present invention adopts above-mentioned production craft step, and described step (2) and step (3) are interrelated, the integration one, constitute characterization step of the present invention jointly.The application of step (2) and step (3) makes this technology have that sintering time is short, the fireballing feature of crystallization, make product have creature dross grain emulated obviously, feature that void content is low.
The key problem in technology of this production technique is: glass melt is made crackle glass, again crackle glass is carried out sintering, crystallization and thermal treatment, make all have bionical thing chip crystal texture in the table, devitrified glass that void content is extremely low.Its technological core is to carry out crystallization and thermal treatment with crackle glass as parent glass.Therefore, the present invention is called this production technique " crackle glass crystallization method ".
This production technique mainly shows with the difference of sintering process, rolling process and casting: sintering process is that the glass metal that will melt flows in the water, through shrend, dry, sieve, make the glass particle material of certain size grading, again particulate material is packed in the mould, with the glass particle is heat treatment object, carries out sintering, crystallization processing; Rolling process and casting are the mode of glass metal by rolling or pouring into a mould that will melt, and make the flawless glass of definite shape, carry out crystallization with this glass as heat treatment object again and handle; And this technology is to utilize traditional glass metal forming method (as calendering, cast, compacting, horizontal drawing or float glass process etc.) moulding, shrend is frightened again splits (or mechanical pressure break, cold air flow is frightened split) becomes crackle glass, and be heat treatment object with crackle glass, carry out sintering, crystallization is handled.
The characteristics and the positively effect of this production technique are as follows:
(1) helps reducing the gas hole defect of devitrified glass.Since crackle glass come down to by countless, that differ in size, contacted with crack surface, closely link together, " split and do not loose " glass cullet particle combines closely and forms, between the glass cullet particle except trickle crack, there is not big hole, therefore, be very easy to sinter into the low devitrified glass of void content.By contrast, the particle sintering process is glass particle to be deposited in carry out sintering in the mould, in any case optimize grain composition and dress mould mode, all between glass particle, there is hole inevitably, the part hole is closed and forms isolated bubble, after polishing, show as pore (or pin hole, pit) defective.Therefore, this technology can solve the inextirpable pore problem of sintering process, and the comparable sintering process of void content reduces more than 95%.
(2) help generating creature dross grain emulated, enriched the superficial makings pattern of devitrified glass.Crackle glass by countless, split and the glass cullet granulometric composition that do not loose, thereby increased specific surface area, surface energy and surface imperfection, reduced the crystal nucleation barrier potential, help crystal and separate out.So when thermal treatment, crystal will be at first separated out on glass cullet particulate surface, also be the preferential crystallization of cracks, grow to the glass cullet granule interior again.Finally obtain a kind of bionical thing chip crystal texture and irregular floating turbid glass body chimeric special texture mutually, enriched the texture kind of devitrified glass.By contrast, the devitrified glass that makes of rolling process and casting does not have texture; And casting can only generate grain usually.
(3) production technique continuously, simply.Raw materials melt becomes glass metal, makes crackle glass again, and global transfer just can directly enter crystallization kiln to mould, make devitrified glass through sintering, crystallization.The entire job object is in the successive operating process, and production technique continuously, simply.By contrast, sintering process after shrend generates glass particle, also will through broken, sieve, sorting, storage, cloth dress mould repeatedly, heat-treat again, whole process of production exhausts the formula operation between being.
(4) raw material range is wide, formula range is wide.As described in characteristics (1) and characteristics (2), this technology helps sintering and crystallization, so some prescription of easy-sintering, crystallization not, and an also available technology reaches good sintering and crystallization effect, thereby makes the range of choice of raw material obtain expanding.Certainly, the prescription that sintering character is good will be more suitable for this technology; And the crystallization ability is strong, also available this technology of prescription of the whole crystallization of energy, produces the devitrified glass of integrally crystallization.(annotate: embodiment 1,2,3,4 and 6 prescription, if use rolling process or casting instead, sheet glass integral body is difficult to separate out crystal in heat treatment process; The prescription of embodiment 6, if use sintering process instead, glass particle is difficult to sintering in heat treatment process, the surface is difficult to molten flat).
(5) there are not the not enough and fried problem of heat of densification depths, yield rate height.The devitrified glass that this technology makes is the same outside and inside, pore is few, so grind, polishing thickness is dark again, also a large amount of pores can not occur.Can remedy whereby the sintering process dense layer thickness thin (usually<2mm), grind, polishing can not too dark deficiency; In addition, this technology is close with casting with rolling process, but owing to passed through hardening crack or fracture treatment, the internal stress of parent glass is released, so can not burst during thermal treatment, the heat that has overcome rolling process and casting is exploded problem.Therefore the yield rate of this technology is than the equal height of current technology.
(6) thermal treatment temp is low, the time is short, can fall the thermal treatment less energy-consumption.As described in characteristics (1) and characteristics (2), this technology helps sintering and crystallization, so can reduce thermal treatment temp, shortening heat treatment time.In addition, because smooth, the no pit of crackle glass self, thickness are even, so compare with sintering process, needn't melt flat glass surface with high temperature when thermal treatment, required maximum heat treatment temperature is relatively low.
(7) can reduce requirement to mould.As described in characteristics (1), (2) and (6), the easy sintering of this technology, crystallization, and needn't be molten flat with high temperature, heat treatment time is short, temperature is low, and available rates is cheap, long service life, mould that refractory temperature is low, even stainless steel mould.
(8) can reduce production costs.Characteristics (3), (4), (5), (6) and (7) show that jointly because this technology has easy-sintering, easy crystallization, thermal treatment temp is low, the time is short, energy consumption is low; Production technique is simple, continuous; It is fried to be difficult for that heat takes place, and the pore inner and top layer is all less, the yield rate height; Formula range is wide, raw material range is wide; Mould is required advantages such as low, production cost is reduced greatly.
(9) the layering technology of preparing that proposes with Chinese patent publication number CN1438192A is compared, this technology also has following characteristics and advantage: 1. product is bionical thing chip devitrified glass, appearance is the pattern after crackle glass sintering, the crystallization, shows as creature dross grain emulated; And the product of CN1438192A is the devitrified glass of grain, and appearance is the pattern after glass particle sintering, the crystallization, shows as the particulate state texture; 2. do not need to prepare separately the glass particle material; And the production technique of CN1438192A need prepare the glass particle material separately; 3. heat treatment object only is a crackle glass, promptly makes the healing of crackle glass, crystallization by sintering, crystallization process, makes the devitrified glass finished product; And the heat treatment object of CN1438192A had both comprised the upper strata glass particle, also comprised the glass baseplate of lower floor, sintering, crystallization process complexity; 4. the finished product integral body forms by crackle glass sintering, crystallization; And the crackle sheet glass that CN1438192A mentions has only constituted the lower floor of the finished product, and function that is play and effect are the carryings to the upper strata glass particle bed of material, and the void content that reduces microcrystal glass plate lower floor; 5. the finished product are the same outside and inside, are the dense structure of low porosity; And the product of CN1438192A is a laminate structure, and it is the particle sintering structure at the middle and upper levels, inevitably has the deficiency of sintering process; 6. this technology also has characteristics (3)~(8) described positively effect; And the upper strata glass particle layer of CN1438192A is consistent with sintering process in fact, has inherited the part deficiency of sintering process, does not have these positively effects.
Description of drawings
Fig. 1 is a technological process of production synoptic diagram of the present invention.
Embodiment
The invention will be further described below in conjunction with accompanying drawing 1 and embodiment.
Embodiment 1: as shown in Figure 1, with weight percent, the used proportioning raw materials of this example is: 32.00% feldspar, 24.70% quartz sand, 25.35% calcite, 0.75% salt of wormwood, 5.40% soda ash, 2.20% boric acid, 0.40% antimonous oxide, 4.25% barium carbonate, 4.95% zinc oxide; The prescription chemical constitution is: 55.96%SiO 2, 6.99%Al 2O 3, 17.46%CaO, 0.07%MgO, 1.97%K 2O, 4.97%Na 2O, 1.50%B 2O 3, 0.48%Sb 2O 3, 3.97%BaO, 5.98%ZnO, 0.02%Fe 2O 3, 0.01%TiO 2, 0.62%Li 2O.By prescription, be mixed with compound, grind evenly, the corundum crucible of packing into uses the Si-Mo rod high-temperature electric resistance furnace at 1550 ℃ of melting 120min.Glass metal is poured in the fireproof die, at the frightened crackle sheet glass that is cleaved into of 950 ℃ of shrends.Put back to electric furnace again and heat-treat, temperature schedule is: 200 ℃ are advanced stove; 200 ℃~810 ℃, 11 ℃/min; 810 ℃ of insulation 40min; 810~1060 ℃, 6 ℃/min; 1060 ℃ of insulation 90min; Self cooling with stove.After grind, polishing, the surface is shown as dendrite texture and irregular floating turbid glass particulate mixing pattern, promptly bionical thing chip pattern.The surface has only less pin hole, does not affect the appearance.
Embodiment 2: with the processing step of embodiment 1, what difference was that the preparation of crackle glass adopts is mechanical fracturing process.Be specially: be poured in the fireproof die after glass smelting is good, move in the air behind 700 ℃ of annealing 30min, naturally cooling becomes sheet glass.Again the sheet glass upper and lower faces is sticked scotch tape, with hydraulic press punching press fragmentation, pressure is 10MPa, makes the crackle sheet glass of " split and do not loose ".The effect of taping in the sheet glass above and below is to prevent that sheet glass from scattering after cracked; Adhesive tape decomposes burning and loses in heat treatment process.The product pattern is with embodiment 1.
Embodiment 3: with the processing step of embodiment 1, what difference was that the preparation of crackle glass adopts is the frightened cracking method of cold air flow.Be specially: be poured in the fireproof die after glass smelting is good, in the time of 1000 ℃, move in the air,, make the cold frightened crackle sheet glass that is fragmented into of sheet glass immediately with the gas blower chilling of drying.The product pattern is with embodiment 1.
Embodiment 4: with weight percent, the used proportioning raw materials of this example is: 4.00% aluminum oxide, 52.10% quartz sand, 26.90% calcite, 5.10% soda ash, 2.20% boric acid, 0.40% antimonous oxide, 4.30% barium carbonate, 5.00% zinc oxide; The prescription chemical constitution is: 62.00%SiO 2, 4.50%Al 2O 3, 18.00%CaO, 3.50%Na 2O, 1.50%B 2O 3, 0.50%Sb 2O 3, 4.00%BaO, 6.00%ZnO.By prescription, be mixed with compound, grind evenly, the corundum crucible of packing into uses the Si-Mo rod high-temperature electric resistance furnace at 1500 ℃ of melting 120min.When glass metal is cooled to 1100 ℃, be poured on the refractory support, be rolled into sheet glass with stainless steel bar, shrend becomes the crackle sheet glass again, and the shrend temperature is 900 ℃.Put back to electric furnace again and heat-treat, temperature schedule is: 200 ℃ are advanced stove; 200 ℃~780 ℃, 11 ℃/min; 780 ℃ of insulation 40min; 780~1040 ℃, 7 ℃/min; 1040 ℃ of insulation 90min; Self cooling with stove.After grind, polishing, the surface is shown as crystal texture and irregular floating turbid glass particulate mixing pattern, promptly bionical thing chip pattern.The surface has only few pin hole, does not affect the appearance.
Embodiment 5: with weight percent, the used proportioning raw materials of this example is: 4.00% aluminum oxide, 51.60% quartz sand, 26.90% calcite, 5.10% soda ash, 2.20% boric acid, 0.40% antimonous oxide, 4.30% barium carbonate, 5.00% zinc oxide, 0.5% chromium sesquioxide; The prescription chemical constitution is: 61.26%SiO 2, 4.54%Al 2O 3, 18.02%CaO, 3.50%Na 2O, 1.49%B 2O 3, 0.47%Sb 2O 3, 3.99%BaO, 6.01%ZnO, 0.72%Cr 2O 3By prescription, be mixed with compound, grind evenly, the corundum crucible of packing into uses the Si-Mo rod high-temperature electric resistance furnace at 1500 ℃ of melting 120min.Glass metal is poured in the fireproof die, at the frightened crackle sheet glass that is cleaved into of 950 ℃ of shrends.Put into silicon molybdenum rod furnace again and heat-treat, temperature schedule is: 100 ℃ are advanced stove; 100 ℃~750 ℃, 11 ℃/min; 750 ℃~860 ℃, 2 ℃/min; 860~1040 ℃, 4 ℃/min; 1040 ℃ of insulation 110min; Self cooling with stove.After grind, polishing, make surperficial existing light green crystal texture, also have irregular green to float the turbid glass particle, present bionical thing chip pattern.The surface does not have pore.
Embodiment 6: with weight percent, the used proportioning raw materials of this example is: 3.90% aluminum oxide, 51.00% quartz sand, 26.20% calcite, 1.80% salt of wormwood, 9.20% soda ash, 2.20% boric acid, 0.40% antimonous oxide, 3.20% barium carbonate, 1.60% zinc oxide, 0.50% Manganse Dioxide; The prescription chemical constitution is: 62.00%SiO 2, 4.50%Al 2O 3, 18.00%CaO, 1.50%K 2O, 6.50%Na 2O, 1.50%B 2O 3, 0.50%Sb 2O 3, 3.00%BaO, 2.00%ZnO, 0.50%MnO 2By prescription, be mixed with compound, grind evenly, the corundum crucible of packing into uses the Si-Mo rod high-temperature electric resistance furnace at 1480 ℃ of melting 120min.Glass metal is poured in the fireproof die, at the frightened crackle sheet glass that is cleaved into of 950 ℃ of shrends.Put into silicon molybdenum rod furnace again and heat-treat, temperature schedule is: 150 ℃ are advanced stove; 150 ℃~870 ℃, 11 ℃/min; 870 ℃ of insulation 40min; 870~1100 ℃, 10 ℃/min; 1100 ℃ of insulation 90min; Self cooling with stove.After grind, polishing, make surperficial existing white crystal texture, also have irregular light beige to float the turbid glass particle, present bionical thing chip pattern.Apparent porosity is extremely low.

Claims (2)

1. crackle glass crystallization method prepares the production technique of bionical thing chip devitrified glass, it is characterized in that production craft step is as follows:
(1) preparation of glass melt: the weighing desired raw material mixes; Utilize conventional glass smelting technology, be dosed in the glass melter, at 1400~1550 ℃ of following melting 1~2.5h; Glass melt is clarified, is all changed in cooling again;
(2) preparation of crackle glass: adopt conventional calendering or cast or horizontal drawing or float glass process or briquetting process that glass melt is made desired shape, split in that 700~1000 ℃ of following shrends are frightened, or cold air flow is frightened splits, or in cooling back pressing machine punching press fragmentation fully, pressure is 5~20MPa, makes the crackle glass of " split and do not loose ";
(3) thermal treatment: the crackle glass that makes is transferred in the fireproof die, enter electric furnace or tunnel furnace or roller kiln or shuttle kiln, carry out sintering, crystallization and thermal treatment, its temperature schedule can be with two kinds of systems, be respectively: 1. the temperature rise rate with 2~15 ℃/min rises to 1000~1180 ℃, insulation 50~120min makes crackle glass sintering, crystallization become devitrified glass; 2. the temperature rise rate with 10~15 ℃/min rises to 710~890 ℃, and insulation 30~90min makes the healing of glass crack sintering; Temperature rise rate with 1~10 ℃/min rises to 950~1180 ℃ again, and insulation 30~120min makes glass crystallization;
(4) the devitrified glass blank is ground, polishes, make bionical thing chip devitrified glass finished product.
2. crackle glass crystallization method according to claim 1 prepares the production technique of bionical thing chip devitrified glass, it is characterized in that: in described step (2) and the step (3), shrend is frightened to be split or frightened temperature or the stamping press that splits of cold air flow controlled crack number, glass cullet granular size by regulating, and then the devitrified glass surface topography after control sintering, the crystallization and thermal treatment, promptly, cold quenching temperature height or stamping press are big, can make the crackle glass that crackle is many, particle is little, after the thermal treatment, creature dross grain emulated intensive, the floating turbid glass particle of complete crystallization is not little; Otherwise, can make the crackle glass that crackle is few, particle is big, creature dross grain emulated loose after the thermal treatment, floating turbid glass particle is big.
CN 200410012997 2004-04-09 2004-04-09 Manufacturing technique for preparing microcrystalline glass of imitating biologic clast through crystallization method of crack glass Expired - Fee Related CN1251982C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100363283C (en) * 2006-01-25 2008-01-23 中国地质大学(武汉) Flow liner crystallite glass composite plate preparation method
CN100383067C (en) * 2006-01-25 2008-04-23 中国地质大学(武汉) Preparation method of creature dross grain emulated crystallite glass composite plate
CN100393651C (en) * 2006-01-25 2008-06-11 中国地质大学(武汉) Preparation method of flow liner crystallite glass
EP2781489A1 (en) * 2013-03-22 2014-09-24 RC eNeM d.o.o. Glass and process for manufacturing of illusion glass

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100363283C (en) * 2006-01-25 2008-01-23 中国地质大学(武汉) Flow liner crystallite glass composite plate preparation method
CN100383067C (en) * 2006-01-25 2008-04-23 中国地质大学(武汉) Preparation method of creature dross grain emulated crystallite glass composite plate
CN100393651C (en) * 2006-01-25 2008-06-11 中国地质大学(武汉) Preparation method of flow liner crystallite glass
EP2781489A1 (en) * 2013-03-22 2014-09-24 RC eNeM d.o.o. Glass and process for manufacturing of illusion glass

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