CN111943701B - Hot-pressing sintering process for improving compactness of ceramic material - Google Patents

Hot-pressing sintering process for improving compactness of ceramic material Download PDF

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CN111943701B
CN111943701B CN202010731405.8A CN202010731405A CN111943701B CN 111943701 B CN111943701 B CN 111943701B CN 202010731405 A CN202010731405 A CN 202010731405A CN 111943701 B CN111943701 B CN 111943701B
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carbon fiber
ceramic
fiber cloth
graphite
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CN111943701A (en
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薛平
陈玉华
董明
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Saifu Nano Technology Xuzhou Co ltd
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    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract

A hot-pressing sintering process for improving the compactness of a ceramic material belongs to the technical field of ceramic manufacturing. The hot-pressing sintering process comprises the following steps: s1, placing the high-strength graphite lower pressing block into a graphite sleeve mold, and fixing the position of the lower pressing block at the bottom of the mold; s2, stacking the carbon fiber cloth and the ceramic green body with the same cross section shape and size in sequence according to the assembly sequence of the carbon fiber cloth, the ceramic green body and the carbon fiber cloth, and placing the stacked carbon fiber cloth and the ceramic green body above a lower pressing block in a graphite sleeve mold; s3, heating to 2400 ℃ of 2000-60 MPa pressure, preserving heat and pressure for 10-60min, pressurizing the ceramic material by pressing the high-strength graphite upper pressure head downwards in the sintering process, and finally sintering the ceramic green body into the bulletproof ceramic plate by hot pressing. The carbon fiber cloth is used to improve the smoothness and uniformity of gas discharge in the ceramic material powder during hot-press sintering, is suitable for manufacturing bulletproof ceramic plates, and can enhance the capability of resisting armor-piercing bullets and armor-piercing combustion bullets of the composite armor based on the bulletproof ceramic plates.

Description

Hot-pressing sintering process for improving density of ceramic material
Technical Field
The invention relates to a technology in the field of ceramic manufacturing, in particular to a hot-pressing sintering process for improving the compactness of a ceramic material.
Background
Hot press sintering is a common process in ceramic material manufacture, and because the longitudinal applied pressure is adopted to supplement the sintering driving force, the densification of the ceramic can be realized in a short sintering time, and a block ceramic material with better densification is obtained. In particular for ceramic materials containing covalent bonds which are difficult to sinter, such as B 4 C、SiC、Si 3 N 4 The process has obvious advantages.
As for the die material for hot-pressing sintering, both a large outer sleeve die and an upper and lower pressing block adopt high-strength graphite materials with superfine particle structures, high purity and high graphitization degree, the structure is compact, the surface smoothness is high, in addition, the oxidation resistance, the electric conduction, the heat conduction and the compression strength at high temperature are high, and the die material can be repeatedly used, so the die material for hot-pressing sintering is the most commonly used die material for hot-pressing sintering at present.
In the existing hot-pressing sintering process, a graphite backing plate, soft graphite paper, a ceramic material green body, the soft graphite paper and the graphite backing plate are sequentially arranged in a graphite mold before mold filling and sintering, and then a hot-pressing sintering furnace is adopted to perform pressure sintering on the ceramic material. Wherein the soft graphite paper on the upper and lower sides of the ceramic green body is used as an isolating material, and has the function of isolating the sintered ceramic material from the graphite gasket, so that the ceramic sample is prevented from being stuck on a mould to cause demoulding difficulty in the high-temperature sintering process, and the influence on repeated use of the high-strength graphite gasket is also avoided.
For hard-to-sinter materials such as carbide and nitride ceramics, the current hot-pressing sintering process needs to set higher temperature and pressure. And the use of the soft graphite paper can cause the phenomenon of uneven sintered structure, namely, the outer edge of the sample obviously has structure layering to the center, and the density of the ceramic material close to the graphite mould is higher than that of the ceramic material at the central position. This non-uniformity leads to a decrease in the hardness of the material and to an unstable performance of the material and is therefore not suitable for the manufacture of bulletproof ceramic plates.
The Chinese patent application with the application number of 201710344144.2 discloses a hot-pressing sintering preparation process for improving the compactness of a ceramic material, and the method is used for replacing a graphite gasket and graphite paper after cutting, crushing and sieving a high-strength graphite block. However, the method has the disadvantages of high difficulty in cutting and crushing the high-strength graphite, low efficiency, poor uniformity of powder thickness after the high-strength graphite powder is added into the graphite sleeve die, easy change of the appearance of the ceramic part and unsuitability for manufacturing bulletproof ceramic plates. In addition, the method can sinter only one ceramic piece at a time, and is not efficient.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a hot-pressing sintering process for improving the density of a ceramic material, which is suitable for manufacturing a bulletproof ceramic plate and can enhance the capability of a composite armor based on the bulletproof ceramic plate in resisting armor-piercing bullets and armor-piercing combustion bullets for multiple strikes.
The invention comprises the following steps:
s1, loading the high-strength graphite lower pressing block into a graphite sleeve die, and fixing the position of the lower pressing block at the bottom of the die to prevent the lower pressing block from loosening;
s2, stacking the carbon fiber cloth with the consistent cross section shape and size and the ceramic green body in sequence according to the assembly sequence of the carbon fiber cloth, the ceramic green body and the carbon fiber cloth, and placing the stacked carbon fiber cloth, the ceramic green body and the carbon fiber cloth above a lower pressing block in a graphite sleeve mold;
s3, heating to 2400 ℃ of 2000-60 MPa pressure, preserving heat and pressure for 10-60min, pressurizing the ceramic material by pressing the high-strength graphite upper pressure head downwards in the sintering process, and finally sintering the ceramic green body into the bulletproof ceramic plate by hot pressing.
Preferably, the thickness of the carbon fiber cloth is 0.05-0.5 mm; the axial thermal conductivity of the carbon fiber is more than 30W/(m.k), and the elastic modulus is more than 310 GPa.
Preferably, a graphite backing plate is arranged between the bottom carbon fiber cloth and the high-strength graphite lower pressing block and/or between the top carbon fiber and the high-strength graphite upper pressing head so as to protect the lower pressing block and the upper pressing head.
Technical effects
Compared with the prior art, the invention has the following technical effects:
1) soft graphite paper which is an isolation material and has poor air permeability in the hot-pressing sintering process is replaced by carbon fiber cloth, so that the smoothness and uniformity of gas discharge inside ceramic material powder in the sintering process are improved, and the bulletproof ceramic material with high density is prepared;
2) the carbon fiber cloth is adopted, so that the surface of the bulletproof ceramic plate obtained by sintering forms a uniformly distributed uneven surface with the texture consistent with that of the carbon fiber cloth, the specific surface area of the ceramic plate is greatly increased, and the bulletproof armor is favorably manufactured by bonding other materials and the bulletproof ceramic plate;
3) a plurality of ceramic green bodies can be simultaneously hot-pressed to prepare the bulletproof ceramic plate, so that the production efficiency is high; adopt carbon cloth, graphite backing plate and carbon cloth to separate between two adjacent ceramic unburned bricks, because of the carbon cloth is unsmooth, can not hinder gaseous discharge when increasing the graphite backing plate in order to guarantee sintering pressure uniformity, the polylith bulletproof ceramic plate density that makes has better uniformity.
Drawings
FIG. 1 is a schematic diagram of a green ceramic structure according to example 1;
FIG. 2 is a schematic view of a hot press sintering process in example 1;
in the figure: the high-strength graphite sleeve die comprises a graphite sleeve die 1, a high-strength graphite lower pressing block 2, a high-strength graphite upper pressing head 3, a graphite backing plate 4, carbon fiber cloth 5 and a ceramic green body 6.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description. The experimental procedures, in which specific conditions are not specified in the examples, were carried out according to the conventional methods and conditions.
Example 1
The embodiment relates to a hot-pressing sintering process for improving the density of a bulletproof ceramic material.
Preparing a green body before hot-pressing sintering, wherein the method comprises the following steps:
20kg of B 4 Uniformly mixing C powder (Cifu nano technology), 2kg of nano carbon fiber (Suzhou first element CNTcr), 580g of water-soluble phenolic resin and 23kg of high-purity water to obtain ceramic slurry; spray drying at air inlet temperature of 200 deg.C and air outlet temperature of 100 deg.C to obtain composite raw material; finally cold pressing under 350MPa to obtain the ceramic green body 6 with the thickness of 20mm as shown in figure 1.
The hot-pressing sintering process comprises the following steps:
s1, adopting a graphite sleeve die 1 with an inner cavity matched with the shape of the ceramic green body, loading the corresponding high-strength graphite lower pressing block 2 into the bottom position in the graphite sleeve die 1, and checking to prevent looseness;
s2, placing the carbon fiber cloth 5 and the ceramic green body 6 above the high-strength graphite lower pressing block 2 in the graphite sleeve mold 1 according to the stacking sequence of the carbon fiber cloth 5, the ceramic green body 6 and the carbon fiber cloth 5, as shown in figure 2; a plurality of ceramic green bodies can be stacked and placed, two adjacent ceramic green bodies are separated by carbon fiber cloth, a graphite backing plate and the carbon fiber cloth, and at most ten ceramic green bodies can be stacked; the shapes and the sizes of the graphite backing plate, the carbon fiber cloth, the ceramic green body and the cross section of the inner cavity are consistent;
and S3, heating to 2200 ℃ under the pressure of 50MPa, preserving heat and pressure for 20min, sintering, and pressurizing the ceramic material by pressing the high-strength graphite upper pressure head downwards in the sintering process to finally obtain ten bulletproof ceramic plates with the thickness of 10 mm.
The top and bottom ceramic plates of this example were tested and compared to prior art ballistic ceramic plates made using soft graphite paper as the spacer material, and the results are shown in table 1 below.
TABLE 1 comparison of Properties
Figure BDA0002603300470000031
Compared with the different areas of the top ceramic plate (or the bottom ceramic plate) in the embodiment 1, the performance of the different areas can be found to be relatively close, and compared with the same area of the top ceramic plate and the bottom ceramic plate, the performance can be found to be consistent, which shows that the carbon fiber cloth is used as an isolation material, is beneficial to the discharge of gas in the hot-pressing sintering process, and ensures the density of the material; and when sintering the multilayer material, the use of the graphite backing plate does not affect the gas discharge based on the carbon fiber cloth.
It is to be emphasized that: the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and all simple modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.

Claims (3)

1. A hot-pressing sintering process for improving the compactness of a ceramic material is characterized by comprising the following steps:
s1, loading the high-strength graphite lower pressing block into a graphite sleeve die, and fixing the position of the lower pressing block at the bottom of the die to prevent the lower pressing block from loosening;
s2, stacking the carbon fiber cloth and the ceramic green body with the same cross section shape and size in sequence according to the assembly sequence of the carbon fiber cloth, the ceramic green body and the carbon fiber cloth, and placing the stacked carbon fiber cloth and the ceramic green body above a lower pressing block in a graphite sleeve mold; the stacking number of the ceramic green bodies is not less than 2, and two adjacent ceramic green bodies are separated by the carbon fiber cloth, the graphite backing plate and the carbon fiber cloth which are sequentially stacked;
s3, heating to 2400 ℃ of 2000-60 MPa pressure, preserving heat and pressure for 10-60min, pressurizing the ceramic material by pressing the high-strength graphite upper pressure head downwards in the sintering process, and finally sintering the ceramic green body into the bulletproof ceramic plate by hot pressing.
2. The hot-pressing sintering process for improving the compactness of the ceramic material according to claim 1, wherein the thickness of the carbon fiber cloth is 0.05-0.5 mm; the axial thermal conductivity of the carbon fiber is more than 30W/(m.k), and the elastic modulus is more than 310 GPa.
3. The hot-pressing sintering process for improving the compactness of the ceramic material according to claim 1, wherein a graphite backing plate is arranged between the bottom carbon fiber cloth and the high-strength graphite lower pressing block and/or between the top carbon fiber and the high-strength graphite upper pressing head.
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CN107140994B (en) * 2017-05-16 2019-11-05 山东大学 A kind of hot pressed sintering preparation process improving ceramic material consistency
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