CN1657492A - Mould material used for preparing texture type ceramic and preparation method - Google Patents

Mould material used for preparing texture type ceramic and preparation method Download PDF

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CN1657492A
CN1657492A CN 200510018252 CN200510018252A CN1657492A CN 1657492 A CN1657492 A CN 1657492A CN 200510018252 CN200510018252 CN 200510018252 CN 200510018252 A CN200510018252 A CN 200510018252A CN 1657492 A CN1657492 A CN 1657492A
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ball milling
preparation
hours
absolute ethyl
ethyl alcohol
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CN1283588C (en
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曹明贺
刘韩星
王万强
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Wuhan University of Science and Engineering WUSE
Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

A template material used for preparing the texture-type ceramic is a regular flaky crystal and has the chemical formula: Bi2O3-xNa2O-yNb2O5, where x=1.3=1.5 and y=1.9-2.1. Its preparing process includes such steps as proportionally mixing Bi2O3, Na2CO3 (or NaHCO3) and Nb2O5, ball grinding, adding flux and absolute alcohol, ball grinding, drying, synthesizing at 950-1200 deg.C for 2-8 hr, washing with hot deionized water multiple times until there is no chlorious, and drying.

Description

A kind of mould material and preparation method who is used to prepare texture ceramic
Technical field
The present invention relates to a kind of mould material and preparation method who is used to prepare texture ceramic.Be template (seed crystal) material and the preparation method of a kind of energy as template grain growth (TGG) and reaction template grain growing method (RTGG).
Background technology
Textured material is under a kind of externally conditioning, each crystal grain that originally is orientated in a jumble is orientated mutually is consistent, and forms a kind of new material that is arranged of preferred orient.Textured material can increase substantially the performance of material.In structural material, can improve toughness and the cutting performance of material by texturing; In functional material, texturing can increase the critical current density of superconductor material, strengthens the electrical conductivity of ion conductor, improves the magnetic performance of magnetic ceramics material and the piezoelectric property that improves piezoelectric ceramics.The preparation method of textured material is many, comprise the directed method of template grain growth (TGG), reaction template grain growing method (RTGG), seed polymorphic transition change method (SPC), induced by magnetic field and directional solidification method or the like, wherein template grain growth (TGG), reaction template grain growing method (RTGG) are two kinds does not need that expensive complex apparatus, technology are relatively simple, the texture satisfactory method of material.In template grain growth and reaction template grain growing method, can prepare well behaved template and be seed crystal and be one of key factor of can processability good textured material.In general, the feature of suitable template has:
1, with similar crystalline structure and the unit cell parameters of bulk material;
2, have suitable shape, for example whisker shape or sheet, suitable size and length-footpath than;
3, has thermodynamic stability.
Summary of the invention
The purpose of this invention is to provide a kind of laminated structure and suitable dimension and length-footpath than mould material, the preparation method of this mould material is provided simultaneously.
The objective of the invention is to realize with following technical proposals:
A kind of mould material that is suitable for template grain growth (TGG) and reaction template grain growth method (RTGG) preparation textured material, it is a kind of mould material (seed crystal material) of texture ceramic, this material is the regular flake crystalline particle shape of 0.5 μ m～40 μ m, and its chemical composition is Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3～1.5 wherein, y=1.9～2.1.
The preparation method of the mould material of described texture ceramic adopts the molten-salt growth method preparation, the steps include:
1st, with purity greater than 99% Bi 2O 3, Na 2CO 3And Nb 2O 5Be initiation material, according to Bi 2O 3: Na 2CO 3: Nb 2O 5=1: 1.3～1.5: 1.9～2.1 chemistry is than batching; Perhaps with purity greater than 99% Bi 2O 3, NaHCO 3And Nb 2O 5Be initiation material, according to Bi 2O 3: NaHCO 3: Nb 2O 5=1: 2x: the chemistry of y is than batching, x=1.3～1.5 wherein, y=1.9～2.1; The material for preparing ball milling 6～12 hours in ball mill, the grinding aid of ball milling is absolute ethyl alcohol, the mass ratio of initiation material and absolute ethyl alcohol=1: 0.8～1.5;
2nd, in the material of step 1 ball milling gained, add fusing assistant, mixing and ball milling oven dry later in 6～12 hours, grinding aid during ball milling is a dehydrated alcohol, described fusing assistant is the combination of any two or three among NaCl or KCl or NaF or KF or four, the quality of fusing assistant is 0.5～2.0: 1 with the ratio of initial reactant total mass, the material of step 1 ball milling gained and the mass ratio of dehydrated alcohol=1: 0.8～1.5;
3rd, the material after step 2 oven dry is added thermal synthesis, 950 ℃～1200 ℃ of synthesis temperatures, generated time 2～8 hours in air or oxygen-enriched atmosphere;
4th, step 3 synthetic powder is inserted in 30～80 ℃ of deionized waters, stirring and washing left standstill 5～10 minutes or adopted ultrasonic cleaner to carry out supersound process 5～10 minutes after 3～5 minutes, remove supernatant liquid then, the repeated washing operating process is up to supernatant liquid AgNO 3Titration does not have muddiness;
5th, the powder drying that step 4 cleaned promptly makes the seed crystal material of required textured material.
Description of drawings
Fig. 1 is Bi 2.5Na 3.5Nb 5O 18XRD figure:
Fig. 2 a, b are Bi 2.5Na 3.5Nb 5O 18The SEM figure of different amplification:
Fig. 1 and the represented Bi of Fig. 2 a, b 2.5Na 3.5Nb 5O 18Preparation condition: with Bi 2O 3, Na 2CO 3And Nb 2O 5Be starting raw material, Bi 2O 3With Na 2CO 3And Nb 2O 5Stoicheiometry is 1: 1.4: 2, and fusing assistant is NaCl, and synthesis temperature is 1100 ℃, and generated time is 5 hours.
Embodiment
Following embodiment is raw materials used to be purity greater than 99% commercial product.
Embodiment 1:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, the preparation of y=2.0
With Bi 2O 3, Na 2CO 3And Nb 2O 5Be initiation material, press Bi 2O 3With Na 2CO 3And Nb 2O 5Stoicheiometry be 1: 1.4: 2.0 the batching, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 6 hours in ball mill, add flux NaCl, ball milling is 12 hours again, NaCl adding quality is 1: 1 with the ratio of initial reactant gross mass, the ball milling post-drying, lower synthetic 5 hours in 1100 ℃ of temperature in air atmosphere, synthetic product dries clean after cleaning by aforesaid stirring and washing method with 50 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5X=1.4 wherein, the y=2.0 crystal.
Embodiment 2:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3 wherein, the preparation of y=2.1
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, Na 2CO 3And Nb 2O 5, Bi 2O 3With Na 2CO 3And Nb 2O 5Stoicheiometry be 1: 1.3: 2.1, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 0.8, the material for preparing ball milling 6 hours in ball mill, add flux NaCl, ball milling is 8 hours again,, the flux quality is 1: 1 with the ratio of initial reactant gross mass, synthesis temperature is 950 ℃, generated time is 6 hours, dries up after synthetic product is clean by aforesaid Ultrasonic Cleaning with 50 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3 wherein, y=2.1 crystal.
Embodiment 3:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, the preparation of y=2.1
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, Na 2CO 3And Nb 2O 5, Bi 2O 3With Na 2CO 3And Nb 2O 5Stoicheiometry be 1.0: 1.3: 2.1, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1.5, the material for preparing ball milling 7 hours in ball mill adds flux NaCl, ball milling is 7 hours again, the flux quality is 1: 1.5 with the ratio of initial reactant gross mass, and synthesis temperature is 1050 ℃, and generated time is 5 hours, synthetic product dries clean after cleaning by aforesaid stirring and washing method with 80 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, y=2.1 crystal.
Embodiment 4:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, the preparation of y=1.9
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1.0: 2.8: 1.9, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1.2, the material for preparing ball milling 9 hours in ball mill adds flux KCl, ball milling is 9 hours again, the flux quality is 1: 1.2 with the ratio of initial reactant gross mass, and synthesis temperature is 1100 ℃, and generated time is 4.5 hours, dry up after synthetic product is clean by aforesaid Ultrasonic Cleaning with 50 ℃ of deionized waters, namely obtain regular sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, y=1.9 crystal.
Embodiment 5:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3 wherein, the preparation of y=2.1
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1: 2.6: 2, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 8 hours in ball mill adds flux KCl, ball milling is 8 hours again, the flux quality is 1: 1 with the ratio of initial reactant gross mass, and synthesis temperature is 1100 ℃, and generated time is 6 hours, synthetic product dries clean after cleaning by aforesaid stirring and washing method with 60 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3 wherein, y=2.1 crystal.
Embodiment 6:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.5 wherein, the preparation of y=2.1
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1.0: 3.0: 2.0, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 12 hours in ball mill adds flux KCl, ball milling is 12 hours again, the flux quality is 1: 1 with the ratio of initial reactant gross mass, and synthesis temperature is 1150 ℃, and generated time is 4 hours, dry up after synthetic product is clean by aforesaid Ultrasonic Cleaning with 60 ℃ of deionized waters, namely obtain 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.5 wherein, y=2.1 crystal.
Embodiment 7:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, the preparation of y=2.0
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1: 2.8: 2, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 12 hours in ball mill, add flux KF, ball milling is 12 hours again, and the flux quality is 1: 1.5 with the ratio of initial reactant gross mass, synthesis temperature is 1100 ℃, generated time is 6 hours, and synthetic product dries clean after cleaning by aforesaid stirring and washing method with 40 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, y=2.0 crystal.
Embodiment 8:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.35 wherein, the preparation of y=2.1
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1: 2.7: 2.1, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 12 hours in ball mill adds flux KF, ball milling is 12 hours again, the flux quality is 1: 2 with the ratio of initial reactant gross mass, and synthesis temperature is 1200 ℃, and generated time is 5.5 hours, dry up after synthetic product is clean by aforesaid Ultrasonic Cleaning with 40 ℃ of deionized waters, namely obtain 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.35 wherein, y=2.1 crystal.
Embodiment 9:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, the preparation of y=1.9
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1: 2.8: 1.9, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 12 hours in ball mill, add flux KCl+NaCl, KCl is 1: 1 with the ratio of NaCl quality, ball milling is 12 hours again, the flux quality is 1: 1 with the ratio of initial reactant gross mass, synthesis temperature is 1100 ℃, generated time is 5 hours, dries up after synthetic product is clean by aforesaid Ultrasonic Cleaning with 45 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.35 wherein, y=2.1 crystal.
Embodiment 10:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, the preparation of y=2.1
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, NaHCO 3And Nb 2O 5, Bi 2O 3With NaHCO 3And Nb 2O 5Stoicheiometry be 1: 2.8: 2.1, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 12 hours in ball mill, add flux KCl+NaCl, KCl is 1: 2 with the ratio of NaCl quality, ball milling is 12 hours again, the flux quality is 1: 1.5 with the ratio of initial reactant gross mass,, synthesis temperature is 1100 ℃, generated time is 4.5 hours, synthetic product dries clean after cleaning by aforesaid stirring and washing method with 45 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.4 wherein, y=2.1 crystal.
Embodiment 11:Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3 wherein, the preparation of y=2.0
The preparation method is identical with embodiment 1, and preparation condition is: initiation material is Bi 2O 3, Na 2CO 3And Nb 2O 5, Bi 2O 3With Na 2CO 3And Nb 2O 5Stoicheiometry be 1: 1.3: 2, be grinding aid with absolute ethyl alcohol, initiation material and absolute ethyl alcohol mass ratio=1: 1, the material for preparing ball milling 12 hours in ball mill adds flux NaF, ball milling is 12 hours again, the flux quality is 1: 2 with the ratio of initial reactant gross mass, and synthesis temperature is 1100 ℃, and generated time is 5 hours, synthetic product dries clean after cleaning by aforesaid stirring and washing method with 45 ℃ of deionized waters, namely obtains 0.5 μ m～40 μ m rule sheet Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3 wherein, y=2.0 crystal.

Claims (2)

1, a kind of mould material of texture ceramic is characterized in that this material is the regular flake crystalline particle shape of 0.5 μ m～40 μ m, and its chemical composition is Bi 2O 3-xNa 2O-yNb 2O 5, x=1.3～1.5 wherein, y=1.9～2.1.
2, the preparation method of the mould material of the described texture ceramic of claim 1 is characterized in that adopting the molten-salt growth method preparation, the steps include:
1st, with purity greater than 99% Bi 2O 3, Na 2CO 3And Nb 2O 5Be initiation material, according to Bi 2O 3: Na 2CO 3: Nb 2O 5=1: 1.3～1.5: 1.9～2.1 chemistry is than batching; Perhaps with purity greater than 99% Bi 2O 3, NaHCO 3And Nb 2O 5Be initiation material, according to Bi 2O 3: NaHCO 3: Nb 2O 5=1: 2x: the chemistry of y is than batching, x=1.3～1.5 wherein, y=1.9～2.1; The material for preparing ball milling 6～12 hours in ball mill, the grinding aid of ball milling is absolute ethyl alcohol, the mass ratio of initiation material and absolute ethyl alcohol=1: 0.8～1.5;
2nd, in the material of step 1 ball milling gained, add fusing assistant, mixing and ball milling oven dry later in 6～12 hours, grinding aid during ball milling is a dehydrated alcohol, described fusing assistant is the combination of any two or three among NaCl or KCl or NaF or KF or four, the quality of fusing assistant is 0.5～2.0: 1 with the ratio of initial reactant total mass, the material of step 1 ball milling gained and the mass ratio of dehydrated alcohol=1: 0.8～1.5;
3rd, the material after step 2 oven dry is added thermal synthesis, 950 ℃～1200 ℃ of synthesis temperatures, 2～8 hours one-tenth time in air or oxygen-enriched atmosphere;
4th, step 3 synthetic powder is inserted in 30～80 ℃ of deionized waters, stirring and washing left standstill 5～10 minutes or adopted ultrasonic cleaner to carry out supersound process 5～10 minutes after 3～5 minutes, remove supernatant liquid then, the repeated washing operating process is up to supernatant liquid AgNO 3Titration does not have muddiness;
5th, the powder drying that step 4 cleaned promptly makes the seed crystal material of required textured material.
CN 200510018252 2005-02-04 2005-02-04 Mould material used for preparing texture type ceramic and preparation method Expired - Fee Related CN1283588C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102115160A (en) * 2011-01-13 2011-07-06 西安工业大学 Method for fast preparing micron-level lamellar barium titanate powder
CN102185098A (en) * 2011-03-21 2011-09-14 武汉理工大学 Preferred orientation type niobate lead-free piezoelectric thick-film material and preparation method thereof
CN107326432A (en) * 2017-06-30 2017-11-07 哈尔滨工业大学 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102115160A (en) * 2011-01-13 2011-07-06 西安工业大学 Method for fast preparing micron-level lamellar barium titanate powder
CN102185098A (en) * 2011-03-21 2011-09-14 武汉理工大学 Preferred orientation type niobate lead-free piezoelectric thick-film material and preparation method thereof
CN107326432A (en) * 2017-06-30 2017-11-07 哈尔滨工业大学 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics
CN107326432B (en) * 2017-06-30 2019-07-02 哈尔滨工业大学 A kind of preparation method and application of the template seed crystal of texture aluminium oxide ceramics

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