CN112441834B - Selective laser melting for preparing Al 2 O 3 -GdAlO 3 -ZrO 2 Method for preparing ternary eutectic ceramics - Google Patents

Selective laser melting for preparing Al 2 O 3 -GdAlO 3 -ZrO 2 Method for preparing ternary eutectic ceramics Download PDF

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CN112441834B
CN112441834B CN202011316115.3A CN202011316115A CN112441834B CN 112441834 B CN112441834 B CN 112441834B CN 202011316115 A CN202011316115 A CN 202011316115A CN 112441834 B CN112441834 B CN 112441834B
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苏海军
申仲琳
刘海方
赵迪
刘园
郭一诺
郭敏
张军
刘林
傅恒志
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Northwestern Polytechnical University
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Abstract

A selective laser melting method of blocky ternary eutectic oxide ceramic adopts CO 2 Laser selective melting method and mixing CO 2 The scanning speed and the laser power of the laser selective melting method are controlled in the range, the melt material in the laser scanning area obtains larger super-cooling degree, and the nucleation rate is increased, so that the eutectic structure is refined, and the mechanical property of the sample is improved. Preparing to obtain large-size blocky Al 2 O 3 ‑GdAlO 3 ‑ZrO 2 Eutectic ceramics, Al prepared therefrom 2 O 3 ‑GdAlO 3 ‑ZrO 2 The size of the eutectic ceramics after wire passing cutting reaches 20 multiplied by 18 multiplied by 3.5mm 3 . The scanning speed of the invention can reach 5000mm/s at most, and the ceramic material has the function of CO treatment 2 The laser has high energy absorption rate, and is more beneficial to the complete melting and solidification forming of the oxide ceramic material. Meanwhile, the laser beam selectively melts and solidifies the powder layer according to the set path and parameters of the computer, and the powder layers are stacked layer by layer, so that the solidified eutectic ceramic sample with large size and complex shape can be prepared.

Description

Selective laser melting for preparing Al 2 O 3 -GdAlO 3 -ZrO 2 Method for preparing ternary eutectic ceramics
Technical Field
The invention relates to the field of ceramic materials, in particular to massive Al 2 O 3 -GdAlO 3 -ZrO 2 Ternary eutectic ceramics and a preparation method thereof.
Background
Experiments prove that the Al prepared by the directional solidification technology 2 O 3 -GdAlO 3 The eutectic ceramic has the characteristics of excellent high-temperature strength, oxidation resistance, creep resistance, high-temperature structural stability and the like, for example, the yield strength of the ceramic material reaches 690MPa from room temperature to 1600 ℃, and the bending strength can be kept almost unchanged within the range of 500-600 MPa. After the ceramic material is exposed for 500 hours in the atmospheric environment at 1700 ℃, the strength is basically unchanged, the solidification structure is not coarsened obviously, and the size, the surface roughness and the weight of a sample are basically unchanged, which shows that the ceramic material has good oxidation resistance, high-temperature structure stability and high-temperature mechanical property. It was found that ZrO 2 The addition of the (A) can obviously improve the fracture toughness of a ceramic sample, and the fracture toughness of the binary eutectic ceramic can be increased from 5-6 MPa.m 1/2 Increased to 8.5 MPa.m 1/2 . Thus, Al 2 O 3 -GdAlO 3 -ZrO 2 The ternary eutectic ceramic has great development potential, and is expected to become a new generation of ultra-high temperature structural material with high performance and high efficiency and stable work in the atmosphere of 1400-1600 ℃.
At present, Al 2 O 3 -GdAlO 3 The preparation method of the eutectic ceramics mainly comprises an improved Bridgman method, a discharge plasma sintering method, a laser suspension zone melting method, a laser base growing method and the like. The improved Bridgman method can prepare large-size eutectic ceramic cast ingots with the diameter of 53mm and the length of 700 mm. However, this technique is inefficient and the use of crucibles increases the cost of the process. In addition, the temperature gradient of the technology is less than 100K/cm and is relatively low, so that the structure of a sample is coarse, and the improvement of the mechanical property of the material is hindered. The micro-drawing method and the laser pedestal growth method are both suitable for preparing fiber or thin rod-shaped samples with the diameter below millimeter, and the microstructure can be regulated and controlled by regulating the drawing speed, so that micron-level or even nano-level microstructures are obtained, and the mechanical property of the material is effectively improved. But the technique is difficult to realize the preparation of large-size samples. The laser suspension zone melting method adopts high-energy laser beams as heat sources, has higher temperature gradient of about 10 DEG 4 K/cm, tissue densification can be obtainedCeramic samples without obvious pores and cracks are obtained, but most of the samples are rod-shaped, and the diameter of the samples is generally less than 5 mm. The laser horizontal zone melting method can melt and process a ceramic preform to obtain a smooth and compact rod-shaped or plate-shaped sample, and the structure can be thinned to be 100nm or less, but the laser horizontal zone melting method is mostly used for surface treatment of materials.
The selective laser melting method is an additive manufacturing technology developed in recent years, and has the advantages of high efficiency, high speed, no need of a mold, flexible manufacturing and the like. The selective laser melting method can rapidly prepare parts with specific geometric shapes in one step by directly melting powder materials and stacking layer by layer. At present, the method is more applied to the preparation of metal materials, and due to the inherent high melting point and the brittle and hard characteristics of ceramic materials, various defects such as air holes, cracks and the like are easily generated in the processing process, so that the preparation difficulty of large-size and high-quality ceramic samples is increased.
The document "Z.Fan, M.Lu, H.Huang.Selective laser scaling of aluminum: A single track study [ J.]The ceramic International 2018,44:9484- 2 O 3 The dendrite structure has a coarse and uneven structure, which hinders the improvement of the mechanical properties of the material.
The patent "liuting, zhayang, zhangchang, Yan, shuai, Liangwenhe, du dao a binderless laser selective melting/sintering process for ceramic slurry]Chinese patent: CN 107973607 a, 2018-05-01, "discloses a forming method for selective laser melting/sintering of a preset slurry layer by using a laser, and the obtained size is 10 × 10 × 2mm 3 The method is complex in operation, firstly, slurry with a certain mass fraction needs to be prepared, the substrate is paved in advance, the thickness is kept to be 30 mu m, then, the slurry layer is preheated by using an induction heating system, and after the water is evaporated by about 95%, selective laser melting is carried out by using a laser. When the processing layer is cooled to 50-130 ℃, powder is repeatedly presetAnd carrying out layer and printing operation until a set three-dimensional solid sample is processed. The method is complicated and time-consuming, and requires repeated slurry preparation, powder layer drying, powder layer preheating and sintering/melting, thereby increasing the complexity of operation.
The documents "J.Guan, Q.Wang, X.Zhang, Y.Jiang, Y.Yan, J.Xiao, B.ren, Selective laser marking of yttria-stabilized zirconia [ J.]Materials Research Express,2019,6:015402-1-9. "selective laser melting of powder material directly with Nd: YAG laser, prepared with dimensions of 10 × 10 × 5mm 3 Cubic bulk zirconia (yttria) ceramics. But the surface and the section of the sample show sintering structure morphology, and the high-temperature mechanical property of the material is seriously influenced.
The documents "H.Liu, H.Su, Z.Shen, D.ZHao, Y.Liu, M.Guo, Y.Guo, J.Zhang, L.Liu, H.Fu. Effect of scanning speed on the geographic process of Al 2 O 3 /GdAlO 3 /ZrO 2 eutectic ceramics in a single track by selective laser melting[J]Ceramic powder is directly melted and rapidly formed by selective laser melting technology 17257, and Al is prepared 2 O 3 -GdAlO 3 -ZrO 2 Ternary eutectic ceramic samples. The method has the advantages of no need of preparing prefabricated body, simplified preparation process, and fine and compact structure. However, only a single-layer powder layer is scanned in the processing process, and the obtained ceramic has a simple shape, a crescent-shaped section and a small thickness which is not more than 2 mm.
The selective laser melting technology adopts a processing mode of powder layer by layer and cladding, a high-energy laser beam selectively melts and solidifies a thin layer of powder material according to a scanning path set in a computer, and solid sample pieces with set shapes are prepared by layer stacking and fusing. The technology has the characteristics of high forming freedom degree, high processing speed, high temperature gradient and the like. At present, various metal sample pieces with complex shapes are prepared by the technology, and the application in the field of oxide eutectic ceramic materials is less. In view of this, the invention provides a selective laser melting method of a bulk ternary eutectic oxide ceramic.
Disclosure of Invention
In order to overcome the defects of difficult ceramic material forming and thick sintering structure in the prior art, the invention provides a selective laser melting method of a blocky ternary eutectic oxide ceramic.
The specific process of the invention is as follows:
step 1, preparing Al of eutectic composition 2 O 3 -Gd 2 O 3 -ZrO 2 Spherical mixed powder material:
al for preparing eutectic composition 2 O 3 -Gd 2 O 3 -ZrO 2 When the spherical mixed powder material is used, Al with the total mass of 400g is weighed 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 Powder; the Al is 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 The proportion of the powder is eutectic molar ratio Al 2 O 3 :Gd 2 O 3 :ZrO 2 58:19: 23. Weighing Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 Mixing the powders, adding alcohol and polyvinyl alcohol solution, and ball milling for 2h to obtain a mixture.
Carrying out spray granulation on the obtained mixture to obtain spherical powder with the particle size distribution of 10-50 microns; and drying the powder material to obtain dry spherical mixed powder with good fluidity. During spray granulation, the air inlet temperature is 250-350 ℃, the air outlet temperature is 100-170 ℃, the rotating frequency of a spray head is 20-25 Hz, and the feeding rotating speed is 5-35 pm.
The dosage of the alcohol is the Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 10 wt.% of the total mass of the powder, the polyvinyl alcohol solution being used in an amount of the Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 5 wt.% of the total mass of the powder.
Step 2, establishing a test piece model:
and establishing the test piece model through Magics preprocessing software.
And the geometric center of the test piece model is positioned at (95,95,2) of the machining platform coordinate system of the PLD laser pulse deposition device.
And slicing the cross section of the established cylinder model in a layered mode. The thickness of the slice is 0.02 mm. And during slicing, sequentially slicing the cylinder model from bottom to top in a layering manner along the axial direction of the cylinder model by taking the contact end of the cylinder model and the surface of the platform as a starting point until the contact end reaches the top end of the cylinder model, and sequentially obtaining a first slicing layer, a second slicing layer, a third slicing layer, … … and an nth slicing layer.
Step 3, determining the laser scanning path of each slice layer:
and arranging a laser scanning path on the surfaces of the first sliced layer to the eighth sliced layer in sequence. The set laser scanning paths are all in a zigzag shape. The paths from the first sliced layer to the eighth sliced layer are the same; the laser scan path on the subsequent slice layer is rotated clockwise by 45 deg. on the basis of the previous slice layer. The scanning paths of the eight slice layers form one scanning period of 360 °.
The specific process for determining the laser scanning path is as follows:
i, setting a scanning path of a first slice layer:
the surface of the first slice layer is used as a scanning surface.
A plurality of scanning strips are set on the scanning surface of the first slice layer, the width k of each scanning strip is 10mm, and the interval h between adjacent scanning strips is 0.1 mm. And enabling a central line in the width direction of a scanning strip positioned in the middle of the end face of the model to pass through the center of the model. The scanning strips are parallel to each other. The joint of each scanning strip and the outer edge of the end face of the model at the position is taken as a scanning starting point.
The width of the strip at the outer edge of the end face is adjusted along with the change of the circumference, and the width is 0-10 mm.
II, setting a scanning path of the second slice layer:
the scanning path of the second slice layer is the same as that of the first slice layer, and the second slice layer is rotated by an angle theta which is 45 degrees in the clockwise direction on the basis of the first slice layer.
III, setting a scanning path of a third slice layer:
the scanning path of the third slice layer is the same as that of the second slice layer, and the third slice layer is rotated by an angle alpha in the clockwise direction on the basis of the second slice layer, wherein the angle alpha is 45 degrees.
And circularly repeating the process of setting the second slice layer scanning path and the third slice layer scanning path to complete the setting of the fourth slice layer scanning path to the eighth slice layer scanning path.
At this point, the first scanning period of 360 ° is formed from the first slice layer scanning path to the eighth slice layer scanning path.
And repeating the process of setting the first scanning period to sequentially obtain the rest scanning periods until the path setting of all the slicing layers is completed.
And 4, setting scanning parameters.
Multi-layer scanning is adopted during scanning. The first scanning layer of the scanning is a surface layer, and the rest scanning layers are filling layers. The scanning parameters of the surface layer are different from the scanning parameters of the filling layers.
The scan parameters include laser power and scan rate.
The laser power of the surface layer is determined to be 150-200W, and the scanning speed is determined to be 250-350 mm/s. Determining the laser power of each filling layer to be 120-145W; the scanning speed is 250-350 mm/s.
And 5, carrying out a selective laser melting test.
The selective laser melting test was performed using a PLD laser pulse deposition apparatus.
The selective scanning is to scan the powder in the scanning area e, and then melt and solidify the powder to form a ceramic sample; the powder outside the scanning area is not scanned and remains in a powder state. The scan area e is the surface area of each slice.
And (4) taking the scanning path of each sliced layer set in the step (3) as the scanning path of each solidified layer in the selective laser melting test. By CO in the PLD laser pulse deposition device 2 And 4, carrying out selective laser melting by the laser according to the scanning parameters set in the step 4.
The specific processing process comprises the following steps:
first, Al is added 2 O 3 The ceramic substrate is placed in the center of a processing platform of the PLD laser pulse deposition device which is horizontally fixed.
And secondly, moving a scraper to the position above the ceramic substrate, and enabling the scraper to be positioned between 400 and 500mm of the X axis of the machining platform coordinate system of the PLD laser pulse deposition device.
The vertical distance between the surface of the processing platform and the lower surface of the scraper is 0.15 mm.
And thirdly, putting the mixed powder obtained in the step 1 into a powder feeding platform of a PLD laser pulse deposition device, and scraping the surface layer of the powder by a scraper to finish the laying of the first layer of powder on the surface of the substrate. The thickness of the first layer of powder was 0.15 mm.
And fourthly, washing gas. And closing the door of the PLD laser pulse deposition device and opening the protective gas valve to start gas washing. The protective gas is argon, and the pressure is 0.5 MPa. The scrubbed condition was maintained until the end of the test.
And fifthly, carrying out a selective laser melting test. The selective laser melting test is carried out in layers in sequence until the number of solidified layers is the same as that of sliced layers. To obtain Al 2 O 3 -GdAlO 3 -ZrO 2 Ternary eutectic ceramics.
The specific process for carrying out the selective laser melting test is as follows:
i preparation of a first solidified layer.
CO for starting the PLD laser pulse deposition device 2 A laser that starts scanning from the beginning of the first slice layer scan path. And taking the surface range of the first cut sheet layer as a scanning area e, and carrying out laser melting on the first layer of powder according to the set scanning path of the first cut sheet layer. Obtaining a first solidified layer; the solidified layer is eutectic ceramic.
The first solidified layer is a surface layer. The laser power of the surface layer was 150W, and the scanning rate was 300 mm/s.
II, preparing a second solidified layer.
Laying a second layer of the mixed powder on the surface of the first solidified layer; the thickness of the mixed powder was 0.02 mm.
And moving a scraper to a position with the X axis of the PLD laser pulse deposition device coordinate system of 676mm to scrape the second layer of mixed powder.
CO for starting the PLD laser pulse deposition device 2 And the laser starts scanning from the starting point of the scanning path of the second slice layer by taking the surface range of the second slice layer as a scanning area e. And carrying out laser melting on the second layer of powder according to the set scanning path of the second sliced layer. A second solidified layer is obtained. The second solidified layer is a filling layer. The laser power of the filling layer is 130W; the scanning rate was 300 mm/s.
III preparing other solidified layers.
And circularly repeating the preparation process of the second solidified layer, and respectively and sequentially preparing the rest solidified layers. Until the number of solidified layers is the same as that of sliced layers; to obtain Al 2 O 3 -GdAlO 3 -ZrO 2 Ternary eutectic ceramics.
To this end, Al is completed 2 O 3 -GdAlO 3 -ZrO 2 And (3) preparing the ternary eutectic ceramic.
The invention can obtain large-size Al 2 O 3 -GdAlO 3 -ZrO 2 Eutectic ceramic, Al produced 2 O 3 -GdAlO 3 -ZrO 2 The size of the eutectic ceramics after wire passing cutting reaches 20 multiplied by 18 multiplied by 3.5mm 3 。
The preparation method provided by the invention adopts CO 2 Laser selective melting method and mixing CO 2 The scanning speed and the laser power of the laser selective melting method are controlled in the range, so that the invention can prepare large-size blocky Al 2 O 3 -GdAlO 3 -ZrO 2 The results of the examples of the eutectic ceramics show that the Al prepared by the invention 2 O 3 -GdAlO 3 -ZrO 2 The size of the eutectic ceramics reaches 20 multiplied by 18 multiplied by 3.5mm 3 And after the parameters are optimized, a eutectic solidification ceramic sample with a larger size is expected to be obtained. As can be seen from the microstructure morphology of the sample shown in FIG. 4, the obtained eutectic ceramicThe microstructure is fine and compact, and the typical intertwined three-dimensional network eutectic solidification structure appearance is presented. High energy CO in selective laser melting 2 The laser directly and rapidly melts the ceramic powder material, the powder material generates eutectic reaction, and a typical eutectic structure is generated in solidification. In addition, the PLD laser pulse deposition apparatus has a high temperature gradient (greater than 10 deg.C) during operation 4 K/cm), the laser scanning area can obtain larger supercooling degree of the melt material, and the nucleation rate is increased, so that the eutectic structure is refined, and the mechanical property of the sample is improved.
Compared with the prior art, the invention has the following advantages:
1. the forming speed is high. Al in the invention 2 O 3 -GdAlO 3 -ZrO 2 The scanning speed of the ternary eutectic ceramic can reach 5000mm/s at most, and Al is prepared by other methods 2 O 3 -GdAlO 3 -ZrO 2 The fastest forming speed reported in the prior art is only 0.8mm/s for ternary eutectic ceramics.
2. Ceramic material to CO 2 The laser has high energy absorption rate. The selective laser melting equipment adopts CO 2 The laser is used as a light source to process the ceramic material, and has greater advantages than the fiber lasers reported in most documents, mainly due to the fact that the laser has high power and high energy, and the oxide ceramic material has high laser absorption rate, so that the full melting and solidification forming of the oxide ceramic material are facilitated.
3. The preparation method provided by the invention has high forming freedom, and the laser beam selectively melts and solidifies the powder layer according to the set path and parameters of the computer, and the powder layer is stacked layer by layer, so that the solidified eutectic ceramic sample with large size and complex shape can be prepared. There is theoretically no limitation on the shape and size of the target structural member. Through the subsequent process optimization, large-size Al with higher quality is expected to be prepared 2 O 3 -GdAlO 3 -ZrO 2 Eutectic ceramic test specimens.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is a diagram of a scan path configured in accordance with the present invention; wherein, FIG. 2a is a schematic diagram of a first layer scanning path; FIG. 2b is a schematic diagram of a second layer scan path; fig. 2c is a third layer scan path diagram.
In the figure: h is the distance between two adjacent strips in the scanning path; k is the width of the strip in the path; e is a scanning area; z is the zig-zag scan path within the strip; theta is the rotation angle of the second layer scanning path; α is the rotation angle of the third layer scan path.
FIG. 3 shows Al prepared in example 1 of the present invention 2 O 3 -GdAlO 3 -ZrO 2 Morphology of eutectic ceramics: FIG. 3a is a graph of the processed profile of a sample; FIG. 3b is the cut topography of FIG. 3 a; figure 3c is a side view of the sample after cutting.
FIG. 4 shows Al prepared 2 O 3 -GdAlO 3 -ZrO 2 The microstructure morphology of the eutectic ceramic.
Detailed Description
The invention relates to a method for preparing Al by selective laser melting 2 O 3 -Gd 2 O 3 -ZrO 2 The method of the ternary eutectic ceramic comprises the following specific processes:
step 1, preparing Al of eutectic composition 2 O 3 -Gd 2 O 3 -ZrO 2 Spherical mixed powder material:
weighing Al in a total mass of 400g 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 Powder; the Al is 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 The proportion of the powder is eutectic molar ratio Al 2 O 3 :Gd 2 O 3 :ZrO 2 ＝58:19:23。
Weighing Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 The powders were mixed and added with alcohol and polyvinyl alcohol solution, and the mixture was ball-milled for 2 hours at a rotation speed of 550rpm using a ball mill to obtain a mixture. The dosage of the alcohol is the Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 10 wt.% of the total mass of the powder, the polyvinyl alcohol solution being used in an amount of the Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 5 wt.% of the total mass of the powder.
The above mixture was spray granulated by a conventional spray granulation method. During spray granulation, the air inlet temperature is 250-350 ℃, the air outlet temperature is 100-170 ℃, the rotating frequency of a spray head is 20-25 Hz, and the feeding rotating speed is 5-35 pm. And after spray granulation, sieving the collected powder to obtain spherical powder with the particle size distribution of 10-50 microns. Drying the powder material at 80 ℃ for 4h to obtain dry spherical mixed powder with good fluidity.
Step 2, establishing a test piece model:
and establishing the test piece model through Magics preprocessing software. The test piece model is a cylinder; the diameter is 50mm and the height is 4 mm.
And the geometric center of the test piece model is positioned at (95,95,2) of the machining platform coordinate system of the PLD laser pulse deposition device.
And slicing the cross section of the established cylinder model in a layered mode. The thickness of the slice is 0.02 mm. And during slicing, sequentially slicing the cylinder model from bottom to top in a layering manner along the axial direction of the cylinder model by taking the contact end of the cylinder model and the surface of the platform as a starting point until the contact end reaches the top end of the cylinder model, and sequentially obtaining a first slicing layer, a second slicing layer, a third slicing layer, … … and an nth slicing layer.
Step 3, determining the laser scanning path of each slice layer:
and arranging a laser scanning path on the surfaces of the first sliced layer to the eighth sliced layer in sequence. The set laser scanning paths are all in a zigzag shape. The paths from the first sliced layer to the eighth sliced layer are the same; the laser scan path on the subsequent slice layer is rotated clockwise by 45 deg. on the basis of the previous slice layer. The scanning paths of the eight sliced layers form one scanning cycle of 360 °.
The specific process for determining the laser scanning path is as follows:
i, setting a scanning path of the first slice layer:
the surface of the first slice layer is used as a scanning surface. A zigzag scanning path is set on the scanning surface, and the scanning of the surface of the first slice layer is completed by means of scanning-folding-scanning. The method comprises the following steps:
a plurality of scanning strips are set on the scanning surface of the slice, the width k of each scanning strip is 10mm, and the interval h between adjacent scanning strips is 0.1 mm. And enabling a central line in the width direction of a scanning strip positioned in the middle of the end face of the model to pass through the center of the model. The scanning strips are parallel to each other. The joint of each scanning strip and the outer edge of the end face of the model at the position is taken as a scanning starting point, as shown in FIG. 2.
The width of the strip at the outer edge of the end face is adjusted along with the change of the circumference, and the width is 0-10 mm.
II, setting a scanning path of the second slice layer:
the scanning path of the second slice layer is the same as that of the first slice layer, and the second slice layer is rotated by an angle theta which is 45 degrees in the clockwise direction on the basis of the first slice layer.
III, setting a scanning path of a third slice layer:
the scanning path of the third slice layer is the same as that of the second slice layer, and the third slice layer is rotated by an angle alpha in the clockwise direction on the basis of the second slice layer, wherein the angle alpha is 45 degrees.
And circularly repeating the process of setting the second slice layer scanning path and the third slice layer scanning path to complete the setting of the fourth slice layer scanning path to the eighth slice layer scanning path.
At this point, the first scanning period of 360 ° is formed from the first slice layer scanning path to the eighth slice layer scanning path.
And repeating the process of setting the first scanning period to sequentially obtain the rest scanning periods until the path setting of all the slicing layers is completed.
And 4, setting scanning parameters.
Multi-layer scanning is adopted during scanning. The first scanning layer of the scanning is a surface layer, and the rest scanning layers are filling layers. The scanning parameters of the surface layer are different from the scanning parameters of the filling layers.
The scan parameters include laser power and scan rate.
Determining the laser power of the surface layer to be 150-200W and the scanning speed to be 250-350 mm/s. Determining the laser power of each filling layer to be 120-145W; the scanning speed is 250-350 mm/s.
And 5, carrying out a selective laser melting test.
A PLD laser pulse deposition apparatus was used for the selective laser melting test.
The selective scanning is to scan the powder in the scanning area e, then melt and solidify the powder into a ceramic sample; the powder outside the scanning area is not scanned and remains in a powder state. The scanning area e is the surface area of each slice.
And (4) taking the scanning path of each sliced layer set in the step (3) as the scanning path of each solidified layer in the selective laser melting test.
By CO in the PLD laser pulse deposition device 2 And 4, carrying out selective laser melting by the laser according to the scanning parameters set in the step 4. The specific processing process comprises the following steps:
in the first step, the size is 100X 10mm 3 95% pure Al 2 O 3 The ceramic substrate is placed in the center of a processing platform of the PLD laser pulse deposition device which is horizontally fixed.
And secondly, moving a scraper to the position above the ceramic substrate, and enabling the scraper to be positioned between 400 and 500mm of the X axis of the machining platform coordinate system of the PLD laser pulse deposition device.
And measuring the vertical distance between the lower surface of the scraper and the ceramic substrate. The height of the processing platform is adjusted to ensure that the vertical distance between the processing platform and the lower surface of the scraper is 0.15 mm.
And thirdly, putting the mixed powder obtained in the step 1 into a powder feeding platform of a PLD laser pulse deposition device, and scraping the surface layer of the powder by a scraper to finish the laying of the first layer of powder on the surface of the substrate. The thickness of the first layer of powder was 0.15 mm.
And moving the scraper along the X axis of the machining platform coordinate system of the PLD laser pulse deposition device to enable the X axis coordinate position of the scraper to be 676mm, and taking the X axis coordinate position as the operation starting point of the scraper.
And fourthly, washing gas. And closing the door of the PLD laser pulse deposition device, opening a protective gas valve and starting gas washing. The protective gas is argon, and the pressure is 0.5 MPa. The scrubbed condition was maintained until the end of the test.
And fifthly, carrying out a selective laser melting test. The selective laser melting test is sequentially carried out in a layered manner, and specifically comprises the following steps:
i preparation of a first solidified layer.
CO for starting the PLD laser pulse deposition device 2 A laser that starts scanning from the beginning of the first slice layer scan path. And taking the surface range of the first cut sheet layer as a scanning area e, and carrying out laser melting on the first layer of powder according to the set scanning path of the first cut sheet layer. Obtaining a first solidified layer; the solidified layer is eutectic ceramic.
The first solidified layer is a surface layer. The laser power of the surface layer was 170W, and the scanning rate was 320 mm/s.
II preparing a second solidified layer.
Laying a second layer of the mixed powder on the surface of the first solidified layer; the mixed powder was laid to a thickness of 0.03 mm.
And moving a scraper to a position with the X axis of the PLD laser pulse deposition device coordinate system of 676mm to scrape the second layer of mixed powder.
CO for starting the PLD laser pulse deposition device 2 And the laser starts scanning from the starting point of the scanning path of the second slice layer by taking the surface range of the second slice layer as a scanning area e. And carrying out laser melting on the second layer of powder according to the set scanning path of the second sliced layer. A second solidified layer is obtained. The second solidified layer is a filling layer. The laser power of the filling layer is 120W; the scanning rate was 300 mm/s.
III preparing the rest of solidified layers.
And circularly repeating the preparation process of the second solidified layer, and respectively and sequentially preparing the rest solidified layers. Up to a solidified layerThe number of layers is the same as the number of layers of the sliced layer. To Al 2 O 3 -GdAlO 3 Binary eutectic ceramics.
To this end, Al is completed 2 O 3 -GdAlO 3 -ZrO 2 And (3) preparing the ternary eutectic ceramic.
The present invention will be specifically described by means of five embodiments. The procedure is the same for each example. The process parameters for each example are shown in Table 1.
TABLE 1
Figure BDA0002791470190000101
Figure BDA0002791470190000111

Claims (6)

1. Selective laser melting preparation of Al 2 O 3 -GdAlO 3 -ZrO 2 The method of the ternary eutectic ceramic is characterized by comprising the following specific steps:
step 1, preparing Al of eutectic composition 2 O 3 -Gd 2 O 3 -ZrO 2 Spherical mixed powder material:
step 2, establishing a cylinder model:
establishing the cylinder model through Magics preprocessing software;
the geometric center of the cylinder model is positioned at (125, 2) of a machining platform coordinate system of the PLD laser pulse deposition device;
cutting the cross section of the established cylinder model into slices; the thickness of the slice is 0.02 mm; during slicing, sequentially cutting the slices from bottom to top along the axial direction of the cylinder model by taking the contact end of the cylinder model and the surface of the processing platform of the PLD laser pulse deposition device as a starting point until the end reaches the top end of the cylinder model, and sequentially obtaining a first slice layer, a second slice layer, a third slice layer, … … and an nth slice layer;
step 3, determining the laser scanning path of each slice:
sequentially arranging a laser scanning path on the surfaces of the first sliced layer to the eighth sliced layer; the set laser scanning paths are all in a zigzag shape; the laser scanning paths from the first sliced layer to the eighth sliced layer are the same; the laser scanning path on the rear slice layer rotates clockwise by 45 degrees on the basis of the front slice layer; the laser scanning paths of the eight slice layers form a scanning period of 360 degrees;
step 4, setting scanning parameters:
multilayer scanning is adopted during scanning; the first scanning layer of the scanning is a surface layer, and the rest scanning layers are filling layers; the scanning parameters of the surface layer are different from the scanning parameters of each filling layer;
the scanning parameters comprise laser power and scanning speed;
determining the laser power of the surface layer to be 150-200W and the scanning speed to be 250-350 mm/s; determining the laser power of each filling layer to be 120-145W; the scanning speed is 250-350 mm/s;
and 5, carrying out a selective laser melting test:
carrying out a selective laser melting test by adopting a PLD laser pulse deposition device;
scanning, namely melting and solidifying the powder positioned in the scanning area into a ceramic sample after scanning; the powder outside the scanning area is not scanned and the powder state is kept; the scanning area is the surface range of each sliced sheet layer;
taking the laser scanning path of each sliced layer set in the step 3 as the laser scanning path of each solidified layer in the selective laser melting test; CO in the PLD laser pulse deposition device according to the scanning parameters set in the step 4 2 Carrying out selective laser melting by a laser;
the specific processing process comprises the following steps:
first, Al is added 2 O 3 The ceramic substrate is placed in the center of a processing platform of a horizontally fixed PLD laser pulse deposition device;
second, moving the scraper to the Al 2 O 3 A scraper is arranged above the ceramic substrate and is positioned at the position PThe LD laser pulse deposition device processes between 400 and 500mm of the X axis of the platform coordinate system;
the vertical distance between the surface of the processing platform of the PLD laser pulse deposition device and the lower surface of the scraper is 0.15 mm;
thirdly, putting the mixed powder obtained in the step 1 into a powder feeding platform of a PLD laser pulse deposition device, and scraping the surface layer of the powder by a scraper to finish Al deposition on the surface of the powder 2 O 3 Laying a first layer of powder on the surface of the ceramic substrate; the thickness of the first layer of powder is 0.15 mm;
fourthly, washing gas; closing a door of the PLD laser pulse deposition device, opening a protective gas valve, and starting gas washing; the protective gas is argon, and the pressure is 0.5 Mpa; keeping the gas washing state until the test is finished;
fifthly, carrying out a selective laser melting test; the selective laser melting test is carried out in layers in sequence until the number of solidified layers is the same as that of sliced layers; to obtain Al 2 O 3 -GdAlO 3 -ZrO 2 Ternary eutectic ceramics;
to this end, Al is completed 2 O 3 -GdAlO 3 -ZrO 2 And (3) preparing the ternary eutectic ceramic.
2. The method of claim 1 for preparing Al by selective laser melting 2 O 3 -GdAlO 3 -ZrO 2 The method for preparing ternary eutectic ceramics is characterized in that Al with eutectic components is prepared 2 O 3 -Gd 2 O 3 -ZrO 2 When the spherical mixed powder material is used, Al with the total mass of 400g is weighed 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 Powder; the Al is 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 The proportion of the powder is eutectic molar ratio Al 2 O 3 :Gd 2 O 3 :ZrO 2 58:19: 23; in the weighed Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 Mixing the powder, adding alcohol and polyvinyl alcohol solution, and ball-milling for 2 hours to obtain a mixture; spraying the resulting mixtureGranulating to obtain spherical powder with the particle size distribution of 10-50 microns; and drying the powder material to obtain dry spherical mixed powder with good fluidity.
3. The method of claim 2 for preparing Al by selective laser melting 2 O 3 -GdAlO 3 -ZrO 2 The method of the ternary eutectic ceramics is characterized in that the using amount of the alcohol is the Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 10 wt.% of the total mass of the powder, the polyvinyl alcohol solution being used in an amount of the Al 2 O 3 Powder of Gd 2 O 3 Powder and ZrO 2 5 wt.% of the total mass of the powder.
4. The method of claim 2 for preparing Al by selective laser melting 2 O 3 -GdAlO 3 -ZrO 2 The method for preparing the ternary eutectic ceramic is characterized in that during spray granulation, the air inlet temperature is 250-350 ℃, the air outlet temperature is 100-170 ℃, the rotating frequency of a spray head is 20-25 Hz, and the feeding rotating speed is 5-35 rpm.
5. The method of claim 1 for preparing Al by selective laser melting 2 O 3 -GdAlO 3 -ZrO 2 The method for preparing the ternary eutectic ceramic is characterized in that the specific process for determining the laser scanning path is as follows:
i, setting a laser scanning path of a first slice layer:
taking any surface of the first slice layer as a scanning surface;
setting a plurality of scanning strips on the scanning surface of the first slice layer, wherein the width k of each scanning strip is 10mm, and the interval h between adjacent scanning strips is 0.1 mm; enabling a central line in the width direction of a scanning strip positioned in the middle of the end face of the cylindrical model to pass through the center of the cylindrical model; each scanning strip is parallel to each other; taking the joint of each scanning strip and the outer edge of the end face of the cylinder model at the position as a scanning starting point;
the width of the strip at the outer edge of the end face is adjusted along with the change of the circumference, and the width is 0-10 mm;
II, setting a laser scanning path of the second slice layer:
the laser scanning path of the second cut sheet layer is the same as that of the first cut sheet layer, and the second cut sheet layer is rotated by an angle theta (theta) of 45 degrees in the clockwise direction on the basis of the first cut sheet layer;
III, setting a laser scanning path of a third slice layer:
the laser scanning path of the third sliced layer is the same as that of the first sliced layer, and the third sliced layer is rotated by an angle alpha along the clockwise direction on the basis of the second sliced layer, wherein the angle alpha is 45 degrees;
the process of setting the second slice layer laser scanning path and the third slice layer laser scanning path is repeated in a circulating mode, and the setting from the fourth slice layer laser scanning path to the eighth slice layer laser scanning path is completed;
forming a first scanning period of 360 degrees from the laser scanning path of the first slice layer to the laser scanning path of the eighth slice layer;
and repeating the process of setting the first scanning period to obtain the rest scanning periods in sequence until the laser scanning path setting of all the slice layers is completed.
6. The method of claim 1 for preparing Al by selective laser melting 2 O 3 -GdAlO 3 -ZrO 2 The method for preparing the ternary eutectic ceramic is characterized in that the specific process for carrying out the selective laser melting test comprises the following steps:
i, preparing a first solidified layer;
moving CO 2 The laser is arranged at the starting point of the laser scanning path of the first cut sheet layer; turning on the CO 2 The laser takes the surface range of the first cut sheet layer as a scanning area and carries out laser melting on the first layer of powder according to the set laser scanning path of the first cut sheet layer; obtaining a first solidified layer; the solidified layer is eutectic ceramic;
the first solidified layer is a surface layer; the laser power of the surface layer is 150W, and the scanning speed is 300 mm/s;
II, preparing a second solidified layer;
laying a second layer of the mixed powder on the surface of the first solidified layer; the laying thickness of the mixed powder is 0.02 mm;
moving a scraper to a position where the X axis of the PLD laser pulse deposition device coordinate system is 1mm to scrape the second layer of mixed powder;
moving CO 2 The laser is arranged at the starting point of the laser scanning path of the second slice layer; turning on the CO 2 The laser takes the surface range of the second slice layer as a scanning area and carries out laser melting on the second layer of mixed powder according to the set laser scanning path of the second slice layer; obtaining a second solidified layer; the second solidified layer is a filling layer; the laser power of the filling layer is 130W; the scanning speed is 300 mm/s;
III, preparing other solidified layers;
circularly repeating the preparation process of the second solidified layer, and respectively and sequentially preparing the rest solidified layers until the number of solidified layers is the same as that of the sliced layer; to obtain Al 2 O 3 -GdAlO 3 -ZrO 2 Ternary eutectic ceramics;
to this end, Al is completed 2 O 3 -GdAlO 3 -ZrO 2 And (3) preparing the ternary eutectic ceramic.
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