CN112743925A - Impact-resistant ceramic material and preparation method and application thereof - Google Patents

Impact-resistant ceramic material and preparation method and application thereof Download PDF

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CN112743925A
CN112743925A CN202011583295.1A CN202011583295A CN112743925A CN 112743925 A CN112743925 A CN 112743925A CN 202011583295 A CN202011583295 A CN 202011583295A CN 112743925 A CN112743925 A CN 112743925A
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layer
impact
oxide
ceramic material
metal
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CN112743925B (en
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王维占
赵太勇
印力魁
付建平
任凯
王保国
陈智刚
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North University of China
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Abstract

The invention relates to the technical field of ceramic materials, in particular to an impact-resistant ceramic material and a preparation method and application thereof, wherein the impact-resistant ceramic material comprises a ceramic layer, a connecting layer and a metal rubber layer, and the ceramic layer is prepared from the following raw materials in percentage by weight: 50-57% of aluminum oxide, 25-30% of zirconia fiber, 8-14% of carbon oxide fiber, 1-3% of sintering aid and 5-8% of rare refractory metal oxide, wherein the sum of the weight percentages of the raw materials is 100%, the connecting layer is a metal layer, and the metal layer is an Nd metal layer or an Mo metal layer; the mass ratio of the ceramic layer to the connecting layer to the metal rubber layer is 1:0.2-0.5: 0.5-0.8. The ceramic layer and the metal rubber layer are connected through the connecting layer to form the composite material, and the mechanical property and the impact resistance of the alumina ceramic are effectively improved under the combined action of the ceramic layer, the connecting layer and the metal rubber layer.

Description

Impact-resistant ceramic material and preparation method and application thereof
Technical Field
The invention relates to the technical field of ceramic materials, in particular to an impact-resistant ceramic material and a preparation method and application thereof.
Background
The impact dynamics is to research the fluctuation generated by the short-time rapid change of a material or a structure under the action of impact load and to enable a solid material to generate the rules of movement, deformation and damage; impact loading refers to a load in which the external load changes rapidly with time, and when a local position of an object is impacted, the disturbance gradually propagates to an undisturbed region.
The metal rubber is a homogeneous elastic porous substance, and is formed by orderly arranging a certain mass of stretched and spiral metal wires in a stamping (or rolling) die and then using a cold stamping method; its raw material is metal wire, which has both the inherent characteristics of the selected metal and the elasticity similar to rubber.
The alumina ceramic has high strength, high hardness and good oxidation resistance and chemical stability, is engineering ceramic with wide application, but the alumina-based ceramic material is combined by ionic bonds and covalent bonds, has high dislocation barrier and large material brittleness, is difficult to bear violent impact, and then influences the wide application of the alumina-based ceramic material; in the prior art, the impact resistance of alumina is often improved by adding a zirconia material into the alumina, the alumina and the zirconia ceramic both have high temperature resistance and high biocompatibility, and the application range of the other oxide cannot be influenced by the application defect of one oxide when the alumina and the zirconia are compounded, so that the zirconia is used as a toughening phase to toughen the substrate alumina, but the phenomena of abnormal growth of alumina grains and crystal crossing and cracking of zirconia grains often occur in the compounding process of the alumina and the zirconia, the technical defect of poor reliability is caused by the uneven internal microstructure of the alumina, and the application of the zirconia ceramic in the preparation of structural ceramics, electronic ceramics and biological ceramic materials is further influenced.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide an impact-resistant ceramic material and a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the impact-resistant ceramic material comprises a ceramic layer, a connecting layer and a metal rubber layer, wherein the ceramic layer is prepared from the following raw materials in percentage by weight: 50-57% of alumina, 25-30% of zirconia fiber, 8-14% of carbon oxide fiber, 1-3% of sintering aid and 5-8% of rare refractory metal oxide, wherein the sum of the weight percentages of the raw materials is 100%;
the connecting layer is a metal layer, and the metal layer is an Nd metal layer or an Mo metal layer;
the mass ratio of the ceramic layer, the connecting layer and the metal rubber layer is 1:0.2-0.5: 0.5-0.8.
Preferably, the metal rubber layer is made of steel wires with the diameter of 0.05-0.1mmCold stampingThe metal rubber prepared by the method.
Preferably, the sintering aid is MnO2-TiO2-a MgO sintering aid.
Preferably, the rare refractory metal oxide is titanium dioxide, oxideZirconiumHafnium oxide, vanadium oxide, niobium oxide, tantalum oxide, molybdenum oxide, or tungsten oxide.
Preferably, the zirconia fibers and the oxidized carbon fibers are each less than 150 μm in length.
Preferably, the oxidized carbon fiber is prepared by the following steps:
(1) soaking the carbon fiber in an acetone solution for 20-28h, taking out, ultrasonically eluting with deionized water, and drying to constant weight to obtain the degumming carbon fiber;
(2) and (2) soaking the degumming carbon fiber obtained in the step (1) in a hydrogen peroxide solution at the temperature of 40-60 ℃ for 1.5-2h, ultrasonically eluting with deionized water, and then drying to constant weight to obtain the oxidized carbon fiber.
The invention also protects an impact-resistant ceramic material, wherein the ceramic layer is prepared by the following method:
(1) weighing: weighing the following raw materials in parts by weight: 50-57% of alumina, 25-30% of zirconia fiber, 8-14% of carbon oxide fiber, 1-3% of sintering aid and 5-8% of rare refractory metal oxide, wherein the sum of the weight percentages of the raw materials is 100% for later use;
(2) preparing a ceramic layer:
s1, uniformly mixing alumina, a sintering aid and a rare refractory metal oxide, ball-milling until the particle size reaches the micron level, and adding zirconia fibers and carbon oxide fibers to obtain a premix;
s2, pre-pressing and molding the premix of S1;
s3, placing the pre-pressed and molded premix into a vacuum hot-pressing sintering furnace for sintering, heating to 1000-1200 ℃ at the heating rate of 5 ℃/min, then preserving heat for 0.5-1h, heating to 1300-1500 ℃ at the heating rate of 2-4 ℃/min, then preserving heat for 1.5-2h, and obtaining the ceramic layer.
The invention also provides a preparation method of the impact-resistant ceramic material, which comprises the following steps:
(1) weighing: weighing the ceramic layer, the connecting layer and the metal rubber layer according to the mass ratio of 1:0.2-0.5: 0.5-0.8;
(2) preparing an impact-resistant ceramic material:
the ceramic layer, the connecting layer and the metal rubber layer are sequentially overlapped together and are jointed for 1.5 to 2 hours at the temperature of 1000-1400 ℃ under the vacuum condition, so as to prepare the impact-resistant ceramic material.
Preferably, the vacuum degree of the vacuum condition in the step (2) is 10-5-10-4Pa。
The invention also protects the application of the impact-resistant ceramic material in the preparation of structural ceramics, electronic ceramics and biological ceramic materials.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention comprises a ceramic layer, a connecting layer and a metal rubber layer, wherein the ceramic layer takes alumina as a base phase, zirconia fiber and carbon oxide fiber as reinforcing materials, MnO is added2-TiO2-MgO as sintering aid, rare refractory metal oxide as flux; the surface oxidation treatment of the carbon fiber can improve the interface condition of the fiber reinforced composite material and the mechanical property of the carbon fiber, and when the carbon oxide fiber and the zirconia fiber are wound and sintered, the mutual action enhances the common mechanical property and the thermal barrier ablation property of the carbon oxide fiber reinforced zirconia fiber; MnO2Can promote sintering, and MgO plays a role of a microstructure stabilizer, and overcomes the defect that alumina grains grow abnormally in MnO2And under the condition of certain MgO content, adding a small amount of TiO2The alumina can be sintered to obtain good mechanical property; the addition of the rare refractory metal oxide effectively improves the mechanical property of the ceramic layer, and the ceramic layer with excellent mechanical and impact resistance is prepared.
2. The invention also comprises a connecting layer and a metal rubber layer, wherein the connecting layer is a metal layer of Nd or Mo, the metal layer is connected with the ceramic layer under the action of the metal layer, and then the impact resistance of the ceramic layer is improved, and the metal rubber layer is selected for the reason that: the thermal expansion coefficients of the zirconium oxide fiber and the steel wire are close, so that the binding force of the zirconium oxide fiber and the steel wire is strong when the zirconium oxide fiber and the steel wire are compounded, and a stable structure is formed.
Detailed Description
Specific embodiments of the present invention are described in detail below with reference to tables 1-2, but it should be understood that the scope of the present invention is not limited to the specific embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. The raw materials used in the invention are not indicated by manufacturers, and are all conventional products which can be obtained by commercial purchase.
Example 1
A preparation method of an impact-resistant ceramic material comprises the steps of preparing a ceramic layer, preparing oxidized carbon fibers and preparing the impact-resistant ceramic material;
the preparation of the ceramic layer comprises the following steps:
(1) weighing: weighing the following raw materials in parts by weight: 50% of alumina, 30% of zirconia fiber, 10% of carbon oxide fiber, 2% of sintering aid and 8% of rare refractory metal oxide for later use;
(2) preparing a ceramic layer:
s1, uniformly mixing alumina, a sintering aid and a rare refractory metal oxide, ball-milling until the particle size reaches the micron level, and adding zirconia fibers and carbon oxide fibers to obtain a premix;
s2, performing compression molding on the premix S1 under 20MPa, then performing compression molding again under 200MPa by using cold isostatic pressure to increase densification, and performing pre-compression molding;
s3, placing the pre-pressed and molded premix into a vacuum hot-pressing sintering furnace for sintering, heating to 1000 ℃ at a heating rate of 5 ℃/min, then preserving heat for 1h, heating to 1500 ℃ at a heating rate of 4 ℃/min, and then preserving heat for 1.5h to obtain a ceramic layer;
the preparation of the oxidized carbon fiber comprises the following steps:
(1) soaking the carbon fiber in an acetone solution for 20 hours, then taking out, ultrasonically eluting with deionized water, and then drying to constant weight to obtain the degumming carbon fiber;
(2) soaking the degumming carbon fiber obtained in the step (1) in a hydrogen peroxide solution at 60 ℃ for 1.5h, ultrasonically eluting with deionized water, and then drying to constant weight to obtain oxidized carbon fiber;
the preparation of the impact-resistant ceramic material comprises the following steps:
(1) weighing: weighing a ceramic layer, a connecting layer and a metal rubber layer according to the mass ratio of 1:0.2: 0.8;
(2) preparing an impact-resistant ceramic material:
sequentially superposing the ceramic layer, the connecting layer and the metal rubber layer together at a vacuum degree of 10-5And (3) bonding for 2h at 1000 ℃ under the vacuum condition of Pa to prepare the impact-resistant ceramic material.
Example 2
A preparation method of an impact-resistant ceramic material comprises the steps of preparing a ceramic layer, preparing oxidized carbon fibers and preparing the impact-resistant ceramic material;
the preparation of the ceramic layer comprises the following steps:
(1) weighing: weighing the following raw materials in parts by weight: 51% of alumina, 27% of zirconia fiber, 14% of carbon oxide fiber, 3% of sintering aid and 5% of rare refractory metal oxide for later use;
(2) preparing a ceramic layer:
s1, uniformly mixing alumina, a sintering aid and a rare refractory metal oxide, ball-milling until the particle size reaches the micron level, and adding zirconia fibers and carbon oxide fibers to obtain a premix;
s2, performing compression molding on the premix S1 under 20MPa, then performing compression molding again under 200MPa by using cold isostatic pressure to increase densification, and performing pre-compression molding;
s3, placing the pre-pressed and molded premix into a vacuum hot-pressing sintering furnace for sintering, heating to 1150 ℃ at a heating rate of 5 ℃/min, then preserving heat for 45min, heating to 1400 ℃ at a heating rate of 3 ℃/min, and then preserving heat for 1.5h to obtain a ceramic layer;
the preparation of the oxidized carbon fiber comprises the following steps:
(1) soaking the carbon fiber in an acetone solution for 24 hours, then taking out, ultrasonically eluting with deionized water, and then drying to constant weight to obtain the degumming carbon fiber;
(2) soaking the degumming carbon fiber obtained in the step (1) in a hydrogen peroxide solution at 50 ℃ for 2h, ultrasonically eluting with deionized water, and then drying to constant weight to obtain oxidized carbon fiber;
the preparation of the impact-resistant ceramic material comprises the following steps:
(1) weighing: weighing a ceramic layer, a connecting layer and a metal rubber layer according to the mass ratio of 1:0.3: 0.7;
(2) preparing an impact-resistant ceramic material:
sequentially stacking a ceramic layer, a connecting layer and a metal rubber layer together under a vacuum degree of 5 multiplied by 10-5And bonding the ceramic materials at 1250 ℃ for 2h under the vacuum condition of Pa to prepare the impact-resistant ceramic material.
Example 3
A preparation method of an impact-resistant ceramic material comprises the steps of preparing a ceramic layer, preparing oxidized carbon fibers and preparing the impact-resistant ceramic material;
the preparation of the ceramic layer comprises the following steps:
(1) weighing: weighing the following raw materials in parts by weight: 57% of aluminum oxide, 25% of zirconia fiber, 11% of carbon oxide fiber, 1% of sintering aid and 6% of rare refractory metal oxide for later use;
(2) preparing a ceramic layer:
s1, uniformly mixing alumina, a sintering aid and a rare refractory metal oxide, ball-milling until the particle size reaches the micron level, and adding zirconia fibers and carbon oxide fibers to obtain a premix;
s2, performing compression molding on the premix S1 under 20MPa, then performing compression molding again under 200MPa by using cold isostatic pressure to increase densification, and performing pre-compression molding;
s3, placing the pre-pressed and molded premix into a vacuum hot-pressing sintering furnace for sintering, heating to 1200 ℃ at a heating rate of 5 ℃/min, then preserving heat for 0.5h, heating to 1300 ℃ at a heating rate of 2 ℃/min, and then preserving heat for 2h to obtain a ceramic layer;
the preparation of the oxidized carbon fiber comprises the following steps:
(1) soaking the carbon fiber in an acetone solution for 28 hours, then taking out, ultrasonically eluting with deionized water, and then drying to constant weight to obtain the degumming carbon fiber;
(2) soaking the degumming carbon fiber obtained in the step (1) in a hydrogen peroxide solution at 40 ℃ for 2h, ultrasonically eluting with deionized water, and then drying to constant weight to obtain oxidized carbon fiber;
the preparation of the impact-resistant ceramic material comprises the following steps:
(1) weighing: weighing a ceramic layer, a connecting layer and a metal rubber layer according to the mass ratio of 1:0.5: 0.5;
(2) preparing an impact-resistant ceramic material:
sequentially superposing the ceramic layer, the connecting layer and the metal rubber layer together at a vacuum degree of 10-4And (3) bonding for 1.5h at 1400 ℃ under the vacuum condition of Pa to prepare the impact-resistant ceramic material.
Comparative example 1
The same procedure as in example 2 was followed except that the weighed raw materials contained only alumina, zirconia fibers and a sintering aid in a mass ratio of alumina to zirconia fibers to the sintering aid of 51:27:3 to prepare a ceramic layer material.
Comparative example 2
The same procedure as in example 2 was followed except that the weighed raw materials contained only alumina, zirconia fibers and a sintering aid, and the mass ratio of the alumina to the zirconia fibers to the sintering aid was 51:27: 3.
Comparative example 3
Ceramic layer material obtained in example 2.
The ceramic materials with excellent impact resistance and mechanical property are prepared in the examples 1 to 3 of the invention, and the properties are similar, the following ceramic material prepared in the example 2 is taken as an example for research, and compared with the comparative examples 1 to 3, the specific research method and results are as follows:
according to the results of the alumina ceramic impact compression damage and the research of the strength test, the volume density, the porosity, the bending strength, the fracture toughness and the hardness of the material prepared by the method are determined, and the specific test results are as follows:
measurement of bulk Density and porosity
When the volume of a material is a real volume (no pores inside the material), it is called true density. The volume density and the open porosity of the sample are measured according to the following steps:
(1) the samples of example 2 and comparative examples 1 to 3 were cleaned in ultrasound, dried in an oven to constant weight, and weighed on an electronic balance Go；
(2) Putting the weighed sample into vacuum for 15min, then putting the sample into water for soaking, and then continuously treating the sample in vacuum for 30 min;
(3) weight G of test specimen suspended in Water2(ii) a Taking out the sample, wiping the surface of the sample, and weighing the wet weight G of the sample strip1；
The bulk density of the sample was: d ═ Gor/(G1-G2) R is the true density of water
The open porosity is: p ═ G1-G0)/(G1-G2)。
Test of bending Strength
The bending strength refers to the capability of the material to resist bending without breaking, a sample is processed into a shape of 3mm multiplied by 4mm multiplied by 50mm, the surface of a sintered body is ground and polished, the sample is placed on two supporting points, then a certain load is applied to the middle position of the sample under the condition that the pressing speed of a pressure head is 0.5mm/min, and the load strength is continuously increased until the unit area load value of the sample when the sample breaks.
Test for fracture toughness
The fracture toughness is an index for measuring the property of the material for preventing the material from generating the instability propagation of the macrocrack, is also a parameter for resisting the material from generating the brittle failure, is an inherent property of the material, and adopts the SENB method in the fracture toughness test of the invention, the size of a sample is 2.5 multiplied by 5 multiplied by 25mm, the depth of a middle crack is 2.5mm, and the width is less than 0.2 mm.
Hardness test
The hardness test adopts an HX-1000 type microhardness tester.
TABLE 1 mechanical Properties study
Figure BDA0002865670430000141
Figure BDA0002865670430000151
The result shows that the material prepared in the embodiment 2 of the invention has excellent mechanical property, and compared with the comparative example 3, the impact resistance and the mechanical property of the material are effectively improved by the combination of the connecting layer and the metal layer; compared with the prior art alumina-zirconia composite material of the comparative example 1, the hardness, the fracture toughness and the bending strength of the composite material of the embodiment 2 are greatly improved, which shows that the material prepared by the preparation method of the invention achieves unexpected technical effects on the basis of the prior art; example 2 compared with comparative example 2, the ceramic material prepared by the invention has more excellent mechanical property and impact resistance compared with the alumina-zirconia composite material in the prior art, and can be applied to the preparation of structural ceramics, electronic ceramics and biological ceramic materials.
TABLE 2 bulk Density and porosity
Figure BDA0002865670430000152
Figure BDA0002865670430000161
The result shows that the density and the porosity of the impact-resistant ceramic material prepared in the embodiment 2 of the invention conform to the performances of structural ceramics, electronic ceramics and biological ceramics, and the mechanical properties are excellent, particularly the porosity and the volume density are both low, and the impact resistance is excellent because a compact microstructure is formed.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (10)

1. The impact-resistant ceramic material is characterized by comprising a ceramic layer, a connecting layer and a metal rubber layer, wherein the ceramic layer is prepared from the following raw materials in percentage by weight: 50-57% of alumina, 25-30% of zirconia fiber, 8-14% of carbon oxide fiber, 1-3% of sintering aid and 5-8% of rare refractory metal oxide, wherein the sum of the weight percentages of the raw materials is 100%;
the connecting layer is a metal layer, and the metal layer is an Nd metal layer or an Mo metal layer;
the mass ratio of the ceramic layer, the connecting layer and the metal rubber layer is 1:0.2-0.5: 0.5-0.8.
2. The impact-resistant ceramic material as claimed in claim 1, wherein said metal rubber layer is made of steel wire with a diameter of 0.05-0.1mmCold stampingThe metal rubber prepared by the method.
3. The impact-resistant ceramic material of claim 1 wherein the sintering aid is MnO2-TiO2-a MgO sintering aid.
4. The impact-resistant ceramic material of claim 1 wherein said rare refractory metal oxide is titanium dioxide, oxidizedZirconiumHafnium oxide, vanadium oxide, niobium oxide, tantalum oxide, molybdenum oxide, or tungsten oxide.
5. An impact resistant ceramic material according to claim 1 wherein the zirconia fibres and the carbon oxide fibres are each less than 150 μm in length.
6. An impact-resistant ceramic material according to claim 1, wherein said oxidized carbon fibers are prepared by the steps of:
(1) soaking the carbon fiber in an acetone solution for 20-28h, taking out, ultrasonically eluting with deionized water, and drying to constant weight to obtain the degumming carbon fiber;
(2) and (2) soaking the degumming carbon fiber obtained in the step (1) in a hydrogen peroxide solution at the temperature of 40-60 ℃ for 1.5-2h, ultrasonically eluting with deionized water, and then drying to constant weight to obtain the oxidized carbon fiber.
7. An impact resistant ceramic material according to any one of claims 1-6, wherein the ceramic layer is prepared according to the following method:
(1) weighing: weighing the following raw materials in parts by weight: 50-57% of alumina, 25-30% of zirconia fiber, 8-14% of carbon oxide fiber, 1-3% of sintering aid and 5-8% of rare refractory metal oxide, wherein the sum of the weight percentages of the raw materials is 100% for later use;
(2) preparing a ceramic layer:
s1, uniformly mixing alumina, a sintering aid and a rare refractory metal oxide, ball-milling until the particle size reaches the micron level, and adding zirconia fibers and carbon oxide fibers to obtain a premix;
s2, pre-pressing and molding the premix of S1;
s3, placing the pre-pressed and molded premix into a vacuum hot-pressing sintering furnace for sintering, heating to 1000-1200 ℃ at the heating rate of 5 ℃/min, then preserving heat for 0.5-1h, heating to 1300-1500 ℃ at the heating rate of 2-4 ℃/min, then preserving heat for 1.5-2h, and obtaining the ceramic layer.
8. The method for preparing an impact-resistant ceramic material according to claim 7, comprising the steps of:
(1) weighing: weighing the ceramic layer, the connecting layer and the metal rubber layer according to the mass ratio of 1:0.2-0.5: 0.5-0.8;
(2) preparing an impact-resistant ceramic material:
the ceramic layer, the connecting layer and the metal rubber layer are sequentially overlapped together and are jointed for 1.5 to 2 hours at the temperature of 1000-1400 ℃ under the vacuum condition, so as to prepare the impact-resistant ceramic material.
9. The method for preparing an impact-resistant ceramic material as claimed in claim 8, wherein the vacuum degree of the vacuum condition in step (2) is 10-5-10-4Pa。
10. Use of an impact-resistant ceramic material according to claim 1 for the preparation of structural, electronic and biological ceramic materials.
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Publication number Priority date Publication date Assignee Title
CN104862634A (en) * 2015-04-30 2015-08-26 苏州统明机械有限公司 Impact-resistant ceramic coating layer for metal-based thermal spraying and spraying method thereof
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CN109161042A (en) * 2018-08-14 2019-01-08 安徽微威胶件集团有限公司 A kind of high-elastic durable automobile rubber shock absorber part material
CN109574638A (en) * 2018-12-29 2019-04-05 山东天汇研磨耐磨技术开发有限公司 A kind of high-bond ceramics section and its manufacturing method applying metal-rubber
CN211254870U (en) * 2019-10-23 2020-08-14 苏才炼 Rubber mat for elevator

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104862634A (en) * 2015-04-30 2015-08-26 苏州统明机械有限公司 Impact-resistant ceramic coating layer for metal-based thermal spraying and spraying method thereof
CN107379672A (en) * 2017-07-24 2017-11-24 苏州宏久航空防热材料科技有限公司 A kind of resistant to elevated temperatures multi-layer ceramics cotton plate
CN109161042A (en) * 2018-08-14 2019-01-08 安徽微威胶件集团有限公司 A kind of high-elastic durable automobile rubber shock absorber part material
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