CN111233479B - Preparation method of high-purity, high-density and large-size boron carbide ceramic - Google Patents
Preparation method of high-purity, high-density and large-size boron carbide ceramic Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation method of high-purity, high-density and large-size boron carbide ceramic. The invention reduces the granularity of the powder to D100 value 0.6 μm on the premise of keeping high purity, and the required sintering pressure is reduced under the condition of not adding any sintering aid, so that the obtained ceramic has stable and uniform performance; by adopting the method of matching the carbon-carbon fiber composite die and the graphite die, the compression strength of the die is improved, the size of the prepared single piece of boron carbide ceramic exceeds 450, the purity of 99.99 percent is ensured, and the density of the boron carbide ceramic exceeds 99.9 percent of the theoretical density. The boron carbide ceramic prepared by the method has the characteristics of large size, low density, high hardness, high bending strength and high fracture toughness, and can be applied to the fields of aircraft bulletproof armor, sputtering target materials and the like with extremely special requirements on ceramics.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a preparation method of high-purity, high-density and large-size boron carbide ceramic.
Background
Boron carbide ceramic is an important special ceramic, has high hardness, low density, good chemical stability and neutron absorption characteristic, and is widely applied to the high-tech fields of aerospace, national defense and military industry, nuclear energy utilization and the like at present. Because the covalent bond proportion in the boron carbide ceramic crystal is as high as 94 percent, the grain boundary moving resistance is very high during sintering, and the sintering difficulty is very high.
The existing preparation method of boron carbide ceramic generally reduces sintering temperature and improves bending strength and fracture toughness of boron carbide ceramic by adding sintering aids containing other elements such as Ti, Si, Al, Y and the like, but the prepared boron carbide ceramic loses the characteristics of low density and high hardness by adding other phases; the conventional common sintering methods of the boron carbide ceramic comprise normal pressure sintering, hot pressing sintering and plasma sintering, the density which can reach more than 99.9 percent of theoretical density cannot be obtained by the current normal pressure sintering, and the obtained boron carbide ceramic is not ideal in performance stability and uniformity due to the limitation of sintering conditions; the ceramic with high density, uniform texture and stable performance can be obtained by hot-pressing sintering, but because the hot-pressing sintering molding of the boron carbide ceramic needs very high pressure, the boron carbide ceramic is limited by the restriction of raw material powder, a graphite mold and sintering equipment, and a single piece of boron carbide ceramic with the size larger than 450 cannot be prepared; the plasma sintering is limited by the limitation of the used equipment and raw materials, the industrialization cannot be realized, and the large-size ceramic piece is difficult to prepare.
Disclosure of Invention
In order to solve the problems, the invention optimizes the preparation method of the raw material powder, reduces the granularity of the powder to D100 value (maximum particle) · 0.6 μm on the premise of keeping high purity, reduces the required sintering pressure under the condition of not adding any sintering aid, and obtains the ceramic with stable and uniform performance; by adopting the method of matching the carbon-carbon fiber composite die and the graphite die, the compression strength of the die is improved, so that the size of the prepared single piece of boron carbide ceramic can exceed 450, the purity of 99.99 percent is ensured, and the density of the boron carbide ceramic exceeds 99.8 percent of the theoretical density. The boron carbide ceramic prepared by the method has the characteristics of large size, low density, high hardness, high bending strength and high fracture toughness, and can be applied to the fields of aircraft bulletproof armor, sputtering target materials and the like which have extremely special requirements on ceramics.
The technical scheme of the invention is as follows:
a preparation method of high-purity, high-density and large-size boron carbide ceramic comprises the following steps:
step 1, mixing high-purity boric acid and high-purity graphite powder according to the mass ratio of 3.5-6: 1, and putting the mixture into an electric arc furnace using a graphite electrode for smelting to obtain a boron carbide crystal block; wherein the high-purity boric acid requires: 99.99% of purity, 0.015% of sulfate, 0.001% of Fe and Cl and other impurities; the requirements of high-purity graphite powder are as follows: ash content of 10ppm and density of 0.3-0.4 g/cm3The granularity D50 is 20-30 μm;
step 2, crushing the boron carbide crystal blocks obtained in the step 1 until D50 is 30-50 microns to obtain boron carbide crystal powder;
step 3, putting the boron carbide crystal powder obtained in the step 2 into a reaction kettle and cleaning with sulfuric acid to remove iron; heating and boiling for more than 2 hours are required during cleaning;
step 4, dehydrating the boron carbide crystal powder obtained after cleaning in the step 3, and repeatedly washing and dehydrating the boron carbide crystal powder by using deionized water until the conductivity of the washed and dehydrated boron carbide crystal powder is 30 mu S/cm;
step 5, putting the dehydrated boron carbide crystal powder in the step 4 into a sorting tank, and selecting D50 & 30 mu m powder;
step 6, dehydrating the powder selected in the step 5, and putting the dehydrated powder into a sand mill to be added with deionized water and milled until the particle size is D100-0.6 mu m; the part of the sand mill, which is required to be contacted with the powder, is coated with a boron carbide ceramic plate, and the grinding medium is a boron carbide ceramic ball which is formed by cold isostatic pressing and sintered at normal pressure; the used boron carbide ceramic plate and boron carbide ceramic ball are single-phase boron carbide and do not contain other elements, and the purity is 99.9 percent; the temperature of the slurry is kept not to exceed 70 ℃ in the whole milling process in a circulating water cooling mode;
step 7, drying and granulating the powder ground in the step 6 by using a spray dryer, and carrying out compression molding by using a hydraulic press to obtain a ceramic green body, wherein no auxiliary agent is added in the drying and compression molding processes;
step 8, pouring the ceramic green body obtained in the step 7 into a graphite mold, isolating the contact surface of the ceramic green body and the graphite mold by using graphite paper, and then sleeving a carbon-carbon fiber composite mold on the outer sleeve of the graphite mold; the carbon-carbon fiber composite material mold used requires 3500MPa of tensile strength and 42000MPa of tensile elastic modulus;
step 9, placing the mold with the ceramic green body in the step 8 into a hot-pressing sintering furnace, vacuumizing to the vacuum degree of 0.05pa, gradually heating to 1900-2100 ℃, heating at the speed of 10 ℃/min, and calculating the pressurizing pressure according to the pressure-bearing area of the hot-pressing ceramic green body multiplied by 20-25 MPa; finally firing to obtain the high-purity, high-density and large-size boron carbide ceramic.
In the step 2, the used crushing equipment is a jaw crusher, a double-roll crusher, a ball mill or an air flow mill.
In the step 4, the used dewatering equipment is a plate-and-frame filter press or a centrifuge.
The invention has the beneficial effects that:
the method has the technical key points that the purity of boron carbide is controlled in the whole process; secondly, the granularity of the powder used for sintering is finer on the basis of maintaining the purity, so as to reduce the pressure required by sintering and stabilize the performance of the ceramic; thirdly, the mould prepared by the carbon-carbon fiber composite material increases the pressure which can be applied by sintering, and improves the compactness of the ceramic. The boron carbide ceramic prepared by the method keeps the characteristics of low density and high hardness, and simultaneously has obviously improved bending strength and fracture toughness compared with the prior hot-pressed sintered boron carbide, and can meet the special requirements of bulletproof armor of aircraft, sputtering target material and the like on the performance of the ceramic. And the used raw materials and equipment are easy to obtain, and the feasibility of industrial mass production is realized.
Drawings
FIG. 1 is a result of particle size analysis of high purity boron carbide powder used for sintering;
Detailed Description
The following further describes a specific embodiment of the present invention with reference to the drawings and technical solutions.
Example 1
Step 1, mixing high-purity boric acid and high-purity graphite powder according to the mass ratio of 3.5:1, and putting the mixture into an electric arc furnace using a high-purity graphite electrode for smelting to obtain a boron carbide crystal block; the requirement of high-purity boric acid is as follows: 99.99% of purity, 0.015% of sulfate, 0.001% of Fe and Cl and other impurities; the high-purity graphite powder is required to be: ash content of 10ppm and density of 0.3-0.4 g/cm3The granularity D50 is 20-30 μm; the results of chemical component detection of the high-purity boron carbide powder are shown in table 1, and the results of particle size analysis of the high-purity boron carbide powder are shown in fig. 1 and table 2.
TABLE 1 results of chemical composition measurements of high purity boron carbide powder used for sintering
TABLE 2 particle size analysis results of high purity boron carbide powders
| Analysis item | Results |
| Specific surface area | 31.22m2/g |
| D(3,2) | 0.343μm |
| D(4,3) | 0.383μm |
| D10 | 0.166μm |
| D50 | 0.346μm |
| D90 | 0.603μm |
Step 2, crushing the boron carbide crystal blocks to D50 of 30 mu m by using a jaw crusher;
step 3, putting the crushed powder into a reaction kettle, and cleaning the powder by using sulfuric acid, wherein the cleaning requires heating to keep a boiling state for more than 2 hours;
step 4, dehydrating by using a plate-and-frame filter press after cleaning, and repeatedly washing and dehydrating by using deionized water until the conductivity of the cleaned and dehydrated water is 30 mu S/cm;
step 5, putting the dehydrated powder into a sorting tank, and preferably selecting the powder with D50 & 30 mu m according to the Stokes sedimentation principle;
step 6, dehydrating the optimized powder, and putting the powder into a sand mill to be ground into D100.0.6 mu m by adding deionized water, wherein the sand mill used in the step requires that parts, such as the inner cavity of a mill body, a stirring paddle and the like, which are in contact with the powder are coated with boron carbide ceramic plates, the grinding medium used in the sand mill is boron carbide ceramic balls which are formed by using cold isostatic pressing and sintered at normal pressure, the used boron carbide ceramic plates and ceramic balls are single-phase boron carbide and contain no other elements, and the purity is 99.9%; the temperature of the slurry is kept not to exceed 70 ℃ in the whole milling process by a circulating water cooling mode;
step 7, drying and granulating the ground powder by using a spray dryer, and carrying out compression molding by using a hydraulic press, wherein no auxiliary agent is added in the drying and compression molding processes;
step 8, placing the molded ceramic green body into a graphite mold, isolating the contact surface of the ceramic green body and the graphite mold by using graphite paper, and sleeving a C-C composite mold on the graphite mold, wherein the carbon-carbon fiber composite mold used in the step requires 3500MPa of tensile strength and 42000MPa of tensile elastic modulus;
step 9, placing the assembled ceramic green body mold into a hot-pressing sintering furnace, vacuumizing to the vacuum degree of 0.05pa, gradually heating to 1900 ℃, heating at the speed of 10 ℃/min, and if the size of the ceramic part is 450 x 20mm, the pressure-bearing area is 0.16m2And pressure 324T is pressurized.
And step 10, cutting the obtained boron carbide ceramic by using an electric spark wire, machining and polishing the boron carbide ceramic by using a plane grinder to manufacture a detection sample, detecting three-point bending strength, fracture toughness and micro Vickers hardness by using an electronic universal tester, and detecting density by using an Archimedes drainage method.
Example 2
The procedure was the same as in example 1, with some parameters controlled as follows:
in the step 1, mixing high-purity boric acid and high-purity graphite powder according to a ratio of 6: 1;
in the step 2, crushing the boron carbide crystal blocks by using a double-roll crusher until D50 is 50 microns;
in step 9, vacuumizing to the vacuum degree of 0.04pa, gradually heating to 2100 ℃, wherein the heating speed is 9 ℃/min, and the applied pressure is 405T.
Example 3
The procedure was the same as in example 1, with some parameters controlled as follows:
in the step 1, mixing high-purity boric acid and high-purity graphite powder according to a ratio of 4: 1;
in the step 2, crushing the boron carbide crystal blocks by using a double-roll crusher until D50 is 45 microns;
in step 9, vacuum is pumped to the vacuum degree of 0.03pa, the temperature is gradually increased to 2000 ℃, the temperature rising speed is 8 ℃/min, and the applied pressure is 355T.
The boron carbide ceramic with high purity, high density and large size can be prepared by three embodiments. And the detection results all meet the following conditions: the density of the ceramic is more than 2.515g/cm measured by using the Archimedes drainage method in GB/T25995-20103The compactness is more than 99.8 percent, the bending strength of the ceramic is more than 550MPa measured by using GB/T6569-2009, and the fracture toughness of the ceramic is more than 5.0 MPa-m measured by using the single-side pre-crack method in GB/T23806-20091/2The Vickers hardness of the ceramic is more than 3600HV1 according to GB/T16534-.
Claims (3)
1. A preparation method of high-purity, high-density and large-size boron carbide ceramic is characterized by comprising the following steps:
step 1, mixing high-purity boric acid and high-purity graphite powder according to the mass ratio of 3.5-6: 1, and putting the mixture into an electric arc furnace using a graphite electrode for smelting to obtain a boron carbide crystal block; wherein the high-purity boric acid requires: 99.99% of purity, 0.015% of sulfate, 0.001% of Fe and Cl and other impurities; the requirements of high-purity graphite powder are as follows: ash content of 10ppm and density of 0.3-0.4 g/cm3The granularity D50 is 20-30 μm;
step 2, crushing the boron carbide crystal blocks obtained in the step 1 until D50 is 30-50 microns to obtain boron carbide crystal powder;
step 3, putting the boron carbide crystal powder obtained in the step 2 into a reaction kettle and cleaning with sulfuric acid to remove iron; heating and boiling for more than 2 hours are required during cleaning;
step 4, dehydrating the boron carbide crystal powder obtained after cleaning in the step 3, and repeatedly washing and dehydrating the boron carbide crystal powder by using deionized water until the conductivity of the washed and dehydrated boron carbide crystal powder is 30 mu S/cm;
step 5, putting the dehydrated boron carbide crystal powder in the step 4 into a sorting tank, and selecting D50 & 30 mu m powder;
step 6, dehydrating the powder selected in the step 5, and putting the dehydrated powder into a sand mill to be added with deionized water and milled until the particle size is D100-0.6 mu m; the part of the sand mill, which is required to be contacted with the powder, is coated with a boron carbide ceramic plate, and the grinding medium is a boron carbide ceramic ball which is formed by cold isostatic pressing and sintered at normal pressure; the used boron carbide ceramic plate and boron carbide ceramic ball are single-phase boron carbide and do not contain other elements, and the purity is 99.9 percent; the temperature of the slurry is kept not to exceed 70 ℃ in the whole milling process in a circulating water cooling mode;
step 7, drying and granulating the powder ground in the step 6 by using a spray dryer, and carrying out compression molding by using a hydraulic press to obtain a ceramic green body, wherein no auxiliary agent is added in the drying and compression molding processes;
step 8, pouring the ceramic green body obtained in the step 7 into a graphite mold, isolating the contact surface of the ceramic green body and the graphite mold by using graphite paper, and then sleeving a carbon-carbon fiber composite mold on the outer sleeve of the graphite mold; the used carbon-carbon fiber composite material mold requires 3500MPa of tensile strength and 42000MPa of tensile elastic modulus;
step 9, placing the mold with the ceramic green body in the step 8 into a hot-pressing sintering furnace, vacuumizing to the vacuum degree of 0.05Pa, gradually heating to the temperature of 1900-2100 ℃, heating at the speed of 10 ℃/min, and calculating the pressurizing pressure according to the pressure-bearing area of the hot-pressing ceramic green body multiplied by 20-25 MPa; finally firing to obtain the high-purity, high-density and large-size boron carbide ceramic.
2. The method for preparing high-purity high-density large-size boron carbide ceramic according to claim 1, wherein in the step 2, the crushing equipment is a jaw crusher, a roller crusher, a ball mill or a jet mill.
3. The method for preparing high-purity high-density large-size boron carbide ceramic according to claim 1 or 2, wherein the dewatering equipment used in the step 4 is a plate-and-frame filter press or a centrifuge.
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| CN102161586A (en) * | 2011-04-26 | 2011-08-24 | 大连金玛硼业科技集团有限公司 | Method for preparing boron carbide ceramic powder with controllable particle size |
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| CN110357634A (en) * | 2019-07-10 | 2019-10-22 | 中国科学院上海硅酸盐研究所 | A kind of application of boron carbide ceramics as pressure-sensitive ceramic material |
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| CN102161586A (en) * | 2011-04-26 | 2011-08-24 | 大连金玛硼业科技集团有限公司 | Method for preparing boron carbide ceramic powder with controllable particle size |
| CN102730689A (en) * | 2012-07-31 | 2012-10-17 | 中国科学院上海硅酸盐研究所 | Surface treatment method of boron carbide powder |
| CN105540591A (en) * | 2016-02-03 | 2016-05-04 | 东北大学 | Method for preparing multi-variety boron carbide micro-powder |
| CN110028321A (en) * | 2019-05-31 | 2019-07-19 | 中南大学 | A kind of energy saving preparation method of the pure boron carbide ceramics material of high-performance and pure boron carbide ceramics material |
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