CN111548162B - Method for preparing ZrC ceramic by compression molding of precursor - Google Patents

Method for preparing ZrC ceramic by compression molding of precursor Download PDF

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CN111548162B
CN111548162B CN202010314190.XA CN202010314190A CN111548162B CN 111548162 B CN111548162 B CN 111548162B CN 202010314190 A CN202010314190 A CN 202010314190A CN 111548162 B CN111548162 B CN 111548162B
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zrc
precursor powder
precursor
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proper amount
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CN111548162A (en
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焦华
宋森
赵康
汤玉斐
张鑫媛
孟庆男
李福平
于晓婧
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Xian University of Technology
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/5607—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 based on refractory metal carbides
    • C04B35/5622—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 based on refractory metal carbides based on zirconium or hafnium carbides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
    • C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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Abstract

The invention discloses a method for preparing ZrC ceramic by utilizing precursor compression molding, which specifically comprises the following steps: step 1, processing ZrC precursor powder: weighing a proper amount of ZrC precursor powder, and sieving the ZrC precursor powder by using a mesh sieve to obtain fine powder; step 2, preparing a PVA binder: weighing a proper amount of PVA in a beaker, adding a proper amount of deionized water, and stirring under heating in a water bath until the solution is transparent and uniform and has no bubbles; step 3, dropping a proper amount of PVA (polyvinyl alcohol) binder into ZrC precursor powder in proportion, and then stirring by using a glass rod until no granular aggregation occurs in the ZrC precursor powder; step 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, and removing the pressing block to obtain a ZrC precursor block; and 5, sintering the prepared precursor block at high temperature under the protection of argon to obtain the ZrC ceramic. The invention has simple production process and lower cost, and is in accordance with large-scale industrial production.

Description

Method for preparing ZrC ceramic by compression molding of precursor
Technical Field
The invention belongs to the field of ZrC ceramic preparation processes, and particularly relates to a method for preparing ZrC ceramic by utilizing precursor compression molding.
Background
ZrC has the properties of high melting point, high hardness, high thermal conductivity, high electrical conductivity, high specific strength, high specific modulus, good chemical stability and the like, and is widely applied to ultrahigh-temperature heat-insulating coatings, high-temperature refractory materials and the like. At present, there are many reports on the synthesis method of ZrC nanopowder, such as the electric arc furnace carbothermic method, the self-propagating high-temperature synthesis method, the sol-gel method, the laser gas phase reaction method, the high-energy ball milling method, etc. However, in practical application, the form of the powder is limited to a certain extent, and the powder is used for more and more ZrC ceramic devices and targets, so that the research on preparing the powder into the ZrC ceramic devices has important significance for the application of the ZrC ceramic devices.
At present, the method for preparing the ZrC ceramic material mainly comprises the following steps: hot pressing sintering method, chemical vapor infiltration method, precursor impregnation cracking method, etc. Wherein the hot-pressing sintering method needs higher sintering temperature, which is usually above 1000 ℃; the chemical vapor infiltration method requires a longer deposition period and high cost; waste gas pollution is often generated in the roasting decomposition process in the precursor impregnation cracking process. Therefore, it is very important to research a ZrC ceramic preparation process which is simple, time-saving, pollution-free in production process and low in cost.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for preparing ZrC ceramic by using precursor pressure, which has the characteristics of simple preparation, low cost and environmental friendliness.
ZrOCl2, glucose and citric acid are used for preparing a ZrC organic precursor through rotary evaporation, and the preparation method is applied for patent and has the patent name: a method for preparing a ZrC organic precursor by rotary evaporation, which is disclosed in the patent application No.: 202010108962.4.
the invention adopts the technical scheme that a method for preparing ZrC ceramic by utilizing precursor compression molding, ZrOCl2And glucose and citric acid are subjected to rotary evaporation to prepare a ZrC organic precursor, and the preparation method is implemented according to the following steps:
step 1, ZrC precursor powder treatment: weighing a proper amount of ZrC precursor powder, and sieving the ZrC precursor powder by using a mesh sieve to obtain ZrC precursor powder;
step 2, preparing a PVA binder: weighing a proper amount of polyvinyl alcohol (PVA) in a beaker, adding a proper amount of deionized water, and stirring in a water bath until the solution is transparent and uniform and has no bubbles, wherein the mass ratio of the PVA to the deionized water is 1-2:8-10, and the water bath heating temperature is 60-70 ℃;
step 3, dropping a proper amount of PVA (polyvinyl alcohol) binder into ZrC precursor powder in proportion, and then stirring by using a glass rod until no granular aggregation occurs in the ZrC precursor powder;
Step 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, and removing the pressing and taking the block to obtain a ZrC precursor block, wherein the proportion of the PVA to the ZrC precursor powder is that 0.5-1.0ml of VA binder is added into each 1.5-2.0g of ZrC precursor powder;
and 5, sintering the prepared ZrC precursor block at high temperature under the protection of argon to obtain the ZrC ceramic.
Further, the mesh used in step 1 is 500-800 mesh.
Further, in the step 4, the pressure condition of the manual press is 10-15MPa, and the dwell time is 1-1.5 min.
Further, in the step 5, the sintering temperature is 1400 ℃, and the sintering time is 8 h.
Compared with the prior art, the invention has the beneficial effects that: the ZrC ceramic is successfully prepared by a simple forming and caking method. The agglomeration method has the characteristics of simple production process and low cost, meets the requirement of large-scale industrial production, and is an excellent choice for ZrC material powder agglomeration.
Drawings
FIG. 1 is a flow chart of a method for preparing ZrC ceramic by adopting precursor compression molding according to the invention;
FIG. 2 is an X-ray diffraction diagram in a method for preparing ZrC ceramic by compression molding of a precursor according to the invention;
FIG. 3(a) is a ZrC precursor block pressed and a ZrC ceramic macroscopic image obtained after high-temperature sintering in the method for preparing ZrC ceramic by precursor press forming of the invention;
FIG. 3(b) is a scanning electron micrograph of ZrC ceramic obtained by high temperature sintering;
FIG. 4 is a graph showing the compressive strength of ZrC ceramics obtained after high-temperature sintering in the method for preparing ZrC ceramics by precursor compression molding according to the invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
A method for preparing ZrC ceramic by using precursor compression molding is specifically implemented according to the following steps as shown in a flow chart of figure 1:
step 1, ZrC precursor powder treatment: weighing a proper amount of ZrC precursor powder, and sieving the ZrC precursor powder by using a 500-plus 800-mesh screen to obtain ZrC precursor powder;
step 2, preparing a PVA binder: weighing a proper amount of polyvinyl alcohol (PVA) in a beaker according to the mass ratio of the PVA to the deionized water of 1-2:8-10, adding a proper amount of deionized water, and heating and stirring in a water bath at 60-70 ℃ until the solution is transparent and uniform and has no bubbles.
And 3, adding a proper amount of PVA binder into 1.5-2.0g of ZrC precursor powder per 0.5-1.0mL of PVA according to the proportion of the PVA to the ZrC precursor powder, and then, stirring by using a glass rod until the ZrC precursor powder does not generate granular aggregation.
And 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, and removing the pressing and taking the block to obtain the ZrC precursor block. The pressure condition of the manual press is 10-15MPa, and the pressure maintaining time is 1-1.5 min.
And 5, sintering the prepared precursor block at high temperature under the protection of argon, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours, so as to obtain the ZrC ceramic.
Example 1
Step 1, ZrC precursor powder treatment: weighing 10 g of ZrC precursor powder, grinding the ZrC precursor powder into fine powder by using a mortar, and screening the fine powder by using a 500-mesh screen after grinding by using the mortar;
step 2, preparing a PVA binder: weighing 1g of PVA in a beaker according to the mass ratio of 1:10 of the PVA to the deionized water, adding 10 mL of deionized water, and stirring the mixture under heating in a water bath at the temperature of 60 ℃ until the solution is transparent, uniform and free of bubbles;
and 3, dripping 5 mL of PVA into the ZrC precursor powder according to the proportion that 1 mL of PVA binder is added into every 2g of ZrC precursor powder, and then stirring by using a glass rod until the ZrC precursor powder does not aggregate in a granular manner.
And 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, wherein the pressure condition of the manual press is 10 MPa, the pressure maintaining time is 1 min, and removing the pressure and the block to obtain the ZrC precursor block.
And 5, sintering the prepared precursor block at high temperature under the protection of argon, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours, so as to obtain the ZrC ceramic.
Example 2
Step 1, processing ZrC precursor powder: weighing 20 g of ZrC precursor powder, grinding the ZrC precursor powder into fine powder by using a mortar, and screening the fine powder by using a 600-mesh screen after grinding by using the mortar;
step 2, preparing a PVA binder: weighing 1.5 g of PVA in a beaker according to the mass ratio of the PVA to the deionized water of 1.5:8.5, adding 8.5mL of deionized water, and stirring the mixture under the water bath heating at 65 ℃ until the solution is transparent, uniform and free of bubbles;
and 3, dripping 5mL of PVA into the ZrC precursor powder according to the proportion of adding 0.5 mL of PVA binder into every 2g of ZrC precursor powder, and stirring by using a glass rod until the ZrC precursor powder does not aggregate in a granular manner.
And 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, wherein the pressure condition of the manual press is 12 MPa, the pressure maintaining time is 1.5 min, and removing the pressure and the block to obtain the ZrC precursor block.
And 5, sintering the prepared precursor block at high temperature under the protection of argon, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours, so as to obtain the ZrC ceramic.
Example 3
Step 1, ZrC precursor powder treatment: weighing 30 g of ZrC precursor powder, grinding the ZrC precursor powder into fine powder by using a mortar, and screening the fine powder by using a 800-mesh screen after grinding by using the mortar;
step 2, preparing a PVA binder: weighing 3g of PVA in a beaker according to the mass ratio of 1:9 of the PVA to the deionized water, adding 27mL of deionized water, and stirring the mixture under the heating of a water bath at 70 ℃ until the solution is transparent, uniform and free of bubbles;
and 3, dropping 20 mL of PVA into the ZrC precursor powder according to the proportion that 1mL of PVA binder is added into every 1.5g of ZrC precursor powder, and stirring by using a glass rod until no granular aggregation occurs in the ZrC precursor powder.
And 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, wherein the pressure condition of the manual press is 15 MPa, the pressure maintaining time is 1 min, and removing the pressure and the block to obtain the ZrC precursor block.
And 5, sintering the prepared precursor block at high temperature under the protection of argon, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours, so as to obtain the ZrC ceramic.
Example 4
Step 1, ZrC precursor powder treatment: weighing 40 g of ZrC precursor powder, grinding the ZrC precursor powder into fine powder by using a mortar, and screening the fine powder by using a 500-mesh screen after grinding by using the mortar;
Step 2, preparing a PVA binder: weighing 4g of PVA in a beaker according to the mass ratio of the PVA to the deionized water of 2:8, adding 16 mL of deionized water, and stirring the mixture under heating in a water bath at 60 ℃ until the solution is transparent, uniform and free of bubbles;
step 3, according to the proportion that 0.5mL of PVA binder is added into every 1.5g of ZrC precursor powder, 13.3 mL of PVA is dripped into the ZrC precursor powder, and then a glass rod is used for stirring until no granular aggregation occurs in the ZrC precursor powder;
step 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, wherein the pressure condition of the manual press is 10 MPa, the pressure maintaining time is 1.5 min, and removing the pressure and the block to obtain a ZrC precursor block;
and 5, sintering the prepared precursor block at high temperature under the protection of argon, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours, so as to obtain the ZrC ceramic.
Example 5
Step 1, ZrC precursor powder treatment: weighing 50 g of ZrC precursor powder, grinding the ZrC precursor powder into fine powder by using a mortar, and screening the fine powder by using a 600-mesh screen after grinding by using the mortar;
step 2, preparing a PVA binder: weighing 6g of PVA in a beaker according to the mass ratio of the PVA to the deionized water of 2:10, adding 30mL of deionized water, and stirring the mixture under water bath heating at 65 ℃ until the solution is transparent, uniform and free of bubbles;
And 3, dripping 25 mL of PVA into the ZrC precursor powder according to the proportion that 1mL of PVA binder is added into every 2.0g of ZrC precursor powder, and then stirring by using a glass rod until the ZrC precursor powder does not have granular aggregation.
And 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, wherein the pressure condition of the manual press is 15 MPa, the pressure maintaining time is 1min, and removing the pressure and the block to obtain the ZrC precursor block.
And 5, sintering the prepared precursor block at high temperature under the protection of argon, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours, so as to obtain the ZrC ceramic.
As shown in FIG. 2, the X-ray diffraction analysis of the ZrC ceramic obtained by the method shows that the characteristic peaks of ZrC appear under the condition of sintering at 1400 ℃ for 8h and correspond to the standard peaks one by one, which shows that the agglomeration method can not change the material structure of ZrC.
As shown in fig. 3 (a), it can be seen that in the macroscopic case, there was no crack and no defect. When the ceramics were analyzed by scanning electron microscopy, as shown in fig. 3 (b), it could be seen that the ZrC ceramics were well bonded.
As shown in FIG. 4, the ZrC ceramic obtained after high-temperature sintering is subjected to a compressive strength test, and the strength average value is 435.20MPa, so that the ZrC ceramic prepared has high compressive strength and can meet basic material application.
The ZrC ceramic is successfully prepared by a simple agglomeration method, and the prepared ZrC ceramic has good bonding degree and high compressive strength. The preparation method has the characteristics of simple production process, low cost and accordance with large-scale industrial production, and the process has important strategic significance and urgent practical value for the development and application of the ZrC device.
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that this is by way of example only, and that the scope of the invention is defined by the appended claims. Various changes and modifications to these embodiments may be made by those skilled in the art without departing from the spirit and scope of the invention, and these changes and modifications are within the scope of the invention.

Claims (3)

1. Method for preparing ZrC ceramic by compression molding of precursor, ZrOCl2The ZrC organic precursor is prepared from glucose and citric acid through rotary evaporation, and is characterized by being implemented according to the following steps:
step 1, ZrC precursor powder treatment: weighing a proper amount of ZrC precursor powder, and sieving the ZrC precursor powder by using a mesh sieve to obtain ZrC precursor powder;
Step 2, preparing a PVA binder: weighing a proper amount of polyvinyl alcohol (PVA) in a beaker, adding a proper amount of deionized water, and stirring in a water bath until the solution is transparent and uniform and has no bubbles, wherein the mass ratio of the PVA to the deionized water is 1-2:8-10, and the water bath heating temperature is 60-70 ℃;
step 3, dropping a proper amount of PVA (polyvinyl alcohol) binder into ZrC precursor powder in proportion, and then stirring by using a glass rod until no granular aggregation occurs in the ZrC precursor powder;
step 4, weighing a proper amount of mixed ZrC precursor powder, placing the ZrC precursor powder in a mold, pressing the ZrC precursor powder into a block by using a manual press, and removing the pressing and taking the block to obtain a ZrC precursor block, wherein the proportion of the PVA to the ZrC precursor powder is that 0.5-1.0ml of VA binder is added into each 1.5-2.0g of ZrC precursor powder;
and 5, sintering the prepared ZrC precursor block at high temperature under the protection of argon to obtain ZrC ceramic, wherein the sintering temperature is 1400 ℃, and the sintering time is 8 hours.
2. The method for preparing ZrC ceramic by pressing and forming a precursor as claimed in claim 1, wherein the mesh used in step 1 is 500-800 mesh.
3. The method for preparing ZrC ceramic by compression molding of a precursor in claim 1, wherein in the step 4, the pressure condition of the manual press is 10-15MPa, and the dwell time is 1-1.5 min.
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