CN107445613B - Preparation method for preparing ceramic matrix composite by vacuum pressure impregnation - Google Patents
Preparation method for preparing ceramic matrix composite by vacuum pressure impregnation Download PDFInfo
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- CN107445613B CN107445613B CN201710679902.6A CN201710679902A CN107445613B CN 107445613 B CN107445613 B CN 107445613B CN 201710679902 A CN201710679902 A CN 201710679902A CN 107445613 B CN107445613 B CN 107445613B
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- C04B35/48—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 zirconium or hafnium oxides, zirconates, zircon or hafnates
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Abstract
The invention relates to the field of ceramic composite processes, in particular to a preparation method for preparing a ceramic matrix composite material by vacuum pressurization impregnation. The method comprises the following steps: 1) carrying out dense forming on a ceramic matrix material and carrying out medium-temperature glue discharging treatment; 2) preparing the solid compound into impregnation liquid with good dispersion performance for later use; 3) putting the impregnation liquid and the ceramic substrate blank into a vacuum pressurization impregnation device for vacuum pressurization impregnation treatment; 4) obtaining the ceramic matrix composite material. Compared with the prior art, the prepared composite exists in the ceramic matrix material in a uniformly dispersed form; the composite and the ceramic substrate particles exist stably in an intrinsic elementary substance active size state; during the sintering of the composite body, the composite serves to improve the inherent defects of the ceramic substrate without interfering with the formation of the inherent crystal structure of the ceramic substrate.
Description
Technical Field
The invention relates to the field of ceramic composite processes, in particular to a preparation method for preparing a ceramic matrix composite material by vacuum pressurization impregnation.
Background
The traditional industrial manufacturing method based on the ceramic material is to obtain ceramic powder particles by a physical and chemical method, then to stack and compact the powder by a specific forming means, and to sinter the compact formed body at high temperature according to a specific sintering system to obtain the material. When a material is to be used to compound the ceramic matrix, the conventional composite method is usually selected from: adding the composite material in a special chemical process in the preparation process of the ceramic powder particles or in a special physical process in the process of compacting and molding the ceramic powder particles; while composites generally have characteristics that include the following three points: the composite exists in a ceramic matrix material in a uniform dispersion state; the composite and the ceramic substrate particles exist stably in an intrinsic elementary substance active size state; the composite should function to improve the inherent defects of the ceramic substrate without interfering with the formation of the inherent crystalline structure of the ceramic substrate during sintering of the composite into a finished product.
The prior traditional method can not simultaneously meet three characteristics of a qualified complex body in the single use process.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, designs a preparation method for preparing the ceramic matrix composite by using vacuum pressurization impregnation, combines the advantages of the traditional composite process method, can selectively control the composite structure, realizes large-scale industrial preparation, and ensures that the prepared composite body meets three qualified characteristics.
In order to achieve the purpose, the preparation method for preparing the ceramic matrix composite by using vacuum pressure impregnation is characterized by comprising the following steps:
1) pretreating a ceramic substrate blank: closely forming a ceramic substrate material to obtain a ceramic substrate forming blank, and performing medium-temperature glue discharging treatment on the forming blank to obtain a ceramic substrate blank for later use;
2) preparing a pre-treated composite material into an impregnation liquid: preparing the solid compound into impregnation liquid with good dispersion performance for later use;
3) vacuum pressure impregnation treatment of the ceramic substrate blank: putting the impregnation liquid and the ceramic substrate blank into a vacuum pressurization impregnation device, and performing vacuum pressurization impregnation treatment under the conditions that the impregnation pressure difference is 0-4kg/cm and the impregnation time is 0-4 hours;
4) obtaining the ceramic matrix composite material.
The temperature of the medium-temperature rubber discharge in the step 1 is 900 ℃.
The compacting and forming mode in the step 1 comprises any one of mould pressing, slurry pouring, 3D printing or tape casting.
The porosity of the ceramic substrate blank prepared in the step 1 is less than 60%, the size of the gap of the ceramic substrate blank is equivalent to the median particle size of the ceramic substrate, and the size of the gap of the ceramic substrate blank and the median particle size of the ceramic substrate are both larger than or equal to 300 nm.
In the step 2, each 100 parts of the impregnating solution comprises 1-10 parts of graphene, 0.5-5 parts of a dispersing agent and the balance of a solvent, and the preparation of the impregnating solution comprises the following steps: 1) taking graphene, and preparing the graphene into powder; 2) mixing graphene powder with a dispersing agent to obtain a mixture; 3) putting the mixed mixture into a ball mill, and grinding the mixture by adopting a mode of combining dry grinding and wet grinding; 4) putting the ground mixture into a solvent, and uniformly mixing under the conditions of a magnetic field, ultrasonic waves and stirring; 5) mixing to obtain the impregnation liquid.
The dispersant is one or more of dimethyl carbonate (DMC), N, N, N ', N' -tetramethyl ethylenediamine, methyl formate or acetonitrile; the solvent is one or more of absolute ethyl alcohol, diethyl ether or acetone.
The particle diameter of the ground graphene of the mixture is less than 250 nm.
The magnetic field intensity is 0.5-5T; the stirring mode is clockwise one minute and anticlockwise one minute, the stirring speed is 50-100r/min, and the stirring time is 0.5-2 h; the control mode of the ultrasonic wave is three seconds on and three seconds off, the frequency of the ultrasonic wave is 20-90KHz, the power of the ultrasonic wave is 1-5KW, and the temperature of the ultrasonic wave is 25 ℃.
Compared with the prior art, the composite prepared by the invention exists in the ceramic matrix material in a uniformly dispersed form; meanwhile, the compound and the ceramic substrate particles exist stably in an intrinsic elementary substance active size state; and the composite plays a role in improving the inherent defects of the ceramic substrate without interfering with the formation of the inherent crystal structure of the ceramic substrate in the process of sintering the composite into a material.
Detailed Description
Example (b):
pretreating a ceramic substrate blank: the 3Y-TZP engineering ceramic granulation powder is used for densely forming the ceramic matrix material by adopting a compression molding mode, and the medium-temperature degumming treatment is carried out on the densely formed ceramic matrix material at the temperature of 900 ℃ to obtain the zirconia ceramic blank.
At the moment, the zirconia ceramic blank can be measured, the density value of the zirconia ceramic blank needs to be larger than 3.04g/cm, the size of a gap of the blank is larger than 300nm, if the blank is qualified, the next step is continued, otherwise, the prepared zirconia ceramic blank is unqualified.
Preparing an impregnating solution, taking 5 parts of graphene, taking 2 parts of acetonitrile as a dispersing agent, and selecting acetone as a solvent. Uniformly mixing a small amount of dispersant acetonitrile and graphene, grinding by using a ball mill, firstly grinding by a dry method at the rotation speed of 30r/min for 30min, then adding the dispersant for wet grinding at the rotation speed of 80r/min for 60min at the temperature of 25 ℃ to obtain a suspension of the graphene and the dispersant, then adding the suspension into an acetone solvent, and carrying out ultrasonic treatment on the stirred solution at the magnetic field intensity of 2T for 20min in a stirring mode of clockwise one minute and anticlockwise one minute, wherein the ultrasonic frequency is 30 KHz, the power is 5KW, the ultrasonic time is 60min, the ultrasonic mode is on for 3s, off for 3s, and the temperature is 25 ℃ to obtain the impregnation liquid.
Carrying out vacuum pressurization dipping treatment on the zirconium oxide ceramic substrate blank, putting the dipping liquid and the zirconium oxide ceramic substrate blank into a vacuum pressurization dipping device, selecting to carry out all dipping treatments on the zirconium oxide substrate, setting the dipping pressure difference to be 0-4kg/cm, and carrying out the dipping treatment for 0-4 hours.
And obtaining the ceramic matrix composite after the completion. In addition, the internal gaps of the zirconium oxide ceramic matrix material after the dipping treatment are completely filled by the dipping liquid, and the suspension liquid dipped into the zirconium oxide ceramic matrix blank keeps the good dispersion state of the graphene, the concentration of the graphene is slightly increased but no agglomeration exists, and the graphene is uniformly dispersed in the zirconium oxide matrix material.
Claims (8)
1. A preparation method for preparing a ceramic matrix composite by using vacuum pressure impregnation is characterized by comprising the following steps:
1) pretreating a ceramic substrate blank: closely forming a ceramic substrate material to obtain a ceramic substrate forming blank, and performing medium-temperature glue discharging treatment on the forming blank to obtain a ceramic substrate blank for later use;
2) preparing a pre-treated composite material into an impregnation liquid: preparing the solid compound into impregnation liquid with good dispersion performance for later use;
3) vacuum pressure impregnation treatment of the ceramic substrate blank: putting the impregnation liquid and the ceramic substrate blank into a vacuum pressurization impregnation device, and performing vacuum pressurization impregnation treatment under the conditions that the impregnation pressure difference is 0-4kg/cm and the impregnation time is 0-4 hours;
4) obtaining the ceramic matrix composite;
in the ceramic matrix composite material obtained in the step 4, the composite exists in the ceramic matrix material in a uniform dispersion state; both the composite and ceramic substrate particles are stable in an intrinsic elemental active size state.
2. The method of claim 1, further comprising the step of: the temperature of the medium-temperature rubber discharge in the step 1 is 900 ℃.
3. The method of claim 1, further comprising the step of: the compacting and forming mode in the step 1 comprises any one of mould pressing, slurry pouring, 3D printing or tape casting.
4. The method of claim 1, further comprising the step of: the porosity of the ceramic substrate blank prepared in the step 1 is less than 60%, the size of the gap of the ceramic substrate blank is equivalent to the median particle size of the ceramic substrate, and the size of the gap of the ceramic substrate blank and the median particle size of the ceramic substrate are both larger than or equal to 300 nm.
5. The method for preparing ceramic matrix composite material by vacuum pressure impregnation according to claim 1, wherein the impregnation liquid in the step 2 comprises 1-10 parts of graphene per 100 parts, 0.5-5 parts of dispersant and the balance of solvent, and the preparation of the impregnation liquid comprises the following steps: 1) taking graphene, and preparing the graphene into powder; 2) mixing graphene powder with a dispersing agent to obtain a mixture; 3) putting the mixed mixture into a ball mill, and grinding the mixture by adopting a mode of combining dry grinding and wet grinding; 4) putting the ground mixture into a solvent, and uniformly mixing under the conditions of a magnetic field, ultrasonic waves and stirring; 5) mixing to obtain the impregnation liquid.
6. The method of claim 5, wherein the step of preparing the ceramic matrix composite material by vacuum pressure impregnation comprises: the dispersant is one or more of dimethyl carbonate (DMC), N, N, N ', N' -tetramethyl ethylenediamine, methyl formate or acetonitrile; the solvent is one or more of absolute ethyl alcohol, diethyl ether or acetone.
7. The method of claim 5, wherein the step of preparing the ceramic matrix composite material by vacuum pressure impregnation comprises: the particle diameter of the ground graphene of the mixture is less than 250 nm.
8. The method of claim 5, wherein the step of preparing the ceramic matrix composite material by vacuum pressure impregnation comprises: the magnetic field intensity is 0.5-5T; the stirring mode is clockwise one minute and anticlockwise one minute, the stirring speed is 50-100r/min, and the stirring time is 0.5-2 h; the control mode of the ultrasonic wave is three seconds on and three seconds off, the frequency of the ultrasonic wave is 20-90KHz, the power of the ultrasonic wave is 1-5KW, and the temperature of the ultrasonic wave is 25 ℃.
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| CN101462219B (en) * | 2009-01-16 | 2010-12-01 | 南开大学 | Method for repairing general-purpose crackle forming based on graphene |
| CN101613202A (en) * | 2009-07-21 | 2009-12-30 | 上海材料研究所 | Adopt glass encapsulating heat and other static pressuring processes to prepare the method for silicon nitride ceramic ball |
| CN101913648A (en) * | 2010-08-05 | 2010-12-15 | 昆明理工大学 | Method for preparing partially stable zirconium oxide by adopting microwave sintering of natural zirconium oxide |
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