CN115180968A - Novel fiber-toughened alumina ceramic and preparation method thereof - Google Patents
Novel fiber-toughened alumina ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of alumina ceramics and discloses a novel fiber-toughened alumina ceramic which comprises the following components in parts by weight: 70-90 parts of alpha-alumina, 20-30 parts of titanium dioxide, 20-30 parts of mullite fiber, 5-10 parts of dispersing agent, 3-7 parts of sintering aid, 2-5 parts of lubricant, 2-5 parts of plasticizer and 1-3 parts of binder. According to the invention, the mullite fiber is soaked and modified, so that the toughness of the mullite fiber is improved, and the modified mullite fiber is pre-laid to form an effective toughening whole, so that the toughness of the whole is greatly enhanced after the alumina ceramic is fired, and in the preparation process, a combined dispersing agent is adopted to further enhance the dispersing effect of alpha-alumina powder, so that the alpha-alumina powder can conveniently enter a mold, and the blank can be conveniently molded and fired through the matching of a lubricating agent and a bonding agent.
Description
Technical Field
The invention relates to the technical field of alumina ceramics, in particular to a novel fiber toughened alumina ceramic and a preparation method thereof.
Background
Alumina ceramics are ceramic materials based on alumina (Al 2O 3) and are used in thick film integrated circuits. The alumina ceramic has better conductivity, mechanical strength and high temperature resistance. It should be noted that washing with ultrasonic waves is required. Alumina ceramics are ceramics with wide application, and because of the superior performance, the alumina ceramics have wider and wider application in modern society and meet the requirements of daily use and special performance.
The Chinese patent network discloses a method for preparing carbon fiber toughened alumina ceramic material with application numbers of CN201710151598.8 and CN107586117A, and the method has good room temperature mechanical property, high densification degree of the material and greatly improved strength and toughness compared with pure alumina prepared by the same process. The method has good application prospect in the aspect of preparing ceramic dies, sand-spraying nozzles, cutters and other parts with higher requirements on wear resistance, in the method, 2.5D woven carbon fibers are adopted to enhance the toughness of the alumina ceramic, and the 2.5D woven carbon fibers are not pretreated and modified, so that the toughness is increased to a limited extent, chinese patent web also discloses a preparation method of fiber-toughened alumina ceramic, and the application number is as follows: 201910675470.0, published as: CN110330350A, the patent introduces carbon source into the alumina ceramic matrix after high temperature pyrolysis of cellulose nanofiber by atmosphere sintering, and synthesizes silicon carbide fiber in situ in the alumina ceramic by adding silicon source to obtain the silicon carbide fiber toughened alumina ceramic, which overcomes the problem that the finished fiber is easy to damage and break in the mixed material preparation process, and simplifies the production flow of composite materials, but the patent pre-mixes the cellulose nanofiber and the alumina matrix, and then carries out forming firing, the process easily causes the cellulose nanofiber not to form effective connection in the firing process, and the improvement degree of the toughness of the alumina ceramic is limited.
Disclosure of Invention
The invention aims to provide a novel fiber-toughened alumina ceramic and a preparation method thereof, which have the advantages that mullite fibers can be soaked and modified to improve the toughness of the mullite fibers, and the modified mullite fibers are pre-laid to form an effective toughened whole body, so that the toughness of the whole body is greatly enhanced after the alumina ceramic is fired, and the problems that the fibers are not modified and the whole body is not fired and formed in the preparation process of the conventional fiber-toughened alumina ceramic are solved.
In order to achieve the purpose, the invention provides the following technical scheme: the novel fiber-toughened alumina ceramic comprises the following components in parts by weight:
70-90 parts of alpha-alumina, 20-30 parts of titanium dioxide, 20-30 parts of mullite fiber, 5-10 parts of dispersing agent, 3-7 parts of sintering aid, 2-5 parts of lubricant, 2-5 parts of plasticizer and 1-3 parts of binder.
Preferably, the novel fiber-toughened alumina ceramic comprises the following components in parts by weight:
75-85 parts of alpha-alumina, 25-28 parts of titanium dioxide, 22-27 parts of mullite fiber, 7-9 parts of dispersing agent, 4-6 parts of sintering aid, 3-4 parts of lubricant, 3-4 parts of plasticizer and 2-3 parts of binder.
Preferably, caO, mgO and SiO are adopted as the dispersing agent 2 CaO accounts for 30-40% of the dispersant by weight, mgO accounts for 10-20% of the dispersant by weight, and SiO 2 Accounting for 40 to 50 percent of the weight of the dispersant.
Preferably, the binder is polyvinyl alcohol, and the binder is previously applied to the pressing mold.
A preparation method of novel fiber-toughened alumina ceramic comprises the following steps:
s1, premixing: mixing alpha-alumina powder with a dispersant, grinding by using a ball mill, sieving the alpha-alumina after grinding, and sieving with a sieve mesh number of 2000-2500;
s2, modification of mullite fiber: pretreating mullite fiber, soaking the mullite fiber in acetone for 2-5h, transferring the mullite fiber, and treating the mullite fiber with Zncl 2 Soaking the mixture in the solution for 3-5h;
s3, crushing mullite fibers: drying the mullite fiber in the S2, drying the mullite fiber for 20-30min at the hot air temperature of a dryer of 350-400 ℃, and crushing the mullite fiber after the mullite fiber is dried;
s4, preprocessing the blank before forming; laying the crushed mullite fiber in a mold, then mixing the alpha-alumina screened in the S1 with other ingredients, uniformly laying the alpha-alumina in the mold, and performing pre-sintering preparation;
s5, firing the blank body by adopting a vacuum hot pressing sintering process.
Preferably, in S1, a grinding aid, namely absolute ethanol, is added during grinding of the α -alumina powder and the dispersant.
Preferably, in S2, zncl is 2 The mass concentration of the substance is 0.5-0.8, and Zncl 2 The solution was saturated.
Preferably, in S3, the mullite fiber is pulverized by a magnetic pulverizer, and the particle size of the pulverized mullite fiber is 0.5 to 1 μm.
Preferably, in S4, the binder is applied to the mold in advance, and then the crushed mullite fiber is uniformly laid in the mold.
Preferably, in S5, the sintering temperature is 1700-1850 ℃ and the sintering pressure is 30-35MPa in the sintering process.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the mullite fiber is soaked and modified, so that the toughness of the mullite fiber is improved, and the modified mullite fiber is pre-laid to form an effective toughening whole, so that the toughness of the whole is greatly enhanced after the alumina ceramic is fired, and in the preparation process, a combined dispersing agent is adopted to further enhance the dispersion effect of alpha-alumina powder, facilitate the alpha-alumina powder to enter a mold, facilitate the molding and firing of a blank body through the matching of a lubricating agent and a binding agent, and solve the problems that the fiber is not modified and the whole is not fired and molded in the preparation process of the existing fiber toughening alumina ceramic.
Drawings
FIG. 1 is a schematic view of the preparation process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example one
A preparation method of novel fiber-toughened alumina ceramic comprises the following steps:
s1, premixing: mixing alpha-alumina powder with a dispersant, grinding by using a ball mill, sieving the alpha-alumina after grinding, and screening with 2500 meshes; and adding a grinding aid absolute ethyl alcohol in the process of grinding the alpha-alumina powder and the dispersing agent.
S2, modification of mullite fiber: pretreating mullite fiber, soaking the mullite fiber in acetone for 3h, transferring the mullite fiber, and using Zncl 2 Soaking the mixture in the solution for 4h; zncl 2 The mass concentration of the substance is 0.8, and Zncl 2 The solution was saturated.
S3, crushing mullite fibers: drying the mullite fiber in the S2 at the hot air temperature of 350 ℃ for 30min, and crushing the mullite fiber after the mullite fiber is dried; the mullite fiber is crushed by a magnetic crusher, and the particle size of the crushed mullite fiber is 0.5 mu m.
S4, preprocessing the blank before forming; laying the crushed mullite fiber in a mold, then mixing the alpha-alumina screened in the step S1 with other ingredients, and uniformly laying the mixture in the mold, wherein 75 parts of alpha-alumina, 25 parts of titanium dioxide, 22 parts of mullite fiber, 7 parts of a dispersing agent, 4 parts of a sintering aid, 3 parts of a lubricant, 3 parts of a plasticizer and 2 parts of a binder are subjected to pre-sintering preparation; the adhesive is coated in the die in advance, and then the crushed mullite fiber is uniformly laid in the die.
S5, firing the blank body, namely firing the blank body by adopting a vacuum hot pressing sintering process, wherein the sintering temperature is 1750 ℃ and the sintering pressure is 30MPa in the sintering process.
Example two
A preparation method of novel fiber-toughened alumina ceramic comprises the following steps:
s1, premixing: mixing alpha-alumina powder with a dispersant, grinding by using a ball mill, sieving the alpha-alumina after grinding, and screening with 2500 meshes; and adding a grinding aid absolute ethyl alcohol in the process of grinding the alpha-alumina powder and the dispersing agent.
S2, modification of mullite fiber: pretreating mullite fiber, soaking the mullite fiber in acetone for 3h, transferring the mullite fiber, and using Zncl 2 Soaking the mixture in the solution for 4h; zncl 2 The mass concentration of the substance is 0.8, and Zncl 2 The solution was saturated.
S3, crushing mullite fibers: drying the mullite fiber in the S2 at the hot air temperature of 350 ℃ for 30min, and crushing the mullite fiber after the mullite fiber is dried; the mullite fiber is pulverized by a magnetic pulverizer, and the particle size of the pulverized mullite fiber is 1 mu m.
S4, preprocessing the blank before forming; laying the crushed mullite fiber in a mold, then mixing the alpha-alumina screened in the step S1 with other ingredients, and uniformly laying the mixture in the mold, wherein 80 parts of alpha-alumina, 25 parts of titanium dioxide, 25 parts of mullite fiber, 8 parts of dispersing agent, 5 parts of sintering aid, 4 parts of lubricant, 4 parts of plasticizer and 2 parts of binder are subjected to pre-sintering preparation; the adhesive is coated in the die in advance, and then the crushed mullite fiber is uniformly laid in the die.
S5, firing the blank body by adopting a vacuum hot-pressing sintering process, wherein in the sintering process, the sintering temperature is 1800 ℃, and the sintering pressure is 35MPa.
EXAMPLE III
A preparation method of novel fiber-toughened alumina ceramic comprises the following steps:
s1, premixing: mixing alpha-alumina powder with a dispersant, grinding by using a ball mill, sieving the alpha-alumina after grinding, and screening with 2500 meshes; and adding a grinding aid absolute ethyl alcohol in the process of grinding the alpha-alumina powder and the dispersing agent.
S2, modification of mullite fiber: pretreating mullite fiber, soaking the mullite fiber in acetone for 3h, transferring the mullite fiber, and using Zncl 2 Soaking the mixture in the solution for 4h; zncl 2 The mass concentration of the substance is 0.8, and Zncl 2 The solution was saturated.
S3, crushing mullite fiber: drying the mullite fiber in the S2 at the hot air temperature of 350 ℃ for 30min, and crushing the mullite fiber after the mullite fiber is dried; the mullite fiber is pulverized by a magnetic pulverizer, and the particle size of the pulverized mullite fiber is 1 mu m.
S4, preprocessing the blank before forming; laying the crushed mullite fiber in a mold, then mixing the alpha-alumina screened in the step S1 with other ingredients, and uniformly laying the mixture in the mold, wherein 85 parts of alpha-alumina, 28 parts of titanium dioxide, 27 parts of mullite fiber, 9 parts of a dispersing agent, 6 parts of a sintering aid, 4 parts of a lubricant, 4 parts of a plasticizer and 3 parts of a binder are subjected to pre-firing preparation; the adhesive is coated in the die in advance, and then the crushed mullite fiber is uniformly laid in the die.
S5, firing the blank body by adopting a vacuum hot-pressing sintering process, wherein in the sintering process, the sintering temperature is 1850 ℃, and the sintering pressure is 35MPa.
Toughness test of alumina ceramics
Bending strength test method adopting GB/T4741-1999 ceramic material
Selecting 10 alumina ceramics prepared by the preparation method in the first to third embodiments, wherein the alumina ceramics have the length of 120mm and the width-thickness ratio of 1:1, and setting the alumina ceramics as group A;
selecting 10 alumina ceramics prepared by a conventional preparation method, wherein the alumina ceramics have the length of 120mm, the width-thickness ratio of 1:1 and are provided with a group B;
the flexural strength is calculated as follows:
б＝3FL÷2bh 2
in the formula: sigma bending strength, MPa;
f- -load at break of the specimen, N;
l-distance of supporting knife edge, mm;
b- -width at the sample fracture, mm;
h-the thickness of the sample at the fracture, mm.
The calculation results are as follows:
the toughness test of the alumina ceramic can obtain that:
(1) The alumina ceramics prepared in the examples can bear bending strength values of 700-800MPa in a bending strength test, and have obviously excellent bending resistance compared with the conventional alumina ceramics.
(2) The preparation method of the invention can obviously improve the bending strength of the alumina ceramic.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising a … …" does not exclude the presence of another identical element in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A novel fiber-toughened alumina ceramic is characterized in that: the novel fiber-toughened alumina ceramic comprises the following components in parts by weight:
70-90 parts of alpha-alumina, 20-30 parts of titanium dioxide, 20-30 parts of mullite fiber, 5-10 parts of dispersing agent, 3-7 parts of sintering aid, 2-5 parts of lubricant, 2-5 parts of plasticizer and 1-3 parts of binder.
2. The novel fiber-toughened alumina ceramic according to claim 1, wherein: the novel fiber-toughened alumina ceramic comprises the following components in parts by weight:
75-85 parts of alpha-alumina, 25-28 parts of titanium dioxide, 22-27 parts of mullite fiber, 7-9 parts of dispersing agent, 4-6 parts of sintering aid, 3-4 parts of lubricant, 3-4 parts of plasticizer and 2-3 parts of binder.
3. A novel fiber-toughened alumina ceramic according to any one of claims 1 to 2, wherein: the dispersing agent adopts CaO, mgO and SiO 2 CaO accounts for 30-40% of the dispersant by weight, mgO accounts for 10-20% of the dispersant by weight, and SiO 2 Accounting for 40 to 50 percent of the weight of the dispersant.
4. A novel fiber-toughened alumina ceramic according to any one of claims 1 to 2, wherein: the binder is polyvinyl alcohol, and the binder is coated in a pressing die in advance.
5. A preparation method of novel fiber-toughened alumina ceramic is characterized by comprising the following steps: the preparation method comprises the following steps:
s1, premixing: mixing alpha-alumina powder with a dispersant, grinding by using a ball mill, sieving the alpha-alumina after grinding, and sieving with a sieve mesh number of 2000-2500;
s2, modification of mullite fiber: pretreating mullite fiber, soaking the mullite fiber in acetone for 2-5h, transferring the mullite fiber, and treating the mullite fiber with Zncl 2 Soaking the mixture in the solution for 3-5h;
s3, crushing mullite fibers: drying the mullite fiber in the S2, drying the mullite fiber for 20-30min at the hot air temperature of a dryer of 350-400 ℃, and crushing the mullite fiber after the mullite fiber is dried;
s4, pre-treating the blank before forming; laying the crushed mullite fiber in a mold, then mixing the alpha-alumina screened in the S1 with other ingredients, uniformly laying the alpha-alumina in the mold, and performing pre-sintering preparation;
s5, firing the blank body by adopting a vacuum hot-pressing sintering process.
6. The preparation method of the novel fiber-toughened alumina ceramic according to claim 1, wherein: in the S1, a grinding aid, namely absolute ethyl alcohol, is added in the process of grinding the alpha-alumina powder and the dispersing agent.
7. The preparation method of the novel fiber-toughened alumina ceramic according to claim 1, wherein: in the S2, zncl 2 The mass concentration of the substance is 0.5-0.8, and Zncl 2 The solution was saturated.
8. The preparation method of the novel fiber-toughened alumina ceramic according to claim 1, wherein: in S3, the mullite fiber is crushed by a magnetic crusher, and the particle size of the crushed mullite fiber is 0.5-1 μm.
9. The preparation method of the novel fiber-toughened alumina ceramic according to claim 1, wherein: in the step S4, the binder is coated in the mold in advance, and then the crushed mullite fiber is uniformly laid in the mold.
10. The preparation method of the novel fiber-toughened alumina ceramic according to claim 1, wherein: in the S5, in the sintering process, the sintering temperature is 1700-1850 ℃, and the sintering pressure is 30-35MPa.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884189A (en) * | 2006-06-21 | 2006-12-27 | 济南大学 | Fiber reinforced alumina ceramic-base composites and method for preparing same |
| US20140148543A1 (en) * | 2012-11-29 | 2014-05-29 | General Electric Company | Methods of making a composite sheet and composite component and a composite |
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