CN109761587A - It is a kind of to prepare Al2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics - Google Patents
It is a kind of to prepare Al2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics Download PDFInfo
- Publication number
- CN109761587A CN109761587A CN201910170459.9A CN201910170459A CN109761587A CN 109761587 A CN109761587 A CN 109761587A CN 201910170459 A CN201910170459 A CN 201910170459A CN 109761587 A CN109761587 A CN 109761587A
- Authority
- CN
- China
- Prior art keywords
- zro
- gdalo
- laser
- ternary eutectic
- ceramics
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
It is a kind of to prepare Al2O3‑GdAlO3‑ZrO2The method of ternary eutectic ceramics, by successively manufacturing/layer upon layer, can obtain the Al that the prior art is difficult to the different shape prepared and size using laser near-net-shape method2O3‑GdAlO3‑ZrO2Ternary eutectic ceramics.In preparation, the present invention is by gradually reducing the method shuttle-scanning sample upper surface of laser power, to realize Al2O3‑GdAlO3‑ZrO2Temperature-compensating of the ternary eutectic ceramics in temperature-fall period, slows down the cooling rate of sample, and making sample, temperature gradually reduces after forming, to reduce the thermal stress in cooling procedure, inhibits the formation of crackle.Forming speed of the present invention is fast, without using using expensive Mo crucible or Ir crucible, avoids the possible pollution of crucible, the Al for reducing production cost, and obtaining2O3‑GdAlO3‑ZrO2The solidified structure of ternary eutectic ceramics refines 25 times or more than sample tissue obtained by Bridgman method, and gained specimen size is 2-3 times of specimen size obtained by realizing laser suspension zone-melting method, widens the application range of such material.
Description
Technical field
It is specifically a kind of using sharp the present invention relates to the laser gain material manufacturing field of high-performance oxide eutectic ceramic material
Light near-net-shape method prepares Al2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics bar samples.
Background technique
Al2O3-GdAlO3Eutectic ceramic has excellent mechanical behavior under high temperature, thermal structure stability outstanding and natural
Antioxygenic property, it is considered to be it is a kind of be widely applied potentiality aerospace superhigh temperature structural material.Document
“Narihito Nakagawa,Hideki Ohtsubo,Atsuyuki Mitani,Kazutoshi Shimizu,Yoshiharu
Waku.High temperature strength and thermal stability for melt growth
Composite [J] .Journal of the European Ceramic Society, 2005,25:1251-1257. " utilization
Bridgman method has prepared the Al of Φ 53mm2O3-GdAlO3Eutectic ceramic column ingot, and investigated its mechanical behavior under high temperature.It grinds
Study carefully the result shows that: its bending strength can be remained to 1600 DEG C by room temperature；Under 1700 DEG C of atmospheric atmosphere after heat exposure 500h, by force
Degree is held essentially constant, and solidified structure is not obviously roughened, and specimen size, surface roughness and weight do not change substantially.Through
Estimation is expected to improve the thermal efficiency of gas turbine 9% by such oxide eutectic ceramic applications in gas turbine nozzle blade.
However, using as structural material, high intensity is not needed only to have, it is also necessary to which there is high toughness, Al2O3-GdAlO3Eutectic
Ceramics belong to typical fragile material, and low fracture toughness greatlys restrict the application prospect of the material.
Document " L é o Mazerolles, Nicolas Piquet, Marie-France Trichet,Perrière,
Denis Boivin,Michel Parlier.New microstructures in ceramic materials from the
melt for high temperature applications[J].Aerospace Science and Technology,
2008,12:499-505. " prepared using directional freeze method and compare Al2O3-GdAlO3Equal binary eutectics ceramics and addition
ZrO2The mechanical property of ternary eutectic ceramics afterwards, the results showed that, ZrO2Addition can be obviously improved the fracture toughness of sample.So
And the maximum shaping rate of the preparation method is 20mm/h, manufacturing cycle is too long, and need to use expensive Mo crucible or Ir earthenware
Crucible, it is not only possible to ceramic droplet can be polluted, and substantially increase production cost.In addition, gained sample tissue is coarse, Eutectic Layer
Piece spacing > 5 μm cause mechanical property limited.Therefore, there is an urgent need to develop new Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics
Preparation process.
Document " Weidan Ma, Jun Zhang, Haijun Su, Qun Ren, Bin Yao, Lin Liu, Hengzhi
Fu.Microstructure transformation from irregular eutectic to complex regular
eutectic in directionally solidified Al2O3/GdAlO3/ZrO2ceramics by laser
floating zone melting[J].Journal of the European Ceramic Society,2016,36:
1447-1454. " using realizing laser suspension zone melting method it is prepared for rodlike Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics.This method
Without the use of crucible, the possible pollution of crucible is not only avoided, and greatly reduces production cost.In addition, using high
Energy laser beam is as heat source, so that temperature gradient is up to 10 in process4K/cm, so as to be adjusted in wider range
Solidification rate.The preparation method solidification rate most reaches 100 μm/s (6mm/min) fastly, far faster than preparations sides such as Bridgman methods
Method, gained sample tissue size is up to submicron-scale.However, this method needs to use special grinding tool compacting prefabricated first
Body then makes precast body obtain certain processing intensity, precast body is finally prepared eutectic using laser fusing again by sintering
Ceramic sample, preparation process is cumbersome, and specimen size is smaller, and maximum is only Φ 3mm × 40mm.
Document " Haifang Liu, Haijun Su, Zhonglin Shen, Enyuan Wang, Di Zhao, Min Guo,
Jun Zhang,Lin Liu,Hengzhi Fu.Direct formation of Al2O3/GdAlO3/ZrO2ternary
eutectic ceramics by selective laser melting:Microstructure evolutions[J]
.Journal of the European Ceramic Society, 2018,38:5144-5152. " is molten using selective laser
The direct processing ceramic powder of change technology, is prepared for Al under the sweep speed of 6mm/min2O3-GdAlO3-ZrO2Ternary eutectic pottery
Porcelain sample.This method is not required to prepare precast body, enormously simplifies preparation section, however, the technique is also immature at present, can only make
The single track monolayer specimens of standby simple shape out.
Laser near-net-shape technology is a kind of laser gain material manufacturing technology based on synchronous powder feeding system, treats the shape of processed sample
There is no limit using the manufacturing philosophy for increasing dimension, successively manufacture, layer upon layer are until obtain target sample for shape and size.The technology
Using high energy laser beam as heat source, temperature gradient is up to 10 in forming process4Therefore K/cm can be adjusted in a wider scope
Solidification rate is saved, to realize the regulation of solidified structure and obtain the solidified structure of nanoscale.Furthermore, it is possible to according to experiment need
It wants, the ancillary equipments such as addition preheating furnace to reduce the thermal stress in forming, and then inhibit the generation of crackle.Therefore, if can incite somebody to action
Laser near-net-shape technology is applied to Al2O3-GdAlO3-ZrO2In the preparation of ternary eutectic ceramics, it will be expected to break through the prior art
It is difficult to prepare labyrinth Al2O3-GdAlO3-ZrO2The bottleneck problem of ternary eutectic ceramics exemplar, thus, to a certain extent
It discharges the application potential of the material and widens its application range.
A kind of laser powder-feeding method is disclosed in the patent of Publication No. CN102557596A prepares alumina base eutectic pottery
The method of porcelain, this method is using laser surface atmosphere heating furnace auxiliary heating eutectic ceramic, to reduce the heat during area is melted
Stress, and then inhibit the formation of crackle in powder fusion process.But the eutectic ceramic using this method preparation is in irregular shape, at
Shape is second-rate, and shaping rate is lower, only 0.6-6mm/min.
Document " Fangyong Niu, Dongjiang Wu, Guangyi Ma, Jiangtian Wang, Minhai Guo,
Bi Zhang.Nanosized microstructure of Al2O3-ZrO2(Y2O3)eutectics fabricated by
Laser engineered net shaping [J] .Scripta Materialia, 2015,95:39-41. " utilize Laser Near
Net forming technique has prepared the Al of column and arc wall-like with nanoscale solidified structure2O3-ZrO2The examination of binary eutectic ceramics
Sample, it was demonstrated that prepare using laser near-net-shape technology the feasibility of various shapes oxide eutectic ceramics.However, preparing
Al in journey2O3And ZrO2Two kinds of raw materials are respectively delivered in molten bath using more barrels of powder feeders, two kinds in rapid solidification
Constituent element may mix unevenly.In addition, whether this method is suitable for other eutectic systems and more multicomponent such as ternary eutectic system
And it does not know.
Summary of the invention
To overcome current Al2O3-GdAlO3-ZrO2The forming technology process-cycle length of ternary eutectic ceramics, production cost
High, the problems such as process is tedious, Al is prepared the invention proposes a kind of2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics.
Detailed process of the invention is:
Step 1, eutectic composition Al is prepared2O3-Gd2O3-ZrO2Spherical powder particle.
Using centrifugal spray drying method, it will be matched by eutectic and be sufficiently mixed uniform Al2O3-Gd2O3-ZrO2Ceramic powders system
For at spherical powder particle.
The particle diameter distribution of obtained spherical powder particle is 30~100 μm.
Step 2, it charges
Obtained spherical powder particle is fitted into spare in the powder feeding bucket of powder feeder.
Step 3, Al is prepared2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
Using laser near-net-shape method, by the resulting spherical powder particle Melting And Solidification of step 1 and layer upon layer shapes,
Prepare Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics, specific preparation process are as follows:
The first step places heating Al in preheating furnace2O3Substrate.
The Al being placed in preheating furnace2O3Vertical range between upper surface of base plate and laser printhead is 10mm；It should
Al2O3The temperature of substrate heating is 700 DEG C.
Second step sets the technological parameter of scanning.
The technological parameter of the scanning includes laser power, sweep speed, the single pass scan distance of laser printhead, laser spray
The processing number of plies of head single layer hoisting depth and sample；Wherein, the laser power of the laser printhead is 200~400W, scanning speed
Rate is 48~192mm/min, and single pass scan distance is 2~4mm, and laser printhead single layer hoisting depth is 0.1~0.2mm, sample
The number of plies be 300~1000 layers；
Third step prepares Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics.Using laser printhead present position as rise
Point.Open laser and powder feeder.Laser beam exports via laser printhead and is radiated Al2O3Substrate surface, Al2O3Substrate is logical
It crosses and absorbs laser energy and melt and form the movement with laser printhead and the molten bath that extends.Meanwhile spherical powder particle passes through rotation
The sending disk of powder turned is transported to powder feeding mouth by powder feeding bucket, then under the promotion of powder feeding gas, via conveyance conduit finally from laser
The powder channel of spray head is sent out and in the bath that enters below laser printhead and is melted；After laser beam leaves, melt in molten bath
Temperature declines and solidifies to form the Al2O3-GdAlO3-ZrO2First layer Al in ternary eutectic ceramics2O3-GdAlO3-ZrO2Three
First eutectic ceramic.
After laser printhead has moved an one way, that is, complete a sweep length.It is high that laser printhead moves up a promotion
Degree, then move linearly to starting point direction, in obtained first layer Al2O3-GdAlO3-ZrO2Continue on the surface of ternary eutectic ceramics
Scanning.In scanning, the first layer Al2O3-GdAlO3-ZrO2The surface melting of ternary eutectic ceramics forms molten bath and with laser
The movement of spray head and extend.Meanwhile spherical powder particle is admitted in the bath and is melted by laser printhead；Work as laser beam
After leaving, melt temperature declines and solidifies to form second layer Al in molten bath2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
Repetition is described to prepare first layer Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics and second layer Al2O3-GdAlO3-ZrO2
The process of ternary eutectic ceramics, until the preparation number of plies of complete design, obtains Al2O3-GdAlO3-ZrO2The examination of ternary eutectic ceramics
Sample.
Step 4, Al2O3-GdAlO3-ZrO2The compensation of ternary eutectic ceramic sample cools down.
By the gradually cooling of laser printhead, to the Al2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample compensates
Cooling；Specifically:
Obtain Al2O3-GdAlO3-ZrO2After ternary eutectic ceramic sample, powder feeder is closed, laser printhead is with 1000mm/
The speed of min moves up 10mm and keeps the height.The laser printhead is to the Al2O3-GdAlO3-ZrO2The examination of ternary eutectic ceramics
The upper surface of sample is scanned.In scanning, the sweep length of one one way of the every movement of laser printhead, laser power reduces
10W, should be until the laser power of laser printhead be down to 50W.Laser is gradually decreased during the scanning process by the laser printhead
Power, to the Al in cooling2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample carries out temperature-compensating, makes the Al2O3-GdAlO3-
ZrO2The temperature of ternary eutectic ceramic sample gradually reduces, to reduce the thermal stress in cooling procedure, inhibits the formation of crackle.
In the compensation cooling, the laser power of laser printhead is 200~400W, and sweep speed is 48~192mm/min.
After the laser power is down to 50W, laser is closed, closes preheating furnace, the forming exemplar on substrate and substrate
With preheating furnace natural cooling, Al is obtained2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
The present invention can slow down sample by the method shuttle-scanning sample upper surface for gradually reducing laser power
Cooling rate, making sample, temperature gradually reduces after forming, to reduce the thermal stress in cooling procedure, inhibits the shape of crackle
At.
Compared with prior art, the present invention has following outstanding feature:
(1) simple process, forming speed are fast.The present invention is not needed using expensive Mo crucible or Ir crucible, not only
The possible pollution of crucible is avoided, production cost is also reduced.In addition, the present invention does not have to suppress and is sintered precast body, adopt
With the theory of increasing material manufacturing, using the direct processing ceramic powder particle of high energy laser beam, and near-net-shape relative density is 98%
Above Al2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample, simplifies manufacturing procedure.In addition, Al in the present invention2O3-
GdAlO3-ZrO2The forming speed of ternary eutectic ceramics reaches as high as 192mm/min, and other methods is used to prepare Al2O3-
GdAlO3-ZrO2When ternary eutectic ceramics, reported most fast forming speed is 6mm/min, highly shortened manufacturing cycle.
(2) Al that flawless forms and has both large scale, fine tissue can be prepared2O3-GdAlO3-ZrO2Ternary eutectic pottery
Porcelain sample.Present invention combination bottom heating furnace continues pre- hot substrate and is persistently swept by gradually reducing laser power after processing is completed
Gained sample upper surface two ways is retouched, the thermal stress in forming process and cooling procedure is reduced, to effectively inhibit crackle
Formation.The rodlike Al that gained flawless is formed2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample is as shown in Figure 1.The prior art
In, the Al of Bridgman method preparation2O3-GdAlO3-ZrO2Ternary eutectic ceramic structure is coarse, and eutectic lamellar spacing > 5 μm cause
Mechanical property is limited；Realizing laser suspension zone-melting method can prepare the Al with sub-micron tissue2O3-GdAlO3-ZrO2Ternary eutectic pottery
Porcelain, but gained specimen size is smaller, reported full-size are Φ 3mm × 40mm, and can only to prepare shape single for this method
Bar samples, greatly restrict the application range and application prospect of such material.Present invention Al prepared at present2O3-
GdAlO3-ZrO2The solidified structure of ternary eutectic ceramics is tiny, and eutectic lamellar spacing is up to 0.2 μm, as shown in Fig. 2, than cloth Ritchie
Sample tissue obtained by graceful method refines 25 times or more, and gained specimen size is the 2-3 of specimen size obtained by realizing laser suspension zone-melting method
Times, as shown in Figure 1.In addition, laser near-net-shape technology used in the present invention does not have the limitation of shape and size to target sample,
Therefore, constantly optimize technique with subsequent, be expected to prepare the bigger and more complicated shape Al of size2O3-GdAlO3-
ZrO2Ternary eutectic ceramic sample, can widen the application range of such material, and discharge its application potential.
Detailed description of the invention
Fig. 1 is rodlike Al prepared by the present invention2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
Fig. 2 is Al prepared by the present invention2O3-GdAlO3-ZrO2Ternary eutectic ceramic microstructures organization chart.
Fig. 3 is flow chart of the invention.
Specific embodiment
The present invention is a kind of using laser near-net-shape manufacture Al2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics, tool
Body process the following steps are included:
Step 1, eutectic composition Al is prepared2O3-Gd2O3-ZrO2Spherical powder particle.
Using centrifugal spray drying method, it will be matched by eutectic and be sufficiently mixed uniform Al2O3-Gd2O3-ZrO2Ceramic powders system
For at spherical powder particle.
The eutectic proportion are as follows: Al2O3Powder is 58%, Gd2O3Powder is 19%, ZrO2Powder is 23%.
The ratio is molar percentage.
The method for preparing spherical powder particle is disclosed in the innovation and creation application No. is CN201810640599,
Detailed process is:
The first step, acquisition are sufficiently mixed uniform eutectic composition oxide ceramic powder；
The eutectic composition oxide ceramic powder is with Al2O3Powder, Gd2O3Powder and ZrO2Powder is initial feed；
By mole weighing initial feed, after poly-vinyl alcohol solution and dehydrated alcohol is added into the initial feed,
With the revolving speed ball milling 5h of 550r/min, it is sufficiently mixed initial feed uniformly, obtains mixed slurry；
Obtained mixed slurry is put into drying box, dry 2h, obtains eutectic composition oxide ceramic at 100 DEG C
End；
Second step prepares slurry；
Distilled water is added into eutectic composition oxide ceramic powder obtained in the first step, is sufficiently stirred, is mixed
Uniform slurry；
Third step, mist projection granulating；
Using drying machine with centrifugal spray, eutectic composition oxide ceramics spheric granules, specific preparation process are prepared are as follows:
I opens drying machine with centrifugal spray, sets 350 DEG C for inlet air temperature, the lower limit value of leaving air temp is set as 140
℃；Open centrifugal blower；Air heater is opened, the air for entering drying machine with centrifugal spray is heated to the inlet air temperature of setting
350 DEG C and 140 DEG C of leaving air temp；
II opens motor, drives centrifugal atomizing nozzle rotation；Feed pump is opened, by the resulting uniformly mixed slurry of second step
Feed pipe through centrifugal atomizing nozzle is sent into centrifugal atomizing nozzle；The revolving speed of the feed pump is 10~20r/min；In 20~25Hz
Interior adjusting electric machine frequency；
The instillation that slurry in the feeding centrifugal atomizing nozzle passes through the feed liquid distributor uniformly continuous in centrifugal atomizing nozzle
The centrifugal pan of centrifugal atomizing nozzle bottom end, and centrifugal atomizing nozzle rotation when generate centrifugal force under the action of be separated into uniform mist
Change drop；After hot air in the atomized drop and drying machine with centrifugal spray, 95%~98% moisture flash evapn,
And the dry spherical oxide ceramic particle to keep droplet-like in 8~10s；Spherical oxide ceramic particle enters centrifugation spray
In the pollination device of the dry motor spindle of mist；
III after slurry completion of processing, closes centrifugal blower, unloads pollination device, collects spherical oxide ceramic particle；Institute
The partial size for obtaining spherical oxide ceramic particle is 30~100 μm；
4th step, dumping；
The resulting spherical oxide ceramic particle of third step is put into chamber type sintering furnace, keeps the temperature 30min at 500 DEG C,
With the polyvinyl alcohol being discharged in the spherical oxide ceramic particle, the spherical oxide ceramics of pure eutectic composition are obtained
Grain.
The particle diameter distribution of obtained spherical powder particle is 30~100 μm.
Step 2, it charges
The resulting spherical powder particle of step 1 is fitted into spare in the powder feeding bucket of powder feeder.
Step 3, Al is prepared2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
Using laser near-net-shape method, by the resulting spherical powder particle Melting And Solidification of step 1 and layer upon layer shapes,
Prepare Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics, specific preparation process are as follows:
The first step opens well formula preheating furnace, and one piece of 100mm × 100mm × 10mm Al is placed in the preheating furnace2O3
Substrate.By the Al2O3Substrate is heated to 700 DEG C.Laser printhead is moved on into Al2O3Right above substrate, adjust the laser printhead with
Al2O3Vertical range between upper surface of base plate is 10mm.
Second step sets technological parameter.The laser power of laser printhead being set as 200~400W, sweep speed is 48~
192mm/min, single pass scan length are 2~4mm, and laser printhead one way hoisting depth is 0.1~0.2mm, and the processing number of plies is 300
~1000 layers.
The open and close of the control process control laser being made up of CNC control routine, laser printhead movement rail
Technological parameter in mark and process.
Third step prepares Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics.Using laser printhead present position as rise
Point.Open laser and powder feeder.Laser beam exports via laser printhead and is radiated Al2O3Substrate surface, Al2O3Substrate is logical
It crosses and absorbs laser energy and melt and form the movement with laser printhead and the molten bath that extends.Meanwhile spherical powder particle passes through rotation
The sending disk of powder turned is transported to powder feeding mouth by powder feeding bucket, then under the promotion of powder feeding gas, via conveyance conduit finally from laser
The powder channel of spray head is sent out and in the bath that enters below laser printhead and is melted；After laser beam leaves, melt in molten bath
Temperature declines and solidifies to form the Al2O3-GdAlO3-ZrO2First layer Al in ternary eutectic ceramics2O3-GdAlO3-ZrO2Three
First eutectic ceramic.
After laser printhead has moved an one way, that is, complete a sweep length.It is high that laser printhead moves up a promotion
Degree, then move linearly to starting point direction, in obtained first layer Al2O3-GdAlO3-ZrO2Continue on the surface of ternary eutectic ceramics
Scanning.In scanning, the first layer Al2O3-GdAlO3-ZrO2The surface melting of ternary eutectic ceramics forms molten bath and with laser
The movement of spray head and extend.Meanwhile spherical powder particle is admitted in the bath and is melted by laser printhead；Work as laser beam
After leaving, melt temperature declines and solidifies to form second layer Al in molten bath2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
Repetition is described to prepare first layer Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics and second layer Al2O3-GdAlO3-ZrO2
The process of ternary eutectic ceramics, until the preparation number of plies of complete design, obtains Al2O3-GdAlO3-ZrO2The examination of ternary eutectic ceramics
Sample.
The laser and powder feeder is all made of the prior art.
Step 4, Al2O3-GdAlO3-ZrO2The compensation of ternary eutectic ceramic sample cools down.
By the gradually cooling of laser printhead, to the Al2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample compensates
Cooling, specifically:
Obtain Al2O3-GdAlO3-ZrO2After ternary eutectic ceramic sample, powder feeder is closed, laser printhead is with 1000mm/
The speed of min moves up 10mm and keeps the height.The laser printhead is along the obtained Al2O3-GdAlO3-ZrO2Ternary eutectic
Straight reciprocating motion is done in the upper surface of ceramic sample, to the Al2O3-GdAlO3-ZrO2The upper surface of ternary eutectic ceramic sample into
Row scanning.In scanning, the sweep length of one one way of the every movement of laser printhead, laser power reduces 10W, should be until swashing
The laser power of light spray head is down to 50W.Laser power is gradually decreased during the scanning process by the laser printhead, in cooling
Al2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample carries out temperature-compensating, makes the Al2O3-GdAlO3-ZrO2Ternary eutectic pottery
The temperature of porcelain sample gradually reduces, to reduce the thermal stress in cooling procedure, inhibits the formation of crackle.
In the compensation temperature-fall period, the laser power of laser printhead is 200~400W, and sweep speed is 48~192mm/
min。
After the laser power is down to 50W, laser is closed, closes preheating furnace, the forming exemplar on substrate and substrate
With preheating furnace natural cooling, Al is obtained2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
Its detailed process is described in detail by six embodiments in the present invention, and the implementation process of each embodiment is identical, difference
It is in the technological parameter of each embodiment.
Table 1: the technological parameter of each embodiment
| Embodiment | Laser power | Sweep speed | Powder feeding disk rotating speed | Single Slice Mode length | Single layer hoisting depth | Process the number of plies |
| 1 | 400W | 192mm/min | 20rpm | 4mm | 0.1mm | 1000 |
| 2 | 350W | 168mm/min | 18rpm | 3mm | 0.15mm | 800 |
| 3 | 300W | 144mm/min | 16rpm | 2mm | 0.1mm | 600 |
| 4 | 250W | 96mm/min | 14rpm | 3mm | 0.2mm | 500 |
| 5 | 200W | 96mm/min | 12rpm | 4mm | 0.15mm | 400 |
| 6 | 300W | 48mm/min | 10rpm | 2mm | 0.2mm | 300 |
Note: the combination by regulating and controlling each technological parameter, it is ensured that the ceramic powders in feeding molten bath are completely melt in forming process,
And guarantee that laser printhead remains at 10mm away from the distance of machined surface, to obtain forming quality good and flawless and stomata shape
At sample.
Claims (4)
1. a kind of prepare Al2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics, which is characterized in that detailed process is:
Step 1, eutectic composition Al is prepared2O3-Gd2O3-ZrO2Spherical powder particle:
It will be matched by eutectic and be sufficiently mixed uniform Al2O3-Gd2O3-ZrO2Ceramic powders are prepared into spherical powder particle；
The particle diameter distribution of obtained spherical powder particle is 30~100 μm；
Step 2, it charges:
Obtained spherical powder particle is fitted into spare in the powder feeding bucket of powder feeder；
Step 3, Al is prepared2O3-GdAlO3-ZrO2Ternary eutectic ceramics:
Using laser near-net-shape method, by the resulting spherical powder particle Melting And Solidification of step 1 and layer upon layer shapes, preparation
Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics, specific preparation process are as follows:
The first step places heating Al in preheating furnace2O3Substrate；
Second step sets the technological parameter of scanning；
Third step prepares Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics；Using laser printhead present position as starting point；It opens
Open laser and powder feeder；Laser beam exports via laser printhead and is radiated Al2O3Substrate surface, Al2O3Substrate passes through absorption
Laser energy melts and forms the movement with laser printhead and the molten bath that extends；Meanwhile spherical powder particle is sent by what is rotated
Powder disk is transported to powder feeding mouth by powder feeding bucket, then under the promotion of powder feeding gas, via conveyance conduit finally from laser printhead
Powder channel is sent out and in the bath that enters below laser printhead and is melted；After laser beam leaves, in molten bath under melt temperature
It drops and solidifies to form the Al2O3-GdAlO3-ZrO2First layer Al in ternary eutectic ceramics2O3-GdAlO3-ZrO2Ternary eutectic
Ceramics；
After laser printhead has moved an one way, that is, complete a sweep length；Laser printhead moves up a hoisting depth, then
It moves linearly to starting point direction, in obtained first layer Al2O3-GdAlO3-ZrO2The surface of ternary eutectic ceramics continues to scan on；
In scanning, the first layer Al2O3-GdAlO3-ZrO2The surface melting of ternary eutectic ceramics forms molten bath and with laser printhead
It moves and extends；Meanwhile spherical powder particle is admitted in the bath and is melted by laser printhead；When laser beam leaves
Afterwards, melt temperature declines and solidifies to form second layer Al in molten bath2O3-GdAlO3-ZrO2Ternary eutectic ceramics；
Repetition is described to prepare first layer Al2O3-GdAlO3-ZrO2Ternary eutectic ceramics and second layer Al2O3-GdAlO3-ZrO2Ternary
The process of eutectic ceramic, until the preparation number of plies of complete design, obtains Al2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample；
Step 4, Al2O3-GdAlO3-ZrO2The compensation of ternary eutectic ceramic sample cools down:
By the gradually cooling of laser printhead, to the Al2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample compensates cooling；
Specifically:
Obtain Al2O3-GdAlO3-ZrO2After ternary eutectic ceramic sample, powder feeder is closed, laser printhead is with the speed of 1000mm/min
Degree moves up 10mm and keeps the height；The laser printhead is to the Al2O3-GdAlO3-ZrO2The upper table of ternary eutectic ceramic sample
Face is scanned；In scanning, the sweep length of one one way of the every movement of laser printhead, laser power reduces 10W, this is straight
Laser power to laser printhead is down to 50W；Laser power is gradually decreased during the scanning process by the laser printhead, to drop
The Al of middle benefit gas2O3-GdAlO3-ZrO2Ternary eutectic ceramic sample carries out temperature-compensating, makes the Al2O3-GdAlO3-ZrO2Ternary is total
The temperature of brilliant ceramic sample gradually reduces, to reduce the thermal stress in cooling procedure, inhibits the formation of crackle；When the laser
After power is down to 50W, laser is closed, closes preheating furnace, the forming exemplar on substrate and substrate is naturally cold with preheating furnace
But, Al is obtained2O3-GdAlO3-ZrO2Ternary eutectic ceramics.
2. preparing Al as claim is a kind of2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics, which is characterized in that the placement
Al in preheating furnace2O3Vertical range between upper surface of base plate and laser printhead is 10mm；By the Al2O3Substrate is heated to
700℃。
3. preparing Al as claim is a kind of2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics, which is characterized in that the scanning
Technological parameter include laser printhead laser power, sweep speed, single pass scan distance, laser printhead single layer hoisting depth and
The processing number of plies of sample；Wherein, the laser power of the laser printhead is 200~400W, and sweep speed is 48~192mm/
Min, single pass scan distance are 2~4mm, and laser printhead single layer hoisting depth is 0.1~0.2mm, the number of plies of sample is 300~
1000 layers.
4. preparing Al as claim is a kind of2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics, which is characterized in that the compensation
In cooling, the laser power of laser printhead is 200~400W, and sweep speed is 48~192mm/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910170459.9A CN109761587B (en) | 2019-03-07 | 2019-03-07 | Preparation of Al2O3-GdAlO3-ZrO2Method for preparing ternary eutectic ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910170459.9A CN109761587B (en) | 2019-03-07 | 2019-03-07 | Preparation of Al2O3-GdAlO3-ZrO2Method for preparing ternary eutectic ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109761587A true CN109761587A (en) | 2019-05-17 |
| CN109761587B CN109761587B (en) | 2021-05-07 |
Family
ID=66457955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910170459.9A Active CN109761587B (en) | 2019-03-07 | 2019-03-07 | Preparation of Al2O3-GdAlO3-ZrO2Method for preparing ternary eutectic ceramics |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109761587B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112441834A (en) * | 2020-11-22 | 2021-03-05 | 西北工业大学 | Selective laser melting for preparing Al2O3-GdAlO3-ZrO2Method for preparing ternary eutectic ceramics |
| CN112895061A (en) * | 2020-11-22 | 2021-06-04 | 西北工业大学 | Selective laser melting preparation of cylindrical Al2O3-GdAlO3Method for binary eutectic ceramics |
| CN113248234A (en) * | 2020-03-09 | 2021-08-13 | 西北工业大学 | Eutectic ceramic coating and preparation method thereof |
| 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 |
| CN115124328A (en) * | 2022-07-05 | 2022-09-30 | 西北工业大学 | Selective laser melting preparation method of high-density blocky eutectic composite ceramic |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531553A (en) * | 2012-01-05 | 2012-07-04 | 西北工业大学 | Method for preparing alumina-based eutectic ceramic |
| CN102557596A (en) * | 2012-01-05 | 2012-07-11 | 西北工业大学 | Method for preparing aluminum oxide-based eutectic ceramic through laser powder feeding method |
| CN102701734A (en) * | 2012-06-02 | 2012-10-03 | 大连理工大学 | Preparation method of self-preheating laser engineered net shaped ZrO2-Al2O3 composite ceramic thin-walled part |
| CN103771837A (en) * | 2013-12-31 | 2014-05-07 | 中国人民解放军第四军医大学 | Aluminum oxide/zirconium oxide SLM (selective laser melting) ceramic powder material and preparation method thereof |
| JP2017071532A (en) * | 2015-10-08 | 2017-04-13 | 日本電気硝子株式会社 | Glass powder for three-dimensional molding |
-
2019
- 2019-03-07 CN CN201910170459.9A patent/CN109761587B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102531553A (en) * | 2012-01-05 | 2012-07-04 | 西北工业大学 | Method for preparing alumina-based eutectic ceramic |
| CN102557596A (en) * | 2012-01-05 | 2012-07-11 | 西北工业大学 | Method for preparing aluminum oxide-based eutectic ceramic through laser powder feeding method |
| CN102701734A (en) * | 2012-06-02 | 2012-10-03 | 大连理工大学 | Preparation method of self-preheating laser engineered net shaped ZrO2-Al2O3 composite ceramic thin-walled part |
| CN103771837A (en) * | 2013-12-31 | 2014-05-07 | 中国人民解放军第四军医大学 | Aluminum oxide/zirconium oxide SLM (selective laser melting) ceramic powder material and preparation method thereof |
| JP2017071532A (en) * | 2015-10-08 | 2017-04-13 | 日本電気硝子株式会社 | Glass powder for three-dimensional molding |
Non-Patent Citations (1)
| Title |
|---|
| HAIFANG LIU: "Direct formation of Al2O3/GdAlO3/ZrO2ternary eutectic ceramics by selective laser melting:Microstructure evolutions", 《JOURNAL OF THE EUROPEAN CERAMIC SOCIETY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248234A (en) * | 2020-03-09 | 2021-08-13 | 西北工业大学 | Eutectic ceramic coating and preparation method thereof |
| 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 |
| CN113248234B (en) * | 2020-03-09 | 2022-05-13 | 西北工业大学 | Eutectic ceramic coating and preparation method thereof |
| CN112441834A (en) * | 2020-11-22 | 2021-03-05 | 西北工业大学 | Selective laser melting for preparing Al2O3-GdAlO3-ZrO2Method for preparing ternary eutectic ceramics |
| CN112895061A (en) * | 2020-11-22 | 2021-06-04 | 西北工业大学 | Selective laser melting preparation of cylindrical Al2O3-GdAlO3Method for binary eutectic ceramics |
| CN115124328A (en) * | 2022-07-05 | 2022-09-30 | 西北工业大学 | Selective laser melting preparation method of high-density blocky eutectic composite ceramic |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109761587B (en) | 2021-05-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109761587A (en) | It is a kind of to prepare Al2O3-GdAlO3-ZrO2The method of ternary eutectic ceramics | |
| CN109760173B (en) | Wall-like Al2O3-GdAlO3-ZrO2Laser melting forming method of ternary eutectic ceramics | |
| US5858037A (en) | Process for the preparation of alumina abrasives | |
| EP0949982B1 (en) | An improved process and apparatus for the preparation of particulate parts | |
| CN107140960B (en) | Method for sintering alumina-based eutectic ceramic composite material by discharge plasma | |
| US11883978B2 (en) | In situ synthesis, densification and shaping of non-oxide ceramics by vacuum additive manufacturing technologies | |
| CN107663081B (en) | Solidification preparation method of aluminum oxide-based ternary nano eutectic/amorphous ceramic | |
| CN108516805A (en) | The preparation method of eutectic composition oxide ceramics spheric granules | |
| JP2004100045A (en) | METHOD FOR PRODUCING Al-SiC COMPOSITE MATERIAL | |
| Zhang et al. | Processing parameters for selective laser sintering or melting of oxide ceramics | |
| CN107140959A (en) | A kind of preparation method of oxide eutectic structural ceramics powder | |
| CN104744051B (en) | A kind of manufacture method of silicon nitride crucible | |
| CN105948722A (en) | Method for assisting in laser engineered net shaping of Al2O3-based eutectic ceramic cutter through ultrasound | |
| Wang et al. | Processing and characterization of laser-sintered Al 2 O 3/ZrO 2/SiO 2 | |
| CN112441834B (en) | Selective laser melting for preparing Al 2 O 3 -GdAlO 3 -ZrO 2 Method for preparing ternary eutectic ceramics | |
| CN112142467A (en) | Al (aluminum)2O3EAG eutectic ceramic and preparation method thereof | |
| CN105755540B (en) | One kind prepares LaB using optics zone-melting technique6-VB2The method of eutectic composites | |
| EP1209137B1 (en) | Method for preparing eutectic ceramics | |
| CN108178632B (en) | ZrB with oriented lamellar microstructure2Preparation method of-SiC eutectic ceramic | |
| CN107032795B (en) | ZrB2Solidification preparation method of-SiC eutectic composite ceramic | |
| CN113264767A (en) | alumina/GAP eutectic ceramic and preparation method thereof | |
| Thakur et al. | Fabrication and characterization of high-purity alumina ceramics doped with zirconia via laser direct deposition | |
| CN111662085B (en) | Preparation method of tungsten carbide ceramic containing diamond based on non-contact flash firing technology | |
| CN102531553B (en) | Method for preparing alumina-based eutectic ceramic | |
| RU2199616C2 (en) | Polycrystalline material, method and device for production of such material and article made from such material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |