CN113880592B - Preparation process of high-hardness high-toughness silicon nitride ceramic complex structural member - Google Patents
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Abstract
The invention discloses a preparation process of a high-hardness high-toughness silicon nitride ceramic complex structural member, which relates to the technical field of preparation processes of silicon nitride ceramic materials and comprises the following steps: step one, preparing silicon nitride composite powder; secondly, carrying out cold isostatic pressing treatment on the silicon nitride composite powder to obtain a silicon nitride ceramic blank; thirdly, cutting the silicon nitride ceramic blank to obtain a silicon nitride ceramic complex structural member blank; fourthly, pre-sintering the silicon nitride ceramic complex structural member blank at low temperature and low pressure; and step five, sintering at high temperature and high pressure. The silicon nitride ceramic complex structural member with high surface hardness and good internal toughness can be obtained by adopting the method, the problem that the high hardness and high toughness of the silicon nitride ceramic structural member cannot be considered in the prior art can be effectively solved, the wear resistance requirement of the silicon nitride ceramic member can be met, the breakage resistance of the structural member can be improved, and the method has great application potential in the fields of wear-resistant structural members, ceramic cutters and the like.
Description
Technical Field
The invention relates to the technical field of preparation processes of silicon nitride ceramic materials, in particular to a preparation process of a high-hardness and high-toughness silicon nitride ceramic complex structural member.
Background
The silicon nitride ceramic has excellent fracture toughness and bending strength, and is successfully applied to wear-resistant structural parts with complex structures, such as high-precision bearing balls, high-speed impellers, ceramic pistons and the like. Atmosphere sintering is a commonly used preparation process for ceramic materials, high-pressure nitrogen is usually adopted as protective gas, densification and batch production of ceramics with complex structures can be realized, and the method is widely applied to preparation of silicon nitride ceramic complex structural parts.
For silicon nitride ceramic materials, the crystal structure typically comprises equiaxed α -Si3N4And hexagonal beta-Si3N4Wherein alpha-Si3N4Can improve the hardness of silicon nitride material and has beta-Si with bimodal distribution3N4The fracture toughness of the silicon nitride material can be improved. beta-Si3N4Is a high-temperature stable phase of silicon nitride, and can generate alpha-Si at the temperature of more than 1400 DEG C3N4To beta-Si3N4Is performed. Therefore, by adjusting the content of the sintering aid, adjusting the sintering temperature, etc., the α -Si can be adjusted3N4With beta-Si3N4The content ratio of the silicon nitride ceramic material to realize the adjustment of the hardness and the fracture toughness of the silicon nitride ceramic material.
Although the performance of the silicon nitride ceramic can be regulated by adjusting the material composition and the sintering temperature, the alpha-Si content is high3N4Or high content of beta-Si3N4The material can not give consideration to both high hardness and high toughness. The gradient composite ceramic and the micro-laminated ceramic material can realize gradient distribution of performance, but are mainly applied to hot press forming of ceramic cutters and other structures with regular shapes at present, and cannot meet the forming of silicon nitride ceramic complex structural parts.
Disclosure of Invention
The invention aims to provide a preparation process of a high-hardness and high-toughness silicon nitride ceramic complex structural member, which solves the problem of performance regulation of the silicon nitride complex structural member, thereby ensuring that the ceramic member has stable and reliable performance indexes so as to meet the service requirement.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a preparation process of a high-hardness and high-toughness silicon nitride ceramic complex structural member, which comprises the following steps of:
step one, preparing silicon nitride composite powder;
secondly, carrying out cold isostatic pressing treatment on the silicon nitride composite powder to obtain a silicon nitride ceramic blank;
thirdly, cutting the silicon nitride ceramic blank to obtain a silicon nitride ceramic complex structural member blank;
fourthly, pre-sintering the silicon nitride ceramic complex structural member blank at low temperature and low pressure;
and fifthly, sintering at high temperature and high pressure to obtain the silicon nitride ceramic complex structural part with high surface hardness and high core toughness.
Preferably, in the first step, silicon nitride and an oxide sintering aid are uniformly mixed in an alcohol medium to obtain the silicon nitride composite powder, wherein the ratio of the silicon nitride to the oxide sintering aid is 90: 10.
preferably, the oxide sintering aid comprises yttrium oxide and aluminum oxide, and the ratio of yttrium oxide to aluminum oxide is 8.5: 1.5.
preferably, in the first step, after the silicon nitride composite powder is obtained, the silicon nitride composite powder is dried and vacuum-packaged.
Preferably, in the second step, the cold isostatic pressing treatment is performed under a pressure of 100 to 200 MPa.
Preferably, in the fourth step, the low-temperature low-pressure pre-sintering is performed in a nitrogen atmosphere, the temperature of the low-temperature low-pressure pre-sintering is 1100 ℃, the pressure of the low-temperature low-pressure pre-sintering is 1-1.5 MPa, and the heat preservation time of the low-temperature low-pressure pre-sintering is 0.5-1.5 hours.
Preferably, in the fourth step, the depth of the surface hardness influence layer of the silicon nitride ceramic complex structural member blank is regulated and controlled by adjusting the heat preservation time, and the longer the heat preservation time is, the greater the depth of the surface hardness influence layer of the silicon nitride ceramic complex structural member blank is.
Preferably, in the fourth step, after the low-temperature low-pressure pre-sintering, the silicon nitride ceramic complex structural member blank needs to be cooled to room temperature.
Preferably, in the fifth step, the high-temperature high-pressure sintering is performed in a nitrogen atmosphere, the temperature of the high-temperature high-pressure sintering is 1850-1950 ℃, and the pressure of the high-temperature high-pressure sintering is 5-10 MPa.
Preferably, the relative density of the obtained silicon nitride ceramic complex structural part with high surface hardness and high core toughness is higher than 99.9 percent, the hardness of the surface layer is 17-20 GPa within 1mm, the core hardness is 14-17 GPa, and the fracture toughness is 9-12 MPa.m1/2。
Compared with the prior art, the invention has the following technical effects:
the preparation process of the high-hardness and high-toughness silicon nitride ceramic complex structural member can obtain the silicon nitride ceramic complex structural member with high surface hardness and good internal toughness, can effectively solve the problem that the high-hardness and high-toughness characteristics of the silicon nitride ceramic structural member cannot be considered in the prior art, can meet the requirement of the wear resistance of the silicon nitride ceramic member, can improve the breakage resistance of the structural member, and has great application potential in the fields of wear-resistant structural members, ceramic cutters and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a process diagram for preparing a high-hardness and high-toughness silicon nitride ceramic complex structural member according to 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 obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
The invention aims to provide a preparation process of a high-hardness and high-toughness silicon nitride ceramic complex structural member, which solves the problem of performance regulation of the silicon nitride complex structural member, thereby ensuring that the ceramic member has stable and reliable performance indexes so as to meet the service requirement.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1: the embodiment provides a preparation process of a high-hardness high-toughness silicon nitride ceramic complex structural member, which comprises the following steps of:
step one, preparing silicon nitride composite powder; in the first step, silicon nitride with a purity of 99.99% and a particle size of 0.5 μm and an oxide sintering aid are uniformly mixed in an alcohol medium to obtain a silicon nitride composite powder, wherein the ratio of the silicon nitride to the oxide sintering aid is 90: 10;
the oxide sintering aid comprises 0.2 mu m yttrium oxide and 0.2 mu m aluminum oxide, and the ratio of yttrium oxide to aluminum oxide is 8.5: 1.5;
after the silicon nitride composite powder is obtained, drying the silicon nitride composite powder in a vacuum drying oven and sieving the dried powder through a 90-mesh stainless steel sieve to obtain the silicon nitride composite powder with fine and uniform granularity, and packaging the silicon nitride composite powder by a vacuum packaging machine to remove redundant gas;
secondly, performing cold isostatic pressing treatment on the silicon nitride composite powder under the pressure of 100-200 MPa to obtain a silicon nitride ceramic blank, wherein the pressure of the embodiment is preferably 150 MPa;
thirdly, cutting, turning and milling the silicon nitride ceramic blank to obtain a silicon nitride ceramic complex structural member blank with certain structural characteristics; in the embodiment, a numerical control milling machine is preferably adopted to mill the silicon nitride ceramic blank subjected to static pressure forming, the cutting speed is 5000rpm, the feeding speed is 100mm/min, and a silicon nitride ceramic complex structural member blank with a cylindrical, hole-shaped and groove-shaped structure is obtained, wherein the size range is 10-30 mm;
putting the processed silicon nitride ceramic complex structural component blank into a vacuum atmosphere sintering furnace, and performing low-temperature low-pressure pre-sintering on the silicon nitride ceramic complex structural component blank;
the low-temperature low-pressure pre-sintering is carried out in a nitrogen atmosphere, the temperature of the low-temperature low-pressure pre-sintering is 1100 ℃, the pressure of the low-temperature low-pressure pre-sintering is 1-1.5 MPa, preferably 1.25MPa, and the heat preservation time of the low-temperature low-pressure pre-sintering is 0.5-1.5 hours, preferably 0.5 hour; the depth of the surface hardness influence layer of the silicon nitride ceramic complex structural member blank can be regulated and controlled by adjusting the heat preservation time, and the longer the heat preservation time is, the greater the depth of the surface hardness influence layer of the silicon nitride ceramic complex structural member blank is;
after low-temperature low-pressure pre-sintering, cooling the silicon nitride ceramic complex structural member blank to room temperature;
step five, sintering at high temperature and high pressure;
the high-temperature high-pressure sintering is carried out in a nitrogen atmosphere, the temperature of the high-temperature high-pressure sintering is 1850-1950 ℃, the preferential temperature is 1850 ℃, and the pressure of the high-temperature high-pressure sintering is 5-10MPa, the preferential pressure is 5 MPa;
the density of the sintered ceramic material was measured using a density balance (DH-120, Japan) using distilled water as a measuring medium; the hardness and the fracture toughness are measured by a Vickers hardness tester (HVS-50, China), the load is selected to be 20kg, and the pressure maintaining time is selected to be 15 s; the 6 points were measured and averaged.
After high-temperature and high-pressure sintering, the obtained nitride has high surface hardness and high core toughnessThe density range of the silicon nitride ceramic complex structural component with various shapes prepared by the embodiment is 3.287-3.302 g/cm3The relative density reaches 99.95 percent, the hardness range from the surface layer to the core part is 19.85-16.30 GPa, the highest hardness value within 1mm of the surface layer is 19.85GPa, and the fracture toughness of the core part is 11.25 +/-0.7 MPa.m1/2。
In the embodiment, the surface layer of the processed ceramic structure blank is processed at low temperature and low pressure to change the structure of the surface layer, and then the densification sintering is performed at high temperature and high pressure to prepare the silicon nitride ceramic structural member with high surface hardness and high core toughness.
The principle and the implementation mode of the present invention are explained by applying specific examples in the present specification, and the above descriptions of the examples are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the foregoing, the description is not to be taken in a limiting sense.
Claims (8)
1. A preparation process of a high-hardness high-toughness silicon nitride ceramic complex structural member is characterized by comprising the following steps of: the method comprises the following steps:
step one, preparing silicon nitride composite powder;
secondly, carrying out cold isostatic pressing treatment on the silicon nitride composite powder to obtain a silicon nitride ceramic blank;
thirdly, cutting the silicon nitride ceramic blank to obtain a silicon nitride ceramic complex structural member blank;
fourthly, pre-sintering the silicon nitride ceramic complex structural member blank at low temperature and low pressure;
fifthly, sintering at high temperature and high pressure to obtain a silicon nitride ceramic complex structural part with high surface hardness and high core toughness;
in the fourth step, the depth of the surface hardness influence layer of the silicon nitride ceramic complex structural member blank is regulated and controlled by adjusting the heat preservation time of the low-temperature low-pressure pre-sintering, and the longer the heat preservation time is, the greater the depth of the surface hardness influence layer of the silicon nitride ceramic complex structural member blank is; after low-temperature low-pressure pre-sintering, the silicon nitride ceramic complex structural component blank needs to be cooled to room temperature.
2. The preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 1, characterized by comprising the following steps of: in the first step, silicon nitride and an oxide sintering aid are uniformly mixed in an alcohol medium to obtain the silicon nitride composite powder, wherein the ratio of the silicon nitride to the oxide sintering aid is 90: 10.
3. the preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 2, characterized by comprising the following steps of: the oxide sintering aid comprises yttrium oxide and aluminum oxide, wherein the ratio of yttrium oxide to aluminum oxide is 8.5: 1.5.
4. the preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 1, characterized by comprising the following steps of: and in the first step, after the silicon nitride composite powder is obtained, drying the silicon nitride composite powder, and carrying out vacuum packaging.
5. The preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 1, characterized by comprising the following steps of: and in the second step, carrying out cold isostatic pressing treatment under the pressure of 100-200 MPa.
6. The preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 1, characterized by comprising the following steps of: in the fourth step, the low-temperature low-pressure pre-sintering is carried out in a nitrogen atmosphere, the temperature of the low-temperature low-pressure pre-sintering is 1100 ℃, the pressure of the low-temperature low-pressure pre-sintering is 1-1.5 MPa, and the heat preservation time of the low-temperature low-pressure pre-sintering is 0.5-1.5 h.
7. The preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 1, characterized by comprising the following steps of: and in the fifth step, high-temperature and high-pressure sintering is carried out in a nitrogen atmosphere, the temperature of the high-temperature and high-pressure sintering is 1850-1950 ℃, and the pressure of the high-temperature and high-pressure sintering is 5-10 MPa.
8. The preparation process of the high-hardness high-toughness silicon nitride ceramic complex structural member according to claim 1, characterized by comprising the following steps of: the relative density of the obtained silicon nitride ceramic complex structural member with high surface hardness and high core toughness is higher than 99.9 percent, the hardness of the surface layer is 17-20 GPa within 1mm, the core hardness is 14-17 GPa, and the fracture toughness is 9-12 MPa.m1/2。
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