CN107032765A - A kind of method of quick high-temp solid-phase sintering aluminium oxide ceramics - Google Patents

A kind of method of quick high-temp solid-phase sintering aluminium oxide ceramics Download PDF

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CN107032765A
CN107032765A CN201710244327.7A CN201710244327A CN107032765A CN 107032765 A CN107032765 A CN 107032765A CN 201710244327 A CN201710244327 A CN 201710244327A CN 107032765 A CN107032765 A CN 107032765A
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aluminium oxide
oxide ceramics
sintering
temp solid
quick high
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CN107032765B (en
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张金咏
汪信志
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/95—Products characterised by their size, e.g. microceramics

Abstract

The invention belongs to ceramic sintering technology field, and in particular to a kind of method of quick high-temp solid-phase sintering aluminium oxide ceramics.Methods described includes：The base substrate of disc-shaped is made after alumina powder is dried；It is rapidly heated under the conditions of without pressure with 500 DEG C/s~600 DEG C/s heating rate to the sintering temperature of setting, the sintering temperature is higher than 200 DEG C~300 DEG C of nominal sintering temperatures but less than the melting temperature of aluminium oxide ceramics, after of short duration insulation, natural cooling obtains the aluminium oxide ceramics of high densification.Quick high-temp solid-phase sintering obtains aluminium oxide ceramics under the conditions of the inventive method realizes no pressure, quick high-temp solid-phase sintering aluminium oxide ceramics technology of the present invention is fast with heating rate compared with conventional sintering means, and sintering temperature is high, sintering time is short, advantage with short production cycle.

Description

A kind of method of quick high-temp solid-phase sintering aluminium oxide ceramics
Technical field
The invention belongs to ceramic sintering technology field, and in particular to a kind of side of quick high-temp solid-phase sintering aluminium oxide ceramics Method.
Background technology
Aluminium oxide ceramics is one of ceramic material that most widely used, purposes is most wide, yield is maximum in oxide ceramics, is had High mechanical strength, resistivity height, good electrical insulation capability, hardness and fusing point are high, corrosion resistance is good, chemical stability is good, Yi Ji There is the superior functions such as good optical and ionic conductivity under certain condition, in machinery, electron and electrician, chemical industry, medical science, build Build and other field has broad application prospects.
Alumina sintering is a very long process, when the sintering temperature height required for traditional non-pressure sintering technology and insulation Between it is long, therefore the problem of existence time and serious energy resource consumption.For such case, numerous researchers proposes a plan to improve Sintering process.First, mix sintering aid.Sintering aid can be with alumina material formation liquid phase, promotion in sintering process Grain is reset and mass transport process, mechanism of mass transfer is changed into liquid phase diffusion by solid-state diffusion.But sintering aid burns to aluminium oxide ceramics Stomata discharge during knot is impacted, such as：Add TiO2Easily alumina article is set to form transgranular hole, so as to influence base substrate Consistency.Second, occur in that some new sintering methods for not needing sintering aid.As discharge plasma sintering (SPS, Spark Plasma Sintering) and flash burning (FS, Flash Sintering).These new sintering methods are extra electric fields Directly by mould or sintering powder, powder is heated using Joule heat, this mode of heating is more efficient.Traditional sintering side Method, such as pressureless sintering and hot pressed sintering, its heating rate are 10~50 DEG C/min, and these new sintering methods are relative to tradition Faster, heating rate reaches more than hundreds of centigrade per minutes to sintering method heating rate, can realize the fast densified of material Change.But, because these new sintering processings depend on electric conductivity, additional auxiliary electric field, impressed pressure and the mould of powder Tool etc., this also limits widely using for these novel sintered methods.Accordingly, it is capable to no without the no any additional auxiliary of pressure Under the conditions of field action, realize that quick densifying is gradually paid close attention to by scholar.Brook et al. proposes a kind of without pressure Fast Sintering Technology (fast firing), sample heating rate under the conditions of without pressure reaches hundreds of centigrade per minutes, it was confirmed that be rapidly heated Promote densification process.But it is this without pressure Fast Sintering technology prepare the densification that sample does not realize material finally, Because there are many sealed porositys in product, it is necessary to which more times could be eliminated.
The content of the invention
The present invention is in view of the shortcomings of the prior art, it is therefore intended that provide a kind of quick high-temp solid-phase sintering aluminium oxide ceramics Method.
For achieving the above object, the technical solution adopted by the present invention is：
A kind of method of quick high-temp solid-phase sintering aluminium oxide ceramics, comprises the following steps：
(1) certain amount of alumina powder is weighed, is dried, crude green body shaping is carried out after the completion of drying, the base substrate of disc-shaped is made；
(2) base substrate of the disc-shaped of step (1) forming is placed in a kind of device for quickly elevating temperature；
(3) it is rapidly heated with certain heating rate to the sintering temperature of setting, after of short duration insulation, natural cooling is obtained High fine and close aluminium oxide ceramics.
In such scheme, the heating rate is 500 DEG C/s~600 DEG C/s.
In such scheme, the sintering temperature is higher than 200~300 DEG C of nominal sintering temperatures but less than aluminium oxide ceramics Melting temperature, specially 1650 DEG C~1850 DEG C.
In such scheme, the time being rapidly heated is 3s~4s.
In such scheme, 1~2min of time of the of short duration insulation.
In such scheme, step (1) described drying is：24h is dried in vacuo under the conditions of being placed in 60 DEG C.
In such scheme, step (1) described crude green body is shaped to：Alumina powder is pressed into circle under 200MPa pressure Flake shaped base substrate, the consistency of the base substrate is 60%.
In such scheme, step (2) described device for quickly elevating temperature is no pressure heat riser.
Beneficial effects of the present invention：(1) quick high-temp solid-phase sintering obtains oxygen under the conditions of the inventive method realizes no pressure Change aluminium ceramics, quick high-temp solid-phase sintering aluminium oxide ceramics technology of the present invention is compared with conventional sintering means, with heating Speed is fast, and sintering temperature is high, short, the with short production cycle advantage of sintering time；(2) it is raw materials used to be in the method for the invention It is pure or for business level powder, for purity and particle diameter no requirement (NR), therefore production cost can be reduced；(3) this method technique Simply, with short production cycle, preparation gained aluminium oxide ceramics consistency is higher, meets the requirement of industrial application, is conducive to a large amount of lifes Produce aluminium oxide ceramics.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention Content is not limited solely to the following examples.
Embodiment 1
A kind of supper-fast preparation method without the standby aluminium oxide ceramics of compacting, it comprises the following steps：
(1) powder handling：By the alumina powder powder stock used in experiment, it is put into drying box and dries 24h.
(2) aluminum oxide crude green body is prepared：Dried alumina powder 1.5g in (1) is weighed, diameter is pressed into tablet press machine For 1.5cm disc-shaped crude green body, pressure is 8MPa, dwell time 2min；The disc-shaped crude green body suppressed is positioned over cold etc. quiet In press, isostatic cool pressing processing, dwell time 5min, with higher initial are carried out to sample under 200MPa pressure Consistency (first base compactness 60% or so), in favor of the sintering of follow-up product.
(3) sinter：By the aluminum oxide handled well in (2), just base is put into the TiB in device for quickly elevating temperature2Sinter heating tank It is interior, start to warm up, heating rate is set to 1693 DEG C in 500~600 DEG C/more than s, sintering temperature the present embodiment, is reached in 3s To sintering temperature, 1min then is incubated in this temperature spot, subsequent natural cooling obtains the aluminium oxide ceramics of high densification, through measurement Relative density reaches 99.4%.
Wherein, the measuring method of above-mentioned relative density is as follows：Open pore and the inside of connection are generally there are in ceramic sample Hole of holding one's breath, the apparent density of measurement sample used, the apparent density=sample mass/(actual volume of sample+open pore volume + pore volume of holding one's breath), nearly all stomata in sample can be all included.Calculating relative density using apparent density can count Calculate accurate consistency.Apparent density and relative density calculate formula：
ρ=ρWaterW1/(W3-W2)
ρRelatively=ρ/ρVery
Wherein, ρ-apparent density；ρWaterThe density of-water, W1The aerial quality of-sample；W2- sample is immersed in water In quality；W3The aerial quality of sample after-immersion；ρVeryThe real density of-aluminium oxide ceramics
Embodiment 2
A kind of supper-fast preparation method without the standby aluminium oxide ceramics of compacting, it comprises the following steps：
(1) powder handling：By the alumina powder powder stock used in experiment, it is put into drying box and dries 24h.
(2) aluminum oxide crude green body is prepared：Dried alumina powder 1.5g, is pressed into a diameter of with tablet press machine in weighing 1) 1.5cm disc-shaped crude green body, pressure is 8MPa, dwell time 2min；The disc-shaped crude green body suppressed is positioned over isostatic cool pressing In machine, isostatic cool pressing processing, dwell time 5min, with higher initial cause are carried out to sample under 200MPa pressure Density, in favor of the sintering of follow-up product.
(3) sinter：The aluminum oxide crude green body handled well in (2) is wrapped with graphite paper, the stone in device for quickly elevating temperature is put into In black mould, start to warm up, heating rate is set to 1798 DEG C in 500~600 DEG C/more than s, sintering temperature the present embodiment, 3 Sintering temperature is reached in~4s, 1min is incubated in this temperature spot, subsequent natural cooling obtains the aluminium oxide ceramics of high densification, warp Measurement relative density reaches 99.6%.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and the not limitation to embodiment.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 change or Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change or change therefore amplified Move within still in the protection domain of the invention.

Claims (9)

1. a kind of method of quick high-temp solid-phase sintering aluminium oxide ceramics, it is characterised in that comprise the following steps：
（1）Certain amount of alumina powder is weighed, is dried, crude green body shaping is carried out after the completion of drying, the base substrate of disc-shaped is made；
（2）By step（1）The base substrate of the disc-shaped of forming is placed in a kind of device for quickly elevating temperature；
（3）It is rapidly heated with certain heating rate to the sintering temperature of setting, after of short duration insulation, natural cooling obtains high cause Close aluminium oxide ceramics.
2. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that the heating Speed is 500 DEG C/s ~ 600 DEG C/s.
3. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that the sintering Temperature is 1650 DEG C ~ 1850 DEG C.
4. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that described quick The time of heating is 3 ~ 4s.
5. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that described of short duration 1 ~ 2min of time of insulation.
6. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that step（1） The drying is：24h is dried in vacuo under the conditions of being placed in 60 DEG C.
7. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that step（1） The crude green body is shaped to：Alumina powder is pressed into disc-shaped base substrate under 200MPa pressure.
8. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that step（1） The consistency of the base substrate is 60%.
9. the method for quick high-temp solid-phase sintering aluminium oxide ceramics according to claim 1, it is characterised in that step（2） The device for quickly elevating temperature is no pressure heat riser.
CN201710244327.7A 2017-04-14 2017-04-14 Method for rapidly sintering alumina ceramic in solid phase at high temperature Expired - Fee Related CN107032765B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174644A (en) * 2020-09-07 2021-01-05 中国科学院上海光学精密机械研究所 Method for pressureless rapid sintering of compact nanocrystalline ceramic

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
FANCHENG MENG等: "Rapid Densification of Nano-Grained Alumina by High Temperature and Pressure with a Very High Heating Rate", 《J. AM. CERAM. SOC.》 *
W. JI等: ""Ultra-fast firing: Effect of heating rate on sintering of 3YSZ, with and without an electric field"", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174644A (en) * 2020-09-07 2021-01-05 中国科学院上海光学精密机械研究所 Method for pressureless rapid sintering of compact nanocrystalline ceramic
CN112174644B (en) * 2020-09-07 2022-05-31 中国科学院上海光学精密机械研究所 Method for rapidly sintering compact nanocrystalline ceramic under no pressure

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