CN106830902A - A kind of method that use phase transition under high pressure method prepares polycrystalline alpha-aluminium oxide - Google Patents

A kind of method that use phase transition under high pressure method prepares polycrystalline alpha-aluminium oxide Download PDF

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CN106830902A
CN106830902A CN201710128089.3A CN201710128089A CN106830902A CN 106830902 A CN106830902 A CN 106830902A CN 201710128089 A CN201710128089 A CN 201710128089A CN 106830902 A CN106830902 A CN 106830902A
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sintering
sample
high pressure
under high
phase transition
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王海阔
仝菲菲
刘俊龙
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Henan University of Technology
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Henan University of Technology
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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
    • C04B35/01—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
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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
    • C04B35/01—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
    • C04B35/111—Fine ceramics
    • C04B35/1115—Minute sintered entities, e.g. sintered abrasive grains or shaped particles such as platelets
    • 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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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract

The present invention relates to a kind of method that use phase transition under high pressure method prepares polycrystalline alpha-aluminium oxide, methods described is with γ Al2O3It is raw material, by carrying out purified treatment and pre-molding to raw material, after assembling sintering unit, at 300 1500 DEG C, is sintered under the conditions of 1 25 GPa superhigh-pressure high-temps, then subsequent sample is processed and performance detection is carried out.This method makes γ Al2O3It is directly translated into polycrystalline α Al2O3, can prepare that thing is mutually single, even structure, with superperformance, the purity such as hardness and consistency high polycrystalline α Al higher2O3Material.

Description

A kind of method that use phase transition under high pressure method prepares polycrystailine alpha alumina
Technical field
The present invention relates to using γ-Al2O3It is raw material, purified treatment is carried out by raw material, under the conditions of superhigh-pressure high-temp High-performance polycrystal Alpha-alumina is prepared by phase transition under high pressure method（That is α-Al2O3）Method.Belong to Inorganic Non-metallic Materials neck Domain.
Technical background
Aluminum oxide has many allomorphisms, and what is be currently known has kind more than 10, mainly there is 3 kinds of crystal formations, i.e. α-Al2O3、β- Al2O3、γ-Al2O3。γ-Al2O3With α-Al2O3It is that aluminum oxide is primarily present form.γ-Al2O3Belong to transitional form oxidation Aluminium, is powdery, microspheroidal or column white solid.Its crystal structure is different from commercial alumina.α-Al2O3It is a kind of important Inorganic Non-metallic Materials, is most stable of thing phase in all aluminum oxide.
Nanometer α-Al2O3Polycrystalline, with good mechanical property（High rigidity, high tenacity, high intensity）；Fracture strength be α- Al2O3The several times of monocrystalline.Due to α-Al2O3Crystal grain is easily grown up and loses its nanostructured at high temperature, and synthesis is this to be caused completely Close nano-multicrystal bulk material is challenging,
The preparation of nano-multicrystal ceramic material is more with nanometer powder as original material, and nanometer powder is present reunites, adsorbs, being difficult to point Scattered problem constrains the mechanical property of sintering gained polycrystalline material.How nanocrystal length in high-temperature sintering process is suppressed Greatly, it is kept nano-meter characteristic and sintered body high-compactness, be also that nano-multicrystal material prepares the technical barrier for facing.
The content of the invention
The purpose of the present invention is just being directed to the weak point in the presence of above-mentioned prior art and is providing one kind and use high pressure The method that phase transition method prepares polycrystailine alpha alumina.
The purpose of the present invention can be realized by following technique measures：
It is of the invention use the method that phase transition under high pressure method prepares polycrystailine alpha alumina with purity higher than 80%, crystallite dimension as 5nm- 500 μm of γ-Al2O3It is raw material, is prepared under high-temperature and high-pressure conditions, its processing step is as follows：
A, Feedstock treating detection：Purity is processed higher than the 80%, γ-Al that crystallite dimension is 5nm-500 μm with absolute ethyl alcohol2O3It is former Material, after pouring out waste liquid, is dried under the conditions of 120 DEG C；Afterwards plus deionized water carries out pre-molding, in vacuum after to be formed Molded samples are vacuum dried in drying oven；
B, assembling sintering unit：The raw material of pre-molding is wrapped up with Metal Inclusions, sample is prevented at high temperature under high pressure It is contaminated；The raw material of the pre-molding after parcel is put into treated metal cup again, being fitted into high-pressure synthesizer is carried out Assembling, the sintering unit that then will be assembled is put into standby in 120 DEG C of baking ovens of freeze-day with constant temperature；
C, HTHP sintering：HTHP sintering is carried out using press, sintering pressure is 1-25GPa, when pressure reaches setting After pressure, heat up heating, heat preservation sintering under conditions of being 300-1500 DEG C in sintering temperature；Soaking time is -50 minutes 10 seconds； After insulation terminates, stop heating, then slowly start step-down；
D, following process treatment：The sample in synthetic cavity is taken out, external metallization inclusion enclave is removed, to inner sample polishing, thrown Light obtains α-Al2O3Polycrystal, α-Al2O3The crystallite dimension of polycrystal is 5nm-500 μm；
E, properties of sample detection：Sample thing phase and sample crystallite dimension are detected by XRD and SEM.
Heretofore described γ-Al2O3The crystal formation of raw material uses XRD determining, and utilizes laser particle size detection assay crystal grain chi It is very little.
In the present invention material of Metal Inclusions described in step b be titanium, molybdenum or tantalum, carried out polishing before parcel and Polishing, then deoiled, ultrasonic wave cleaning, infrared drying.
Unit is sintered in the present invention described in step b with graphite-pipe as heater element, magnesia and pyrophyllite are pressure transmission Jie Matter.
Beneficial effects of the present invention are as follows：
Nano-multicrystal α-Al prepared by the present invention2O3Material, the raw material of use is the γ-Al of pure phase2O3In powder, and sample not Containing other impurity, with purity it is high, thing is mutually single the characteristics of.
Nano-multicrystal α-Al prepared by the present invention2O3Material, it is possible to use micron-scale γ-Al2O3It is raw material.Avoid With manocrystalline powders as original material, the reunion that exists, adsorb, be difficult to scattered problem.
Nano-multicrystal α-Al prepared by the present invention2O3Material, is prepared using superhigh-pressure high-temp phase transition method.Using super High pressure makes raw material be broken into uniform crystal grain, and ultra-high pressure condition can suppress the crystal grain that high temperature orders about and grow up problem.This method Successfully solve nanocrystal growing up in high-temperature sintering process.
Brief description of the drawings
Fig. 1 is sintering unit assembling schematic diagram.
Sequence number in figure：1 is plug, and 2 is dolomite sleeve pipe, and 3 is pyrophyllite in lumps, and 4 is graphite flake, and 5 is graphite-pipe, and 6 is sample Product, 7 is magnesia tube, and 8 is oxidation magnesium sheet, and 9 is titanium sheet.
Specific embodiment
The present invention is below with reference to embodiment（Accompanying drawing）It is further described：
Embodiment 1：
A, Feedstock treating detection：It is the γ-Al that 99%, crystallite dimension is 5 μm by purity2O3Raw material is processed with absolute ethyl alcohol, Go out waste liquid, the raw material after treatment is put into 120 DEG C of drying in baking oven；Raw material after drying adds deionized water as binding agent, precompressed Shaping；Molded samples are put into vacuum drying oven and are vacuum dried；Crystal formation by XRD, grain size analysis with laser grain size analyzer raw material is four Square γ-Al2O3。
B, assembling sintering unit：The raw material of pre-molding is wrapped up with Metal Inclusions, prevents sample high in high temperature Pressure is contaminated；The raw material of the pre-molding after parcel is put into treated metal cup again, is fitted into high-pressure synthesizer Assembled, the sintering unit that then will be assembled is put into standby in 120 DEG C of baking ovens of freeze-day with constant temperature；Described sintering unit with Graphite-pipe is heater element, and magnesia and pyrophyllite are transmission medium.As shown in figure 1, being burnt according to the installation diagram assembling of sintering unit Statement of account unit.
C, HTHP sintering：HTHP sintering is carried out using press, sintering pressure is 3GPa, and pressure reaches setting pressure After power, heat temperature raising, under conditions of being 1300 DEG C in sintering temperature, soaking time is 5 minutes；After insulation terminates, stop adding Heat, then slowly starts step-down.
D, following process treatment：The sample in synthetic cavity is taken out, external metallization inclusion enclave is removed, inner sample is beaten Mill, polishing obtain α-Al2O3Polycrystal, α-Al2O3The crystallite dimension of polycrystal is 5nm-500 μm.
E, properties of sample detection：Sample thing phase and sample crystallite dimension are detected by XRD and SEM.
Show that sample has high rigidity and high tenacity by hardness and toughness test.By XRD diffraction pattern analysis, sample Comprise only α-Al2O3Single-phase, and crystalline phase stabilization, the average crystal grain size of SEM detection samples is nano particle, and sample is microcosmic Structure is than more uniform.High quality alpha-the Al prepared using this technique2O3Material thing is mutually single, even structure, with hardness high and Consistency, heat endurance high.
Embodiment 2
A, Feedstock treating detection：It is the γ-Al that 99.5%, crystallite dimension is 20 μm by purity2O3Raw material is used at absolute ethyl alcohol Reason, pours out waste liquid, and the raw material after treatment is put into 120 DEG C of drying in baking oven；Raw material after drying adds deionized water as bonding Agent, pre-molding；Molded samples are put into vacuum drying oven and are vacuum dried；By XRD, the crystalline substance of grain size analysis with laser grain size analyzer raw material Type is square γ-Al2O3。
The step of the present embodiment, b was same as Example 1, was not repeated.
C, HTHP sintering：HTHP sintering is carried out using press, sintering pressure is 5GPa, and pressure reaches setting pressure After power, heat temperature raising, under conditions of being 1500 DEG C in sintering temperature, soaking time is 50 minutes；After insulation terminates, stop adding Heat, then slowly starts step-down.
The step of the present embodiment, d, e were same as Example 1, were not repeated.

Claims (4)

1. a kind of method that use phase transition under high pressure method prepares polycrystailine alpha alumina, it is characterised in that:Methods described processing step is such as Under：
A, Feedstock treating detection：Purity is processed higher than the 80%, γ-Al that crystallite dimension is 5nm-500 μm with absolute ethyl alcohol2O3It is former Material, after pouring out waste liquid, is dried under the conditions of 120 DEG C；Afterwards plus deionized water carries out pre-molding, in vacuum after to be formed Molded samples are vacuum dried in drying oven；
B, assembling sintering unit：The raw material of pre-molding is wrapped up with Metal Inclusions, sample is prevented at high temperature under high pressure It is contaminated；The raw material of pre-molding after parcel is put into treated metal cup again, being fitted into high-pressure synthesizer carries out group Dress, the sintering unit that then will be assembled is put into standby in 120 DEG C of baking ovens of freeze-day with constant temperature；
C, HTHP sintering：HTHP sintering is carried out using press, sintering pressure is 1-25GPa, when pressure reaches setting After pressure, heat up heating, heat preservation sintering under conditions of being 300-1500 DEG C in sintering temperature；Soaking time is -50 minutes 10 seconds； After insulation terminates, stop heating, then slowly start step-down；
D, following process treatment：The sample in synthetic cavity is taken out, external metallization inclusion enclave is removed, to inner sample polishing, thrown Light obtains α-Al2O3Polycrystal, α-Al2O3The crystallite dimension of polycrystal is 5nm-500 μm；
E, properties of sample detection：Sample thing phase and sample crystallite dimension are detected by XRD and SEM.
2. the method that use phase transition under high pressure method according to claim 1 prepares polycrystailine alpha alumina, it is characterised in that:It is described γ-Al2O3The crystal formation of raw material uses XRD determining, and utilizes laser particle size detection assay crystallite dimension.
3. the method that use phase transition under high pressure method according to claim 1 prepares polycrystailine alpha alumina, it is characterised in that:Step The material of Metal Inclusions described in b is titanium, molybdenum or tantalum, carries out needing grinding and buffing to process before parcel, is then gone Oil, ultrasonic wave cleaning, infrared drying.
4. the method that use phase transition under high pressure method according to claim 1 prepares polycrystailine alpha alumina, it is characterised in that:Step Unit is sintered described in b with graphite-pipe as heater element, magnesia and pyrophyllite are transmission medium.
CN201710128089.3A 2017-03-06 2017-03-06 A kind of method that use phase transition under high pressure method prepares polycrystalline alpha-aluminium oxide Pending CN106830902A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111592360A (en) * 2020-06-09 2020-08-28 欧阳晓平 Polycrystal B4C-diamond double-layer composite material and preparation method thereof
CN111606711A (en) * 2020-06-09 2020-09-01 欧阳晓平 Polycrystal B4C-SiC double-layer composite material and preparation method thereof
CN113754431A (en) * 2021-09-09 2021-12-07 浙江大学 Method for preparing nano polycrystalline composite phase zirconia by ultrahigh pressure/high temperature phase change method

Citations (3)

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Publication number Priority date Publication date Assignee Title
KR20050068439A (en) * 2003-12-30 2005-07-05 한국기계연구원 Method for manufacturing alumium based alloyed powder having superior compactability
CN101704680A (en) * 2009-11-18 2010-05-12 中国地质大学（北京） Submicron alumina ceramic material and preparation method thereof
CN106007687A (en) * 2016-05-11 2016-10-12 河南工业大学 Method for preparing nano-polycrystalline coesite through high-pressure phase transition method

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CN101704680A (en) * 2009-11-18 2010-05-12 中国地质大学（北京） Submicron alumina ceramic material and preparation method thereof
CN106007687A (en) * 2016-05-11 2016-10-12 河南工业大学 Method for preparing nano-polycrystalline coesite through high-pressure phase transition method

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111592360A (en) * 2020-06-09 2020-08-28 欧阳晓平 Polycrystal B4C-diamond double-layer composite material and preparation method thereof
CN111606711A (en) * 2020-06-09 2020-09-01 欧阳晓平 Polycrystal B4C-SiC double-layer composite material and preparation method thereof
CN113754431A (en) * 2021-09-09 2021-12-07 浙江大学 Method for preparing nano polycrystalline composite phase zirconia by ultrahigh pressure/high temperature phase change method

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