CN105314971B - A kind of method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base ternary eutectic - Google Patents
A kind of method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base ternary eutectic Download PDFInfo
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Abstract
A kind of method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base ternary eutectic, is related to a kind of method for preparing alumina base eutectic ceramic in situ composite.The present invention is to solve the preparation method of existing alumina base eutectic ceramic in situ composite and be difficult to prepare big-size complicated shape eutectic ceramic, eutectic ceramic organizational coarseness anisotropy and the low technical problem of production efficiency.The present invention: one, the pre-heat treatment raw material；Two, mechanical alloying；Three, cold moudling；Four, pulsed discharge plasma assists consolidation.The present invention is applied to prepare the spontaneous composite ceramics of big-size complicated shape alumina base ternary eutectic.
Description
Technical field
The present invention relates to a kind of methods for preparing alumina base eutectic ceramic in situ composite.
Background technique
With the development of the development of the national economy and national science and techniques of defence, import before the engine turbine that thrust ratio is 10 or more
Temperature proposes more stringent want to the research and development of high-temperature structural material of new generation and its technology of preparing more than 1700 DEG C
It asks.Alumina base eutectic ceramic in situ composite because of its high-melting-point, high specific strength, high antioxidant and excellent corrosion resistance, and
Good mechanical property and structure stability can be kept under the superhigh temperature oxidation environment close to fusing point (> 1650 DEG C), be recognized
For be most be potential become a new generation can under high temperature oxidation stability atmosphere long service preferred superhigh temperature structural material.
Currently, oxide eutectic ceramics processing is broadly divided into two classes: using crucible directional solidification technique and be not necessarily to
The directional solidification technique of crucible, the former specifically includes that Bridgman method, epitaxial growth method etc.；The latter include: floating zone method,
Laser zone remelting method and micro- pull method etc..Above-mentioned technology of preparing is in the presence of can not prepare oversized shape complexity ceramic component, micro-
Drawbacks, the Bridgman methods such as sight tissue height texture orientation and production efficiency are low can prepare large-size ceramic component, but
Since temperature gradient and the speed of growth are very low, the technology is significantly limited in preparation superhigh temperature oxide eutectic ceramic component side
The application in face.
Summary of the invention
The present invention is to solve the preparation method of existing alumina base eutectic ceramic in situ composite and be difficult to prepare large scale
Complex-shaped eutectic ceramic, eutectic ceramic organizational coarseness anisotropy and the low technical problem of production efficiency, and one kind is provided
The method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base ternary eutectic.
It is spontaneous compound that a kind of pulsed discharge plasma auxiliary remelting of the invention prepares alumina base ternary eutectic
The method of ceramics carries out according to the following steps:
One, the pre-heat treatment raw material: by nanometer Al2O3Powder temperature be 800 DEG C~1500 DEG C under conditions of heating 1h~
For 24 hours, it cools to room temperature with the furnace, obtains preheated treated Al2O3Powder；By nanometer ZrO2Powder temperature be 800 DEG C~
1h~for 24 hours is heated under conditions of 1500 DEG C, cools to room temperature with the furnace, obtains preheated treated ZrO2Powder；By nanometer Y2O3
Powder heating 1h~for 24 hours under conditions of temperature is 800 DEG C~1500 DEG C, cools to room temperature with the furnace, after obtaining preheated processing
Y2O3Powder；
Two, mechanical alloying: by preheated treated Al2O3Powder, preheated treated ZrO2Powder and preheated
Treated Y2O3Powder is placed in the same ball grinder, and dehydrated alcohol and aluminium oxide abrading-ball is added, is in rotational speed of ball-mill
Ball milling 12h~100h under conditions of 300rpm~500rpm obtains eutectic proportion ball milling activation powdery pulp；Described in step 2
Preheated treated Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3The total weight of powder
Weight ratio with dehydrated alcohol is 1:(1~2)；Preheated treated Al described in step 22O3After powder, preheated processing
ZrO2Powder and preheated treated Y2O3The total weight of powder and the weight ratio of aluminium oxide abrading-ball are 1:(1~10)；Step
Preheated treated ZrO described in two2Powder and preheated treated Al2O3The molar ratio of powder is 1:(3.4~3.5)；
Preheated treated Y described in step 22O3Powder and preheated treated Al2O3The molar ratio of powder be 1:(4~
4.1)；
Three, cold moudling: the eutectic proportion ball milling activation powdery pulp that step 2 is obtained is 100 DEG C~200 in temperature
Dry 20min~100min, then crosses 100 mesh~500 meshes under conditions of DEG C, in the pressure that pressure is 10MPa~100MPa
Lower cold pressing 1min~60min, obtains ceramic body；
Four, pulsed discharge plasma assist consolidation: the ceramic body that step 3 is obtained pressure be 10MPa~
100MPa, pulsed discharge plasma heating and heating rate be 50 DEG C/min~200 DEG C/min under conditions of from room temperature
To 500 DEG C~1000 DEG C, pressure be 10MPa~100MPa, pulsed discharge plasma heating and temperature be 500 DEG C~1000
Under conditions of DEG C keep the temperature 1min~10min, then pressure be 1MPa~20MPa, pulsed discharge plasma heating and heating
Rate is is warming up to 1800 DEG C~2000 DEG C from 500 DEG C~1000 DEG C under conditions of 100 DEG C/min~600 DEG C/min, in pressure
For 0.5MPa~20MPa, pulsed discharge plasma heating and temperature be 1800 DEG C~2000 DEG C under conditions of keep the temperature 1min~
10min obtains fused ceramic, stops being heated and pressurizeed, and opens circulating water cooling system and carries out rapid condensation to fused ceramic, obtains
Al2O3/Y3Al5O12/ZrO2The spontaneous composite ceramics of ternary eutectic.
Pulsed discharge plasma auxiliary consolidation technology of the invention is solidifying using strong convection circulating water cooling system control melt
Gu behavior, therefore the problems such as overcome traditional fused craft eutectic ceramic there are organizational coarseness anisotropy.
Pulsed discharge plasma auxiliary consolidation technology of the invention is realized using aux. pressure system stage by stage to eutectic
Ceramic microstructures organization optimization and regulation.
The advantages of the method for the present invention:
(1) the method for the present invention is related to a kind of pulsed discharge plasma auxiliary consolidation technology, realizes to large scale (such as diameter
Greater than 60mm, highly the cylinder for being 5mm) complex-shaped high-melting-point eutectic ceramic material consolidation integration quickly preparation；
(2) the method for the present invention passes through regulation heating rate, temperature, the application technical parameters such as pressure and dwell time, success
Prepare that synusia spacing is small and the preparation of isotropic eutectic ceramic in situ composite component；
(3) the method for the present invention using multiple step format be rapidly heated control high-melting-point alumina base eutectic composite ceramics melting and
Solidification behavior realizes the large scale oxide eutectic ceramic component compared with low residual stress.
Detailed description of the invention
Fig. 1 is the Al for testing a preparation2O3/Y3Al5O12/ZrO2The XRD diagram of the spontaneous composite ceramics of ternary eutectic；
Fig. 2 is the Al for testing a preparation2O3/Y3Al5O12/ZrO2The SEM of the spontaneous composite ceramics of ternary eutectic schemes.
Specific embodiment
Specific embodiment 1: present embodiment is that a kind of pulsed discharge plasma assists remelting to prepare aluminium oxide
The method of the spontaneous composite ceramics of base ternary eutectic, specifically carries out according to the following steps:
One, the pre-heat treatment raw material: by nanometer Al2O3Powder temperature be 800 DEG C~1500 DEG C under conditions of heating 1h~
For 24 hours, it cools to room temperature with the furnace, obtains preheated treated Al2O3Powder；By nanometer ZrO2Powder temperature be 800 DEG C~
1h~for 24 hours is heated under conditions of 1500 DEG C, cools to room temperature with the furnace, obtains preheated treated ZrO2Powder；By nanometer Y2O3
Powder heating 1h~for 24 hours under conditions of temperature is 800 DEG C~1500 DEG C, cools to room temperature with the furnace, after obtaining preheated processing
Y2O3Powder；
Two, by preheated treated Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3
Powder is placed in the same ball grinder, and dehydrated alcohol and aluminium oxide abrading-ball is added, and is 300rpm~500rpm in rotational speed of ball-mill
Under conditions of ball milling 12h~100h, obtain eutectic proportion ball milling activation powdery pulp；It is preheated described in step 2 that treated
Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3The total weight of powder and the weight of dehydrated alcohol
Amount is than being 1:(1~2)；Preheated treated Al described in step 22O3Powder, preheated treated ZrO2Powder and warp
Y after the pre-heat treatment2O3The total weight of powder and the weight ratio of aluminium oxide abrading-ball are 1:(1~10)；It is preheated described in step 2
Treated ZrO2Powder and preheated treated Al2O3The molar ratio of powder is 1:(3.4~3.5)；Warp described in step 2
Y after the pre-heat treatment2O3Powder and preheated treated Al2O3The molar ratio of powder is 1:(4~4.1)；
Three, cold moudling: the eutectic proportion ball milling activation powdery pulp that step 2 is obtained is 100 DEG C~200 in temperature
Dry 20min~100min, then crosses 100 mesh~500 meshes under conditions of DEG C, in the pressure that pressure is 10MPa~100MPa
Lower cold pressing 1min~60min, obtains ceramic body；
Four, pulsed discharge plasma assist consolidation: the ceramic body that step 3 is obtained pressure be 10MPa~
100MPa, pulsed discharge plasma heating and heating rate be 50 DEG C/min~200 DEG C/min under conditions of from room temperature
To 500 DEG C~1000 DEG C, pressure be 10MPa~100MPa, pulsed discharge plasma heating and temperature be 500 DEG C~1000
Under conditions of DEG C keep the temperature 1min~10min, then pressure be 1MPa~20MPa, pulsed discharge plasma heating and heating
Rate is is warming up to 1800 DEG C~2000 DEG C from 500 DEG C~1000 DEG C under conditions of 100 DEG C/min~600 DEG C/min, in pressure
For 0.5MPa~20MPa, pulsed discharge plasma heating and temperature be 1800 DEG C~2000 DEG C under conditions of keep the temperature 1min~
10min obtains fused ceramic, stops being heated and pressurizeed, and opens circulating water cooling system and carries out rapid condensation to fused ceramic, obtains
Al2O3/Y3Al5O12/ZrO2The spontaneous composite ceramics of ternary eutectic.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is: described in step 1 to receive
Rice Al2O3The granularity d of powder50For 50nm~500nm.Other are same as the specific embodiment one.
Specific embodiment 3: the difference of present embodiment and specific embodiment one or two is: described in nanometer
ZrO2The granularity d of powder50For 50nm~500nm.Other are the same as one or two specific embodiments.
Specific embodiment 4: the difference of present embodiment and specific embodiment one to three is: described in step 1
Nanometer Y2O3The granularity d of powder50For 50nm~500nm.Other are identical as specific embodiment one to three.
Specific embodiment 5: the difference of present embodiment and specific embodiment one to four is: described in step 2
Aluminium oxide abrading-ball diameter be 3mm~10mm.Other are identical as specific embodiment one to four.
Beneficial effects of the present invention are verified by following tests:
Test one: this test is that a kind of pulsed discharge plasma assists remelting to prepare alumina base ternary eutectic certainly
The method of raw composite ceramics, specifically carries out according to the following steps:
One, the pre-heat treatment raw material: by nanometer Al2O3Powder heats 2h under conditions of temperature is 1000 DEG C, cools to the furnace
Room temperature obtains preheated treated Al2O3Powder；By nanometer ZrO2Powder heats 2h under conditions of temperature is 1000 DEG C, with
Furnace is cooled to room temperature, and obtains preheated treated ZrO2Powder；By nanometer Y2O3Powder adds under conditions of temperature is 1000 DEG C
Hot 2h, cools to room temperature with the furnace, obtains preheated treated Y2O3Powder；
Two, by preheated treated Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3
Powder is placed in the same ball milling bottle, and dehydrated alcohol and aluminium oxide abrading-ball is added, under conditions of rotational speed of ball-mill is 500rpm
Ball milling 12h obtains eutectic proportion ball milling activation powdery pulp；Preheated treated Al described in step 22O3Powder, through pre-
ZrO after heat treatment2Powder and preheated treated Y2O3The total weight of powder and the weight ratio of dehydrated alcohol are 1:1.5；Step
Preheated treated Al described in rapid two2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3Powder
The total weight of body and the weight ratio of aluminium oxide abrading-ball are 1:4；Preheated treated ZrO described in step 22Powder and warp are pre-
Al after heat treatment2O3The molar ratio of powder is 1:3.42；Preheated treated Y described in step 22O3Powder with it is preheated
Treated Al2O3The molar ratio of powder is 1:4；
Three, cold moudling: the condition that the eutectic proportion ball milling activation powdery pulp that step 2 is obtained is 200 DEG C in temperature
Then lower dry 20min crosses 200 meshes, be cold-pressed 5min in the case where pressure is the pressure of 50MPa, obtain ceramic body；
Four, pulsed discharge plasma assists consolidation: the ceramic body that step 3 is obtained is 100MPa, pulse in pressure
Discharge plasma heating and heating rate be 100 DEG C/min under conditions of from room temperature to 800 DEG C, be in pressure
100MPa, pulsed discharge plasma heating and temperature be 800 DEG C under conditions of keep the temperature 2min, then pressure be 0.5MPa,
Pulsed discharge plasma heating and heating rate are in pressure to be warming up to 1800 DEG C from 800 DEG C under conditions of 300 DEG C/min
0.5MPa~20MPa, pulsed discharge plasma heating and temperature keep the temperature 1min under conditions of being 1800 DEG C, obtain melting pottery
Porcelain stops being heated and pressurizeed, and opens circulating water cooling system and carries out rapid condensation to fused ceramic, obtains Al2O3/Y3Al5O12/
ZrO2The spontaneous composite ceramics of ternary eutectic.
Nanometer Al described in step 12O3The granularity d of powder50For 50nm~100nm；Nanometer described in step 1
ZrO2The granularity d of powder50For 50nm~100nm；Nanometer Y described in step 12O3The granularity d of powder50For 50nm~
100nm；The diameter of aluminium oxide abrading-ball described in step 2 is 10mm.
Fig. 1 is the Al for testing a preparation2O3/Y3Al5O12/ZrO2The XRD diagram of the spontaneous composite ceramics of ternary eutectic, ● it is α-
Al2O3, ■ is Y3Al5O12, is c-ZrO2, as can be seen from the figure test the Al of a preparation2O3/Y3Al5O12/ZrO2Ternary is total
Brilliant spontaneous composite ceramics have preferable crystallinity, by α-Al2O3、Y3Al5O12(YAG) and c-ZrO2It constitutes, does not find other
Impurity phase generates.
Fig. 2 is the Al for testing a preparation2O3/Y3Al5O12/ZrO2The SEM of the spontaneous composite ceramics of ternary eutectic schemes, from figure
It can be seen that the Al of one preparation of test2O3/Y3Al5O12/ZrO2The spontaneous composite ceramics of ternary eutectic do not find crackle and stomata.
Al prepared by test one2O3/Y3Al5O12/ZrO2The spontaneous composite ceramics of ternary eutectic carry out hardness determination, hard
Degree is up to 18.7 ± 0.6GPa.
Test two: for a kind of pulsed discharge plasma asistance consolidation, to prepare alumina base ternary eutectic spontaneous compound for this test
The method of ceramics, specifically carries out according to the following steps:
One, the pre-heat treatment raw material: by nanometer Al2O3Powder heats 2h under conditions of temperature is 1000 DEG C, cools to the furnace
Room temperature obtains preheated treated Al2O3Powder；By nanometer ZrO2Powder heats 2h under conditions of temperature is 1000 DEG C, with
Furnace is cooled to room temperature, and obtains preheated treated ZrO2Powder；By nanometer Y2O3Powder adds under conditions of temperature is 1000 DEG C
Hot 2h, cools to room temperature with the furnace, obtains preheated treated Y2O3Powder；
Two, by preheated treated Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3
Powder is placed in the same ball milling bottle, and dehydrated alcohol and aluminium oxide abrading-ball is added, under conditions of rotational speed of ball-mill is 500rpm
Ball milling 12h obtains eutectic proportion ball milling activation powdery pulp；Preheated treated Al described in step 22O3Powder, through pre-
ZrO after heat treatment2Powder and preheated treated Y2O3The total weight of powder and the weight ratio of dehydrated alcohol are 1:1.5；Step
Preheated treated Al described in rapid two2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3Powder
The total weight of body and the weight ratio of aluminium oxide abrading-ball are 1:4；Preheated treated ZrO described in step 22Powder and warp are pre-
Al after heat treatment2O3The molar ratio of powder is 1:3.42；Preheated treated Y described in step 22O3Powder with it is preheated
Treated Al2O3The molar ratio of powder is 1:4；
Three, cold moudling: the condition that the eutectic proportion ball milling activation powdery pulp that step 2 is obtained is 200 DEG C in temperature
Then lower dry 20min crosses 200 meshes, be cold-pressed 15min in the case where pressure is the pressure of 30MPa, obtain ceramic body；
Four, pulsed discharge plasma asistance consolidation: by ceramic body that step 3 obtains pressure is 80MPa, pulse is put
Electro-plasma heating and heating rate be 60 DEG C/min under conditions of from room temperature to 1000 DEG C, pressure be 80MPa, arteries and veins
Impulse electricity plasma heating and temperature keep the temperature 2min under conditions of being 1000 DEG C, are then 2MPa, pulsed discharge etc. in pressure
Gas ions heating and heating rate are 2MPa, pulse in pressure to be warming up to 1850 DEG C from 1000 DEG C under conditions of 300 DEG C/min
Discharge plasma heating and temperature keep the temperature 2min under conditions of being 1850 DEG C, obtain fused ceramic, stop being heated and pressurizeed, open
It opens circulating water cooling system and rapid condensation is carried out to fused ceramic, obtain Al2O3/Y3Al5O12/ZrO2The spontaneous composite ceramic of ternary eutectic
Porcelain.
Nanometer Al described in step 12O3The granularity d of powder50For 50nm~100nm；Nanometer described in step 1
ZrO2The granularity d of powder50For 50nm~100nm；Nanometer Y described in step 12O3The granularity d of powder50For 50nm~
100nm；The diameter of aluminium oxide abrading-ball described in step 2 is 10mm.
Al prepared by test two2O3/Y3Al5O12/ZrO2The spontaneous composite ceramics of ternary eutectic carry out hardness test, hard
Degree is up to 20.5 ± 0.7GPa.
Claims (1)
1. a kind of method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base ternary eutectic,
It is characterized in that the method that pulsed discharge plasma auxiliary remelting prepares the spontaneous composite ceramics of alumina base ternary eutectic
It carries out according to the following steps:
One, the pre-heat treatment raw material: by nanometer Al2O3Powder heats 2h under conditions of temperature is 1000 DEG C, cools to room with the furnace
Temperature obtains preheated treated Al2O3Powder；By nanometer ZrO2Powder heats 2h under conditions of temperature is 1000 DEG C, with furnace
It is cooled to room temperature, obtains preheated treated ZrO2Powder；By nanometer Y2O3Powder heats under conditions of temperature is 1000 DEG C
2h cools to room temperature with the furnace, obtains preheated treated Y2O3Powder；
Two, by preheated treated Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3Powder
It is placed in the same ball milling bottle, dehydrated alcohol and aluminium oxide abrading-ball is added, ball milling under conditions of rotational speed of ball-mill is 500rpm
12h obtains eutectic proportion ball milling activation powdery pulp；Described preheated treated the Al2O3Powder, preheated treated
ZrO2Powder and preheated treated Y2O3The total weight of powder and the weight ratio of dehydrated alcohol are 1:1.5；Described is preheated
Treated Al2O3Powder, preheated treated ZrO2Powder and preheated treated Y2O3The total weight and oxidation of powder
The weight ratio of aluminium abrading-ball is 1:4；Preheated treated ZrO described in step 22Powder and preheated treated Al2O3Powder
The molar ratio of body is 1:3.42；Preheated treated Y described in step 22O3Powder and preheated treated Al2O3Powder
Molar ratio be 1:4；
Three, cold moudling: the eutectic proportion ball milling activation powdery pulp that step 2 is obtained is dry under conditions of temperature is 200 DEG C
Then dry 20min crosses 200 meshes, be cold-pressed 15min in the case where pressure is the pressure of 30MPa, obtain ceramic body；
Four, pulsed discharge plasma asistance consolidation: the ceramic body that step 3 is obtained is 80MPa, pulsed discharge etc. in pressure
Gas ions heating and heating rate be 60 DEG C/min under conditions of from room temperature to 1000 DEG C, be that 80MPa, pulse are put in pressure
Electro-plasma heating and temperature keep the temperature 2min under conditions of being 1000 DEG C, are then 2MPa, pulsed discharge plasma in pressure
Body heating and heating rate are 2MPa, pulsed discharge in pressure to be warming up to 1850 DEG C from 1000 DEG C under conditions of 300 DEG C/min
Plasma heating and temperature keep the temperature 2min under conditions of being 1850 DEG C, obtain fused ceramic, stop being heated and pressurizeed, unlatching follows
Ring water-cooling system carries out rapid condensation to fused ceramic, obtains Al2O3/Y3Al5O12/ZrO2The spontaneous composite ceramics of ternary eutectic.
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| WO2011012765A2 (en) * | 2009-07-31 | 2011-02-03 | Consejo Superior De Investigaciones Científicas (Cisc) | Method for obtaining a nanostructured composite material having a ceramic matrix, which can be machined by electroerosion, and resulting product |
| CN102674819A (en) * | 2012-05-16 | 2012-09-19 | 台州学院 | High-toughness aluminum oxide ceramic, and preparation method and application thereof |
| CN103586296A (en) * | 2013-10-23 | 2014-02-19 | 大连理工大学 | Mosaic ceramic drawing die and making method thereof |
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| WO2011012765A2 (en) * | 2009-07-31 | 2011-02-03 | Consejo Superior De Investigaciones Científicas (Cisc) | Method for obtaining a nanostructured composite material having a ceramic matrix, which can be machined by electroerosion, and resulting product |
| CN102674819A (en) * | 2012-05-16 | 2012-09-19 | 台州学院 | High-toughness aluminum oxide ceramic, and preparation method and application thereof |
| CN103586296A (en) * | 2013-10-23 | 2014-02-19 | 大连理工大学 | Mosaic ceramic drawing die and making method thereof |
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