CN108298991A - The manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die - Google Patents
The manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die Download PDFInfo
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- CN108298991A CN108298991A CN201810150121.2A CN201810150121A CN108298991A CN 108298991 A CN108298991 A CN 108298991A CN 201810150121 A CN201810150121 A CN 201810150121A CN 108298991 A CN108298991 A CN 108298991A
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Abstract
The present invention relates to the manufacturing methods of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, belong to boron nitride ceramics technical field of mold.It is an object of the invention to solve the problems, such as that use graphite to manufacture bend glass hot bending die in the prior art provides one kind to be commercialized powder BN powders as raw material intolerant to oxidative attack, normal pressure-sintered legal system makes h BN ceramics bend glass hot bending dies.BN ceramics have thermal conductivity is high, coefficient of thermal expansion is low, with outside the not wellability of glass and easy processing characteristic, high-temperature oxidation resistance is well many than graphite material, just start to aoxidize in air under 1200 DEG C or more hot conditions, is far below the hot bending temperature of 800 DEG C of softening points of glass.In addition, the manufacturing approach craft of the normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die is simple, cost is relatively low, it can be achieved that industrialization large-scale production, is suitble to promote the use of.
Description
Technical field
The present invention relates to the manufacturing methods of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, belong to boron nitride
Ceramic mold field.
Background technology
Hexagonal phase boron nitride（h-BN）There is the title of " white graphite ", because it has the layered crystal structure similar to graphite,
Also have and physical and chemical performance as graphite-phase, such as good lubricating properties and thermal conductivity.H-BN structural ceramics is because of its thermal conductivity
Rate is high, electrical insulation capability is good, coefficient of thermal expansion is low and the not wellability with most metals, thus high-temperature insulation component,
The fields such as atomic energy, metallurgy, aviation are widely used.Utilize the high temperature resistant of boron nitride, electrical insulating property, h-BN products
The heat shielding of the high-temperature insulation component of plasma soldering appliance, the bushing of a variety of heaters, spaceship can be used for making
Material etc..In addition high-termal conductivity, can make underground coal mine fire-proof motor insulating radiation piece, high-temp thermal couple protective casing pipe.Profit
With h-BN to glass, the nonwetting property of metal bath and erosion resisting, may be used as a variety of non-ferrous metals of melting in special smelting,
The components such as the vessel of noble metal and rare metal, crucible, delivery pump.
With the continuous upgrading of the electronic products such as mobile phone, tablet computer, the screen of this electronic product has begun largely
Using bend glass（Such as 2.5D glass screens, 3D glass screens）.Bend glass of the bend glass generally by being arranged in hot-bending machine
Hot bending die manufactures, and the basic step of manufacturing method is：First, mold is assembled into compacting readiness, at this point, in mold
Equipped with glass blank；Then, the mold for suppressing readiness is heated, to keep glass blank contained in mold soft
Change；Hereafter, the glass blank after softening is suppressed by mold, glass blank is made to be shaped to bend glass；Finally, to mould
Tool is cooled down, and bend glass product is removed from the molds after cooling.
Above-mentioned manufacturing method proposes high requirement for the material of bend glass hot bending die.In general, curved surface glass
The material of glass hot bending die need to meet the following conditions：One, enough intensity is kept under glass blank softening point temperature, is not occurred
High temperature deformation or creep；Two, under a certain pressure under the glass blank of softening maintain interface inertia, do not infiltrate mutually；Three, have
Quickly heating and cooling can be repeated in good thermal conductance and thermal shock resistance；Four, it is milled and is polished with good
Performance wants the harshness of bend glass surface smoothness, dimensional accuracy etc. to make the bend glass of manufacture meet electronic product
It asks；Five, the similar thermal expansion coefficient with glass, in order to avoid when heated due to coefficient of thermal expansion difference cause glass occur explosion or
Fold.
Bend glass hot bending die made of currently used graphite disclosure satisfy that above-mentioned condition.But general glass
Hot bending is carried out in the glass softening point temperature of 800 DEG C of glass, at this temperature, since graphite is intolerant to oxidative attack, bend glass
Manufacturing process in need mold being placed under protective atmosphere (such as nitrogen, argon gas), lead to mould to reduce air and be contacted with mold
Has ablation.The manufacturing cost of bend glass is not only a significant increase using protective atmosphere, and there are still molds in weak oxygen
Under atmosphere the phenomenon that gradual ablation.Therefore, the surface of mold needs discontinuity polishing to repair, until final because oxidation leads to stone
There is the insufficient integrity failure of intensity in the decline of smoky quartz interparticle bond strength.According to used graphite performance difference, existing song
The access times of surface glass hot bending die are generally 1000-3000 times.
BN ceramics are had not yet to see to apply on bend glass hot bending die.BN ceramics are used for bend glass by the present invention
Hot bending technical field is related to the purposes of BN ceramics, the manufacturing method of BN ceramics bend glass hot bending dies.
Invention content
The technical solution adopted in the present invention is：The manufacture of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die
Method, step are：
（1）, pretreatment of raw material, it is spare after BN powders are handled 0.5~2 hour at air atmosphere and temperature >=1200 DEG C；
（2）, mixed powder prepare, by weight Al2O3：Y2O3=0.75~1.8 ratio has weighed Al2O3And Y2O3Powder,
And be uniformly mixed, AY powders are denoted as, as sintering aid；By step（1）The BN powders and AY powders prepared is uniformly mixed system
For at mixed powder, BN powder contents >=90wt% is made in mixed powder（Weight percent）；
（3）, prepare slurry, using water or alcohol as solvent, PVA or PVB are binder, binder content≤mixed powder
2wt%（Weight percent）, it is 40~60wt% to be made into solid content as solute using mixed powder and binder（Weight percent）'s
Slurry；Then with Al2O3Slurry is uniformly mixed by ball as mill ball；
（4）, powder prepare, by step（3）In prepared slurry drying, crushing, sieving, or through mist projection granulating BN to be made multiple
Powder is closed, and controls 100 ± 10 microns of the average grain diameter of mist projection granulating；
（5）, processing and forming, by step（4）In BN composite granules obtained through dry-pressing and/or isostatic pressing, form BN ceramics
Biscuit；
（6）, unsticking sintering, by step（5）In BN biscuit of ceramics vacuum unsticking or air atmosphere unsticking obtained, then in N2
It is sintered under gas atmosphere, BN ceramics is prepared；
（7）, finishing and polishing, by step（6）The BN ceramics of preparation are processed to obtain finishing workpiece by numerically-controlled machine tool,
And it is polished to get to normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die.
The preferred step（1）The grain size of middle BN powders is 1~2 micron.
The preferred step（2）Middle Al2O3And Y2O3Average grain diameter≤1 micron of powder.
The preferred step（3）In mill ball Al2O3Dosage be 1~5 times of mixed powder weight, slurry it is mixed
It is 24 hours to close the time.
The preferred step（4）Middle drying temperature is 60~80 DEG C, and sieving process selects the sieve of 100 mesh.
The preferred step（4）The outlet temperature of middle mist projection granulating is 60~80 DEG C.
The preferred step（5）Middle dry-pressing pressure is 20 ~ 100 megapascal, and hydrostatic pressure is 200 ~ 300 megapascal.
The preferred step（6）Middle unsticking temperature is 500-1200 DEG C, and the unsticking soaking time is 60-120 minutes.
The preferred sintering temperature is 1700-1900 DEG C, and the sintered heat insulating time is 30-90 minutes.
The present invention devises the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, this method sheet
The purpose of invention be to solve the problems, such as in the prior art using graphite manufacture bend glass hot bending die intolerant to oxidative attack and
One kind is provided to be commercialized powder BN powders as raw material, normal pressure-sintered legal system makes h-BN ceramics bend glass hot bending dies.BN makes pottery
Porcelain is high with thermal conductivity, coefficient of thermal expansion is low, with outside the not wellability of glass and easy processing characteristic, and high-temperature oxidation resistance compares stone
Ink material is well very much, just starts to aoxidize in air under 1200 DEG C or more hot conditions, is far below 800 DEG C of softening points of glass
Hot bending temperature.In addition, the manufacturing approach craft of the normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die is simple, at
This is relatively low, it can be achieved that industrialization large-scale production, is suitble to promote the use of.
Specific implementation mode
Specific embodiment one, the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, step
For：
（1）, pretreatment of raw material, it is spare after BN powders are handled 1 hour at 1200 DEG C of air atmosphere and temperature；
（2）, mixed powder prepare, by weight Al2O3：Y2O3=1.5 ratio has weighed Al2O3And Y2O310 grams of powder, and
It is uniformly mixed, AY powders is denoted as, as sintering aid；By step（1）90 grams of the BN powders prepared and AY powders are uniformly mixed
It is prepared into mixed powder；
（3）, prepare slurry, using water as solvent, PVA is binder, and binder is 1 gram, using mixed powder and binder as solute
It is 45wt% to be made into solid content（Weight percent）Slurry；Then with Al2O3Slurry is uniformly mixed by ball as mill ball；
（4）, powder prepare, by step（3）In prepared slurry drying, crushing, sieving；
（5）, processing and forming, by step（4）In BN composite granules obtained through dry-pressing and isostatic pressing, form BN ceramics elements
Base；
（6）, unsticking sintering, by step（5）In BN biscuit of ceramics air atmosphere unsticking obtained, then in N2It is burnt under gas atmosphere
BN ceramics are prepared in knot；
（7）, finishing and polishing, by step（6）The BN ceramics of preparation are processed to obtain finishing workpiece by numerically-controlled machine tool,
And it is polished to get to normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die.
The step（1）The grain size of middle BN powders is 1~2 micron, the step（2）Middle Al2O3And Y2O3Powder is put down
Equal grain size≤1 micron, the step（3）In mill ball Al2O3Dosage be 180 grams, the incorporation time of slurry is 24 hours,
The step（4）Middle drying temperature is 70 DEG C, and sieving process selects the sieve of 100 mesh, the step（5）Middle dry-pressing pressure is 20
Megapascal, hydrostatic pressure are 250 megapascal, the step（6）Middle unsticking temperature is 600 DEG C, and the unsticking soaking time is 60 points
Clock, the sintering temperature are 1750 DEG C, and the sintered heat insulating time is 60 minutes.
The density for the normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die that the embodiment obtains is 1.85gcm-3,
Compression strength is 220MPa, coefficient of thermal expansion 6.5*10-6/K。
Specific embodiment two, the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, step
For：
（1）, pretreatment of raw material, it is spare after BN powders are handled 1.2 hours at 1250 DEG C of air atmosphere and temperature；
（2）, mixed powder prepare, by weight Al2O3：Y2O3=1 ratio has weighed Al2O3And Y2O35 grams of powder, and mix
Uniformly, AY powders are denoted as, as sintering aid；By step（1）95 grams of the BN powders prepared and AY powders, which are uniformly mixed, to be prepared
At mixed powder；
（3）, prepare slurry, using alcohol as solvent, PVB is binder, and consumption of binder is 2 grams, with mixed powder and binder
It is 45wt% to be made into solid content for solute（Weight percent）Slurry；Then with Al2O3Ball mixes slurry equal as mill ball
It is even；
（4）, powder prepare, by step（3）In prepared slurry BN composite granules are made through mist projection granulating, and control spraying and make
100 ± 10 microns of the average grain diameter of grain；
（5）, processing and forming, by step（4）In BN composite granules obtained through dry-pressing and isostatic pressing, form BN ceramics elements
Base；
（6）, unsticking sintering, by step（5）In BN biscuit of ceramics vacuum unsticking obtained, then in N2It is sintered, makes under gas atmosphere
It is standby to obtain BN ceramics；
（7）, finishing and polishing, by step（6）The BN ceramics of preparation are processed to obtain finishing workpiece by numerically-controlled machine tool,
And it is polished to get to normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die.
The step（1）The grain size of middle BN powders is 1~2 micron, the step（2）Middle Al2O3And Y2O3Powder is put down
Equal grain size≤1 micron, the step（3）In mill ball Al2O3Dosage be 200 grams, the incorporation time of slurry is 24 hours,
The step（4）The outlet temperature of middle mist projection granulating is 65 DEG C, the step（5）Middle dry-pressing pressure, 50 megapascal, hydrostatic pressure
For 250 megapascal, the step（6）Middle unsticking temperature, 600 DEG C, the unsticking soaking time is 60 minutes, and the sintering temperature is
1850 DEG C, the sintered heat insulating time is 60 minutes.
The density for the normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die that the embodiment obtains is 1.75gcm-3,
Compression strength is 195MPa, coefficient of thermal expansion 4.8*10-6/K。
Specific embodiment three, the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, step
For：
（1）, pretreatment of raw material, it is spare after BN powders are handled 1 hour at 1200 DEG C of air atmosphere and temperature；
（2）, mixed powder prepare, by weight Al2O3：Y2O3=1 ratio has weighed Al2O3And Y2O32 grams of powder, and mix
Uniformly, AY powders are denoted as, as sintering aid；By step（1）98 grams of the BN powders prepared and AY powders, which are uniformly mixed, to be prepared
At mixed powder；
（3）, prepare slurry, using alcohol as solvent, PVB is binder, and binder is molten with mixed powder and binder with 2 grams
It is 45wt% that matter, which is made into solid content,（Weight percent）Slurry；Then with Al2O3Slurry is uniformly mixed by ball as mill ball；
（4）, powder prepare, by step（3）In prepared slurry BN composite granules are made through mist projection granulating, and control spraying and make
100 ± 10 microns of the average grain diameter of grain；
（5）, processing and forming, by step（4）In BN composite granules obtained through dry-pressing and isostatic pressing, form BN ceramics elements
Base；
（6）, unsticking sintering, by step（5）In BN biscuit of ceramics vacuum unsticking obtained, then in N2It is sintered, makes under gas atmosphere
It is standby to obtain BN ceramics；
（7）, finishing and polishing, by step（6）The BN ceramics of preparation are processed to obtain finishing workpiece by numerically-controlled machine tool,
And it is polished to get to normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die.
The step（1）The grain size of middle BN powders is 1~2 micron, the step（2）Middle Al2O3And Y2O3Powder is put down
Equal grain size≤1 micron, the step（3）In mill ball Al2O3Dosage be 220 grams, the incorporation time of slurry is 24 hours,
The step（4）The outlet temperature of middle mist projection granulating is 70 DEG C, the step（5）Middle dry-pressing pressure, 50 megapascal, hydrostatic pressure
For 250 megapascal, the step（6）Middle unsticking temperature, 1100 DEG C, the unsticking soaking time is 120 minutes, the sintering temperature
It it is 1900 DEG C, the sintered heat insulating time is 90 minutes.
The density for the normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die that the embodiment obtains is 1.71gcm-3,
Compression strength is 180Mpa, coefficient of thermal expansion 4.2*10-6/K。
The present invention devises the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, this method sheet
The purpose of invention be to solve the problems, such as in the prior art using graphite manufacture bend glass hot bending die intolerant to oxidative attack and
One kind is provided to be commercialized powder BN powders as raw material, normal pressure-sintered legal system makes h-BN ceramics bend glass hot bending dies.BN makes pottery
Porcelain is high with thermal conductivity, coefficient of thermal expansion is low, with outside the not wellability of glass and easy processing characteristic, and high-temperature oxidation resistance compares stone
Ink material is well very much, just starts to aoxidize in air under 1200 DEG C or more hot conditions, is far below 800 DEG C of softening points of glass
Hot bending temperature.In addition, the manufacturing approach craft of the normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die is simple, at
This is relatively low, it can be achieved that industrialization large-scale production, is suitble to promote the use of.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (9)
1. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die, it is characterised in that its step is：
（1）, pretreatment of raw material, it is spare after BN powders are handled 0.5~2 hour at air atmosphere and temperature >=1200 DEG C；
（2）, mixed powder prepare, by weight Al2O3：Y2O3=0.75~1.8 ratio has weighed Al2O3And Y2O3Powder, and
It is uniformly mixed, AY powders is denoted as, as sintering aid；By step（1）The BN powders and AY powders prepared, which is uniformly mixed, to be prepared
At mixed powder, so that BN powder contents >=90wt% in mixed powder（Weight percent）；
（3）, prepare slurry, using water or alcohol as solvent, PVA or PVB are binder, binder content≤mixed powder
2wt%（Weight percent）, it is 40~60wt% to be made into solid content as solute using mixed powder and binder（Weight percent）'s
Slurry；Then with Al2O3Slurry is uniformly mixed by ball as mill ball；
（4）, powder prepare, by step（3）In prepared slurry drying, crushing, sieving, or through mist projection granulating BN to be made multiple
Powder is closed, and controls 100 ± 10 microns of the average grain diameter of mist projection granulating；
（5）, processing and forming, by step（4）In BN composite granules obtained through dry-pressing and/or isostatic pressing, form BN ceramics
Biscuit；
（6）, unsticking sintering, by step（5）In BN biscuit of ceramics vacuum unsticking or air atmosphere unsticking obtained, then in N2
It is sintered under gas atmosphere, BN ceramics is prepared；
（7）, finishing and polishing, by step（6）The BN ceramics of preparation are processed to obtain finishing workpiece by numerically-controlled machine tool,
And it is polished to get to normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die.
2. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（1）The grain size of middle BN powders is 1~2 micron.
3. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（2）Middle Al2O3And Y2O3Average grain diameter≤1 micron of powder.
4. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（3）In mill ball Al2O3Dosage be 1~5 times of mixed powder weight, the incorporation time of slurry
It is 24 hours.
5. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（4）Middle drying temperature is 60~80 DEG C, and sieving process selects the sieve of 100 mesh.
6. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（4）The outlet temperature of middle mist projection granulating is 60~80 DEG C.
7. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（5）Middle dry-pressing pressure is 20 ~ 100 megapascal, and hydrostatic pressure is 200 ~ 300 megapascal.
8. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the step（6）Middle unsticking temperature is 500-1200 DEG C, and the unsticking soaking time is 60-120 minutes.
9. the manufacturing method of normal pressure-sintered hexagonal boron nitride ceramics bend glass hot bending die according to claim 1,
It is characterized in that, the sintering temperature is 1700-1900 DEG C, and the sintered heat insulating time is 30-90 minutes.
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| CN111410539A (en) * | 2020-03-03 | 2020-07-14 | 哈尔滨工业大学 | Y-Al-Si-O multi-element glass phase reinforced hexagonal boron nitride-based multiphase ceramic and preparation method thereof |
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