CN109608173A - A kind of Al2O3Base complex phase ceramic sintered sample and shape control method - Google Patents

A kind of Al2O3Base complex phase ceramic sintered sample and shape control method Download PDF

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CN109608173A
CN109608173A CN201811618700.1A CN201811618700A CN109608173A CN 109608173 A CN109608173 A CN 109608173A CN 201811618700 A CN201811618700 A CN 201811618700A CN 109608173 A CN109608173 A CN 109608173A
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complex phase
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zro
control method
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CN109608173B (en
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马斌
马丽莉
马国俊
张谦信
苏科
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Qinghai University
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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
    • C04B35/622—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
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C04B35/62615—High energy or reactive ball milling
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C04B2235/3246—Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia
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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
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    • 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
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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    • 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
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Abstract

The invention belongs to ceramic sintering technology fields, disclose a kind of Al2O3Base complex phase ceramic sintered sample and shape control method.Take the Al of certain mass2O3Powder and SiC powder are placed in ball mill, then micro ZrO is added into ball mill2A small amount of dehydrated alcohol is added dropwise after powder, mixing and ball milling 10-15h obtains Al2O3Base complex phase powder；This complex phase powder is put into punching block and passes through cold isostatic compaction under a certain pressure；Green body after cold isostatic compaction is subjected to the pre-heat treatment in a vacuum, removes moisture and volatile material in green body；Ceramic material is sintered after ceramic post sintering equipment is set corresponding temperature increasing schedule.The present invention is in Al2O3Micro ZrO is added in-SiC complex phase powder2Powder effectively inhibits Al2O3The deformation of SiC ceramic green body during the sintering process, has promoted the normal use of material, can substantially reduce the defect rate of this kind of ceramic material.

Description

A kind of Al2O3Base complex phase ceramic sintered sample and shape control method
Technical field
The invention belongs to ceramic sintering technology field more particularly to a kind of Al2O3The shape control of base complex phase ceramic sintered sample Method processed.
Background technique
Currently, the prior art commonly used in the trade is such that
Ceramic material has a wide range of applications in many fields.But its most fatal weakness is high brittleness and low reliable Property, especially Al2O3Ceramics, brittleness is big, thermal shock resistance is poor, to limit its application in many occasions.Furthermore ceramics The crystal grain that material necessarily occurs when sintering at high temperature, which is recrystallized, brings obstacle to the preparation of single phase ceramic material, therefore, complex phase pottery The conception of porcelain is come into being.It is present in the inside configuration or crystal boundary of the matrix of micron order or submicron order with the second phase of nanoscale In, so that it may while effect to the strengthening and toughening of material is played, and can be improved its thermal shock resistance.In addition, it is material again Expect a good object of design.Therefore, complex phase ceramic also just becomes the ceramic material of most Practical significance.
Al2O3Base complex phase ceramic is a kind of extremely important and basic engineering ceramics material in practical application and scientific research Material, system includes Al2O3-SiC、Al2O3-ZrO2Etc..And preparing the most commonly used sintering method of these ceramics is exactly air It is normal pressure-sintered under atmospheric condition.However, this preparation method is in sintering Al2O3When-SiC complex phase ceramic, specimen surface and inside are few It is SiO that oxidation transformation, which can occur, for the SiC of amount2, therefore, sample can deform bending, lead to material not and can be carried out normally to answer With.
In conclusion problem of the existing technology is:
Ceramic material can not be machined after the completion of sintering as metal, therefore it is required that the shape of green body Stability wants high.For Al2O3The sintering of-SiC complex phase ceramic generally requires the protection of inert gas, and not only equipment investment is big, and And it is produced into also higher.Using common heating equipment to Al2O3- SiC complex phase ceramic, which is sintered, can reduce equipment and production Cost, but molding green body often due to the oxidation of SiC and deform, cause the shape stability of ceramic body compared with Difference.
More Al is applied at present2O3Base complex phase ceramic system includes Al2O3-SiC、Al2O3-ZrO2, it is being sintered system Standby Al2O3When-SiC complex phase ceramic, oxidation transformation can occur for specimen surface and internal a small amount of SiC for SiO2, therefore, sample meeting Deform bending, leads to material not and can be carried out normal application.
Solve the difficulty and meaning of above-mentioned technical problem:
To Al under its empty atmosphere2O3When-SiC complex phase ceramic carries out normal pressure-sintered, how to inhibit green body under hot conditions Shape distortion generally can inhibit the sintering method deformed using gravity using slinging green body, but the method can be to agglomerating plant There is particular/special requirement, and can also propose more harsh requirement in powder mixing and blank forming technical process.How not Change Al2O3In the case that-SiC complex phase ceramic mainly forms, using the sintering method that cost is minimum, inhibit the shape of ceramic There is presently no good methods for shape deformation.The invention patent is proposed in Al2O3With a small amount of Y is added in SiC powder2O3Part is steady Fixed tetragonal phase ZrO2, utilize Y2O3Partially stabilized tetragonal phase ZrO2Volumetric expansion in temperature-fall period, to inhibit The deformation of the ceramic material, it is entirely avoided the dependence to equipment reduces costs.
Avoid Al2O3Base complex phase ceramic Al2O3Bending of-SiC the system in sintering, can greatly improve material Utilization rate, reduction in the numbers of seconds, while the use scope of ceramics has also been enlarged.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of Al2O3Base complex phase ceramic sintered sample and shape control Method processed.
The invention is realized in this way a kind of Al2O3The shape control method of base complex phase ceramic sintered sample are as follows:
Step 1: the Al of certain mass is taken2O3Powder and SiC powder are placed in ball mill (Al2O3Mass ratio with SiC is 1:1~9:1, Al2O3Powder is nano powder, 99% or more purity；The granularity of SiC powder is more than 300 mesh, 98% or more purity), then Micro ZrO is added into ball mill2Powder (ZrO2Powder is micron powder, and composition is 2~8%Y2O3Partially stabilized four Square phase ZrO2, additive amount Al2O3With the 0.5~2% of SiC gross mass), a small amount of nothing is added dropwise in mixed powder later Water-ethanol；Mixing and ball milling 10-15h, mill, which is situated between, uses ZrO2Abrading-ball；It is final to obtain complex phase powder；
Step 2: mixing complex phase powder is put through punching block cold isostatic compaction under a certain pressure, and briquetting pressure 200~ 300Mpa；
Step 3: the green body after cold isostatic compaction is carried out to the pre-heat treatment (heat treatment temperature 400~600 in a vacuum DEG C), remove the moisture and volatile material in green body；
Step 4: setting corresponding temperature increasing schedule for ceramic post sintering equipment, specifically: room temperature~600 DEG C: 3 DEG C/min, 600~1000 DEG C: 5 DEG C/min, and in 1000 DEG C of heat preservation 1~2h, 1000 DEG C~sintering temperature (1400~1650 DEG C): 10~15 ℃/min；Green body is put into sintering furnace and is sintered according to temperature increasing schedule, cooled to room temperature obtains Al2O3Base complex phase ceramic Sintered sample.
Further, the Al2O3The shape control method of base complex phase ceramic sintered sample, which is characterized in that the Al2O3 Powder and SiC powder carry out a small amount of dehydrated alcohol of dropwise addition that must be used when ball milling, to prevent powder hardened.
Further, the pressure when cold isostatic compaction is 200~300MPa.
Further, the sintering schedule of the ceramic post sintering equipment setting is room temperature~600 DEG C: 3 DEG C/min, 600~1000 DEG C: 5 DEG C/min, and in 1000 DEG C of heat preservation 1~2h, 1000 DEG C~sintering temperature (1400~1650 DEG C): 10~15 DEG C/min.It burns Junction temperature keeps the temperature 2~6h.
The Al is utilized another object of the present invention is to provide a kind of2O3The shape of base complex phase ceramic sintered sample controls Al made from method2O3Base complex phase ceramic sintered sample.
In conclusion advantages of the present invention and good effect are as follows: by adding a small amount of Y2O3Partially stabilized tetragonal phase ZrO2 Changes in crystal structure in temperature-fall period, the Volumetric expansion of generation.Inhibit ceramic body volume during the sintering process Diminution and metamorphosis.This method does not have particular/special requirement to agglomerating plant, reduces cost, improves yield rate and materials'use rate.
The present invention using conventional agglomerating plant in the case where not utilizing specific process and condition, in Al2O3- SiC complex phase Micro ZrO is added in powder2Powder effectively inhibits Al2O3The deformation of SiC ceramic green body during the sintering process, promotes The normal use of material can substantially reduce the defect rate of this ceramic material.
Detailed description of the invention
Fig. 1 is Al provided in an embodiment of the present invention2O3The shape control method flow chart of base complex phase ceramic sintered sample.
Fig. 2 is Al provided in an embodiment of the present invention2O3The XRD spectrum of-SiC complex phase ceramic.
Fig. 3 is the sintered shape comparison diagram of complex phase ceramic provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Application principle of the invention is described in detail with reference to the accompanying drawing.
As shown in Figure 1, Al provided in an embodiment of the present invention2O3The shape control method of base complex phase ceramic sintered sample are as follows:
S101: the Al of certain mass is taken2O3Powder and SiC powder are placed in ball mill (Al2O3Mass ratio with SiC is 1: 1~9:1, Al2O3Powder is nano powder, 99% or more purity；The granularity of SiC powder is more than 300 mesh, 98% or more purity), then to Micro ZrO is added in ball mill2Powder (ZrO2Powder is micron powder, and composition is 2~8%Y2O3Partially stabilized four directions Phase ZrO2, additive amount Al2O3With the 0.5~2% of SiC gross mass), it is added dropwise in mixed powder later a small amount of anhydrous Ethyl alcohol；Mixing and ball milling 10-15h, mill, which is situated between, uses ZrO2Abrading-ball；It is final to obtain complex phase powder；
S102: mixing complex phase powder is put through punching block cold isostatic compaction under a certain pressure, and briquetting pressure 200~ 300Mpa；
S103: the green body after cold isostatic compaction is carried out to the pre-heat treatment (heat treatment temperature 400~600 in a vacuum DEG C), remove the moisture and volatile material in green body；
S104: after green body is put into sintering furnace, setting the corresponding temperature increasing schedule of equipment, specifically: room temperature~600 DEG C: 3 DEG C/min, 600~1000 DEG C: 5 DEG C/min, and in 1000 DEG C of heat preservation 1~2h, 1000 DEG C~sintering temperature (1400~ 1650 DEG C): 10~15 DEG C/min；Green body is put into sintering furnace and is sintered according to temperature increasing schedule, sintering temperature heat preservation 2~ 6h, cooled to room temperature obtain Al2O3Base complex phase ceramic sintered sample.
Al2O3Powder and SiC powder carry out a small amount of dehydrated alcohol of dropwise addition that must be used when ball milling, to prevent powder hardened.
The pressure when cold isostatic compaction is 200~300MPa.
The sintering schedule of the ceramic post sintering equipment setting is room temperature~600 DEG C: 3 DEG C/min, 600~1000 DEG C: 5 DEG C/ Min, and in 1000 DEG C of heat preservation 1~2h, 1000 DEG C~sintering temperature (1400~1650 DEG C): 10~15 DEG C/min.
The present invention provides a kind of utilization the Al2O3Al made from the shape control method of base complex phase ceramic sintered sample2O3 Base complex phase ceramic sintered sample.
The invention will be further described with experiment combined with specific embodiments below.
With above-mentioned Al2O3Powder, SiC powder and ZrO2Powder is raw material, carries out Al according to specific embodiment2O3- SiC pottery The sintering of porcelain, the main object for obtaining the following gained ceramic material of result mutually remain as Al2O3With SiC (Fig. 2).
It can clearly be seen that corresponding ZrO is added from Fig. 32Shape distortion suppression sintered for ceramic body after powder Production is with clearly.It is being added without ZrO2When powder, apparent bending is presented in ceramics after the completion of sintering；ZrO is being added2 When powder；Rectangular column shape when remaining as molding after the completion of ceramic post sintering is substantially identical as molding blank shape.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (5)

1. a kind of Al2O3The shape control method of base complex phase ceramic sintered sample, which is characterized in that the Al2O3Base complex phase ceramic The shape control method of sintered sample are as follows:
Step 1: the Al of certain mass is taken2O3Powder and SiC powder are placed in ball mill, then micro ZrO is added into ball mill2 A small amount of dehydrated alcohol is added dropwise in powder in mixed powder later；Mixing and ball milling 10-15h, mill, which is situated between, uses ZrO2Abrading-ball； It is final to obtain complex phase powder；
Step 2: mixing complex phase powder is put through punching block cold isostatic compaction under a certain pressure, and briquetting pressure 200~ 300Mpa；
Step 3: the green body after cold isostatic compaction is subjected to the pre-heat treatment in a vacuum, 400~600 DEG C of heat treatment temperature, is removed Remove the moisture and volatile material in green body；
Step 4: ceramic post sintering equipment is set into corresponding temperature increasing schedule；Green body is put into sintering furnace according to temperature increasing schedule It is sintered, cooled to room temperature obtains Al2O3Base complex phase ceramic sintered sample.
2. Al as described in claim 12O3The shape control method of base complex phase ceramic sintered sample, which is characterized in that step 1 In, Al2O3Mass ratio with SiC is 1:1~9:1, Al2O3Powder is nano powder, 99% or more purity；The granularity of SiC powder is being greater than 300 mesh, purity are greater than 98%；
ZrO2Powder is micron powder, and group becomes 2%~8%Y2O3Partially stabilized tetragonal phase ZrO2, ZrO2Powder additive amount For Al2O3With the 0.5~2% of SiC gross mass.
3. Al as described in claim 12O3The shape control method of base complex phase ceramic sintered sample, which is characterized in that described cold etc. Hydrostatic profile pressure is 200~300MPa.
4. Al as described in claim 12O3The shape control method of base complex phase ceramic sintered sample, which is characterized in that the ceramics The sintering schedule of agglomerating plant setting are as follows: room temperature~600 DEG C: 3 DEG C/min；600~1000 DEG C: 5 DEG C/min；And it is protected at 1000 DEG C Temperature 1~2h, 1000 DEG C~sintering temperature (1400~1650 DEG C): 10~15 DEG C/min；Sintering temperature keeps the temperature 2~6h.
5. a kind of utilize Al described in claim 12O3The shape control method of base complex phase ceramic sintered sample adds in material powder Enter 2~8%Y of gross mass2O3Partially stabilized tetragonal phase ZrO2Al is made2O3- SiC complex phase ceramic sintered sample.
CN201811618700.1A 2018-12-28 2018-12-28 Al (aluminum)2O3Complex phase ceramic sintered sample and shape control method Expired - Fee Related CN109608173B (en)

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* Cited by examiner, † Cited by third party
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US4796127A (en) * 1986-04-23 1989-01-03 Sumitomo Special Metals Co., Ltd. Recording head slider
JPH04104944A (en) * 1990-08-21 1992-04-07 Nitsukatoo:Kk Al2o3-sic-zro2 composite sinter
JPH04243960A (en) * 1991-01-30 1992-09-01 Toray Ind Inc Composite ceramics
CN1986483A (en) * 2006-12-25 2007-06-27 西南科技大学 Nano-nano type Al2O3-base heterogeneous ceramic and its preparing method
CN102515720A (en) * 2011-12-08 2012-06-27 西安交通大学 Preparation method of transparent alumina ceramic
CN107417286A (en) * 2017-08-22 2017-12-01 东北大学 One kind enhancing Ultra-low carbon Al2O3‑ZrO2The preparation method of SiC C refractory materials
CN108358614A (en) * 2018-03-05 2018-08-03 段高峰 Creep resistant abrasion-proof stick and preparation method thereof

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* Cited by examiner, † Cited by third party
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JP4104944B2 (en) * 2002-09-18 2008-06-18 淳 小泉 Prediction method of displacement behavior of structures in underpinning
JP4243960B2 (en) * 2003-02-25 2009-03-25 ヤマハファインテック株式会社 Work sorting apparatus and sorting method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4796127A (en) * 1986-04-23 1989-01-03 Sumitomo Special Metals Co., Ltd. Recording head slider
JPH04104944A (en) * 1990-08-21 1992-04-07 Nitsukatoo:Kk Al2o3-sic-zro2 composite sinter
JPH04243960A (en) * 1991-01-30 1992-09-01 Toray Ind Inc Composite ceramics
CN1986483A (en) * 2006-12-25 2007-06-27 西南科技大学 Nano-nano type Al2O3-base heterogeneous ceramic and its preparing method
CN102515720A (en) * 2011-12-08 2012-06-27 西安交通大学 Preparation method of transparent alumina ceramic
CN107417286A (en) * 2017-08-22 2017-12-01 东北大学 One kind enhancing Ultra-low carbon Al2O3‑ZrO2The preparation method of SiC C refractory materials
CN108358614A (en) * 2018-03-05 2018-08-03 段高峰 Creep resistant abrasion-proof stick and preparation method thereof

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