CN102557595B - Method for performing laser solid forming on aluminum oxide-based eutectic authigenic composite ceramic - Google Patents
Method for performing laser solid forming on aluminum oxide-based eutectic authigenic composite ceramic Download PDFInfo
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Abstract
The invention relates to a method for performing laser solid forming on aluminum oxide-based eutectic authigenic composite ceramic. Large-volume eutectic ceramic is prepared by performing laser solid forming on the oxide eutectic ceramic material. A method for paving ceramic powder layer by layer is adopted; the Al2O3-based eutectic ceramic is adopted; the heat-preserving temperature is commonly controlled to be 800 to 1,300 DEG C; and different cooling speed and temperature gradient are realized by adjusting the heat-preserving temperature. Powder is repeatedly molten into a matrix by a method of repeated accumulation and multi-time cladding, so that the eutectic ceramic can be prepared, the high-melting-point material is quickly molten, the temperature gradient is more than 3,000 K/cm, and thermal stress is reduced and crack is completely eliminated in the laser forming process of materials. High-purity inert gas is introduced in the heating and forming process, so that air in the furnace body is escaped completely, air holes in the forming material are eliminated and stable growth of the crystal is realized. Temperature difference between the forming material and the ambient environment and thermal stress of the material are effectively reduced.
Description
Technical field
The present invention relates to high performance material laser fast forming preparation field, specifically be a kind of surface atmosphere heating furnace auxiliary laser shop powder solid forming that utilizes, realize that high-melting-point, high-compactness, low thermal stress particularly have the technology of preparing of larger volume eutectic ceramic material.
Background technology
The spontaneous pottery of oxide eutectic has excellent elevated temperature strength, heat endurance, creep resistant characteristic and high-temperature oxidation resistance, is the long-term superhigh temperature structural material that uses under adverse circumstances more than 1650 ℃ that is expected to of development in recent years.Yet the main technology of preparing of oxide ceramic material is still powder sintering up to now.Because powder sintered ceramic material is the polycrystalline tissue, usually can't obtain monocrystalline and form phase, ceramic particle, matrix and other composition phases (as wild phase or toughness reinforcing phase) and each all exist a large amount of weak linkage interfaces between forming mutually, the porosity of microstructure uniformity and stability and material all is difficult to eliminate, cause the ceramic material mechanical behavior under high temperature to fall sharply, limited the application of ceramic material under ultra-high temperature condition greatly.Utilize the solid technology of laser zone consolidation can obtained performance oxide eutectic pottery preferably, but this method produces bigger thermal stress in the process that laser melts fast and solidifies, easily cause the sample cracking, and eutectic ceramic belongs to fragile material, more easy to crack, therefore to be melt into the shape eutectic ceramic be the comparison difficulty in the laser levitation district, only limits to prepare the sample of reduced size.
People such as the Li Gang of Liaoning Project Technology University have proposed the method for the synthetic in-situ formed ceramic particle reinforced iron-aluminum-based composites of a kind of laser combustion in the patent No. is the patent of CN201010267573.2, belong to the material technology field, carry out according to the following steps: place the ball mill ball milling to obtain mixed powder tungsten ore stone flour, iron powder, aluminium powder and carbon dust; Mixed powder is pressed into pressed compact, adopts CO
2Laser machine emission high energy laser beam is lighted the pressed compact surface, causes pressed compact from spreading sintering, generates in-situ formed ceramic particle reinforced iron-aluminum-based composites.Laser output power is 550～650W, and the laser burning time is 10～25s.Method of the present invention generates two kinds of ceramic particle wild phases simultaneously on a kind of matrix, shortened composite preparation technology's flow process, reduced the material preparation cost, but be subjected to the restriction of materials chemistry reaction, can not realize the preparation of oxide ceramics.
Laser has very high energy density, can melt very dystectic material fast, and temperature gradient of solid-liquid interface can reach 10 when being used for directional solidification
3～10
4/ cm the order of magnitude is far above 10 of routine techniques
1～10
2The K/cm order of magnitude.The laser fast forming technology is a kind ofly to utilize high energy laser beam that metal or nonmetallic materials are carried out oneself the Quench slewing of quenching of laser surface fusing and the conduction of no interface Rapid Thermal to solidify, not only can directly obtain to have outside the skin-material of rapid solidification tissue signature and specific physical chemistry and mechanical property, and can realize the no mould of high-performance labyrinth part, fast, complete fine and close near-net-shape, has the smelting temperature height, the thermograde height, freezing rate control accuracy height, material and environmental suitability are extensive, characteristics such as pollution-free have been subjected to lot of domestic and foreign scholar's great attention.Be in the patent application of CN 102115882A at publication number; Shanghai University Of Engineering Science has proposed a kind of way of laser-based surface cladding alloy of Materialbearbeitung mit Laserlicht technical field; this method is when laser cladding forming; under the protection of inert gas, adopt the way of laser melting coating at metal base surface cladding single track or multiple tracks alloy.The metal for preparing has good cladding layer, but this technology only limits to prepare metal material.Yet, to compare with metal material, oxide ceramic material has higher fusing point and high fragility.Therefore, need to develop the technology of preparing that new prepared high-melting-point, high-compactness, low thermal stress particularly have larger volume eutectic ceramic material in above-mentioned technical foundation.
Summary of the invention
For overcome exist in the prior art or easily cause sample cracking, perhaps only limit to prepare the sample of reduced size, perhaps can not realize the deficiency of the preparation of oxide ceramics, the present invention proposes the method for the spontaneous composite ceramics of a kind of laser solid forming alumina base eutectic.
The present invention includes following steps:
Step 1, preparation eutectic ceramic powder;
Step 2, the shop powder of eutectic ceramic powder and the heating of surface atmosphere heating furnace; The part eutectic ceramic powder that obtains evenly is layered on forms substrate on the metal substrate; The metal substrate that is covered with substrate is placed on the heating plate of surface atmosphere heating furnace; Open the airometer valve and in burner hearth, feed protective gas N
2Gas; N
2Throughput 100～150ml/min; Eutectic powder being heated to 1200 ℃, adding and pine for, is the heating of 20% speed with conduction ratio below 600 ℃, more than 600 ℃ is 40% speed heating with conduction ratio; Specimen temperature is consistent with temperature of heating plate in the heating; Add and pine for continuing to feed N
2Gas; Al after obtaining heating
2O
3The substrate of/YAG eutectic ceramic;
Step 3, the shaping eutectic ceramic; Adopt the process of laser zone melting method shaping eutectic ceramic, its detailed process is:
Make laser instrument be positioned at the starting point place of eutectic ceramic substrate surface shaping eutectic ceramic, level is carried out in the eutectic ceramic substrate after the heating line by line scan; After laser instrument is finished first line scanning, along the translation of eutectic ceramic substrate surface width, carry out the horizontal sweep of second row, obtain the second road eutectic ceramic that forms at the eutectic ceramic substrate surface; By that analogy, laser instrument advances to the width of eutectic ceramic substrate gradually, forms the ground floor eutectic ceramic until whole eutectic ceramic substrate surface; After the shaping of ground floor eutectic ceramic is finished, remaining eutectic ceramic powder is evenly overlayed on the ground floor eutectic ceramic shop; Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues shaping second layer eutectic ceramic on the ground floor eutectic ceramic surface that obtains; After the shaping of second layer eutectic ceramic is finished, continue remaining eutectic ceramic powder is evenly overlayed on the second layer eutectic ceramic shop; Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues the 3rd layer of eutectic ceramic that be shaped on the second layer eutectic ceramic surface that obtains; Repeat the process that above-mentioned laser zone is melt into the shape eutectic ceramic, obtain required eutectic ceramic; In the shaping eutectic ceramic, laser power is 500W, laser scanning speed 6mm/min, and laser spot diameter is 12mm.In the molten process of laser zone, the surface atmosphere heating furnace continues heating to sample, makes the temperature of sample remain on 1200 ℃, and feeds N
2Gas.The spacings of laser instrument adjacent two row center lines after the translation of eutectic ceramic base widths are 10mm.
Step 4, eutectic pottery cooling, after obtaining volume required eutectic ceramic, after the surface atmosphere heating furnace was cooled to 800 ℃ with the cooling rate of 10 ℃/min, the eutectic ceramic that obtains cooled to room temperature with the furnace, thereby obtains the spontaneous composite ceramics of eutectic.
The present invention obtains large volume eutectic ceramic body by laser solid forming oxide eutectic ceramic material, uses bottleneck problem thereby solve laser forming large scale alumina-based ceramic material through engineering approaches.This is because the pool depth of laser zone blow body ceramics preparative body is limited usually, adopts the method for successively spreading ceramic powder, and the restriction that can effectively solve size is the effective ways of realizing the large volume ceramics forming.But the molten ceramic material inside of laser zone easily cracks the deficiency with pore or material cracking in the powder process of shop, reduce material internal thermal stress and defective, improve quality and the serviceability of shaping sample, proposed to add the method for laser fast forming surface atmosphere heating furnace Assisted Preparation dense oxide eutectic ceramic.This preparation method utilizes surface atmosphere heating furnace device to combine with laser shop powder solid forming technology, can melt materials with high melting point fast, realize high thermograde (＞3000K/cm), and can guarantee in the material laser forming process to reduce thermal stress and eliminate crackle fully.In addition, in heating and forming process, charge into high purity inert gas simultaneously, make that the air in the body of heater is overflowed fully, eliminated the pore of moulding material inside, can obtain stable crystal growth, thereby be convenient to solidification theory research.
The cooldown rate that the laser rapid solidification is high causes material to produce big thermal stress usually in forming process, when particularly preparation is shaped, a large amount of crackle even the crackings of the inner generation of product, simultaneously under high cooling velocity, material internal non-equilibrium phase and metastable phase volume fraction increase, pore forms simultaneously, cause under the high temperature the unstable and mechanical property of material structure to fall sharply, had a strong impact on the application of laser fast forming technology on ceramic material, laser fast forming surface atmosphere heating furnace effectively reduces the temperature difference of moulding material and surrounding environment and the thermal stress of material internal by the adjusting to holding temperature.At Al
2O
3The base eutectic ceramic, holding temperature is generally controlled at 800～1300 ℃.In addition, according to different materials, can realize different cooldown rate and thermograde by adjusting holding temperature.
Laser scanning speed has material impact to the eutectic ceramic microstructure, improve laser scanning speed and can reduce the eutectic lamellar spacing, thereby significantly improve the mechanical property of eutectic ceramic material, but the too fast pool depth that causes of sweep speed is not enough, is unfavorable for the preparation pottery.Laser scanning speed is set at 0.6～6mm/min.
The present invention can be selected from Al as the powder of raw-material eutectic composition
2O
3With Y
2O
3Binary eutectic, Al
2O
3With ZrO
2Binary eutectic, Al
2O
3With Gd
2O
3Binary eutectic, Al
2O
3With Er
2O
3Binary eutectic, Al
2O
3With Y
2O
3, Gd
2O
3, Er
2O
3And ZrO
2Ternary eutectic.
Because the present invention takes technique scheme, make laser fast forming surface atmosphere heating furnace by relatively poor to toughness, the material that thermal stress is big carries out soak to be handled, and effectively reduces the temperature difference of moulding material and surrounding environment and the thermal stress of material internal.When high energy laser irradiation during to the moulding material upper surface, lower surface is elevated to higher temperature simultaneously under the effect of heating furnace, the upper and lower surface temperature difference significantly reduces (ceramic material), even approach, thereby guarantee that base material can not swash the heat cracking, can guarantee again simultaneously that melt can not crack and defective because of Quench in the process of cooling, quality and the performance of material forming have been improved greatly, and make the laser fast forming technology prepare fragile material to become possibility, according to different materials, can realize different cooldown rate and thermograde by adjusting holding temperature.Because crackle disappears and thermal stress reduces, melt growth is more stable, is conducive to carry out laser rapid solidification Study on Theory.Utilization repeats to pile up, the method for cladding repeatedly, makes powder repeat to be fused to matrix, thereby realizes the preparation of eutectic ceramic.
The present invention simultaneously feeds inert protective gas in two road direction stoves in heating; make steam and air in the stove to discharge fully; the inner pore that produces when eliminating the melt rapid solidification; improve the compactness of material, accompanying drawing 1 shows that adopting surface atmosphere heating furnace auxiliary laser to spread powder solid forming single track Multi Slice Mode prepares Al
2O
3/ YAG/YSZ ternary eutectic pottery can obtain consolidation rear surface flawless, has unfused powder particle to be attached to the eutectic ceramic on surface.Through measuring, the thickness of consolidation layer is 8.2mm, and length is 65mm, and width is that 45mm reaches the dimensional requirement that large volume is shaped.Measure sample density by Archimedes' principle, reach 99.8% of solid density.By Metallographic Analysis, the ceramic material interior solid, the cross section of consolidation layer and longitudinal section smooth and flawless and hole, as shown in Figure 2, prepared Al
2O
3The smooth flawless of/YAG eutectic ceramic specimen surface but have at the edge not that the powder of penetration exists.For easy oxidation and volatile material, this device can also prevent that oxidation and composition change in the material laser forming process.
Description of drawings
Accompanying drawing 1. surface atmosphere heating furnace auxiliary lasers shop powder solid forming Al
2O
3/ YAG/YSZ ternary eutectic pottery photomacrograph.
Accompanying drawing 2 is surface atmosphere heating furnace auxiliary laser shop powder solid forming Al
2O
3/ YAG eutectic ceramic photomacrograph.
Accompanying drawing 3 is process charts of the present invention.
The specific embodiment
Embodiment one
Present embodiment is the method for the spontaneous composite ceramics of a kind of solid forming alumina base eutectic.Present embodiment adopts this method to prepare Al
2O
3/ YAG eutectic ceramic, its detailed process may further comprise the steps:
Step 1, preparation Al
2O
3/ YAG eutectic ceramic powder.With high-purity Al
2O
3, Y
2O
3Powder is raw material, according to eutectic molar percentage Al
2O
3: Y
2O
3=81: 19 ratio raw materials weighing adds the PVA binding agent in load weighted raw material; The PVA binding agent that adds is 10% of raw material total amount.The above-mentioned raw material that configures placed in the comprehensive planetary ball mill of PMQW shape mix 4h.Drum's speed of rotation is 100r/min.The Al that obtains preparing after powder is even
2O
3/ YAG eutectic ceramic powder.
Step 2, the shop powder of eutectic powder and the heating of surface atmosphere heating furnace.The part powder that obtains evenly is layered on forms substrate on the metal substrate, substrate thickness is 2～4mm, and length is 70mm, and width is 50mm.The metal substrate that is covered with substrate is placed on the heating plate of surface atmosphere heating furnace, and squeeze into the hole with insulation with the laser that heat-preservation cotton covers on the surface atmosphere heating furnace.Open the airometer valve and in burner hearth, feed protective gas N
2Gas; N
2Throughput 100～150ml/min.By Elema heating plate is heated, and then by heating plate powder is heated to 1200 ℃.Adding and pine for, is the heating of 20% speed with conduction ratio below 600 ℃, more than 600 ℃ is 40% speed heating with conduction ratio.Add and pine for continuing insulation, make specimen temperature consistent with temperature of heating plate.Add and pine for continuing to feed N
2Gas.Al after obtaining heating
2O
3The substrate of/YAG eutectic ceramic.Add and pine for setting heating power and heating-up temperature by regulating temperature controller.
Step 3, the shaping eutectic ceramic.Adopt the process of laser zone melting method shaping eutectic ceramic, its detailed process is:
Make laser instrument be positioned at Al
2O
3The starting point place of/YAG eutectic ceramic substrate surface shaping eutectic ceramic starts laser instrument, to the Al after the heating
2O
3The substrate of/YAG eutectic ceramic is carried out level and is lined by line scan.After laser instrument is finished first line scanning, along Al
2O
3The horizontal sweep of second row is carried out in the translation of/YAG eutectic ceramic substrate surface width, obtains at Al
2O
3The second road eutectic ceramic that/YAG eutectic ceramic substrate surface forms.By that analogy, laser instrument is gradually to Al
2O
3The width of/YAG eutectic ceramic substrate advances, until whole Al
2O
3/ YAG eutectic ceramic substrate surface forms the ground floor eutectic ceramic.After the shaping of ground floor eutectic ceramic is finished, with residual A l
2O
3/ YAG eutectic ceramic powder evenly shop overlays on the ground floor eutectic ceramic, and the thickness that the shop is covered is 2～4mm, and length is 70mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues shaping second layer eutectic ceramic on the ground floor eutectic ceramic surface that obtains.After the shaping of second layer eutectic ceramic is finished, continue residual A l
2O
3/ YAG eutectic ceramic powder evenly shop overlays on the second layer eutectic ceramic, and the thickness that the shop is covered is 2～4mm, and length is 70mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues the 3rd layer of eutectic ceramic that be shaped on the second layer eutectic ceramic surface that obtains.Repeat the process that above-mentioned laser zone is melt into the shape eutectic ceramic, obtain required eutectic ceramic.Above-mentioned shaping eutectic ceramic laser power is 500W, laser scanning speed 6mm/min, and laser spot diameter is 12mm, laser instrument is along Al
2O
3The spacing of adjacent two row center lines is 10mm after the translation of/YAG eutectic ceramic base widths.In the present embodiment, Al
2O
3/ YAG eutectic ceramic base widths is 50mm, and the laser scanning passage is 5 roads.In the molten process of laser zone, the surface atmosphere heating furnace continues heating to sample, makes the temperature of sample remain on 1200 ℃, and feeds N
2Gas.
Step 4, the cooling of eutectic pottery after obtaining volume required eutectic ceramic, is closed laser.After the surface atmosphere heating furnace was cooled to 800 ℃ with the cooling rate of 10 ℃/min, the eutectic ceramic that obtains cooled to room temperature with the furnace, thereby obtains the Al of surperficial flawless, interior solid
2O
3The spontaneous composite ceramic body of/YAG eutectic.
Embodiment two
Present embodiment is the method for the spontaneous composite ceramics of a kind of solid forming alumina base eutectic.Present embodiment adopts this method to prepare Al
2O
3/ YAG/YSZ ternary eutectic pottery, its detailed process may further comprise the steps:
Step 1, preparation Al
2O
3/ YAG/YSZ eutectic ceramic powder.With high-purity Al
2O
3, Y
2O
3, ZrO
2Powder is raw material, according to eutectic molar percentage Al
2O
3: Y
2O
3: ZrO
2=65.8: 15.6: 18.6 ratio raw materials weighing adds the PVA binding agent in load weighted raw material; The PVA binding agent that adds is 10% of raw material total amount.The above-mentioned raw material that configures placed in the comprehensive planetary ball mill of PMQW shape mix 4h.Drum's speed of rotation is 100r/min.Obtain preparing Al after powder is even
2O
3/ YAG/YSZ eutectic ceramic powder.
Step 2, the shop powder of eutectic powder and the heating of surface atmosphere heating furnace.The part powder that obtains evenly is layered on forms substrate on the metal substrate, substrate thickness is 3mm, and length is 80mm, and width is 50mm.The metal substrate that is covered with substrate is placed on the heating plate of surface atmosphere heating furnace, and squeeze into the hole with insulation with the laser that heat-preservation cotton covers on the surface atmosphere heating furnace.Open the airometer valve and in burner hearth, feed protective gas N
2Gas; N
2Throughput 100～150ml/min.By Elema heating plate is heated, and then by heating plate powder is heated to 1200 ℃.Adding and pine for, is the heating of 20% speed with conduction ratio below 600 ℃, more than 600 ℃ is 40% speed heating with conduction ratio.Add and pine for continuing insulation, make specimen temperature consistent with temperature of heating plate.Add and pine for continuing to feed N
2Gas.Al after obtaining heating
2O
3The substrate of/YAG eutectic ceramic.Add and pine for setting heating power and heating-up temperature by regulating temperature controller.
Step 3, the shaping eutectic ceramic.Adopt the process of laser zone melting method shaping eutectic ceramic, its detailed process is:
Make laser instrument be positioned at Al
2O
3The starting point place of/YAG/YSZ eutectic ceramic substrate surface shaping eutectic ceramic starts laser instrument, to the Al after the heating
2O
3The substrate of/YAG/YSZ eutectic ceramic is carried out level and is lined by line scan.After laser instrument is finished first line scanning, along Al
2O
3The horizontal sweep of second row is carried out in the translation of/YAG/YSZ eutectic ceramic substrate surface width, obtains at Al
2O
3The second road eutectic ceramic that/YAG/YSZ eutectic ceramic substrate surface forms.By that analogy, laser instrument is gradually to Al
2O
3The width of/YAG/YSZ eutectic ceramic substrate advances, until whole Al
2O
3/ YAG/YSZ eutectic ceramic substrate surface forms the ground floor eutectic ceramic.After the shaping of ground floor eutectic ceramic is finished, with residual A l
2O
3/ YAG/YSZ eutectic ceramic powder evenly shop overlays on the ground floor eutectic ceramic, and the thickness that the shop is covered is 3mm, and length is 800mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues shaping second layer eutectic ceramic on the ground floor eutectic ceramic surface that obtains.After the shaping of second layer eutectic ceramic is finished, continue residual A l
2O
3/ YAG/YSZ eutectic ceramic powder evenly shop overlays on the second layer eutectic ceramic, and the thickness that the shop is covered is 3mm, and length is 80mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues the 3rd layer of eutectic ceramic that be shaped on the second layer eutectic ceramic surface that obtains.Repeat the process that above-mentioned laser zone is melt into the shape eutectic ceramic, obtain required eutectic ceramic.Above-mentioned shaping eutectic ceramic laser power is 600W, laser scanning speed 3mm/min, and laser spot diameter is 12mm, laser instrument is along Al
2O
3The spacing of adjacent two row center lines is 10mm after the translation of/YAG/YSZ eutectic ceramic base widths.In the present embodiment, Al
2O
3/ YAG/YSZ eutectic ceramic base widths is 50mm, and the laser scanning passage is 5 roads.In the molten process of laser zone, the surface atmosphere heating furnace continues heating to sample, makes the temperature of sample remain on 1200 ℃, and feeds N
2Gas.
Step 4, the cooling of eutectic pottery after obtaining volume required eutectic ceramic, is closed laser.After the surface atmosphere heating furnace was cooled to 800 ℃ with the cooling rate of 20 ℃/min, the eutectic ceramic that obtains cooled to room temperature with the furnace, thereby obtains the Al of surperficial flawless, interior solid
2O
3The spontaneous composite ceramic body of/YAG/YSZ eutectic.
Embodiment three
Present embodiment is the method for the spontaneous composite ceramics of a kind of solid forming alumina base eutectic.Present embodiment adopts this method to prepare Al
2O
3/ GdAlO
3(GAP) eutectic ceramic, its detailed process may further comprise the steps:
Step 1, preparation Al
2O
3/ GAP eutectic ceramic powder.With high-purity Al
2O
3, Gd
2O
3Powder is raw material, according to eutectic molar percentage Al
2O
3: Gd
2O
3=77: 23 ratio raw materials weighing adds the PVA binding agent in load weighted raw material; The PVA binding agent that adds is 10% of raw material total amount.The above-mentioned raw material that configures placed in the comprehensive planetary ball mill of PMQW shape mix 4h.Drum's speed of rotation is 100r/min.Obtain preparing Al after powder is even
2O
3/ GAP eutectic ceramic powder.
Step 2, the shop powder of eutectic powder and the heating of surface atmosphere heating furnace.The part powder that obtains evenly is layered on forms substrate on the metal substrate, substrate thickness is 2～4mm, and length is 60mm, and width is 50mm.The metal substrate that is covered with substrate is placed on the heating plate of surface atmosphere heating furnace, and squeeze into the hole with insulation with the laser that heat-preservation cotton covers on the surface atmosphere heating furnace.Open the airometer valve and in burner hearth, feed protective gas N
2Gas; N
2Throughput 100～150ml/min.By Elema heating plate is heated, and then by heating plate powder is heated to 1200 ℃.Adding and pine for, is the heating of 20% speed with conduction ratio below 600 ℃, more than 600 ℃ is 40% speed heating with conduction ratio.Add and pine for continuing insulation, make specimen temperature consistent with temperature of heating plate.Add and pine for continuing to feed N
2Gas.Al after obtaining heating
2O
3The substrate of/GAP eutectic ceramic.Add and pine for setting heating power and heating-up temperature by regulating temperature controller.
Step 3, the shaping eutectic ceramic.Adopt the process of laser zone melting method shaping eutectic ceramic, its detailed process is:
Make laser instrument be positioned at Al
2O
3The starting point place of/GAP eutectic ceramic substrate surface shaping eutectic ceramic starts laser instrument, to the Al after the heating
2O
3The substrate of/GAP eutectic ceramic is carried out level and is lined by line scan.After laser instrument is finished first line scanning, along Al
2O
3The horizontal sweep of second row is carried out in the translation of/GAP eutectic ceramic substrate surface width, obtains at Al
2O
3The second road eutectic ceramic that/GAP eutectic ceramic substrate surface forms.By that analogy, laser instrument is gradually to Al
2O
3The width of/GAP eutectic ceramic substrate advances, until whole Al
2O
3/ GAP eutectic ceramic substrate surface forms the ground floor eutectic ceramic.After the shaping of ground floor eutectic ceramic is finished, with residual A l
2O
3/ GAP eutectic ceramic powder evenly shop overlays on the ground floor eutectic ceramic, and the thickness that the shop is covered is 2mm, and length is 60mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues shaping second layer eutectic ceramic on the ground floor eutectic ceramic surface that obtains.After the shaping of second layer eutectic ceramic is finished, continue residual A l
2O
3/ GAP eutectic ceramic powder evenly shop overlays on the second layer eutectic ceramic, and the thickness that the shop is covered is 2mm, and length is 60mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues the 3rd layer of eutectic ceramic that be shaped on the second layer eutectic ceramic surface that obtains.Repeat the process that above-mentioned laser zone is melt into the shape eutectic ceramic, obtain required eutectic ceramic.Above-mentioned shaping eutectic ceramic laser power is 400W, laser scanning speed 0.6mm/min, and laser spot diameter is 10mm, laser instrument is along Al
2O
3The spacing of adjacent two row center lines is 8mm after the translation of/GAP eutectic ceramic base widths.In the present embodiment, Al
2O
3/ GAP eutectic ceramic base widths is 50mm, and the laser scanning passage is 7 roads.In the molten process of laser zone, the surface atmosphere heating furnace continues heating to sample, makes the temperature of sample remain on 1200 ℃, and feeds N
2Gas.
Step 4, the cooling of eutectic pottery after obtaining volume required eutectic ceramic, is closed laser.After the surface atmosphere heating furnace was cooled to 800 ℃ with the cooling rate of 15 ℃/min, the eutectic ceramic that obtains cooled to room temperature with the furnace, thereby obtains the Al of surperficial flawless, interior solid
2O
3The spontaneous composite ceramic body of/GAP eutectic.
Embodiment four
Present embodiment is the method for the spontaneous composite ceramics of a kind of solid forming alumina base eutectic.Present embodiment adopts this method to prepare Al
2O
3/ Er
3Al
5O
12(EAG) eutectic ceramic, its detailed process may further comprise the steps:
Step 1, preparation Al
2O
3/ EAG eutectic ceramic powder.With high-purity Al
2O
3, Er
2O
3Powder is raw material, according to eutectic molar percentage Al
2O
3: Er
2O
3=81: 19 ratio raw materials weighing adds the PVA binding agent in load weighted raw material; The PVA binding agent that adds is 10% of raw material total amount.The above-mentioned raw material that configures placed in the comprehensive planetary ball mill of PMQW shape mix 4h.Drum's speed of rotation is 100r/min.Obtain preparing Al after powder is even
2O
3/ EAG eutectic ceramic powder.
Step 2, the shop powder of eutectic powder and the heating of surface atmosphere heating furnace.The part powder that obtains evenly is layered on forms substrate on the metal substrate, substrate thickness is 1.5mm, and length is 70mm, and width is 50mm.The metal substrate that is covered with substrate is placed on the heating plate of surface atmosphere heating furnace, and squeeze into the hole with insulation with the laser that heat-preservation cotton covers on the surface atmosphere heating furnace.Open the airometer valve and in burner hearth, feed protective gas N
2Gas; N
2Throughput 100～150ml/min.By Elema heating plate is heated, and then by heating plate powder is heated to 1200 ℃.Adding and pine for, is the heating of 20% speed with conduction ratio below 600 ℃, more than 600 ℃ is 40% speed heating with conduction ratio.Add and pine for continuing insulation, make specimen temperature consistent with temperature of heating plate.Add and pine for continuing to feed N
2Gas.Al after obtaining heating
2O
3The substrate of/EAG eutectic ceramic.Add and pine for setting heating power and heating-up temperature by regulating temperature controller.
Step 3, the shaping eutectic ceramic.Adopt the process of laser zone melting method shaping eutectic ceramic, its detailed process is:
Make laser instrument be positioned at Al
2O
3The starting point place of/EAG eutectic ceramic substrate surface shaping eutectic ceramic starts laser instrument, to the Al after the heating
2O
3The substrate of/EAG eutectic ceramic is carried out level and is lined by line scan.After laser instrument is finished first line scanning, along Al
2O
3The horizontal sweep of second row is carried out in the translation of/EAG eutectic ceramic substrate surface width, obtains at Al
2O
3The second road eutectic ceramic that/EAG eutectic ceramic substrate surface forms.By that analogy, laser instrument is gradually to Al
2O
3The width of/EAG eutectic ceramic substrate advances, until whole Al
2O
3/ EAG eutectic ceramic substrate surface forms the ground floor eutectic ceramic.After the shaping of ground floor eutectic ceramic is finished, with residual A l
2O
3/ EAG eutectic ceramic powder evenly shop overlays on the ground floor eutectic ceramic, and the thickness that the shop is covered is 1.5mm, and length is 70mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues shaping second layer eutectic ceramic on the ground floor eutectic ceramic surface that obtains.After the shaping of second layer eutectic ceramic is finished, continue residual A l
2O
3/ EAG eutectic ceramic powder evenly shop overlays on the second layer eutectic ceramic, and the thickness that the shop is covered is 1.5mm, and length is 70mm, and width is 50mm.Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues the 3rd layer of eutectic ceramic that be shaped on the second layer eutectic ceramic surface that obtains.Repeat the process that above-mentioned laser zone is melt into the shape eutectic ceramic, obtain required eutectic ceramic.Above-mentioned shaping eutectic ceramic laser power is 200W, laser scanning speed 2.4mm/min, and laser spot diameter is 8mm, laser instrument is along Al
2O
3The spacing of adjacent two row center lines is 7mm after the translation of/EAG eutectic ceramic base widths.In the present embodiment, Al
2O
3/ EAG eutectic ceramic base widths is 50mm, and the laser scanning passage is 8 roads.In the molten process of laser zone, the surface atmosphere heating furnace continues heating to sample, makes the temperature of sample remain on 1200 ℃, and feeds N
2Gas.
Step 4, the cooling of eutectic pottery after obtaining volume required eutectic ceramic, is closed laser.After the surface atmosphere heating furnace was cooled to 800 ℃ with the cooling rate of 10 ℃/min, the eutectic ceramic that obtains cooled to room temperature with the furnace, thereby obtains the Al of surperficial flawless, interior solid
2O
3The spontaneous composite ceramic body of/EAG eutectic.
Claims (2)
1. the method for the spontaneous composite ceramics of laser solid forming alumina base eutectic is characterized in that, may further comprise the steps: step 1, preparation eutectic ceramic powder;
Step 2, the shop powder of eutectic ceramic powder and the heating of surface atmosphere heating furnace; The part eutectic ceramic powder that obtains evenly is layered on forms substrate on the metal substrate; The metal substrate that is covered with substrate is placed on the heating plate of surface atmosphere heating furnace; Open the airometer valve and in burner hearth, feed protective gas N
2Gas; N
2Throughput 100～150ml/min; Eutectic powder being heated to 1200 ℃, adding and pine for, is the heating of 20% speed with conduction ratio below 600 ℃, more than 600 ℃ is 40% speed heating with conduction ratio; Specimen temperature is consistent with temperature of heating plate in the heating; Add and pine for continuing to feed N
2Gas; Al after obtaining heating
2O
3The substrate of/YAG eutectic ceramic;
Step 3, the shaping eutectic ceramic; Adopt the process of laser zone melting method shaping eutectic ceramic, its detailed process is: make laser instrument be positioned at the starting point place of eutectic ceramic substrate surface shaping eutectic ceramic, level is carried out in the eutectic ceramic substrate after the heating line by line scan; After laser instrument is finished first line scanning, along the translation of eutectic ceramic substrate surface width, carry out the horizontal sweep of second row, obtain the second road eutectic ceramic that forms at the eutectic ceramic substrate surface; By that analogy, laser instrument advances to the width of eutectic ceramic substrate gradually, forms the ground floor eutectic ceramic until whole eutectic ceramic substrate surface; After the shaping of ground floor eutectic ceramic is finished, remaining eutectic ceramic powder is evenly overlayed on the ground floor eutectic ceramic shop; Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues shaping second layer eutectic ceramic on the ground floor eutectic ceramic surface that obtains; After the shaping of second layer eutectic ceramic is finished, continue remaining eutectic ceramic powder is evenly overlayed on the second layer eutectic ceramic shop; Laser instrument is got back to starting point, by the method for shaping ground floor eutectic ceramic, continues the 3rd layer of eutectic ceramic that be shaped on the second layer eutectic ceramic surface that obtains; Repeat the process that above-mentioned laser zone is melt into the shape eutectic ceramic, obtain required eutectic ceramic; In the shaping eutectic ceramic, laser power is 200～600W, laser scanning speed 0.6～6mm/min, and laser spot diameter is 8～12mm; In the molten process of laser zone, the surface atmosphere heating furnace continues heating to sample, makes the temperature of sample remain on 1200 ℃, and feeds N
2Gas;
Step 4, eutectic pottery cooling, after obtaining volume required eutectic ceramic, after the surface atmosphere heating furnace was cooled to 800 ℃ with the cooling rate of 10～20 ℃/min, the eutectic ceramic that obtains cooled to room temperature with the furnace, thereby obtains the spontaneous composite ceramics of eutectic.
2. the method for the spontaneous composite ceramics of a kind of laser solid forming alumina base eutectic according to claim 1 is characterized in that, laser instrument spacings of adjacent two row center lines after the translation of eutectic ceramic base widths are 10mm.
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| CN107235731B (en) * | 2017-05-12 | 2020-04-03 | 西南交通大学 | Eutectic structure ultra-high temperature ZrB2-SiC complex phase ceramic and preparation method thereof |
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| CN113264767A (en) * | 2020-03-09 | 2021-08-17 | 西北工业大学深圳研究院 | alumina/GAP eutectic ceramic and preparation method thereof |
| CN112441834B (en) * | 2020-11-22 | 2022-08-02 | 西北工业大学 | Selective laser melting for preparing Al 2 O 3 -GdAlO 3 -ZrO 2 Method for preparing ternary eutectic ceramics |
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