CN107778009B - Pressure-bearing preparation of Ti3SiC2Method for synthesizing ceramics by reverse thermal expansion - Google Patents
Pressure-bearing preparation of Ti3SiC2Method for synthesizing ceramics by reverse thermal expansion Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000002194 synthesizing effect Effects 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 58
- 229910009817 Ti3SiC2 Inorganic materials 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 22
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- 238000001308 synthesis method Methods 0.000 claims abstract description 7
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
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Abstract
The invention belongs to the field of ceramic material preparation processes, and particularly relates to Ti3SiC2The synthesis method of ceramic by reverse thermal expansion. The method comprises the following seven steps of raw material refining, sieving and drying, powder purification, green body preparation, pressure-bearing fixation, atmosphere sintering and mechanical treatment; solves the problem of the existing Ti3SiC2Expensive equipment, low yield and limited size in the ceramic synthesis process; provides a high-purity Ti for industrial production3SiC2The simple preparation method of the ceramic has the remarkable advantages of high purity of the prepared ceramic, unlimited size and shape of the prepared ceramic and the like.
Description
Technical Field
The invention belongs to the field of ceramic material preparation processes, and particularly relates to a pressure-bearing Ti preparation method3SiC2The synthesis method of ceramic by reverse thermal expansion.
Background
Ti3SiC2Is an important compound in MAX system, and belongs to typical ternary system metal ceramic materials. Ti3SiC2Has the characteristic of hexagonal layered structure with space octahedron connection and has the dual characteristics of metal and ceramic. On one hand, the material has the metal-like characteristics of excellent electrical conductivity and thermal conductivity, higher elastic modulus, thermal shock resistance, high-temperature plasticity, machinability and the like; on the other hand, it has typical ceramic properties of high yield strength, high melting point, high thermal stability, high resistance to oxidation and corrosion. The excellent characteristics endow the material with potential application value space in the fields of electromechanics, metallurgy, chemical engineering, automobiles, ships, petrifaction, spaceflight, national defense and the like.
Albeit Ti3SiC2The excellent performance of the composite material attracts wide attention at home and abroad. But because in the Ti-Si-C ternary phase diagram, single Ti3SiC2The phase stability region is narrow, and thus the preparation process is relatively complicated. The common preparation methods at present include a hot pressing sintering method, a hot isostatic pressing sintering method, a discharge plasma sintering method, a self-propagating high-temperature synthesis method, a laser melting method and the like. These methods are currently used to synthesize large-size Ti3SiC2Ceramics and large size Ti3SiC2Various problems exist with ceramic profiles. Hot-pressing sintering is currently the most common synthetic Ti3SiC2Ceramic method, but subject to the size of the press head, hot press sintering can only produce small size, single shape Ti3SiC2Ceramic, long preparation time, low yield and is not suitable for industrial production. The hot isostatic pressing sintering method can prepare small Ti3SiC2Ceramic special-shaped pieces, but the requirements for the blank are high, and the energy consumption of equipment is large. The discharge plasma method has rapid reaction, simple process and Ti synthesis3SiC2The ceramic has high compactness, but the size of the synthesized ceramic has high equipment price and high maintenance cost. High-temperature self-propagating synthesis method, rapid reaction and low energy consumption, but the reaction process is difficult to control, and Ti is synthesized3SiC2The purity of the ceramic is low. And thus the laser melting method is only suitable for preparing Ti with specific size3SiC2A film material. At present, the method is lack of the method which can be really applied to the mass production of large-size and high-purity Ti3SiC2A technical method of ceramic materials.
Disclosure of Invention
In view of the above-mentioned problems, the present invention is provided to solve the existing Ti3SiC2Expensive equipment, low yield and limited size in the ceramic synthesis process. Provides a high-purity Ti for industrial production3SiC2Simple preparation method of ceramics.
Specifically, the technical scheme of the invention is realized by the following ways:
in general, the reverse thermal expansion method bears pressure to prepare Ti3SiC2The ceramic synthesis method comprises the following seven steps of raw material refining, sieving and drying, powder purification, green body preparation, pressure-bearing fixation, atmosphere sintering and mechanical treatment; refining raw materials: firstly, commercial Ti3SiC2Mixing the powder with ethanol of the same mass, and adding Ti of the same mass3SiC22-5 times of agate balls or zirconia balls of the powder are ball-milled for 4-12 hours on a high-speed ball mill to obtain ball-milled slurry; sieving and drying: sieving the ball-milled slurry, keeping the temperature of the sieved slurry in an oven for 12-24h, controlling the temperature of the oven to be 30-45 ℃, and recovering after the powder is completely dried; powder purification: recovering the above-mentioned Ti3SiC2Adding the powder into hot phosphoric acid for acidification for 30-60min, cooling and separating, adding the powder treated by the hot phosphoric acid into a mixed solution of hydrochloric acid and hydrofluoric acid, controlling the treatment temperature at 50-60 ℃, treating for 30-60min to obtain secondarily acidified powder, cooling and diluting, and centrifugally recovering and purifying; preparing a green body: adding a small amount of 3-5% PVA into the purified powder for granulation, placing the mixture into a mold with a fixed shape for primary pressing, controlling the mold pressing pressure to be 15-35MPa to obtain a rough blank, placing the rough blank into a cold isostatic press, and carrying out lining for 5-10min under the pressure of 120-200MPa to obtain a green blank with certain strength; pressure-bearing fixation: putting the obtained green body into a corundum mold, adding inert pressure-bearing powder, adding an outer cover, and screwing down the high-strength ceramic bolt; atmosphere sintering: placing the corundum mold into an atmosphere furnace for sintering, wherein the sintering temperature is 1300-1400 ℃, and the reaction time is 1400 DEG CControlling the reaction time to be 0.5-2h, cooling the die to room temperature along with the furnace after the reaction, unscrewing the ceramic bolt, and recovering a sample; mechanical treatment: the sample obtained above is subjected to mechanical processing and appropriate surface treatment to finally obtain the required Ti3SiC2A ceramic;
the commercial Ti3SiC2The diameter of the powder is 200 meshes, and the purity is 96% -98%;
the slurry is sieved, wherein the specification of a selected screen is 400-800 meshes;
in the mixed solution of the hydrochloric acid and the hydrofluoric acid, the volume ratio of the hydrochloric acid to the hydrofluoric acid is controlled to be 2: 1-4: 1;
the mixture is initially pressed in a mould, and the mould pressing pressure is controlled to be 15-35 MPa;
the surface pressure bearing of the outer cover is 1-5 MPa.
The invention provides a pressure-bearing Ti preparation method3SiC2Reverse thermal expansion synthesis method of ceramic and hot pressing sintering method, hot isostatic pressing sintering method and the like widely adopted at present for preparing Ti3SiC2Compared with the method, the method has the following advantages: (1) the reaction sintering process is simple and low in cost: the synthesis technology only adopts the method of fixing by external pressure bearing of a die and utilizing the pressure formed by sintering self thermal expansion reverse to a blank to compact and sinter the blank, and the Ti can be finished by only a simple atmosphere sintering furnace3SiC2The ceramic has simple sintering preparation and low synthesis cost. (2) The prepared ceramic has high purity: the technology adopts powder thinning and binary acidification treatment, can remove trace metal compounds and solid solution metal impurities in the powder, and the purity of the actually synthesized ceramic can reach more than 99 percent. (3) The size and shape of the prepared ceramic are not limited: the process of sintering and densifying the blank body is formed by reaction in the die, and the synthesized Ti can be formed as long as the size of the pressure-bearing ceramic die is large enough3SiC2The ceramic can be free of size and shape limitations, and is particularly suitable for larger size Ti3SiC2And (4) preparing a ceramic special-shaped piece.
Drawings
The invention is described in further detail below with reference to the following figures and embodiments:
FIG. 1 is a schematic view of a pressure-bearing mold assembly;
wherein, A: and (3) a ceramic bolt B: and (4) pressing a cover C of the upper die: buffer ceramic gasket
D: pressure-bearing powder E: ti3SiC2A ceramic green body F, a lower die container.
FIG. 2 shows synthesized Ti3SiC2And (5) XRD detection results of the ceramics.
Detailed Description
Example 1
Weighing 300g of Ti3SiC2Adding 400mL of ethanol and 600g of agate balls into powder, putting the powder into a ball milling tank, ball milling for 4h at the speed of 400r/min, passing the ball-milled slurry through a 500-mesh sieve by a wet method, keeping the temperature of the sieved slurry in an oven for 12h, setting the temperature of the oven at 45 ℃, acidifying the dried powder for 30min by hot phosphoric acid, cooling and separating, adding the powder subjected to hot phosphoric acid treatment into a mixed solution of hydrochloric acid and hydrofluoric acid with the volume ratio of 2:1 for binary acid washing, cooling, diluting, centrifuging, recovering and purifying the powder obtained after acid washing, adding a small amount of 3% PVA into the purified powder for granulation, putting the powder into a mold for 20MPa pressure treatment, carrying out 120MPa treatment by using a cold isostatic press after mold pressing, and keeping the pressure for 5min to obtain a green body; placing the obtained green body into a corundum mold, adding 500g of inert pressure-bearing powder, adding a 1MPa pressure-bearing fixed mold, placing the obtained green body into a high-temperature atmosphere furnace at 1400 ℃ for reaction for 0.5h as the schematic view of the assembly of the pressure-bearing mold shown in figure 1, cooling to room temperature, performing mechanical processing and proper surface treatment on the obtained sample, and finally obtaining high-purity Ti3SiC2Ceramic, FIG. 2 is synthetic Ti3SiC2And (5) XRD detection results of the ceramics.
Example 2
Weighing 400g of Ti3SiC2Adding 500mL of ethanol and 600g of agate balls into powder, putting the powder into a ball milling tank, ball milling for 12h at the speed of 500r/min, sieving the ball-milled slurry through a 600-mesh sieve by a wet method, keeping the temperature of the sieved slurry in an oven for 24h, setting the temperature of the oven at 30 ℃, acidifying the dried powder for 60min by hot phosphoric acid, cooling and separating, and adding the powder treated by the hot phosphoric acid into the volume ratioCarrying out binary acid pickling in a mixed solution of hydrochloric acid and hydrofluoric acid with the ratio of 3:1, cooling, diluting, centrifugally recovering and purifying the powder obtained after acid pickling, adding a small amount of 3% PVA into the purified powder for granulation, putting the powder into a mould for 25MPa pressurization treatment, carrying out 120MPa treatment by using a cold isostatic press after mould pressing, and keeping the pressure for 8min to obtain a green body. Putting the obtained green body into a corundum mold, adding 600g of inert pressure-bearing powder, adding a 2MPa pressure-bearing fixed mold, putting the mixture into a high-temperature atmosphere furnace for reacting for 1.5h at 1350 ℃, cooling to room temperature, carrying out mechanical processing and appropriate surface treatment on the obtained sample, and finally obtaining high-purity Ti3SiC2A ceramic.
Example 3
Weighing 250g of Ti3SiC2Adding 350mL of ethanol and 350g of zirconia grinding balls into powder, ball-milling the powder for 2.5h in a ball-milling tank at the speed of 350r/min, passing the ball-milled slurry through a 800-mesh sieve by a wet method, keeping the temperature of the screened slurry in an oven for 15h, setting the temperature of the oven at 40 ℃, acidifying the dried powder for 45min by hot phosphoric acid, cooling and separating, adding the powder subjected to hot phosphoric acid treatment into a mixed solution of hydrochloric acid and hydrofluoric acid with the volume ratio of 4:1 for binary acid washing, cooling, diluting, centrifugally recovering and purifying the powder obtained after acid washing, adding a small amount of 3% PVA into the purified powder for granulation, putting the powder into a mold for 15MPa pressure treatment, carrying out pressure treatment by a cold isostatic press for 180MPa after mold pressing, and keeping the pressure for 5min to obtain a green body. Putting the obtained green body into a corundum mold, adding 600g of inert pressure-bearing powder, adding a 1MPa pressure-bearing fixed mold, putting the mixture into a high-temperature atmosphere furnace for reaction at 1300 ℃ for 2h, cooling to room temperature, carrying out mechanical processing and appropriate surface treatment on the obtained sample, and finally obtaining high-purity Ti3SiC2A ceramic.
Example 4
Weighing 1000g of Ti3SiC2Adding 1000mL of ethanol and 1200g of zirconia grinding balls into powder, putting the powder into a ball milling tank, ball milling for 6h at the speed of 400r/min, screening the ball milled slurry through a 500-mesh sieve by a wet method, keeping the temperature of the screened slurry in an oven for 16h, setting the temperature of the oven at 35 ℃, acidifying the powder obtained after drying for 50min by hot phosphoric acid, cooling and separating, and then adding the powder into a reactorAdding the powder treated by hot phosphoric acid into a mixed solution of hydrochloric acid and hydrofluoric acid with a volume ratio of 2.5:1 for binary acid cleaning, cooling and diluting the powder obtained after acid cleaning, centrifugally recovering and purifying, adding a small amount of 3% PVA into the purified powder for granulation, then putting the powder into a mould for 30MPa pressurization treatment, carrying out 200MPa treatment by using a cold isostatic press after mould pressing, and maintaining the pressure for 5min to obtain a green body. Putting the obtained green body into a corundum mold, adding 800g of inert pressure-bearing powder, adding a 3MPa pressure-bearing fixed mold, putting the mixture into a high-temperature atmosphere furnace, sintering at 1400 ℃ for 1.5h, cooling to room temperature, carrying out mechanical processing and appropriate surface treatment on the obtained sample, and finally obtaining high-purity Ti3SiC2A ceramic.
Claims (1)
1. Pressure-bearing preparation of Ti3SiC2The synthesis method of ceramic with reverse thermal expansion includes the following steps:
firstly, refining raw materials: firstly, Ti3SiC2Mixing the powder with ethanol of the same mass, and adding Ti of the same mass3SiC22-5 times of agate balls or zirconia balls of the powder are ball-milled for 4-12 hours on a high-speed ball mill to obtain ball-milled slurry;
step two, sieving and drying: sieving the ball-milled slurry, keeping the temperature of the sieved slurry in an oven for 12-24h, controlling the temperature of the oven to be 30-45 ℃, and recovering after the powder is completely dried;
step three, powder purification: recovering the above-mentioned Ti3SiC2Adding the powder into hot phosphoric acid for acidification for 30-60min, cooling and separating, adding the primarily acidified powder into a mixed solution of hydrochloric acid and hydrofluoric acid for secondary acidification treatment, controlling the temperature at 50-60 ℃ and the acidification time at 30-60min, cooling and diluting the treated powder, and centrifuging and recovering;
step four, green body preparation: adding 3-5% of PVA into the purified powder for granulation, placing the mixture into a mold with a fixed shape for primary pressing to obtain a rough blank, placing the obtained rough blank into a cold isostatic press, and treating for 5-10min under the pressure of 120-200MPa to obtain a green blank with certain strength;
fifthly, bearing and fixing: putting the obtained green body into a corundum mold, adding inert pressure-bearing powder, adding an outer cover, and screwing down the high-strength ceramic bolt;
sixthly, atmosphere sintering: placing the corundum mold into an atmosphere furnace for sintering, wherein the sintering temperature is 1300-1400 ℃, reacting for 0.5-2h, cooling the mold to room temperature along with the furnace after the reaction, unscrewing the ceramic bolt, and recovering a sample;
seventh step, mechanical treatment: machining and surface treating the sample to obtain Ti3SiC2A ceramic;
ti described in the first step3SiC2The diameter of the powder is 200 meshes, and the purity is 96-98%;
the slurry is sieved in the second step, wherein the specification of the selection of a screen is 400-800 meshes;
in the mixed solution of the hydrochloric acid and the hydrofluoric acid in the third step, the volume ratio of the hydrochloric acid to the hydrofluoric acid is controlled to be between 2:1 and 4: 1;
the fourth step is that the mixture is initially pressed in a mould, and the mould pressing pressure is controlled to be 15-35 MPa;
and in the fifth step, the surface pressure bearing of the outer cover is 1-5 MPa.
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