CN107326432A - A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics - Google Patents

A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics Download PDF

Info

Publication number
CN107326432A
CN107326432A CN201710523918.8A CN201710523918A CN107326432A CN 107326432 A CN107326432 A CN 107326432A CN 201710523918 A CN201710523918 A CN 201710523918A CN 107326432 A CN107326432 A CN 107326432A
Authority
CN
China
Prior art keywords
aluminium oxide
oxide ceramics
seed crystal
texture
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201710523918.8A
Other languages
Chinese (zh)
Other versions
CN107326432B (en
Inventor
常云飞
张敏敏
吴杰
孙媛
刘迎春
杨彬
曹文武
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harbin Institute of Technology
Original Assignee
Harbin Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Harbin Institute of Technology filed Critical Harbin Institute of Technology
Priority to CN201710523918.8A priority Critical patent/CN107326432B/en
Publication of CN107326432A publication Critical patent/CN107326432A/en
Application granted granted Critical
Publication of CN107326432B publication Critical patent/CN107326432B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B9/00—Single-crystal growth from melt solutions using molten solvents
    • C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
    • C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
    • C30B9/12—Salt solvents, e.g. flux growth
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • 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
    • C04B35/111—Fine ceramics
    • C04B35/1115—Minute sintered entities, e.g. sintered abrasive grains or shaped particles such as platelets
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/20—Aluminium oxides

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics, the present invention relates to the preparation method and application of template seed crystal.The invention solves the problems that there is the problem of production equipment requires poor height, production cycle length, complex process, microcrystalline dispersion, grain size distribution width, small radius-thickness ratio, difficult Morphological control and high production cost in existing tabular alumina crystallite preparation technology.Method：Aluminum-containing raw material is mixed with fused salt, growth auxiliary agent is then added, ball milling obtains mixed material；Mixed material is placed in the alumina crucible of lid, calcines, obtains reaction product；Reaction product is cleaned with hot water stirs and uses ultrasonic wave to be disperseed, is dried.Applied to preparing texture aluminium oxide ceramics, metal/ceramic/high polymer composite material toughener, heat-conduction-type polymer filler, grinding and polishing powder and the pigment base material field that crystal grain is small and the degree of orientation is high.

Description

A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics
Technical field
The present invention relates to the preparation method and application of template seed crystal.
Background technology
Advanced structural ceramic has an excellent performance because of it, for example high temperature resistant, corrosion-resistant, anti-oxidant, wear-resistant, high-strength Degree, high rigidity, the good, insulation of heat conduction etc., progressively turn into Aero-Space, new energy, electronic information, metallurgy, petrochemical industry, vapour The indispensable critical material of the industrial technical fields such as car, bio-mechanical.It is used as one of 21 century sciemtifec and technical sphere basic material Aluminum oxide (Al2O3) be typical material in advanced structural ceramic, be also in modern society most widely used ceramic material it One.Al2O3Though it is many more than having the advantages that, it is big with fatal weakness, i.e. fragility itself as well as other ceramics, it is right Defect is very sensitive, and toughness is low.Which dictates that it is poor using reliability and survivability, constrain its further development with Large-scale engineer applied.
Make each crystal grain edge [0001] in ceramics by template seed crystal oriented growth technology (TGG)cHeight preferred orientation is simultaneously Oriented growth into pattern be piece (plate) shape Al2O3Textured ceramic, can make its intensity and fracture toughness etc. produce anisotropy, at it The mechanical property significantly improved than conventional ceramic is obtained on predominant direction.Its corresponding toughening mechanism mainly by crackle bridging with splitting The deflecting mechanism (along texture plane) of line is to the outstanding contributions produced by the raising of toughness.Wherein, the texture quality of textured ceramic I.e. the crystallite dimension of the degree of orientation and different growth is to Al2O3The Effect on Mechanical Properties of textured ceramic is maximum, improves the degree of orientation and drops Low crystallite dimension is expected to that its performance is significantly increased.
The general thought of template seed crystal oriented growth technology (TGG) be by anisotropic template seed crystal shearing field work With lower uniform and directionally in embedment matrix fine powder, in subsequent heat treatment process, in matrix freedom different with template surface Under the driving of energy, template-directed matrix oriented growth, so as to be formed with anisotropic textured ceramic.Aluminum oxide texture is made pottery For porcelain, the topographical property (particle size, radius-thickness ratio, particle size distribution range, dispersiveness etc.) of its sheet template seed crystal is to determine The key factor of its texture quality and ceramic crystalline grain size.Successfully to prepare that crystal grain is small and texture quality high using TGG methods Aluminium oxide ceramics, its tabular alumina crystallite template needs to meet following condition：(1) template microcrystalline dispersion will get well, and footpath is thick Than it is high (>10), thus ensure its in matrix fine powder can uniformly and high orientation arrange；(2) template crystallite particle diameter is small In 15 microns, and particle size distribution range is narrow, so as to ensure that textured ceramic has the characteristics of crystallite dimension is small.
At present, preparing the technique of tabular alumina crystallite has hydro-thermal method, Mechanical Method, pyrolysismethod, agglutinating nature yeast and fused salt Method etc..Wherein, hydro-thermal method preparation process needs to react in the environment of HTHP, requires high to production equipment, and produce Cycle is long.Although Mechanical Method can carry out the production of mass, the physicochemical properties for being easily caused alumina particle occur Change, it is difficult to control the pattern and size of crystallite；Pyrolysismethod and agglutinating nature yeast are needed using expensive metal in process of production Organic salt etc. is used as the raw material reacted so that production cost is significantly raised.Have that equipment requirement is low, the reaction time with molten-salt growth method The advantages of short, reaction temperature is relatively low, crystal morphology is easily controlled, its technique is simple, it is easy to industrialized production, is to prepare aluminum oxide The comparatively ideal method of sheet-like crystallite.
However, being difficult to meet textured ceramic to propose template seed crystal at present using the tabular alumina prepared by molten-salt growth method Whole requirements, it need further improvement in its pattern control aspect.For example, part microcrystalline dispersion prepared by molten-salt growth method Property is poor, there is serious reunion or crossover phenomenon, causes it can not be uniformly distributed in matrix fine powder；Part crystallite radius-thickness ratio is small (<10), cause its directionality in matrix fine powder poor；Part crystallite particle diameter is too big (>=20 microns), causes it in slurry template Easily snapped off in mixed process；Also some crystallite particle diameter distributions are too wide, can cause textured ceramic grain size heterogeneity.These The presence of problem limits application of these sheet-like crystallites in little crystal grain, high-quality textured ceramic is prepared, and hinders texture pottery The further raising of porcelain mechanical property.
The content of the invention
The invention solves the problems that there is production equipment in existing tabular alumina crystallite preparation technology requires the high, production cycle Length, complex process, microcrystalline dispersion are poor, grain size distribution is wide, radius-thickness ratio is small, Morphological control is difficult and production cost is high asks Topic, and a kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics are provided.
A kind of preparation method of the template seed crystal of texture aluminium oxide ceramics of the present invention is completed according to the following steps：
First, aluminum-containing raw material is mixed with fused salt, then adds growth auxiliary agent, mixture is obtained, using absolute ethyl alcohol as ball milling Medium, using alumina balls as abrading-ball, by mixture ball milling 12h~48h, dries slurry after ball milling, obtains mixed material；
Described aluminum-containing raw material is γ-Al2O3、γ-AlO(OH)、Al2(SO4)3With α-Al (OH)3In one kind or wherein Several mixtures；
Described fused salt is Na2SO4、K2SO4, NaCl and one kind or wherein several mixtures in KCl；
Described growth auxiliary agent is SiO2、SiO2- CaO mixed aids or SiO2-CaO-TiO2Mixed aid；Described SiO2SiO in-CaO mixed aids2Mol ratio with CaO is 1:(0.2~2)；Described SiO2-CaO-TiO2In mixed aid SiO2Mol ratio with CaO is 1:(0.2~1)；Described SiO2-CaO-TiO2SiO in mixed aid2With TiO2Mol ratio be 1:(0.2~1)；
Described aluminum-containing raw material and the mol ratio of fused salt are 1:(2~10)；
2nd, mixed material is placed in the alumina crucible of lid, under conditions of temperature is 900 DEG C~1200 DEG C, forged 1h~8h is burnt, reaction product is obtained；
3rd, reaction product is cleaned with temperature for 60 DEG C~95 DEG C of hot water stirs and uses ultrasonic wave to be disperseed, dried It is dry, obtain the template seed crystal of texture aluminium oxide ceramics；The template seed crystal grain size of described texture aluminium oxide ceramics is 0.5 μm~15 μm, radius-thickness ratio is 12~25；
The matter of the template seed crystal of the texture aluminium oxide ceramics prepared in growth auxiliary agent and step 3 described in step one Amount is than being (0.1~3):100.
The template seed crystal of texture aluminium oxide ceramics prepared by preparation method of the present invention is applied to prepare that crystal grain is small and orientation The high texture aluminium oxide ceramics of degree, the texture aluminium oxide ceramics crystallite dimension of preparation is 5 μm~20 μm, along [0001] orientation texture Quality is more than 93%, and fracture toughness is more than 2 times of conventional ceramic, can also be applied to metal/ceramic/high polymer composite material Toughener, heat-conduction-type polymer filler, grinding and polishing powder and pigment base material field.
The template seed crystal of texture aluminium oxide ceramics prepared by the present invention is aluminum oxide sheet-like crystallite.
The beneficial effects of the invention are as follows：The present invention is by adding SiO2、SiO2- CaO or SiO2-CaO-TiO2In one kind Auxiliary agent is grown, good dispersion, narrow size distribution, regular shape, table are successfully prepared for using the molten-salt growth method of growth auxiliary agent auxiliary Face flat smooth, radius-thickness ratio can adjust between 12~25, grain size adjustable tabular alumina between 0.5~15 μm Crystallite, the crystallite disclosure satisfy that whole requirements that preparation little crystal grain, high-quality textured ceramic are proposed to template seed crystal.With There is technology to compare, the cost of material that preparation method of the invention is used is cheap, without addition crystal seed, without using phosphoric acid or hydrogen The acid such as fluoric acid, without using alkali such as sodium hydroxides, without using phosphate or fluoride salt, without using special calcination atmosphere, Technological process is simple and safe, low for equipment requirements, with short production cycle, can be applied to the production of scale.Using the present invention's Sheet-like crystallite good dispersion prepared by the molten-salt growth method of auxiliary agent auxiliary, soilless sticking and crossover phenomenon are grown, narrow size distribution, surface is put down Whole smooth, radius-thickness ratio is adjustable between 12~25, and crystallite dimension can be adjusted between 0.5~15 μm.Use the inventive method institute Whole requirements that the aluminum oxide sheet-like crystallite of preparation meets little crystal grain, the textured ceramic of high-orientation is proposed to crystallite template, The texture aluminium oxide ceramics crystallite dimension of preparation is 5~20 μm, is more than 93% along [0001] orientation texture quality, so that significantly Degree improves the ceramic mechanical property, and fracture toughness is significantly increased, and is 2 times of conventional ceramic, in addition, can also answer For metal/ceramic/high polymer composite material toughener, heat-conduction-type polymer filler, grinding and polishing powder and pigment base material etc. Field, so as to increase substantially mechanics/physics/functional performance of its practical application.
Brief description of the drawings
Fig. 1 is a kind of preparation method process chart of the template seed crystal of texture aluminium oxide ceramics of the present invention；
Fig. 2 is the XRD spectrum of aluminum oxide sheet-like crystallite prepared by embodiment one；
Fig. 3 is the microscopic appearance figure of aluminum oxide sheet-like crystallite prepared by embodiment two；
Fig. 4 is the microscopic appearance figure of aluminum oxide sheet-like crystallite prepared by embodiment three；
Fig. 5 is the texture aluminium oxide ceramics XRD spectrum prepared by template of aluminum oxide sheet-like crystallite prepared by example IV；
Fig. 6 schemes for Fracture Toughness comparison, and a is conventional ceramic, and b is example IV preparation using aluminum oxide sheet-like crystallite as mould Texture aluminium oxide ceramics prepared by plate.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it Between any combination.
Embodiment one：Present embodiment is illustrated according to Fig. 1, a kind of texture oxidation described in present embodiment The preparation method of the template seed crystal of aluminium ceramics is completed according to the following steps：
First, aluminum-containing raw material is mixed with fused salt, then adds growth auxiliary agent, mixture is obtained, using absolute ethyl alcohol as ball milling Medium, using alumina balls as abrading-ball, by mixture ball milling 12h~48h, dries slurry after ball milling, obtains mixed material；
Described aluminum-containing raw material is γ-Al2O3、γ-AlO(OH)、Al2(SO4)3With α-Al (OH)3In one kind or wherein Several mixtures；
Described fused salt is Na2SO4、K2SO4, NaCl and one kind or wherein several mixtures in KCl；
Described growth auxiliary agent is SiO2、SiO2- CaO mixed aids or SiO2-CaO-TiO2Mixed aid；Described SiO2SiO in-CaO mixed aids2Mol ratio with CaO is 1:(0.2~2)；Described SiO2-CaO-TiO2In mixed aid SiO2Mol ratio with CaO is 1:(0.2~1)；Described SiO2-CaO-TiO2SiO in mixed aid2With TiO2Mol ratio be 1:(0.2~1)；
Described aluminum-containing raw material and the mol ratio of fused salt are 1:(2~10)；
2nd, mixed material is placed in the alumina crucible of lid, under conditions of temperature is 900 DEG C~1200 DEG C, forged 1h~8h is burnt, reaction product is obtained；
3rd, reaction product is cleaned with temperature for 60 DEG C~95 DEG C of hot water stirs and uses ultrasonic wave to be disperseed, dried It is dry, obtain the template seed crystal of texture aluminium oxide ceramics；The template seed crystal grain size of described texture aluminium oxide ceramics is 0.5 μm~15 μm, radius-thickness ratio is 12~25；
The matter of the template seed crystal of the texture aluminium oxide ceramics prepared in growth auxiliary agent and step 3 described in step one Amount is than being (0.1~3):100.
The template seed crystal of texture aluminium oxide ceramics prepared by present embodiment is aluminum oxide sheet-like crystallite.
The beneficial effect of present embodiment is：Present embodiment is by adding SiO2、SiO2- CaO or SiO2- CaO-TiO2In a kind of growth auxiliary agent, good dispersion, size point are successfully prepared for using the molten-salt growth method of growth auxiliary agent auxiliary Cloth is narrow, regular shape, surfacing are smooth, radius-thickness ratio can adjust between 12~25, grain size can between 0.5~15 μm The tabular alumina crystallite of regulation, the crystallite disclosure satisfy that preparation little crystal grain, high-quality textured ceramic are carried to template seed crystal The whole requirements gone out.Compared with the prior art, the cost of material that the preparation method of present embodiment is used is cheap, Wu Xutian Plus crystal seed, without using acid such as phosphoric acid or hydrofluoric acid, without using alkali such as sodium hydroxides, without using phosphate or fluorination Salt, without using special calcination atmosphere, technological process is simple and safe, low for equipment requirements, with short production cycle, can be applied to rule The production of modelling.The sheet-like crystallite good dispersion prepared using the molten-salt growth method of the growth auxiliary agent auxiliary of the present invention, soilless sticking and friendship Phenomenon is pitched, narrow size distribution, surfacing is smooth, and radius-thickness ratio is adjustable between 12~25, and crystallite dimension can be at 0.5~15 μm Between adjust.Little crystal grain, high-orientation is met with the aluminum oxide sheet-like crystallite prepared by present embodiment method to knit Whole requirements that structure ceramic is proposed to crystallite template, the texture aluminium oxide ceramics crystallite dimension of preparation is 5~20 μm, along [0001] Orientation texture quality is more than 93%, so as to increase substantially the ceramic mechanical property, fracture toughness has been obtained significantly Improve, be 2 times of conventional ceramic, gather in addition, applying also for metal/ceramic/high polymer composite material toughener, heat-conduction-type The fields such as compound filler, grinding and polishing powder and pigment base material, so as to increase substantially mechanics/physics/function of its practical application Performance.
Embodiment two：Present embodiment from unlike embodiment one：Contain aluminium described in step one The mol ratio of raw material and fused salt is 1:(2~6).It is other identical with embodiment two.
Embodiment three：Unlike one of present embodiment and embodiment one or two：Institute in step one The mass ratio of the growth auxiliary agent stated and the template seed crystal of the texture aluminium oxide ceramics prepared in step 3 is (0.1~2.5): 100.It is other identical with embodiment one or two.
Embodiment four：Unlike one of present embodiment and embodiment one to three：Institute in step one The mass ratio of the growth auxiliary agent stated and the template seed crystal of the texture aluminium oxide ceramics prepared in step 3 is (0.1~2.25): 100.It is other identical with embodiment two to four.
Embodiment five：Unlike one of present embodiment and embodiment one to four：Institute in step one The mass ratio of the growth auxiliary agent stated and the template seed crystal of the texture aluminium oxide ceramics prepared in step 3 is (0.15~2.25): 100.It is other identical with embodiment one to four.
Embodiment six：Unlike one of present embodiment and embodiment one to five：In step one when Described fused salt is Na2SO4And K2SO4Mixture when, Na2SO4With K2SO4Mol ratio be 1:(0.5~5).It is other with it is specific Embodiment one to five is identical.
Embodiment seven：Unlike one of present embodiment and embodiment one to six：In step one when Described fused salt is Na2SO4And K2SO4Mixture when, Na2SO4With K2SO4Mol ratio be 1:(1~5).Other and specific reality Apply mode one to six identical.
Embodiment eight：Unlike one of present embodiment and embodiment one to seven：In step one when When described fused salt is NaCl and KCl mixture, NaCl and KCl mol ratio are 1:(1~5).Other and specific embodiment party Formula one to seven is identical.
Embodiment nine：Unlike one of present embodiment and embodiment one to eight：In step one when When described fused salt is NaCl and KCl mixture, NaCl and KCl mol ratio are 1:(2~5).Other and specific embodiment party Formula one to eight is identical.
Embodiment ten：Crystal grain is small and the degree of orientation is high applied to preparing for the template seed crystal of texture aluminium oxide ceramics Texture aluminium oxide ceramics, the texture aluminium oxide ceramics crystallite dimension of preparation is 5 μm~20 μm, is along [0001] orientation texture quality More than 93%, fracture toughness is more than 2 times of conventional ceramic, can also be applied to metal/ceramic/high polymer composite material toughness reinforcing Agent, heat-conduction-type polymer filler, grinding and polishing powder and pigment base material field.
Beneficial effects of the present invention are verified using following examples：
Embodiment one：A kind of preparation method of the template seed crystal of texture aluminium oxide ceramics is completed according to the following steps：
First, aluminum-containing raw material is mixed with fused salt, then adds growth auxiliary agent, mixture is obtained, using absolute ethyl alcohol as ball milling Medium, using alumina balls as abrading-ball, by mixture ball milling 12h, dries slurry after ball milling, obtains mixed material；
Described aluminum-containing raw material is Al2(SO4)3；
Described fused salt is K2SO4；
Described growth auxiliary agent is SiO2-CaO-TiO2Mixed aid；Described SiO2-CaO-TiO2SiO in mixed aid2 Mol ratio with CaO is 1:1；Described SiO2-CaO-TiO2SiO in mixed aid2With TiO2Mol ratio be 1:0.2；
Described aluminum-containing raw material and the mol ratio of fused salt are 1:6；
2nd, mixed material is placed in the alumina crucible of lid, under conditions of temperature is 1100 DEG C, calcines 1h, obtain To reaction product；
3rd, reaction product is cleaned with temperature for 90 DEG C of hot water stirs and uses ultrasonic wave to be disperseed, dried, obtain The template seed crystal of texture aluminium oxide ceramics；The texture aluminum oxide prepared in growth auxiliary agent and step 3 described in step one is made pottery The mass ratio of the template seed crystal of porcelain is 1:100.
The template seed crystal of texture aluminium oxide ceramics manufactured in the present embodiment is aluminum oxide sheet-like crystallite.
Fig. 2 is the XRD spectrum of aluminum oxide sheet-like crystallite prepared by embodiment one；As seen from the figure, prepared sheet-like crystallite For the α-Al of pure phase2O3。
Aluminum oxide sheet microcrystalline product good dispersion manufactured in the present embodiment, narrow size distribution, regular shape, surfacing Smooth, radius-thickness ratio is 13.2, and average grain diameter is 14.9 microns.
Embodiment two：
A kind of preparation method of the template seed crystal of texture aluminium oxide ceramics is completed according to the following steps：
First, aluminum-containing raw material is mixed with fused salt, then adds growth auxiliary agent, mixture is obtained, using absolute ethyl alcohol as ball milling Medium, using alumina balls as abrading-ball, by mixture ball milling 32h, dries slurry after ball milling, obtains mixed material；
Described aluminum-containing raw material is γ-Al2O3；
Described fused salt is Na2SO4-K2SO4；Described Na2SO4With K2SO4Mol ratio be 1:1；
Described growth auxiliary agent is SiO2；
Described aluminum-containing raw material and the mol ratio of fused salt are 1:2；
2nd, mixed material is placed in the alumina crucible of lid, under conditions of temperature is 1200 DEG C, calcines 4h, obtain To reaction product；
3rd, reaction product is cleaned with temperature for 85 DEG C of hot water stirs and uses ultrasonic wave to be disperseed, dried, obtain The template seed crystal of texture aluminium oxide ceramics；The texture aluminum oxide prepared in growth auxiliary agent and step 3 described in step one is made pottery The mass ratio of the template seed crystal of porcelain is 0.5:100.
The template seed crystal of texture aluminium oxide ceramics manufactured in the present embodiment is aluminum oxide sheet-like crystallite.
Fig. 3 is the microscopic appearance figure of aluminum oxide sheet-like crystallite prepared by embodiment two；As seen from the figure, the microcrystalline dispersion Good, aclusion and agglomeration, narrow size distribution, regular shape, surfacing are smooth, and average grain diameter is 9.8 microns, radius-thickness ratio For 23.7.
Embodiment three：
A kind of preparation method of the template seed crystal of texture aluminium oxide ceramics is completed according to the following steps：
First, aluminum-containing raw material is mixed with fused salt, then adds growth auxiliary agent, mixture is obtained, using absolute ethyl alcohol as ball milling Medium, using alumina balls as abrading-ball, by mixture ball milling 48h, dries slurry after ball milling, obtains mixed material；
Described aluminum-containing raw material is γ-Al2O3；
Described fused salt is Na2SO4-K2SO4；Described Na2SO4With K2SO4Mol ratio be 1:1；
Described growth auxiliary agent is SiO2- CaO mixed aids；Described SiO2SiO in-CaO mixed aids2With rubbing for CaO You are than being 1:1；
Described aluminum-containing raw material and the mol ratio of fused salt are 1:2；
2nd, mixed material is placed in the alumina crucible of lid, under conditions of temperature is 1150 DEG C, calcines 4h, obtain To reaction product；
3rd, reaction product is cleaned with temperature for 90 DEG C of hot water stirs and uses ultrasonic wave to be disperseed, dried, obtain The template seed crystal of texture aluminium oxide ceramics；The texture aluminum oxide prepared in growth auxiliary agent and step 3 described in step one is made pottery The mass ratio of the template seed crystal of porcelain is 1:100.
The template seed crystal of texture aluminium oxide ceramics manufactured in the present embodiment is aluminum oxide sheet-like crystallite.
Fig. 4 is the microscopic appearance figure of aluminum oxide sheet-like crystallite prepared by embodiment three；As seen from the figure, the microcrystalline dispersion Good, aclusion and agglomeration, narrow size distribution, regular shape, surfacing are smooth, and average grain diameter is 3.6 microns, radius-thickness ratio For 12.3.
Example IV：The aluminum oxide sheet-like crystallite prepared by the use of embodiment three as template, according to document [M.D.Snel, J.van Hoolst etc., Influence of tape cast parameters on texture formation in alumina by templated grain growth,Journal of the European Ceramic Society 29 (2009) 2757-2763] disclosed in template seed crystal oriented growth technology prepare texture aluminium oxide ceramics, obtain with alumina wafer Shape crystallite is texture aluminium oxide ceramics prepared by template；The texture aluminium oxide ceramics prepared by template of aluminum oxide sheet-like crystallite is brilliant Particle size is 10 microns.
Fig. 5 is the texture aluminium oxide ceramics XRD spectrum prepared by template of aluminum oxide sheet-like crystallite prepared by example IV, As can be seen that its 0006 and 00012 peak is especially strong from figure, whole XRD has been dominated, has illustrated that the textured ceramic is high along [0001] Preferred orientation is spent, the ceramic texture quality calculated according to XRD spectrum i.e. [0001] degree of orientation is up to more than 93%.
Fig. 6 schemes for Fracture Toughness comparison, and a is conventional ceramic, and b is example IV preparation using aluminum oxide sheet-like crystallite as mould Texture aluminium oxide ceramics prepared by plate.As seen from the figure, what prepared by example IV prepares by template of aluminum oxide sheet-like crystallite The fracture toughness of texture aluminium oxide ceramics be significantly increased, be 2 times of conventional ceramic.

Claims (10)

1. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics, it is characterised in that a kind of texture aluminium oxide ceramics is used The preparation method of template seed crystal complete according to the following steps：
First, aluminum-containing raw material is mixed with fused salt, then adds growth auxiliary agent, obtain mixture, using absolute ethyl alcohol as ball-milling medium, Using alumina balls as abrading-ball, by mixture ball milling 12h~48h, slurry is dried after ball milling, mixed material is obtained；
Described aluminum-containing raw material is γ-Al2O3、γ-AlO(OH)、Al2(SO4)3With α-Al (OH)3In one kind or wherein several Mixture；
Described fused salt is Na2SO4、K2SO4, NaCl and one kind or wherein several mixtures in KCl；
Described growth auxiliary agent is SiO2、SiO2- CaO mixed aids or SiO2-CaO-TiO2Mixed aid；Described SiO2-CaO SiO in mixed aid2Mol ratio with CaO is 1:(0.2~2)；Described SiO2-CaO-TiO2SiO in mixed aid2With CaO Mol ratio be 1:(0.2~1)；Described SiO2-CaO-TiO2SiO in mixed aid2With TiO2Mol ratio be 1:(0.2~ 1)；
Described aluminum-containing raw material and the mol ratio of fused salt are 1:(2~10)；
2nd, mixed material is placed in the alumina crucible of lid, under conditions of temperature is 900 DEG C~1200 DEG C, calcines 1h ~8h, obtains reaction product；
3rd, reaction product is cleaned with temperature for 60 DEG C~95 DEG C of hot water stirs and uses ultrasonic wave to be disperseed, dried, obtain To the template seed crystal of texture aluminium oxide ceramics；The template seed crystal grain size of described texture aluminium oxide ceramics is 0.5 μm ~15 μm, radius-thickness ratio is 12~25；
The mass ratio of the template seed crystal of the texture aluminium oxide ceramics prepared in growth auxiliary agent and step 3 described in step one For (0.1~3):100.
2. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： The mol ratio of aluminum-containing raw material and fused salt described in step one is 1:(2~6).
3. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： The mass ratio of growth auxiliary agent and the template seed crystal of the texture aluminium oxide ceramics prepared in step 3 described in step one is (0.1~2.5):100.
4. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： The mass ratio of growth auxiliary agent and the template seed crystal of the texture aluminium oxide ceramics prepared in step 3 described in step one is (0.1~2.25):100.
5. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： The mass ratio of growth auxiliary agent and the template seed crystal of the texture aluminium oxide ceramics prepared in step 3 described in step one is (0.15~2.25):100.
6. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： When described fused salt is Na in step one2SO4And K2SO4Mixture when, Na2SO4With K2SO4Mol ratio be 1:(0.5~5).
7. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： When described fused salt is Na in step one2SO4And K2SO4Mixture when, Na2SO4With K2SO4Mol ratio be 1:(1~5).
8. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： In step one when described fused salt is NaCl and KCl mixture, NaCl and KCl mol ratio are 1:(1~5).
9. a kind of preparation method of the template seed crystal of texture aluminium oxide ceramics according to claim 1, it is characterised in that： In step one when described fused salt is NaCl and KCl mixture, NaCl and KCl mol ratio are 1:(2~5).
10. the application of the template seed crystal of texture aluminium oxide ceramics prepared by preparation method as claimed in claim 1, its feature It is that the template seed crystal of texture aluminium oxide ceramics is applied to prepare the texture aluminium oxide ceramics that crystal grain is small and the degree of orientation is high, prepares Texture aluminium oxide ceramics crystallite dimension be 5 μm~20 μm, be more than 93% along [0001] orientation texture quality, fracture toughness is More than 2 times of conventional ceramic, can also be applied to metal/ceramic/high polymer composite material toughener, heat-conduction-type polymer and fill out Material, grinding and polishing powder and pigment base material field.
CN201710523918.8A 2017-06-30 2017-06-30 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics Active CN107326432B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710523918.8A CN107326432B (en) 2017-06-30 2017-06-30 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710523918.8A CN107326432B (en) 2017-06-30 2017-06-30 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics

Publications (2)

Publication Number Publication Date
CN107326432A true CN107326432A (en) 2017-11-07
CN107326432B CN107326432B (en) 2019-07-02

Family

ID=60199576

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710523918.8A Active CN107326432B (en) 2017-06-30 2017-06-30 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics

Country Status (1)

Country Link
CN (1) CN107326432B (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650888A (en) * 2018-12-27 2019-04-19 哈尔滨工业大学 A kind of high electric property ternary system lead titanate relaxor ferroelectric orientation ceramic of low temperature texture and its preparation method and application
CN112194490A (en) * 2020-10-16 2021-01-08 南京工业大学 Layered high-texture ceramic and preparation method thereof
CN115784279A (en) * 2022-12-12 2023-03-14 苏州锦艺新材料科技股份有限公司 Preparation method of alpha-photo-like nano aluminum oxide
CN116924774A (en) * 2022-04-02 2023-10-24 中国科学院上海硅酸盐研究所 High-strength low-dielectric composite microwave dielectric ceramic material and preparation method thereof
CN116924782A (en) * 2022-04-02 2023-10-24 中国科学院上海硅酸盐研究所 Microwave dielectric material with bionic structure and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657492A (en) * 2005-02-04 2005-08-24 武汉理工大学 Mould material used for preparing texture type ceramic and preparation method
CN1800024A (en) * 2006-01-13 2006-07-12 中国科学院上海硅酸盐研究所 Plate-like aluminum oxide granule preparation method
CN101575209A (en) * 2009-06-05 2009-11-11 武汉理工大学 Textured ceramic niobate template material with controllable thickness and radial dimension and preparation method thereof
CN104628379A (en) * 2013-11-06 2015-05-20 同济大学 Highly-oriented lead-free piezoelectric textured ceramic material and preparation method and application thereof
CN104947193A (en) * 2014-10-29 2015-09-30 中南大学 Sheet template seed crystal for textured leadless piezoelectric ceramics, and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1657492A (en) * 2005-02-04 2005-08-24 武汉理工大学 Mould material used for preparing texture type ceramic and preparation method
CN1800024A (en) * 2006-01-13 2006-07-12 中国科学院上海硅酸盐研究所 Plate-like aluminum oxide granule preparation method
CN101575209A (en) * 2009-06-05 2009-11-11 武汉理工大学 Textured ceramic niobate template material with controllable thickness and radial dimension and preparation method thereof
CN104628379A (en) * 2013-11-06 2015-05-20 同济大学 Highly-oriented lead-free piezoelectric textured ceramic material and preparation method and application thereof
CN104947193A (en) * 2014-10-29 2015-09-30 中南大学 Sheet template seed crystal for textured leadless piezoelectric ceramics, and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LI-HUI ZHU等: "Molten salt synthesis of a-Al2O3 platelets using NaAlO2 as raw material", 《CERAMICS INTERNATIONAL》 *
YUNFEI CHANGA等: "Molten salt synthesis of morphology controlled α-alumina platelets", 《CERAMICS INTERNATIONAL》 *
YUNFEI CHANG等: "Fabrication of Highly Textured Fine-Grained a-Alumina by Templated Grain Growth of Nanoscale Precursors", 《J. AM. CERAM. SOC.》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109650888A (en) * 2018-12-27 2019-04-19 哈尔滨工业大学 A kind of high electric property ternary system lead titanate relaxor ferroelectric orientation ceramic of low temperature texture and its preparation method and application
CN112194490A (en) * 2020-10-16 2021-01-08 南京工业大学 Layered high-texture ceramic and preparation method thereof
CN116924774A (en) * 2022-04-02 2023-10-24 中国科学院上海硅酸盐研究所 High-strength low-dielectric composite microwave dielectric ceramic material and preparation method thereof
CN116924782A (en) * 2022-04-02 2023-10-24 中国科学院上海硅酸盐研究所 Microwave dielectric material with bionic structure and preparation method thereof
CN115784279A (en) * 2022-12-12 2023-03-14 苏州锦艺新材料科技股份有限公司 Preparation method of alpha-photo-like nano aluminum oxide

Also Published As

Publication number Publication date
CN107326432B (en) 2019-07-02

Similar Documents

Publication Publication Date Title
CN107326432B (en) A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics
CN109455936B (en) Non-slip matt glaze with silk texture, preparation method and ceramic tile using non-slip matt glaze
CN104310978B (en) A kind of refractory ceramics powder coating material and preparation method thereof
CN104829218B (en) Bimodal active alumina micropowder and preparation method
CN104986786B (en) A kind of controllable sheet α Al of particle size2O3Powder and preparation method thereof
CN109336556B (en) A kind of enhancing of architectural pottery prestressing force coating paste and preparation method thereof and architectural pottery product
CN101775659B (en) Process for preparing mullite whisker or flaky alumina by using coal ash
CN112939582B (en) Zirconia-doped alumina ceramic and preparation method thereof
CN115521073B (en) Nano-calcium feldspar powder, anorthite microcrystalline frit and transparent microcrystalline glaze ceramic tile
CN111423124B (en) Wear-resistant transparent glaze, wear-resistant polished glazed brick and preparation method thereof
CN110563010A (en) preparation method of low-sodium regular hexagonal flaky alpha-alumina micro powder
CN107298453A (en) The nanocrystalline preparation method of boehmite
CN115557781B (en) Nano strengthened and toughened building ceramic and preparation method thereof
CN115838245A (en) Microcrystalline micro-gloss glaze, micro-gloss ceramic rock plate with ultra-flat and fine glaze and preparation method thereof
Ye et al. Effect of different preparation methods on the microstructure and mechanical properties of Si3N4 ceramic composites
CN1500733A (en) alpha-aluminium oxide powder and production method
CN114715925A (en) Flaky alpha alumina and preparation method thereof
Xia et al. Reactive hot pressing and mechanical properties of B4C/Li2O–Al2O3–SiO2 composites
CN112225557B (en) Preparation method of zirconia ceramic with pearl effect and product prepared by preparation method
CN102649576B (en) Preparation process for flaky alumina with great diameter-thickness ratio
CN112456525A (en) Preparation method of boehmite with low water absorption
CN116814118A (en) Ceramic ink capable of producing relief effect
CN114656249B (en) High-strength tawnite-based thin ceramic plate and preparation method thereof
CN106430984A (en) Method for preparing microcrystal wollastonite glass from wollastonite
CN107720764B (en) Method for preparing high-purity superfine tricalcium silicate powder by wet chemical method

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant