CN107140960A - The method of discharge plasma sintering alumina-based eutectic ceramic composite - Google Patents

The method of discharge plasma sintering alumina-based eutectic ceramic composite Download PDF

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CN107140960A
CN107140960A CN201710279867.9A CN201710279867A CN107140960A CN 107140960 A CN107140960 A CN 107140960A CN 201710279867 A CN201710279867 A CN 201710279867A CN 107140960 A CN107140960 A CN 107140960A
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eutectic
powder
sample
sintering
ceramic composite
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CN107140960B (en
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苏海军
任俊飞
张军
刘林
黄太文
郭敏
傅恒志
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Northwestern Polytechnical University
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Abstract

A kind of method of discharge plasma sintering alumina-based eutectic ceramic composite, the uniform ROD EUTECTIC sample of fine microstructures is prepared for using realizing laser suspension zone-melting directional solidification technology；The internal eutectic powder for including eutectic structure is obtained by pulverizing and sieving；The internal alumina-based eutectic ceramic composite for remaining with eutectic structure is prepared using discharge plasma sintering.Sintering eutectic composites prepared by the present invention remain the eutectic structure among initial eutectic sample, and eliminate most of crystal boundary and interface amorphous phase, and the preparation for large scale alumina-based eutectic ceramic composite provides a kind of new approaches.The tissue that the present invention is obtained is in typical " pictograph " Eutectic Morphology, and eutectic particle size distribution is at 4~12 μm and more than eutectic lamellar spacing, and particle inside can be effectively retained the eutectic structure among initial eutectic sample.Because sintering time is short, effectively suppresses the tissue during sintering and grow up, be conducive to obtaining the eutectic ceramic of uniform fine tissue.

Description

The method of discharge plasma sintering alumina-based eutectic ceramic composite
Technical field
The present invention relates to superhigh temperature structural ceramics field, there is eutectic structure particular by discharge plasma sintering inside Eutectic powder prepare blocks of large alumina-based eutectic ceramic composite.
Technical background
Alumina-based composite ceramics with its excellent mechanical behavior under high temperature, natural oxidation resistance and relatively low density, It is expected to use in high temperature oxidation stability environment as superhigh temperature structural material, thus in aviation and ground gas turbine high-temperature heat-resistance Field of components has wide application potential.Up to now, the main preparation method of alumina-based composite ceramics is powder sintered Method, but its material prepared is general in polycrystalline structure, and there is crystal boundary, stomata and interface amorphous phase in material internal, cause material Uniformity and bad stability under high temperature water oxygen environment are organized in, so that intensity declines rapidly, its work is significantly limit Used for superhigh temperature structural material.Document (Oelgardt C, Anderson J, Heinrich J G, et al.Sintering, Microstructure and Mechanical Properties of Al2O3/Y2O3/ZrO2(AYZ)Eutectic Composition Ceramic Microcomposites[J].Journal of the European Ceramic Society,2010,30(3):649-656), by sintering nanoscale Al respectively without pressure and hot pressing2O3/Y2O3/ZrO2Eutectic composition Powder, obtains the block materials of the eutectic composition of high densification, the hardness of material is 16~19GPa, slightly above congruent fixed To solidification eutectic material (15~17GPa), and fracture toughness is broken for 2.3~4.7MPa.m1/2, it is solidifying relative to congruent orientation Gu material (3~9MPa.m1/2) relatively low.In addition, as a result showing, relative to pressureless sintering, hot pressed sintering can be in lower sintering temperature It is lower to obtain high fine and close material, while reducing the degree that crystal grain is grown up in sintering process, but pass through hot pressed sintering eutectic composition powder End can only prepare particulate composite, and the crystal boundary and interface amorphous phase that material internal is present cause its mechanical property at high temperature It is deteriorated with structure stability.
And preparing oxide eutectic ceramics using directional solidification technique can be such that materials microstructure is arranged by specific direction, altogether Brilliant two-phase is spontaneous compound from melt, and monocrystalline mutually runs through on three dimensions, mutually wound, so that it is clean to form interface Only the irregular eutectic solidification structures, being well combined, while eliminating the hole and interface amorphous phase in sintered powder material.Text Offer (Su H, Zhang J, Cui C, et al.Rapid solidification of Al2O3/Y3Al5O12/ZrO2, eutectic in situ composites by laser zone remelting[J].Journal of Crystal Growth,2007,307(2):448-456.), it is prepared for using realizing laser suspension zone-melting with the bar-shaped of different eutectic structure sizes Al2O3/YAG/ZrO2Eutectic sample, wherein when withdrawing rate is 1000 μm/s, synusia spacing is decreased to 0.15 μm.Meanwhile, make Person tests its hardness and fracture toughness, the Al of acquisition using indentation method2O3/YAG/ZrO2Eutectic hardness is 16.67GPa, is broken Split toughness and reach 8.01MPa.m1/2, with external highest level 9MPa.m1/2Quite.However, being melted because oxide ceramics is higher The limitation of point and current directional solidification technique, it is more difficult to larger-size alumina-based eutectic ceramic is prepared, so as to limit eutectic The application of material.So, in the urgent need to conducting a research with independent intellectual property right and the oxidation that disclosure satisfy that commercial Application condition The technology of preparing of aluminium base eutectic material.
Therefore, researcher, which has turned one's attention to, can prepare the sintering technology of large dimension specimen, and propose by crushing Melt growth eutectic sample prepares eutectic powder, and the new preparation of large scale eutectic ceramic is then prepared by the way of sintering Method.Document (Mah Tai-Il, Parthasarathy Triplicane A, Kerans Ronald J.Processing, Microstructure,and Strength of Alumina–YAG Eutectic Polycrystals[J].Journal of the American Ceramic Society,2010,83(8):2088-2090.), it is prepared for by electric arc melting Al2O3/ YAG eutectics, then obtain the eutectic powder particle that particle diameter is less than 150 μm, finally hot pressing at high temperature by crushing Sintering is so as to obtain the sintering eutectic composite ceramics of high densification, and it remains the eutectic knot in eutectic powder particle in organizing Structure, while bending strength is 270 ± 61MPa at room temperature, higher than congruent sintered particle composite material, but because it was prepared Without the removal less eutectic powder particle of particle diameter in journey, thus substantial amounts of monophased particles can be introduced in sintering process, so obtaining To sintering eutectic ceramic material in occur in that more thick polycrystalline tissue.Document (the quick .ZrB of Chen Si2- SiC eutectic sintered bodies Preparation and its performance study [D] Wuhan University of Technologys, 2011.), with ZrB2- SiC meltings body is raw material, using crushing, grind Mill and repeatedly sieving are prepared for the eutectic powder of different-grain diameter, are then prepared for densification using discharge plasma sintering technique ZrB2- SiC sinters eutectic, and its Fracture Toughness is compared and direct sintering ZrB2, SiC powder improve 15%, but electric arc is molten The microstructure of the standby initial eutectic sample of refining is uneven, causes tissue of sintered body uneven, so that material property can be limited Performance.
So, in view of the application to alumina-based eutectic ceramic needs, the present invention proposes one kind and prepares large scale oxidation The novel method of thing eutectic ceramic.This method prepares tissue, eutectic sample of good performance using realizing laser suspension zone-melting technology, so Afterwards by having the eutectic powder of eutectic structure to prepare large-sized alumina base eutectic composite wood inside discharge plasma sintering Material.
The content of the invention
To overcome the microstructure of initial eutectic sample present in prior art uneven, cause tissue of sintered body uneven Even, so that the deficiency of the performance of material property can be limited, the present invention proposes a kind of discharge plasma sintering alumina base eutectic The method of ceramic composite.
The present invention detailed process be：
Step 1, sample prefabricated body blank is prepared.
It is described when preparing sample prefabricated body blank, with Al2O3And Y2O3Or Er2O3Or Gd2O3For raw material, or with Al2O3、 Y2O3And ZrO2Powder is raw material, described Al2O3、Y2O3、Er2O3、Gd2O3And ZrO2It is powdered.
When with Al2O3And Y2O3During for raw material, according to Al2O3/Y2O3The eutectic point proportioning of phasor；
When with Al2O3And Er2O3During for raw material, according to Al2O3/Er2O3Phasor eutectic point is matched；
When with Al2O3And Gd2O3During for raw material, according to Al2O3/Gd2O3Phasor eutectic point is matched；
Or with Al2O3、Y2O3And ZrO2Powder is raw material, according to Al2O3/Y2O3/ZrO2Phasor eutectic point is matched；
Described ratio is mol ratio.
Poly-vinyl alcohol solution and absolute ethyl alcohol are added in load weighted mixed-powder and carries out being sufficiently mixed stirring；Ball milling The rotating speed of machine is 550r/min, and mixing time is 5h, obtains well mixed mixed-powder.The addition of the polyvinyl alcohol is 10~15ml poly-vinyl alcohol solution is added in raw material described in per 100g；The addition of the absolute ethyl alcohol is per in 100g raw materials Add 50~60ml.
Described poly-vinyl alcohol solution is 5g polyvinyl alcohol to be added in 100ml pure water and heating makes polyvinyl alcohol molten Solution is obtained.
Drying and processing is carried out to obtained mixed-powder, well mixed ceramic powders are obtained；Drying temperature is 80 DEG C, is dried The dry time is 12h.It will be put into by the ceramic powders of drying and processing in mould, 100MPa uniaxial tensions applied to the powder, protected Unloading pressure after 3min is pressed, sample is obtained.Obtained sample is put into sintering furnace, 2h, sintering temperature are sintered in atmospheric environment Spend for 1400~1500 DEG C, obtain the precast body of an eutectic ceramic in situ composite sample.
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple sample prefabricated body bases are obtained Material.
Step 2, sample is prepared.
Repeated melting-- draw process, the sample prefabricated body blank that step 1 is obtained, which prepares to turn into, has fine uniform The sample of eutectic structure.Using the obtained average eutectic lamellar spacing of the sample as between the average eutectic lamellar of all samples Away from.
Preparing the detailed process of sample is：
The precast body of obtained eutectic ceramic in situ composite sample is respectively cut as precast body.One of those is prefabricated Body is fixed on the specimen mounting of realizing laser suspension zone-melting pull system.Open laser to heat the precast body, make the precast body Melt and form stable melting zone.Pull system is opened, pull is carried out to the melting zone with 50~200 μm/s withdrawing rate, Complete the directional solidification of sample.
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so that Obtain multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure.
Arbitrarily take one of sample and metallographic processing is carried out to it.Pass through the tissue of the scanning electron microscopic observation sample.Adopt With method of scoring, the average eutectic lamellar spacing of the sample is obtained.
Step 3, eutectic particle is prepared.The particle diameter of described eutectic particle is 4~12 μm, is remained inside individual particle Eutectic structure tissue.
It is described prepare eutectic particle detailed process be：
All samples obtained using ultrasonic wave to step 2 are cleaned.By all broken after cleaning and sieve, obtain Particle size is less than 1mm coarse granule.
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball It is 10 with coarse grained mass ratio:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/ of the ball milling tank volume 5.Ball mill is opened, with 500r/min rotating speed to coarse granule 3~4h of ball milling, eutectic powder is obtained.To obtained eutectic powder Drying is to being completely dried.
During the eutectic powder being completely dried described in vibrosieve, the eutectic powder is placed in the screen cloth that aperture is 12 μm, The screen cloth that aperture is 4 μm is placed in the lower section of 12 μm of screen clothes.Continue to add nothing into the eutectic powder in vibrosieve Water-ethanol；The addition of absolute ethyl alcohol described in vibrosieve is advisable so that the eutectic powder in screen cloth is flooded.
Step 4, the preparation of block eutectic ceramic composite.Block eutectic is prepared by the method for discharge plasma sintering Ceramic composite, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder.One layer is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron nitride；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove；To the plasma discharging stove evacuation extremely Vacuum is higher than 5 × 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure.Start heating electricity Source is to the plasma discharging stove heat.
3rd, plasma discharging stove is warming up to 500~600 DEG C with 120~200 DEG C/min speed.Hot pressing furnace continue with 100~150 DEG C/min speed is warming up to 1550~1580 DEG C, and is incubated 5~10min.Insulation terminate after, stop heating and with Stove is cooled to room temperature, obtains the internal block eutectic ceramic composite for remaining with eutectic structure.In cooling procedure, when described When the temperature of plasma discharging stove is down to 500 DEG C, removal pressure obtains block eutectic ceramic composite.Obtained block is total to The relative density of brilliant ceramic composite is 97.9~98.8%.
In order to prepare large scale and the tiny alumina-based eutectic ceramic composite of interior tissue, the present invention utilizes laser Floating zone melts directional solidification technique and is prepared for the uniform ROD EUTECTIC sample of fine microstructures, then obtains internal by pulverizing and sieving Include the eutectic powder of eutectic structure, the internal aluminum oxide for remaining with eutectic structure is finally prepared using discharge plasma sintering Base eutectic ceramic composite.
In contrast to congruent Particles dispersed ceramics, sintering eutectic composites prepared by the present invention remain initial eutectic Eutectic structure among sample, and most of crystal boundary and interface amorphous phase are eliminated, and then be large scale alumina base eutectic The preparation of ceramic composite provides a kind of new approaches.
Compared with prior art, the present invention achieves following beneficial effect：
(1) it is prepared for that surface is smooth, flawless alumina base eutectic is total to using realizing laser suspension zone-melting directional solidification technology Brilliant spontaneous composite ceramics, its outward appearance using ESEM as shown in figure 1, analyzed its interior tissue, its tissue is in simultaneously Typical " pictograph " Eutectic Morphology, as shown in Figure 2.
(2) effectively the original eutectic structure of the overwhelming majority is retained again by choosing suitable eutectic powder particle diameter In agglomerated material.Wherein, when withdrawing rate is 200 μm/s, eutectic lamellar spacing is 0.66~1.23 μm, eutectic grain graininess It is distributed in 4~12 μm and more than eutectic lamellar spacing, therefore particle inside can be effectively retained the eutectic among initial eutectic sample Structure, as shown in Figure 3.
(3) eutectic powder is densified by discharge plasma sintering, preparation remains with a large amount of tiny eutectic structures Alumina-based eutectic ceramic composite, its outward appearance is as shown in Figure 4.In addition, Fig. 5 is the institutional framework in Fig. 4 Sample As region, As can be seen that including the eutectic powder of eutectic structure by sintering inside, so as to remain being total among initial eutectic sample Crystal structure, it organizes same in typical " pictograph " Eutectic Morphology.
(4) in discharge plasma sintering technique, due to its faster heating rate, powder can heat up in several minutes To sintering temperature, sintering time is substantially reduced, is grown up therefore, it is possible to effectively suppress the tissue during sintering, so as to be beneficial to obtain Obtain the eutectic ceramic of uniform fine tissue.
Brief description of the drawings
Fig. 1 is the Al prepared by realizing laser suspension zone-melting when freezing rate is 200 μm/s and heating power is 400W2O3/YAG The spontaneous ceramic macrospecimen picture of ROD EUTECTIC.
Fig. 2 is the Al that realizing laser suspension zone-melting is obtained when freezing rate is 200 μm/s2O3The cross section of/YAG club-shaped materials Solidified structure scanning electron microscopic picture.
Fig. 3 is by the scanning electron microscopic picture of 4~12 μm of eutectic particles obtained after crushing and screening in the present invention.
Fig. 4 is the block Al of 4~12 μm of eutectic particle preparations of sintering2O3The photomacrograph of/YAG eutectic ceramic composites.
Fig. 5 is Al shown in Fig. 42O3The macrograph in/YAG eutectic ceramic composite As region
Fig. 6 is the process chart of the present invention.
Embodiment
Embodiment one
This implementation is that one kind prepares Al2O3The method of/YAG block eutectic ceramic composites, detailed process includes following step Suddenly：
Step 1, Al2O3The preparation of the sample prefabricated body of/YAG eutectic ceramic in situ composite.Al using purity as 99.99%2O3 And Y2O3Powder is raw material, according to Al2O3/Y2O3The eutectic point proportioning of phasor, polyethylene is added in load weighted mixed-powder Alcoholic solution and absolute ethyl alcohol simultaneously carry out being sufficiently mixed stirring；The rotating speed of ball mill is 550r/min, and mixing time is 5h, is mixed Close uniform mixed-powder.The polyvinyl alcohol that the addition of the polyvinyl alcohol is addition 15ml in raw material described in per 100g is molten Liquid；The addition of the absolute ethyl alcohol is to add 50ml per in 100g raw materials.The poly-vinyl alcohol solution added is by the poly- second of 5g Enol, which is added in 100ml pure water and heated, makes polyvinyl alcohol be obtained after dissolving.
Drying and processing is carried out to obtained mixed-powder, well mixed Al is obtained2O3/Y2O3Ceramic powders；Drying temperature For 80 DEG C, drying time is 12h.8g is passed through to the Al of drying and processing2O3/Y2O3Ceramic powders are put into by alcohol washes not In steel mold of becoming rusty, unloading pressure after 100MPa uniaxial tensions, pressurize 3min is applied to powder by forcing press, length and width high score is obtained Not Wei 70mm × 12mm × 4mm plate tensile sample.Obtained plate tensile sample is put into sintering furnace, sintered in atmospheric environment 2h, sintering temperature is 1500 DEG C, obtains Al2O3The precast body of/YAG eutectic ceramic in situ composite samples.In sintering, Al2O3With Y2O3Solid phase reaction occurs for powder, and the phase composition of material is changed into Al2O3With YAG two-phases.
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple Al are obtained2O3/ YAG eutectics The precast body blank of spontaneous composite ceramics sample.In the present embodiment, the precast body blank of preparation is 40.
Step 2, sample is prepared.Using diamond precision gas cutting machine by obtained multiple Al2O3The spontaneous composite ceramic of/YAG eutectics The precast body of porcelain sample is respectively cut as a height of 70mm × 4mm of length and width × 4mm strip precast body.By one of precast body On the specimen mounting for being placed in realizing laser suspension zone-melting pull system, clamping is reinforced.Laser is opened, the power of laser is risen to 400W, is heated to the precast body, melts the precast body, and forms stable melting zone.Pull system is opened, with 200 μm/s Withdrawing rate to the melting zone carry out pull, complete sample directional solidification.
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so that Obtain multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure.The sample A diameter of 2.8 ± 0.2mm, high 5 ± 0.5cm.
Arbitrarily take one of sample and metallographic processing is carried out to it.Pass through the tissue of the scanning electron microscopic observation sample.Adopt With method of scoring, the average eutectic lamellar spacing for obtaining the bar samples is 1.23 μm.It is total to obtained the average of the bar samples Crystal layer piece spacing as all bar samples average eutectic lamellar spacing.
Step 3, Al is prepared2O3/ YAG eutectic particles.The particle diameter of described eutectic particle is 4~12 μm.Detailed process is：
All bar samples obtained using ultrasonic wave to step 2 are cleaned.All bar samples after cleaning are put In the jaw crusher that jaw is high-purity zirconia and Mechanical Crushing is graininess.By obtained pellet through sieves, particle is obtained Size is less than 1mm Al2O3/ YAG coarse granules.
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball It is 10 with coarse grained mass ratio:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/ of the ball milling tank volume 5.Ball mill is opened, with 500r/min rotating speed to coarse granule ball milling 4h, eutectic powder is obtained.Eutectic powder drying to obtaining To being completely dried.
The eutectic powder of drying is sieved.Specifically, the eutectic powder of drying is placed in the screen cloth that aperture is 12 μm In, the screen cloth that aperture is 4 μm is placed in the lower section of 12 μm of screen clothes, vibrosieve is carried out.Continue in vibrosieve to described Absolute ethyl alcohol is added in eutectic powder；The addition of absolute ethyl alcohol described in vibrosieve is so that the eutectic powder in screen cloth to be flooded It is advisable.
After screening, the powder in 4 μm of screen clothes is taken out, the Al that targeted particle size is 4~12 μm is obtained2O3/ YAG eutectic powders. Because obtained Al2O3The size of/YAG eutectic powders is more than the eutectic spacing of club-shaped material, so being protected inside individual particle Eutectic structure tissue is stayed.
Step 4, block Al2O3The preparation of/YAG eutectic ceramic composites.Prepared by the method for discharge plasma sintering Block Al2O3/ YAG eutectic ceramic composites, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder.One layer is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron nitride；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove, is closed furnace chamber, is vacuumized, work as vacuum Higher than 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure.Start heating power supply to put this Electric plasma heating furnace heating.
3rd, plasma discharging stove is warming up to 600 DEG C with 150 DEG C/min speed.Hot pressing furnace continues with 100 DEG C/min's Speed is warming up to 1580 DEG C, and is incubated 10min.After insulation terminates, stop heating and cooling to the furnace room temperature, obtain internal retain There is the block eutectic ceramic composite of eutectic structure.In cooling procedure, when the temperature of the plasma discharging stove is down to 500 DEG C when, removal pressure.
Obtained block eutectic ceramic composite is tested through Archimedes's drainage, the block eutectic ceramic composite wood Relative density is 98.8%.
Embodiment two
This implementation is that one kind prepares Al2O3/YAG/ZrO2The method of block eutectic composite ceramic material, detailed process includes Following steps：
Step 1, Al2O3/YAG/ZrO2The preparation of the sample prefabricated body of eutectic ceramic in situ composite.Using purity as 99.99% Al2O3、Y2O3And ZrO2Powder is raw material, according to Al2O3/Y2O3/ZrO2Phasor eutectic point is matched.In load weighted mixed-powder Middle addition poly-vinyl alcohol solution and absolute ethyl alcohol simultaneously carry out being sufficiently mixed stirring；The rotating speed of ball mill is 550r/min, during stirring Between be 5h, obtain well mixed mixed-powder.The addition of the polyvinyl alcohol adds 10ml in the raw material described in per 100g Poly-vinyl alcohol solution；The addition of the absolute ethyl alcohol is to add 55ml per in 100g raw materials.The polyvinyl alcohol added is molten Liquid is that 5g polyvinyl alcohol is added in 100ml pure water and heated polyvinyl alcohol is obtained after dissolving.
Drying and processing is carried out to obtained mixed-powder, well mixed Al is obtained2O3/Y2O3/ZrO2Ceramic powders；Drying Temperature is 80 DEG C, and drying time is 12h.10g is passed through to the Al of drying and processing2O3/Y2O3/ZrO2Ceramic powders are put into by alcohol In the stainless steel mould of cleaning, unloading pressure after 100MPa uniaxial tensions, pressurize 3min is applied to powder by forcing press, obtained Length, width and height are respectively 70mm × 12mm × 4mm plate tensile sample.Obtained plate tensile sample is put into sintering furnace, in atmospheric environment Middle sintering 2h, sintering temperature is 1400 DEG C, obtains Al2O3/YAG/ZrO2The precast body of eutectic ceramic in situ composite sample.Sintering In, Al2O3And Y2O3Solid phase reaction occurs for powder, and the phase composition of material is changed into Al2O3With YAG two-phases.
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple Al are obtained2O3/YAG/ ZrO2The precast body blank of eutectic ceramic in situ composite sample.In the present embodiment, the precast body blank of preparation is 40.
Step 2, sample is prepared.Using diamond precision gas cutting machine by obtained multiple Al2O3/YAG/ZrO2Eutectic is spontaneous The precast body of composite ceramics sample is respectively cut as a height of 70mm × 4mm of length and width × 4mm strip precast body.By one of those Precast body is placed on the specimen mounting of realizing laser suspension zone-melting pull system, reinforces clamping.Laser is opened, by the power liter of laser To 300W, the precast body is heated, the precast body is melted, and forms stable melting zone.Pull system is opened, with 50 μm/s Withdrawing rate to the melting zone carry out pull, complete sample directional solidification.
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so that Obtain multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure.The sample A diameter of 2.8 ± 0.2mm, high 5 ± 0.5cm.
Arbitrarily take one of sample and metallographic processing is carried out to it.Pass through the tissue of the scanning electron microscopic observation sample.Adopt With method of scoring, the average eutectic lamellar spacing for obtaining the bar samples is 0.66 μm.It is total to obtained the average of the bar samples Crystal layer piece spacing as all bar samples average eutectic lamellar spacing.
Step 3, Al is prepared2O3/YAG/ZrO2Eutectic particle.The particle diameter of described eutectic particle is 4~12 μm.Specific mistake Cheng Shi：
All bar samples obtained using ultrasonic wave to step 2 are cleaned.All bar samples after cleaning are put In the jaw crusher that jaw is high-purity zirconia and Mechanical Crushing is graininess.By obtained pellet through sieves, particle is obtained Size is less than 1mm Al2O3/YAG/ZrO2Coarse granule.
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball It is 10 with coarse grained mass ratio:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/ of the ball milling tank volume 5.Ball mill is opened, with 500r/min rotating speed to coarse granule ball milling 3h, eutectic powder is obtained.Eutectic powder drying to obtaining To being completely dried.
The eutectic powder of drying is sieved.Specifically, the eutectic powder of drying is placed in the screen cloth that aperture is 12 μm In, the screen cloth that aperture is 4 μm is placed in the lower section of 12 μm of screen clothes, vibrosieve is carried out.Continue in vibrosieve to described Absolute ethyl alcohol is added in eutectic powder；The addition of absolute ethyl alcohol described in vibrosieve is so that the eutectic powder in screen cloth to be flooded It is advisable.
After screening, the powder in 4 μm of screen clothes is taken out, the Al that targeted particle size is 4~12 μm is obtained2O3/YAG/ZrO2Eutectic Powder.Because obtained Al2O3/YAG/ZrO2The size of eutectic powder is more than the eutectic lamellar spacing of club-shaped material, so Eutectic structure tissue is remained inside individual particle.
Step 4, block Al2O3/YAG/ZrO2The preparation of eutectic ceramic composite.Pass through the side of discharge plasma sintering Method prepares block Al2O3/YAG/ZrO2Eutectic ceramic composite, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder.One layer is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron nitride；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove, is closed furnace chamber, is vacuumized, work as vacuum Higher than 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure.Start heating power supply to put this Electric plasma heating furnace heating.
3rd, plasma discharging stove is warming up to 500 DEG C with 120 DEG C/min speed.Hot pressing furnace continues with 100 DEG C/min's Speed is warming up to 1550 DEG C, and is incubated 10min.After insulation terminates, stop heating and cooling to the furnace room temperature, obtain internal retain There is the block eutectic ceramic composite of eutectic structure.In cooling procedure, when the temperature of the plasma discharging stove is down to 500 DEG C when, removal pressure.
Obtained block eutectic ceramic composite is tested through Archimedes's drainage, the block eutectic ceramic composite wood Relative density is 97.9%.
Embodiment three
This implementation is that one kind prepares Al2O3/YAG/ZrO2The method of block eutectic composite ceramic material, detailed process includes Following steps：
Step 1, Al2O3/YAG/ZrO2The preparation of the sample prefabricated body of eutectic ceramic in situ composite.Using purity as 99.99% Al2O3、Y2O3And ZrO2Powder is raw material, according to Al2O3/Y2O3/ZrO2Phasor eutectic point is matched.In load weighted mixed-powder Middle addition poly-vinyl alcohol solution and absolute ethyl alcohol simultaneously carry out being sufficiently mixed stirring；The rotating speed of ball mill is 550r/min, during stirring Between be 5h, obtain well mixed mixed-powder.The addition of the polyvinyl alcohol adds 13ml in the raw material described in per 100g Poly-vinyl alcohol solution；The addition of the absolute ethyl alcohol is to add 60ml per in 100g raw materials.The polyvinyl alcohol added is molten Liquid is that 5g polyvinyl alcohol is added in 100ml pure water and heated polyvinyl alcohol is obtained after dissolving.
Drying and processing is carried out to obtained mixed-powder, well mixed Al is obtained2O3/Y2O3/ZrO2Ceramic powders；Drying Temperature is 80 DEG C, and drying time is 12h.10g is passed through to the Al of drying and processing2O3/Y2O3/ZrO2Ceramic powders are put into by alcohol In the stainless steel mould of cleaning, unloading pressure after 100MPa uniaxial tensions, pressurize 3min is applied to powder by forcing press, obtained Length, width and height are respectively 70mm × 12mm × 4mm plate tensile sample.Obtained plate tensile sample is put into sintering furnace, in atmospheric environment Middle sintering 2h, sintering temperature is 1450 DEG C, obtains Al2O3/YAG/ZrO2The precast body of eutectic ceramic in situ composite sample.Sintering In, Al2O3And Y2O3Solid phase reaction occurs for powder, and the phase composition of material is changed into Al2O3With YAG two-phases.
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple Al are obtained2O3/YAG/ ZrO2The precast body blank of eutectic ceramic in situ composite sample.In the present embodiment, the precast body blank of preparation is 40.
Step 2, sample is prepared.Using diamond precision gas cutting machine by obtained multiple Al2O3/YAG/ZrO2Eutectic is spontaneous The precast body of composite ceramics sample is respectively cut as a height of 70mm × 4mm of length and width × 4mm strip precast body.By one of those Precast body is placed on the specimen mounting of realizing laser suspension zone-melting pull system, reinforces clamping.Laser is opened, by the power liter of laser To 300W, the precast body is heated, the precast body is melted, and forms stable melting zone.Open pull system, with 100 μm/ S withdrawing rate carries out pull to the melting zone, completes the directional solidification of sample.
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so that Obtain multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure.The sample A diameter of 2.8 ± 0.2mm, high 5 ± 0.5cm.
Arbitrarily take one of sample and metallographic processing is carried out to it.Pass through the tissue of the scanning electron microscopic observation sample.Adopt With method of scoring, the average eutectic lamellar spacing for obtaining the bar samples is 0.49 μm.It is total to obtained the average of the bar samples Crystal layer piece spacing as all bar samples average eutectic lamellar spacing.
Step 3, Al is prepared2O3/YAG/ZrO2Eutectic particle.The particle diameter of described eutectic particle is 4~12 μm.Specific mistake Cheng Shi：
All bar samples obtained using ultrasonic wave to step 2 are cleaned.All bar samples after cleaning are put In the jaw crusher that jaw is high-purity zirconia and Mechanical Crushing is graininess.By obtained pellet through sieves, particle is obtained Size is less than 1mm Al2O3/YAG/ZrO2Coarse granule.
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball It is 10 with coarse grained mass ratio:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/ of the ball milling tank volume 5.Ball mill is opened, with 500r/min rotating speed to coarse granule ball milling 3.5h, eutectic powder is obtained.Obtained eutectic powder is dried Do to being completely dried.
The eutectic powder of drying is sieved.Specifically, the eutectic powder of drying is placed in the screen cloth that aperture is 12 μm In, the screen cloth that aperture is 4 μm is placed in the lower section of 12 μm of screen clothes, vibrosieve is carried out.Continue in vibrosieve to described Absolute ethyl alcohol is added in eutectic powder；The addition of absolute ethyl alcohol described in vibrosieve is so that the eutectic powder in screen cloth to be flooded It is advisable.
After screening, the powder in 4 μm of screen clothes is taken out, the Al that targeted particle size is 4~12 μm is obtained2O3/YAG/ZrO2Eutectic Powder.Because obtained Al2O3/YAG/ZrO2The size of eutectic powder is more than the eutectic lamellar spacing of club-shaped material, so Eutectic structure tissue is remained inside individual particle.
Step 4, block Al2O3/YAG/ZrO2The preparation of eutectic ceramic composite.Pass through the side of discharge plasma sintering Method prepares block Al2O3/YAG/ZrO2Eutectic ceramic composite, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder.One layer is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron nitride；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove, is closed furnace chamber, is vacuumized, work as vacuum Higher than 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure.Start heating power supply to put this Electric plasma heating furnace heating.
3rd, plasma discharging stove is warming up to 550 DEG C with 130 DEG C/min speed.Hot pressing furnace continues with 120 DEG C/min's Speed is warming up to 1560 DEG C, and is incubated 5min.After insulation terminates, stop heating and cooling to the furnace room temperature, obtain internal retain There is the block eutectic ceramic composite of eutectic structure.In cooling procedure, when the temperature of the plasma discharging stove is down to 500 DEG C when, removal pressure.
Obtained block eutectic ceramic composite is tested through Archimedes's drainage, the block eutectic ceramic composite wood Relative density is 98.1%.
Example IV
This implementation is that one kind prepares Al2O3The method of/EAG block eutectic composite ceramic materials, detailed process includes following step Suddenly：
Step 1, Al2O3The preparation of the sample prefabricated body of/EAG eutectic ceramic in situ composite.Al using purity as 99.99%2O3 And Er2O3Powder is raw material, according to Al2O3/Er2O3Phasor eutectic point is matched.
Poly-vinyl alcohol solution and absolute ethyl alcohol are added in load weighted mixed-powder and carries out being sufficiently mixed stirring；Ball milling The rotating speed of machine is 550r/min, and mixing time is 5h, obtains well mixed mixed-powder.The addition of the polyvinyl alcohol is 15ml poly-vinyl alcohol solution is added in raw material described in per 100g；The addition of the absolute ethyl alcohol is to be added per in 100g raw materials 60ml.The poly-vinyl alcohol solution added is 5g polyvinyl alcohol to be added in 100ml pure water and heating makes polyvinyl alcohol molten Obtained after solution.
Drying and processing is carried out to obtained mixed-powder, well mixed Al is obtained2O3/Er2O3Ceramic powders；Drying temperature Spend for 80 DEG C, drying time is 12h.8g is passed through to the Al of drying and processing2O3/Er2O3Ceramic powders are put into by alcohol washes In stainless steel mould, unloading pressure after 100MPa uniaxial tensions, pressurize 3min is applied to powder by forcing press, length, width and height are obtained Respectively 70mm × 12mm × 4mm plate tensile sample.Obtained plate tensile sample is put into sintering furnace, sintered in atmospheric environment 2h, sintering temperature is 1500 DEG C, obtains Al2O3The precast body of/EAG eutectic ceramic in situ composite samples.In sintering, Al2O3With Er2O3Solid phase reaction occurs for powder, and the phase composition of material is changed into Al2O3With EAG two-phases.
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple Al are obtained2O3/ EAG eutectics The precast body blank of spontaneous composite ceramics sample.In the present embodiment, the precast body blank of preparation is 40.
Step 2, sample is prepared.Using diamond precision gas cutting machine by obtained multiple Al2O3The spontaneous composite ceramic of/EAG eutectics The precast body of porcelain sample is respectively cut as a height of 70mm × 4mm of length and width × 4mm strip precast body.By one of precast body On the specimen mounting for being placed in realizing laser suspension zone-melting pull system, clamping is reinforced.Laser is opened, the power of laser is risen to 400W, is heated to the precast body, melts the precast body, and forms stable melting zone.Pull system is opened, with 150 μm/s Withdrawing rate to the melting zone carry out pull, complete sample directional solidification.
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so that Obtain multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure.The sample A diameter of 2.8 ± 0.2mm, high 5 ± 0.5cm.
Arbitrarily take one of sample and metallographic processing is carried out to it.Pass through the tissue of the scanning electron microscopic observation sample.Adopt With method of scoring, the average eutectic lamellar spacing for obtaining the bar samples is 0.81 μm.It is total to obtained the average of the bar samples Crystal layer piece spacing as all bar samples average eutectic lamellar spacing.
Step 3, Al is prepared2O3/ EAG eutectic particles.The particle diameter of described eutectic particle is 4~12 μm.Detailed process is：
All bar samples obtained using ultrasonic wave to step 2 are cleaned.All bar samples after cleaning are put In the jaw crusher that jaw is high-purity zirconia and Mechanical Crushing is graininess.By obtained pellet through sieves, particle is obtained Size is less than 1mm Al2O3/ EAG coarse granules.
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball It is 10 with coarse grained mass ratio:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/ of the ball milling tank volume 5.Ball mill is opened, with 500r/min rotating speed to coarse granule ball milling 4h, eutectic powder is obtained.Eutectic powder drying to obtaining To being completely dried.
The eutectic powder of drying is sieved.Specifically, the eutectic powder of drying is placed in the screen cloth that aperture is 12 μm In, the screen cloth that aperture is 4 μm is placed in the lower section of 12 μm of screen clothes, vibrosieve is carried out.Continue in vibrosieve to described Absolute ethyl alcohol is added in eutectic powder；The addition of absolute ethyl alcohol described in vibrosieve is so that the eutectic powder in screen cloth to be flooded It is advisable.
After screening, the powder in 4 μm of screen clothes is taken out, the Al that targeted particle size is 4~12 μm is obtained2O3/ EAG eutectic powders. Because obtained Al2O3The size of/EAG eutectic powders is more than the eutectic spacing of club-shaped material, so being protected inside individual particle Eutectic structure tissue is stayed.
Step 4, block Al2O3The preparation of/EAG eutectic ceramic composites.Prepared by the method for discharge plasma sintering Block Al2O3/ EAG eutectic ceramic composites, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder.One layer is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron nitride；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove, is closed furnace chamber, is vacuumized, work as vacuum Higher than 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure.Start heating power supply to put this Electric plasma heating furnace heating.
3rd, plasma discharging stove is warming up to 580 DEG C with 180 DEG C/min speed.Hot pressing furnace continues with 140 DEG C/min's Speed is warming up to 1570 DEG C, and is incubated 8min.After insulation terminates, stop heating and cooling to the furnace room temperature, obtain internal retain There is the block eutectic ceramic composite of eutectic structure.In cooling procedure, when the temperature of the plasma discharging stove is down to 500 DEG C when, removal pressure.
Obtained block eutectic ceramic composite is tested through Archimedes's drainage, the block eutectic ceramic composite wood Relative density is 98.4%.
Embodiment five
This implementation is that one kind prepares Al2O3The method of/GAP block eutectic composite ceramic materials, detailed process includes following step Suddenly：
Step 1, Al2O3The preparation of the sample prefabricated body of/GAP eutectic ceramic in situ composite.Al using purity as 99.99%2O3 And Gd2O3Powder is raw material, according to Al2O3/Gd2O3Phasor eutectic point is matched.
Poly-vinyl alcohol solution and absolute ethyl alcohol are added in load weighted mixed-powder and carries out being sufficiently mixed stirring；Ball milling The rotating speed of machine is 550r/min, and mixing time is 5h, obtains well mixed mixed-powder.The addition of the polyvinyl alcohol is 14ml poly-vinyl alcohol solution is added in raw material described in per 100g；The addition of the absolute ethyl alcohol is to be added per in 100g raw materials 60ml.The poly-vinyl alcohol solution added is 5g polyvinyl alcohol to be added in 100ml pure water and heating makes polyvinyl alcohol molten Obtained after solution.
Drying and processing is carried out to obtained mixed-powder, well mixed Al is obtained2O3/Gd2O3Ceramic powders；Drying temperature Spend for 80 DEG C, drying time is 12h.8g is passed through to the Al of drying and processing2O3/Gd2O3Ceramic powders are put into by alcohol washes In stainless steel mould, unloading pressure after 100MPa uniaxial tensions, pressurize 3min is applied to powder by forcing press, length, width and height are obtained Respectively 70mm × 12mm × 4mm plate tensile sample.Obtained plate tensile sample is put into sintering furnace, sintered in atmospheric environment 2h, sintering temperature is 1500 DEG C, obtains Al2O3The precast body of/GAP eutectic ceramic in situ composite samples.Al in sintering2O3With Gd2O3Solid phase reaction occurs for powder, and the phase composition of material is changed into Al2O3With GAP two-phases.
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple Al are obtained2O3/ GAP eutectics The precast body blank of spontaneous composite ceramics sample.In the present embodiment, the precast body blank of preparation is 40.
Step 2, sample is prepared.Using diamond precision gas cutting machine by obtained multiple Al2O3The spontaneous composite ceramic of/GAP eutectics The precast body of porcelain sample is respectively cut as a height of 70mm × 4mm of length and width × 4mm strip precast body.By one of precast body On the specimen mounting for being placed in realizing laser suspension zone-melting pull system, clamping is reinforced.Laser is opened, the power of laser is risen to 400W, is heated to the precast body, melts the precast body, and forms stable melting zone.Pull system is opened, with 200 μm/s Withdrawing rate to the melting zone carry out pull, complete sample directional solidification.
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so that Obtain multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure.The sample A diameter of 2.8 ± 0.2mm, high 5 ± 0.5cm.
Arbitrarily take one of sample and metallographic processing is carried out to it.Pass through the tissue of the scanning electron microscopic observation sample.Adopt With method of scoring, the average eutectic lamellar spacing for obtaining the bar samples is 1.12 μm.It is total to obtained the average of the bar samples Crystal layer piece spacing as all bar samples average eutectic lamellar spacing.
Step 3, Al is prepared2O3/ GAP eutectic particles.The particle diameter of described eutectic particle is 4~12 μm.Detailed process is：
All bar samples obtained using ultrasonic wave to step 2 are cleaned.All bar samples after cleaning are put In the jaw crusher that jaw is high-purity zirconia and Mechanical Crushing is graininess.By obtained pellet through sieves, particle is obtained Size is less than 1mm Al2O3/ GAP coarse granules.
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball It is 10 with coarse grained mass ratio:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/ of the ball milling tank volume 5.Ball mill is opened, with 500r/min rotating speed to coarse granule ball milling 3.5h, eutectic powder is obtained.Obtained eutectic powder is dried Do to being completely dried.
The eutectic powder of drying is sieved.Specifically, the eutectic powder of drying is placed in the screen cloth that aperture is 12 μm In, the screen cloth that aperture is 4 μm is placed in the lower section of 12 μm of screen clothes, vibrosieve is carried out.Continue in vibrosieve to described Absolute ethyl alcohol is added in eutectic powder；The addition of absolute ethyl alcohol described in vibrosieve is so that the eutectic powder in screen cloth to be flooded It is advisable.
After screening, the powder in 4 μm of screen clothes is taken out, the Al that targeted particle size is 4~12 μm is obtained2O3/ GAP eutectic powders. Because obtained Al2O3The size of/GAP eutectic powders is more than the eutectic spacing of club-shaped material, so being protected inside individual particle Eutectic structure tissue is stayed.
Step 4, block Al2O3The preparation of/GAP eutectic ceramic composites.Prepared by the method for discharge plasma sintering Block Al2O3/ GAP eutectic ceramic composites, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder.One layer is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron nitride；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove, is closed furnace chamber, is vacuumized, work as vacuum Higher than 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure.Start heating power supply to put this Electric plasma heating furnace heating.
3rd, plasma discharging stove is warming up to 580 DEG C with 200 DEG C/min speed.Hot pressing furnace continues with 150 DEG C/min's Speed is warming up to 1570 DEG C, and is incubated 8min.After insulation terminates, stop heating and cooling to the furnace room temperature, obtain internal retain There is the block eutectic ceramic composite of eutectic structure.In cooling procedure, when the temperature of the plasma discharging stove is down to 500 DEG C when, removal pressure.
Obtained block eutectic ceramic composite is tested through Archimedes's drainage, the block eutectic ceramic composite wood Relative density is 98.6%.

Claims (6)

1. a kind of method of discharge plasma sintering alumina-based eutectic ceramic composite, it is characterised in that detailed process is：
Step 1, sample prefabricated body blank is prepared；
Step 2, sample is prepared；
Repeated melting-- draw process, the sample prefabricated body blank that step 1 is obtained, which prepares to turn into, has fine uniform eutectic The sample of tissue；The average eutectic lamellar spacing of all samples is used as using the obtained average eutectic lamellar spacing of the sample；
Step 3, eutectic particle is prepared；The particle diameter of described eutectic particle is 4~12 μm, and eutectic is remained inside individual particle Structure organization；
Step 4, the preparation of block eutectic ceramic composite；Block eutectic ceramic is prepared by the method for discharge plasma sintering Composite, detailed process is：
First, graphite paper is spread in the region contacted in graphite jig with eutectic powder；One layer of nitridation is sprayed on the graphite paper top layer Eutectic powder is positioned over mould inside after boron；
Second, the graphite jig that will be equipped with powder is placed in plasma discharging stove；To the plasma discharging stove evacuation to vacuum Degree is higher than 5 × 10-1During Pa, apply 30MPa axial compressive force to the eutectic powder and keep the pressure；Start heating power supply pair The plasma discharging stove heat；
3rd, plasma discharging stove is warming up to 500~600 DEG C with 120~200 DEG C/min speed；Hot pressing furnace continues with 100~ 150 DEG C/min speed is warming up to 1550~1580 DEG C, and is incubated 5~10min；After insulation terminates, stop heating and cold with stove But to room temperature, the internal block eutectic ceramic composite for remaining with eutectic structure is obtained；In cooling procedure, when the electric discharge When the temperature of plasma heating furnace is down to 500 DEG C, removal pressure obtains block eutectic ceramic composite；Obtained block eutectic pottery The relative density of porcelain composite is 97.9~98.8%.
2. the preparation method of block alumina-based eutectic ceramic composite as claimed in claim 1, it is characterised in that the system During standby sample prefabricated body blank, with Al2O3And Y2O3Or Er2O3Or Gd2O3For raw material, or with Al2O3、Y2O3And ZrO2Powder is Raw material, described Al2O3、Y2O3、Er2O3、Gd2O3And ZrO2It is powdered；Polyethylene is added in load weighted mixed-powder Alcoholic solution and absolute ethyl alcohol simultaneously carry out being sufficiently mixed stirring；The rotating speed of ball mill is 550r/min, and mixing time is 5h, is mixed Close uniform mixed-powder；The polyvinyl alcohol that the addition of the polyvinyl alcohol is 10~15ml of addition in raw material described in per 100g Solution；The addition of the absolute ethyl alcohol is per 50~60ml of addition in 100g raw materials；
Drying and processing is carried out to obtained mixed-powder, well mixed ceramic powders are obtained；Drying temperature is 80 DEG C, during drying Between be 12h；It will be put into by the ceramic powders of drying and processing in mould, 100MPa uniaxial tensions, pressurize applied to the powder Unloading pressure after 3min, obtains sample；Obtained sample is put into sintering furnace, 2h, sintering temperature are sintered in atmospheric environment For 1400~1500 DEG C, the precast body of an eutectic ceramic in situ composite sample is obtained；
Dispensing-- stirring-- drying-- pressurization-- the sintering process is repeated, multiple sample prefabricated body blanks are obtained.
3. the preparation method of block alumina-based eutectic ceramic composite as claimed in claim 1, it is characterised in that the step Rapid 2 detailed processes for preparing sample are：
The precast body of obtained eutectic ceramic in situ composite sample is respectively cut as precast body；One of precast body is consolidated On the specimen mounting for being scheduled on realizing laser suspension zone-melting pull system；Open laser to heat the precast body, melt the precast body And form stable melting zone；Pull system is opened, pull is carried out to the melting zone with 50~200 μm/s withdrawing rate, is completed The directional solidification of sample；
Clamping-- fusing-- the draw process is repeated, the directional solidification to all precast bodies is completed one by one, so as to obtain Multiple uniform diameters, the smooth flawless in surface and the internal bar samples with fine uniform eutectic structure；
Arbitrarily take one of sample and metallographic processing is carried out to it；Pass through the tissue of the scanning electron microscopic observation sample；Using draw Collimation method, obtains the average eutectic lamellar spacing of the sample.
4. the preparation method of block alumina-based eutectic ceramic composite as claimed in claim 1, it is characterised in that
It is described prepare eutectic particle detailed process be：
All samples obtained using ultrasonic wave to step 2 are cleaned；By all broken after cleaning and sieve, obtain particle Size is less than 1mm coarse granule；
Obtained coarse granule is placed in the high purity aluminium oxide ball grinder of planetary ball mill, and makes high-purity zirconia abrading-ball and thick The mass ratio of particle is 10:1；Add absolute ethyl alcohol；The addition of the absolute ethyl alcohol is the 1/5 of the ball milling tank volume；Open Ball mill is opened, with 500r/min rotating speed to coarse granule 3~4h of ball milling, eutectic powder is obtained；Eutectic powder drying to obtaining To being completely dried；
During the eutectic powder being completely dried described in vibrosieve, the eutectic powder is placed in the screen cloth that aperture is 12 μm, by hole Footpath is that 4 μm of screen cloth is placed in the lower section of 12 μm of screen clothes；Continue to add anhydrous second into the eutectic powder in vibrosieve Alcohol；The addition of absolute ethyl alcohol described in vibrosieve is advisable so that the eutectic powder in screen cloth is flooded.
5. the preparation method of block alumina-based eutectic ceramic composite as claimed in claim 2, it is characterised in that
When with Al2O3And Y2O3During for raw material, according to Al2O3/Y2O3The eutectic point proportioning of phasor；
When with Al2O3And Er2O3During for raw material, according to Al2O3/Er2O3Phasor eutectic point is matched；
When with Al2O3And Gd2O3During for raw material, according to Al2O3/Gd2O3Phasor eutectic point is matched；
Or with Al2O3、Y2O3And ZrO2Powder is raw material, according to Al2O3/Y2O3/ZrO2Phasor eutectic point is matched；
Described ratio is mol ratio.
6. the preparation method of block alumina-based eutectic ceramic composite as claimed in claim 2, it is characterised in that described Poly-vinyl alcohol solution is that 5g polyvinyl alcohol is added in 100ml pure water and heated to obtain polyvinyl alcohol dissolving.
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CN113582726A (en) * 2020-04-30 2021-11-02 Toto株式会社 Composite structure and semiconductor manufacturing apparatus provided with composite structure
CN113462924A (en) * 2021-06-18 2021-10-01 中国地质大学（武汉） Titanium-plated diamond copper composite material and preparation method thereof
CN113462924B (en) * 2021-06-18 2022-03-29 中国地质大学（武汉） Titanium-plated diamond copper composite material and preparation method thereof
CN113683420A (en) * 2021-07-27 2021-11-23 中国科学院金属研究所 Large-size Al2O3LuAG directional solidification eutectic ceramic and light suspension zone melting preparation method thereof
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