CN102050617A - Method for obtaining microstructure of alumina-based binary eutectic melt-grown ceramic - Google Patents
Method for obtaining microstructure of alumina-based binary eutectic melt-grown ceramic Download PDFInfo
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- CN102050617A CN102050617A CN2010105355859A CN201010535585A CN102050617A CN 102050617 A CN102050617 A CN 102050617A CN 2010105355859 A CN2010105355859 A CN 2010105355859A CN 201010535585 A CN201010535585 A CN 201010535585A CN 102050617 A CN102050617 A CN 102050617A
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Abstract
The invention provides a method for obtaining the microstructure of an alumina-based binary eutectic melt-grown ceramic. A plurality of alumina-based oxide preforms are directionally solidified through a laser leviation region melting directional solidification device; and after the routine metallographic treatment, gold is sprayed on the surface of the longitudinal section and on the surface of the cross section of each directionally-solidified preform, so as to obtain the microstructures of the alumina-based binary eutectic melt-grown ceramic at different growth rates. During the directional solidification process, the laser power is 200 W, the rotation speed of the sample rotating system is 50 Rpm, and the drawing speed of each preform ranges from 1 Mum/s to 300 Mum/s. The invention achieves the purpose that the front temperature field of the solid-liquid interface of the preform is uniform and straight, overcomes the problems of high manufacturing cost and complex structure of the prior art, and is applied to the researches on evolution of directionally-solidified microstructure of non-conductive materials with high melting-points.
Description
Technical field
The present invention relates to materials processing engineering field, specifically is a kind of method that obtains alumina base two component eutectic melt growth pottery tissue topography.
Background technology
In recent years, the oxide melt growth pottery of directional solidification process acquisition has been subjected to Chinese scholars and engineering technical personnel's extensive concern.Because the chemical stability of its intrinsic, oxide compound has at first overcome the insufficient problem of oxidation-resistance that a lot of metals at high temperature show.Secondly, oxide compound is used for one of bottleneck of high-temperature structural material-creep-resistant property and has also obtained solving largely researching and producing.Its fracture toughness property is also progressively improving.As ionophore, proton conductor and selectivity high temperature emissive material, oxide compound all demonstrates great potential.But but seldom, it is still indeterminate that main restraining factors are exactly its tissue topography and the relation of solidifying between the parameter in engineering for oxide melt growth ceramic applications.
At present, generally obtain the oxide melt ceramic tissue topography of growing by Bridgman method and epitaxial growth method.
Bridgman method, the advantage of this method are to prepare the large size bulk material, and the limiting factor of specimen size has only crucible size, and its thermograde is greatly about 10
2The K/cm order of magnitude.Oxide melt generally is positioned in the crucible of high-purity molybdenum, tungsten and iridium, realizes directional freeze by slowly extracting crucible out hot-zone.
Little daraf(reciprocal of farad) is applicable to that preparation has character of the same race and the eutectic spacing is controlled at the interior eutectic structure of micrometer range, especially is fit to be used for preparing to have the eutectic ceramic fiber of diameter below millimeter.Its thermograde can reach 10
3K/cm, growth velocity can reach 1000mm/h, and specimen finish is in 0.3～5mm scope.
Epitaxial growth method, this method are to utilize the wicking action of liquid and a kind of directional solidification process of developing.The pattern that high melting point alloy is made partly immerses in the crucible that fills eutectic melt, when formwork enters half left and right sides of melt, under wicking action, melt rises to the upper surface of pattern wetting along the pore in the formwork, lift simultaneously and the contacted seed crystal of pattern upper surface, can prepare the melt growth pottery continuously.Its thermograde can reach 400～1600K/cm.
The thermograde of Bridgman method and epitaxial growth method is lower, can only obtain under the low solidification rate oxide melt ceramic tissue topography of growing.And when adopting the Bridgman method to obtain oxide melt to grow ceramic tissue topography, all need to change crucible after each the production, very expensive is not suitable for the usefulness that makes a search.And also complex structure of the device that is used for epitaxial growth method, production cost is higher.
People such as the breadboard Sayir of U.S. NASA Green utilize the cam-like speculum of two high speed rotating, realized the high speed scan round of laser beam on the precast body surface, thereby guarantee that the temperature field is even, successfully grow directional freeze oxide eutectic fiber with uniform formation.But employed apparatus structure complexity, the accuracy requirement height, cost is very high.
Spain CSIC university and solidification technology National Key Laboratory of Northwestern Polytechnical University utilize making of horizontal zone-melting technique success the bar-shaped and thickness of 4-6mm diameter reach the oxide platelet eutectic sample of 3mm, the laser level district melting temperatur gradient that this method obtained can reach 10
4Level, but isothermal surface is not straight, the oxide melt of the acquisition ceramic tissue topography of growing can't cause the great difficulty of interpretation with to solidify parameter corresponding.
Summary of the invention
For overcome exist in the prior art or complex structure, of a high price, perhaps isothermal surface is not straight, the perhaps not high deficiency of thermograde the present invention proposes a kind of method that obtains alumina base two component eutectic melt growth pottery tissue topography.
The present invention adopts the tissue topography of the method acquisition oxide compound two component eutectic melt growth pottery of directional freeze by the molten device for directionally solidifying in laser levitation district, and its detailed process may further comprise the steps:
The first step is made precast body; By batch mixing, grinding, compacting, sintering and shaping, obtain a plurality of precast bodies;
In second step, a plurality of precast bodies are carried out directional freeze respectively; The detailed process of a plurality of precast bodies being carried out directional freeze respectively is, with one of them precast body clamping in the pull system, adjust the position of convex lens by adjusting the convex lens translating device, make between convex lens mirror body center and the two bundle laser intersection points apart from being 270～310mm; Open laser apparatus, make laser power progressively be increased to 200W with the speed of 50W/min; Start sample pull rotational system, realize the directional freeze of first precast body; With second precast body clamping in the pull system; And make that distance is 270～310mm between convex lens mirror body center and the two bundle laser intersection points; Open laser apparatus, make laser power progressively be increased to 200W with the speed of 50W/min; Start sample pull rotational system, realize the directional freeze of second precast body; Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; In the directional freeze, the rotating speed of sample rotational system is 50Rpm; The withdrawing rate of each precast body is respectively 1～300 μ m/s;
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After the vertical section of a plurality of samples of obtaining and cross section handled through conventional metallographic, surperficial metal spraying obtained the tissue topography of oxide melt growth pottery under different growth velocitys.
Described oxide compound two component eutectic is the alumina base two component eutectic melt growth pottery that is formed by aluminum oxide and rare earth oxide.
The present invention adopts quality laser beam such as two-way molten to the precast body district, rotate precast body simultaneously, reach and make evenly straight purpose of temperature field, precast body solid-liquid interface forward position, it is high to have overcome the cost in the traditional method, complex structure and other problems, and well solved problem with comparatively easy method.Al when being illustrated in figure 2 as solidification rate that the present invention obtains and being 2 μ m/s
2O
3/ YAG eutectic solid-liquid interface is organized picture, can find out that the interface is more smooth in diameter range, has clear improvement with respect to the molten thermoisopleth in the laser level district shown in Fig. 3.The present invention can carry out oriented freezing organization evolution research to fusing point height, electrically nonconducting material.
Description of drawings
Accompanying drawing 2 is solidification rate that the present invention obtains Al when being 2 μ m/s
2O
3/ YAG eutectic solid-liquid interface is organized picture.
Accompanying drawing 3 is molten picture and the isothermal surface synoptic diagram organized in laser level district.
Accompanying drawing 4 is solidification rate that the present invention obtains Al when being 10 μ m/s
2O
3/ YAG eutectic structure picture.
Accompanying drawing 5 is solidification rate that the present invention obtains Al when being 24 μ m/s
2O
3/ EAG eutectic structure picture.
Accompanying drawing 6 is solidification rate that the present invention obtains Al when being 100 μ m/s
2O
3/ GAP eutectic structure picture.
Accompanying drawing 7 is structural representations of the molten device for directionally solidifying in laser levitation district.
Accompanying drawing 8 is that the A of device for directionally solidifying structural representation is melted to attempting in the laser levitation district.Wherein:
1. laser apparatus 2. spectroscopes 3. first speculums 4. second speculums 5. the 3rd speculum 6. convex lens 7. convex lens translating devices 8. plano lens 9. vacuum chambers 10. pull rotational systems 11. group of motors 12. tack bolts 13. precast bodies 14. melting zone a. solidify direction b. laser scanning direction c. and solidify the e.2 thermoisopleth after second of direction d. thermoisopleth
Embodiment
Embodiment one
Present embodiment is a kind of acquisition Al
2O
3The method of the oriented freezing organization pattern of/YAG oxide compound two component eutectic melt growth pottery under different growth velocitys, carry out the precast body of directional freeze quantity be 5, its detailed process may further comprise the steps:
The first step is made 5 precast bodies; The making processes of each precast body is, with Al
2O
3And Y
2O
3The powder that two kinds of purity is 4N is according to Al
2O
3/ YAG eutectic composition mixes also puts into mortar, adds 10% PVA binding agent, powder is mixed and is ground to no reunion lump by ordinary method; Get the mixed powder of 10 grams and put into the mould that inner cavity size is 68 * 10mm, matched moulds pressurization 25MPa, pressurize 5 minutes with the plate of pressed by powder into about 68 * 10 * 5mm, forms the blank of precast body; Blank to the precast body that presses under atmosphere carries out sintering, and to increase the intensity of precast body, sintering temperature is 1400 ℃, heat preservation sintering 2 hours; Furnace cooling.The precast body blank that sinters is cut into the strip of two 68mm * 4mm * 4mm with cutting piece made from diamond.With sand paper its corner angle are ground off, form the subcircular rod, obtain two precast bodies.Repeat said process, 5 required precast bodies complete.
In second step, precast body is carried out directional freeze; Clamping is distinguished on the upper grip and lower chuck of pull system in the two ends of one of them precast body, adjust the position of convex lens by adjusting the convex lens translating device, making convex lens mirror body central point to being 310mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects, is the hot spot of 4mm at precast body surface formation diameter; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 2 μ m/s speed, realize the directional freeze of oxide eutectic.With the two ends of second precast body wherein respectively clamping on the upper grip and lower chuck of pull system; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 16 μ m/s speed, realize the directional freeze of oxide eutectic.Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; Convex lens mirror body central point is the hot spot of 4mm to being 310mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects at precast body surface formation diameter; Laser power all progressively is increased to 200W with the speed of 50W/min; Pull rotational system rotating speed is 50Rpm, and the withdrawing rate of all the other each precast bodies is respectively 10,60,120 μ m/s.Finish the directional freeze of precast body.
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After 5 sample vertical sections obtaining and cross section handled through conventional metallographic, surperficial metal spraying; Thereby obtain Al
2O
3The tissue topography of/YAG two component eutectic oxide melt growth pottery under different growth velocitys.
Embodiment two
Present embodiment is a kind of acquisition Al
2O
3The method of the oriented freezing organization pattern of/EAG oxide compound two component eutectic melt growth pottery under different growth velocitys, carry out the precast body of directional freeze quantity be 6, its detailed process may further comprise the steps:
The first step is made precast body; With Al
2O
3, Er
2O
3Two kinds of powder Al that purity is 4N
2O
3/ EAG eutectic composition mixes also puts into mortar, adds 10% PVA binding agent, powder is mixed and is ground to no reunion lump by ordinary method; The mixed powder of 10 grams is put into the mould that inner cavity size is 68 * 10mm, matched moulds pressurization 20MPa, pressurize 7 minutes with the plate of pressed by powder into about 68 * 10 * 5mm, forms the blank of precast body; Blank to the precast body that presses under atmosphere carries out sintering, and to increase the intensity of precast body, sintering temperature is 1600 ℃, heat preservation sintering 2 hours, furnace cooling; The precast body blank that sinters is cut into the strip of two 68mm * 4mm * 4mm with cutting piece made from diamond.With sand paper its corner angle are ground off, form the subcircular rod, obtain two precast bodies.Repeat said process, 6 required precast bodies complete.
In second step, precast body is carried out directional freeze; With the two ends clamping of precast body on the upper grip and lower chuck of pull system, adjust the position of convex lens by adjusting the convex lens translating device, making convex lens mirror body central point to being 310mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects, is the hot spot of 4mm at precast body surface formation diameter; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 100Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 2 μ m/s speed, realize the directional freeze of oxide eutectic.With the two ends of second precast body wherein respectively clamping on the upper grip and lower chuck of pull system; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 100Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 6 μ m/s speed, realize the directional freeze of oxide eutectic.Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; Convex lens mirror body central point is the hot spot of 4mm to being 310mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects at precast body surface formation diameter; Laser power all progressively is increased to 200W with the speed of 50W/min; Pull rotational system rotating speed is 100Rpm, and the withdrawing rate of all the other each precast bodies is respectively 8,24,80,150 μ m/s.Finish the directional freeze of precast body.
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After 6 sample vertical sections obtaining and cross section handled through conventional metallographic, surperficial metal spraying, thus obtain Al
2O
3The tissue topography of/EAG eutectic melt growth pottery under different growth velocitys.
Embodiment three
Present embodiment is a kind of acquisition Al
2O
3The method of the oriented freezing organization pattern of/GAP oxide compound two component eutectic under different growth velocitys, carry out the precast body of directional freeze quantity be 7, its detailed process may further comprise the steps:
The first step is made precast body; With Al
2O
3, Gd
2O
3The powder that two kinds of purity is 4N is according to Al
2O
3/ GAP eutectic composition mixes also puts into mortar, adds 10% PVA binding agent, powder is mixed and is ground to no reunion lump by ordinary method; The mixed powder of 10 grams is put into the mould that inner cavity size is 68 * 10mm, matched moulds pressurization 22MPa, pressurize 6 minutes with the plate of pressed by powder into about 68 * 10 * 5mm, forms the blank of precast body; Blank to the precast body that presses under atmosphere carries out sintering, and to increase the intensity of precast body, sintering temperature is 1600 ℃, heat preservation sintering 2 hours, furnace cooling; The precast body blank that sinters is cut into the strip of two 68mm * 4mm * 4mm with cutting piece made from diamond.With sand paper its corner angle are ground off, form the subcircular rod, obtain two precast bodies.Repeat said process, 7 required precast bodies complete.
In second step, precast body is carried out directional freeze; With the two ends clamping of precast body on the upper grip and lower chuck of pull system, adjust the position of convex lens by adjusting the convex lens translating device, making convex lens mirror body central point to being 270mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects, is the hot spot of 3mm at precast body surface formation diameter; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 1 μ m/s speed, realize the directional freeze of oxide eutectic.With the two ends of second precast body wherein respectively clamping on the upper grip and lower chuck of pull system; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 5 μ m/s speed, realize the directional freeze of oxide eutectic.Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; Convex lens mirror body central point is the hot spot of 3mm to being 270mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects at precast body surface formation diameter; Laser power all progressively is increased to 200W with the speed of 50W/min; Pull rotational system rotating speed is 50Rpm, and the withdrawing rate of all the other each precast bodies is respectively 10,20,50,100,300 μ m/s.Finish the directional freeze of precast body.
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After 7 sample vertical sections obtaining and cross section handled through conventional metallographic, surperficial metal spraying, thus obtain Al
2O
3The tissue topography of/GAP eutectic under different growth velocitys.
Embodiment four
Present embodiment is a kind of acquisition Al
2O
3/ EuAlO
3The method of the oriented freezing organization pattern of oxide compound two component eutectic melt growth pottery under different growth velocitys, carry out the precast body of directional freeze quantity be 8, its detailed process may further comprise the steps:
The first step is made precast body; With Al
2O
3And Eu
2O
3The powder that two kinds of purity is 4N is according to Al
2O
3/ EuAlO
3Eutectic composition mixes also puts into mortar, adds 10% PVA binding agent, powder is mixed and is ground to no reunion lump by ordinary method; The mixed powder of 10 grams is put into the mould that inner cavity size is 68 * 10mm, matched moulds pressurization 25MPa, pressurize 6 minutes with the plate of pressed by powder into about 68 * 10 * 5mm, forms the blank of precast body; Blank to the precast body that presses under atmosphere carries out sintering, and to increase the intensity of precast body, sintering temperature is 1400 ℃, heat preservation sintering 2 hours, furnace cooling; The precast body blank that sinters is cut into the strip of two 68mm * 4mm * 4mm with cutting piece made from diamond.With sand paper its corner angle are ground off, form the subcircular rod, obtain two precast bodies.Repeat said process, make 8 precast bodies.
In second step, precast body is carried out directional freeze; With the two ends clamping of precast body on the upper grip and lower chuck of pull system, adjust the position of convex lens by adjusting the convex lens translating device, making convex lens mirror body central point to being 290mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects, is the hot spot of 3.5mm at precast body surface formation diameter; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 3 μ m/s speed, realize the directional freeze of oxide eutectic.With the two ends of second precast body wherein respectively clamping on the upper grip and lower chuck of pull system; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 9 μ m/s speed, realize the directional freeze of oxide eutectic.Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; Convex lens mirror body central point is the hot spot of 3.5mm to being 290mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects at precast body surface formation diameter; Laser power all progressively is increased to 200W with the speed of 50W/min; Pull rotational system rotating speed is 50Rpm, and the withdrawing rate of all the other each precast bodies is respectively 25,50,70,140,210,280 μ m/s.Finish the directional freeze of precast body.
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After 8 sample vertical sections obtaining and cross section handled through conventional metallographic, surperficial metal spraying, thus obtain Al
2O
3/ EuAlO
3The tissue topography of two component eutectic melt growth pottery under different growth velocitys.
Embodiment five
Present embodiment is a kind of acquisition Al
2O
3/ SmAlO
3The method of the oriented freezing organization pattern of oxide compound two component eutectic melt growth pottery under different growth velocitys, carry out the precast body of directional freeze quantity be 9, its detailed process may further comprise the steps:
The first step is made precast body; With Al
2O
3, Sm
2O
3The powder that two kinds of purity is 4N is according to Al
2O
3/ SmAlO
3Eutectic composition mixes also puts into mortar, adds 10% PVA binding agent, powder is mixed and is ground to no reunion lump by ordinary method; The mixed powder of 10 grams is put into the mould that inner cavity size is 68 * 10mm, matched moulds pressurization 20MPa, pressurize 7 minutes with the plate of pressed by powder into about 68 * 10 * 5mm, forms the blank of precast body; Blank to the precast body that presses under atmosphere carries out sintering, and to increase the intensity of precast body, sintering temperature is 1600 ℃, heat preservation sintering 2 hours, furnace cooling; The precast body blank that sinters is cut into the strip of two 68mm * 4mm * 4mm with cutting piece made from diamond.With sand paper its corner angle are ground off, form the subcircular rod, obtain two precast bodies.Repeat said process, make 9 precast bodies.
In second step, precast body is carried out directional freeze; With the two ends clamping of precast body on the upper grip and lower chuck of pull system, adjust the position of convex lens by adjusting the convex lens translating device, making convex lens mirror body central point to being 290mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects, is the hot spot of 3.5mm at precast body surface formation diameter; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 3 μ m/s speed, realize the directional freeze of oxide eutectic.With the two ends of second precast body wherein respectively clamping on the upper grip and lower chuck of pull system; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 7 μ m/s speed, realize the directional freeze of oxide eutectic.Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; Convex lens mirror body central point is the hot spot of 3.5mm to being 290mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects at precast body surface formation diameter; Laser power all progressively is increased to 200W with the speed of 50W/min; Pull rotational system rotating speed is 50Rpm, and the withdrawing rate of all the other each precast bodies is respectively 14,28,56,112,224,252,280 μ m/s.9 required precast bodies complete.
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After 9 sample vertical sections obtaining and cross section handled through conventional metallographic, surperficial metal spraying, thus obtain Al
2O
3/ SmAlO
3The tissue topography of two component eutectic melt growth pottery under different growth velocitys.
Embodiment six
Present embodiment is a kind of acquisition Al
2O
3/ Dy
3Al
5O
12The method of the oriented freezing organization pattern of oxide compound two component eutectic melt growth pottery under different growth velocitys, carry out the precast body of directional freeze quantity be 10, its detailed process may further comprise the steps:
The first step is made precast body; With Al
2O
3And Dy
2O
3The powder that two kinds of purity is 4N is according to Al
2O
3/ Dy
3Al
5O
12Eutectic composition mixes also puts into mortar, adds 10% PVA binding agent, powder is mixed and is ground to no reunion lump by ordinary method; The mixed powder of 10 grams is put into the mould that inner cavity size is 68 * 10mm, matched moulds pressurization 20MPa, pressurize 7 minutes with the plate of pressed by powder into about 68 * 10 * 5mm, forms the blank of precast body; Blank to the precast body that presses under atmosphere carries out sintering, and to increase the intensity of precast body, sintering temperature is 1500 ℃, heat preservation sintering 2 hours, furnace cooling; The precast body blank that sinters is cut into the strip of two 68mm * 4mm * 4mm with cutting piece made from diamond.With sand paper its corner angle are ground off, form the subcircular rod, obtain two precast bodies.Repeat said process, 10 required precast bodies complete.
In second step, precast body is carried out directional freeze; With the two ends clamping of precast body on the upper grip and lower chuck of pull system, adjust the position of convex lens by adjusting the convex lens translating device, making convex lens mirror body central point to being 270mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects, is the hot spot of 3mm at precast body surface formation diameter; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 4 μ m/s speed, realize the directional freeze of oxide eutectic.With the two ends of second precast body wherein respectively clamping on the upper grip and lower chuck of pull system; Open laser apparatus and move synchronous chuck, the wavelength that laser apparatus is produced is that the red laser cross-over of 630nm drops on the precast body bottom, opens the laser beam of 10.6 mum wavelengths then, makes the laser beam intersection point drop on the precast body bottom; Burst for preventing that precast body is shock heating, required power when making laser power progressively be increased to the oxide eutectic directional freeze with the speed of 50W/min, in the present embodiment, laser power progressively is increased to 200W, and this moment, precast body was melted by laser zone; Open the rotating mechanism in the pull rotational system, this rotating mechanism rotating speed is 50Rpm; Open the pull-out mechanism in the pull rotational system, precast body is moved from top to bottom by 8 μ m/s speed, realize the directional freeze of oxide eutectic.Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; Convex lens mirror body central point is the hot spot of 3mm to being 270mm by the distance between the intersection point of the laser beam of second speculum and the 3rd mirror reflects at precast body surface formation diameter; Laser power all progressively is increased to 200W with the speed of 50W/min; Pull rotational system rotating speed is 50Rpm, and the withdrawing rate of all the other each precast bodies is respectively 16,32,64,96,128,192,256,300 μ m/s.Finish the directional freeze of precast body.
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After 10 sample vertical sections obtaining and cross section handled through conventional metallographic, surperficial metal spraying, thus obtain Al
2O
3/ Dy
3Al
5O
12The tissue topography of two component eutectic melt growth pottery under different growth velocitys.
Embodiment seven
Present embodiment is a kind of grow device of the molten directional freeze in laser levitation district of method of ceramic tissue topography of acquisition oxide melt that the various embodiments described above propose that is used for implementing.The device of the molten directional freeze in described laser levitation district comprises laser apparatus 1, spectroscope 2, speculum, two convex lens 6, two plano lens 8 and convex lens translating device 7, vacuum chamber 9, pull rotational system 10 and two group of motors 11.In the present embodiment, three of plane mirrors comprise first speculum 3, second speculum 4 and the 3rd speculum 5, and spectroscope 2, first speculum 3, second speculum 4 and the 3rd speculum 5 are distributed in vacuum chamber 9 neighborings successively.Laser apparatus 1 is positioned at vacuum chamber 9 one sides.The plano lens 8 of two circles is inlaid in respectively on 9 liang of side bodies of vacuum chamber; The central axis of this plano lens 8 is crossed the axis of pull rotational system 10 and perpendicular to the axis of pull rotational system 10, drop on the axis of pull rotational system 10 after making two bundle laser after focusing on through two convex lens 6 enter vacuum chamber 9 by two plano lens 8, realization is to being installed in the fusion of precast body 13 on the pull rotational system 10, and then forms melting zone 14 on precast body 13.
The width between centers laser apparatus light-emitting window of spectroscope 2 is 1m, and with laser beam angle at 45, the laser level that laser apparatus 1 produces is by spectroscope 2, after be divided into the laser of quality such as mutually perpendicular two bundles, two restraint laser planar horizontal of living in.Distance between first speculum, 3 centers and spectroscope 2 centers is 1m, with laser angle through spectroscope 2 transmissions be 45 °.Second speculum 4 is centered close to by first speculum, 3 beam reflected centers, and its center and first speculum, 3 width between centerss are 1m, and become 50 ° of angles with laser beam.The 3rd speculum 5 is centered close to by spectroscope 2 beam reflected centers, and its center and spectroscope 2 width between centerss are 1m, and become 50 ° of angles with laser beam, and finally two bundle laser angles after second speculum 4 and 5 reflections of the 3rd speculum are 160 °.
The central point of two convex lens 6 mirror bodies is respectively through the intrafascicular heart of second speculum 4 the 3rd speculum 5 laser light reflected, central point to two bundle laser intersection point distance by two convex lens, 6 mirror bodies can be adjusted by convex lens translating device 7, in the present embodiment, described convex lens mirror body central point is 270～310mm by the distance between the intersection point of second speculum 4 and the 3rd speculum 5 laser light reflected bundles extremely.The focal length of selected convex lens 6 is 200mm.
Pull rotational system 10 comprises upper grip and lower chuck, and the axis of pull rotational system 10 is vertical, and the two ends of this pull rotational system 10 are connected with two group of motors 11 respectively, realizes being synchronized with the movement of pull systems and rotates by group of motors 11.The upper grip of pull rotational system 10 and lower chuck are circular rod member, and an end of this upper grip and lower chuck excircle all has the step of protrusion, make its profile be "T"-shaped; Have the end face center of step one end of protrusion that blind hole is all arranged at upper grip and lower chuck, the internal diameter of this blind hole is slightly larger than the external diameter of precast body 13.
The two ends of precast body 13 are respectively charged into the blind hole that is positioned at pull system 10 upper grips and lower chuck one end end face center, and screw tack bolt 12 with the fastening location of precast body.Precast body 13 is coaxial with pull rotational system 10.
Claims (3)
1. a method that obtains alumina base two component eutectic melt growth pottery tissue topography is characterized in that, the grow method of ceramic tissue topography of described acquisition oxide melt may further comprise the steps:
The first step is made precast body; By batch mixing, grinding, compacting, sintering and shaping, obtain a plurality of precast bodies;
In second step, a plurality of precast bodies are carried out directional freeze respectively; The detailed process of a plurality of precast bodies being carried out directional freeze respectively is, one of them precast body clamping in the pull system, and is made that distance is 270～310mm between convex lens mirror body center and the two bundle laser intersection points; Open laser apparatus, it is molten with prefabricated tagma to make laser power progressively be increased to 200W with the speed of 50W/min; Start sample rotational system and pull-out mechanism, realize the directional freeze of first precast body; With second precast body clamping in the pull system; And make that distance is 270～310mm between convex lens mirror body center and the two bundle laser intersection points; Open laser apparatus, make laser power progressively be increased to 200W with the speed of 50W/min; Repeat said process, one by one all the other each precast bodies are carried out directional freeze until end; In the directional freeze, the rotating speed of sample rotational system is 50Rpm; The withdrawing rate of each precast body is 1～300 μ m/s; Obtain the sample after a plurality of directional freezes;
In the 3rd step, get the vertical section and the cross section of each sample after the directional freeze; The central axis of sample is crossed in the vertical section of each sample; The cross section of each sample is perpendicular to the central axis of sample; After the vertical section of a plurality of samples of obtaining and cross section handled through conventional metallographic, surperficial metal spraying; Obtain the tissue topography of alumina base two component eutectic melt growth pottery under different growth velocitys.
2. a kind of according to claim 1 method that obtains alumina base two component eutectic melt growth pottery tissue topography is characterized in that described oxide compound two component eutectic is the alumina base two component eutectic melt growth pottery that is formed by aluminum oxide and rare earth oxide.
3. a kind of according to claim 1 method that obtains alumina base two component eutectic melt growth pottery tissue topography is characterized in that laser beam is 3～4mm at the spot diameter that the precast body surface forms.
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| CN104790037A (en) * | 2015-03-30 | 2015-07-22 | 江苏舒适照明有限公司 | Growth method of cerium doped alumina-terbium aluminum garnet cocrystal |
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| CN107858750A (en) * | 2017-11-05 | 2018-03-30 | 西北工业大学 | A kind of Al2O3‑YAG:Ce3+The preparation method of eutectic fluorescence ceramics |
| CN111235629A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学深圳研究院 | Preparation method of alumina-YAG eutectic melt growth composite material |
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