CN103204683B - Laser near-net forming method for Al2O3 ceramic parts different in colors - Google Patents

Laser near-net forming method for Al2O3 ceramic parts different in colors Download PDF

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CN103204683B
CN103204683B CN201310086487.5A CN201310086487A CN103204683B CN 103204683 B CN103204683 B CN 103204683B CN 201310086487 A CN201310086487 A CN 201310086487A CN 103204683 B CN103204683 B CN 103204683B
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laser
powder
sweep velocity
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lifting capacity
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CN103204683A (en
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吴东江
孙贝
张垚磊
牛方勇
马广义
郭东明
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Dalian University of Technology
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Abstract

The invention discloses a technical method for laser near-net forming method for Al2O3 ceramic parts different in colors. By adopting a laser stereoscopic forming system and the coaxial powder feeding method, sample parts are accumulated on a substrate layer by layer, forming scanning tracks are changed by adjusting defocusing, composite ceramic matrixes are optionally formed, and Al2O3 ceramic parts different in colors are formed by optimizing technical parameters. With no adding of colored elements or compounds, black, gray and white Al2O3 ceramic parts compact in structure and uniform in formation can be directly formed by changing the technique method.

Description

Different colours Al 2o 3the Laser Near net-shape method of ceramic member
Technical field
The present invention relates to a kind of different colours Al 2o 3the near-net-shape method of ceramic member, particularly high-purity Al 2o 3the Laser Near net-shape method of ceramic member.
Background technology
Along with the development of the top science technology such as the energy, aerospace, electronics, military project, part bears strong friction abrasive action conventionally under the mal-condition such as high temperature oxidation, thermal etching, and service condition is very severe, and material property is had to very high requirement, therefore high strength, high rigidity, high temperature resistant, wear-resistant, anticorrosive, the advanced ceramics material that heat insulating ability is good arises at the historic moment, and plays an important role in these technological revolutions, has greatly promoted development and the application of ceramic science.It is high that alumina-ceramic has physical strength, insulation resistance is large, hardness is high, a series of premium propertiess such as wear-resisting, corrosion-resistant and high temperature resistant, and there is good optical and ionic conductivity under certain condition, be widely used in the high-technology fields such as the traditional industries such as pottery, weaving, oil, chemical industry, building and electronics and aerospace, national defence.Existing ceramic structure, mainly by thermal sintering, utilizes high-temperature and high-pressure conditions to make ceramic powder press forming, but the method exists sintering structure tissue looseness, loaded down with trivial details with defect, aftertreatment technology, the shortcomings such as the complicated ceramic structure difficulty of sintering.
Laser near-net-shape (Laser Engineered Net Shaping, LENS) is a kind of advanced manufacturing methods that utilizes high energy beam direct forming object construction, can realize high-performance complex structural member without mould, quick, complete fine and close near-net-shape.SNL company of the U.S., Los Alamos National Laboratory, the Huang Weidong of NORTHWEST CHINA polytechnical university all uses the method to obtain dense internal organization, good, the flawless hardware of surface quality.
At present, the V.K.Balla group of the document Zhong Jin U.S. of open report adopts the LENS method compact structure that is shaped, the ceramic member of homogeneous microstructure.Wherein use white high-purity Al 2o 3the structural part that powder obtains is but rendered as grey black, in document, this phenomenon is not analyzed.Conventionally the acquisition of different colours pottery is to add some coloring compounds or introduce some coloring ions in the powder stage material microstructure is changed, and the method needs strict powder chemistry proportioning components and the generation temperature controlled, and causes to produce to take time and effort.Shaping and ceramic color change about ceramic member all have report with Publication about Document:
V.K.Balla, S.Bose, A.Bandvopadhvav: " block aluminum oxide laser near-net-shape (Processing of Bulk Alumina Ceramics Using Laser Engineered Net Shaping) ", " application ceramic technology international magazine (International Journal of Applied Ceramic Technology) ", 5 volumes in 2008.
Sheldon A.Bernard, V.K.Balla, S.Bose, A.Bandvopadhvav: " Laser Direct Deposition lead zirconate-titanate ceramic (Direct laser processing of bulk lead zirconate titanate ceramics) ", " Materials Science and Engineering (Materials Science and Engineering B) ", 172 volumes in 2010.
Z.H.Liu, J.J.Nolte, J.I.Packard, G.Hilmas, F.Dogan, M.C.Leu: " selective sintering high density aluminum oxide ceramic member (Selective Laser Sintering of High-density Alumina Ceramics Parts) ", " the 35th MATADOR international conference minutes (Proceedings of the 35th international MATADOR conference) ", 2007 351st~354 pages.
Tang Yaxin, Deng Qilin, Zhang Hong: " research of laser sintered ceramics forming technology ", " electromachining ", the 1st phase in 1997.
Zhang little Feng, Liu Weiliang, Jiang Linwen: " researchs of alumina ceramic of black color preparation and dielectric properties ", " Chinese pottery industry ", 17 volumes in 2010.
Chinese scholar Li Yuan is strong, Xu Jie: " research of painted Y-TZP pottery ", " sparking plug and special cermacis ", 4 phases in 1993.
Adopt LENS technology shaping different colours Al 2o 3ceramic member not only can avoid the intrinsic defect of sintering method to obtain the structural part of dense structure, uniform ingredients, and do not need to adjust powder chemistry proportioning and can directly obtain the different ceramic member of different colours performance, colour-change reason that more can the clean drip molding of comparative analysis Laser Near, and then determine more rational process program, improve drip molding performance, improve drip molding quality.
Summary of the invention
For the high-purity Al of shaping different colours 2o 3ceramic member the defect of avoiding existing method to exist, the invention provides a kind of different colours Al 2o 3the Laser Near net-shape method of ceramic member is adjusted direct forming black, grey and white Al 2o 3ceramic member.
The technical solution adopted for the present invention to solve the technical problems is:
1, matrix is Ti-6Al-4V or pure Ti, and selection diameter is the spherical ceramic powder of 20~100 μ m and is dried, adjusts laser beam spot identical with the diameter of flow of powder focal position overlapping position.
2, selected parameter Z axle pulling speed is 1000~1200mm/min;
3,, for distinct colors, adjusting process parameter is shaped ceramic part on matrix:
A. black Al is shaped 2o 3when exemplar, defocusing amount is 0mm, and laser power is between 170~298W, and sweep velocity is 300~500mm/min, and it is 2.0~3.2g/min that powder sending quantity is selected interval, and Z axis lifting capacity is 0.15~0.2mm.
B. the grey that is shaped Al 2o 3when exemplar, defocusing amount is 8~9mm, it is 1.2~1.61g/min that powder sending quantity is selected interval, 1st~6 layers of laser power are selected between 520~566W, sweep velocity is 800~1000mm/min, and Z axis lifting capacity is 0mm, and the 7th layer is finished to being shaped, laser power is selected between 250~454W, and sweep velocity is 200~500mm/min.
C. white Al is shaped 2o 3when exemplar, defocusing amount is 8~9mm; Shaping whiteware part needs preshaped ZrO 2and Al 2o 3composite ceramics, its processing parameter is: laser power is between 318~466W, and sweep velocity is 400~500mm/min, powder sending quantity Q zrO2and Q al2O3selection interval be respectively 1.85~2.1g/min and 0.6~0.62g/min, Z axis lifting capacity is 0.15~0.3mm; White Al 2o 3exemplar forming parameters is: laser power between 398~520W, powder sending quantity Q al2O3zone of reasonableness is 1.0~1.6g/min, and Z axis lifting capacity is 0.05~0.15mm, and the 1st layer of sweep velocity is 400~520mm/min, and the 2nd, 3 layers of sweep velocity are 1100~1300mm/min, and every three layers is a loop cycle.
D. open rare gas element, adjusting powder feeding air pressure is 0.15~0.25MPa, and flow is 4~7L/min; protection air pressure is selected 0.08~0.15MPa; flow is 12~20L/min, starts powder feeder and laser apparatus, and laser head completes shaping according to the path movement of programming in advance.
Analyze laser fast forming Al in the present invention 2o 3ceramic member presents the reason of different colours, detects starting powder, black exemplar and white exemplar composition phase.Wherein, white exemplar is identical with starting powder phase composite and black exemplar has more CaAl compared with the two 2si 2o 8, CaAl 12o 19, NaAl 9o 14three-phase.In forming process, the oxide impurity (Na that starting powder contains in the time that rate of cooling is too fast 2o, CaO, Fe 2o 3, SiO 2) can not volatilize completely, with Al 2o 3reaction forms cenotype.CaAl 12o 19belong to β-Al 2o 3, its structure is by basic metal or alkaline-earth metal ions layer and [ Al 11o 12? +the overlapping accumulation in type spinel unit forms, O 2+be arranged in cubic close packing, Ca +be completely contained in the loose depos-its plane perpendicular to C axle, metal ion can rapid diffusion in this plane.Ca element can be at β-Al in diffusion process 2o 3deposition and then cause stupalith blackening in the lattice of pottery or in the crystal boundary of polycrystalline material.In the present invention, processing parameter, shaping track while scan and preshaped composite ceramics matrix three aspects: all affect in various degree rate of cooling and then affect oxide impurity volatilization, and then affect drip molding composition phase composition, and different colours Al is finally shaped 2o 3ceramic member.
The present invention does not need to add element or compound only just can be realized Al of the same race by processing method 2o 3the shaping of ceramic powder different colours exemplar; Drip molding compact structure, mechanical property, mechanical property are high compared with sintering process shaped ceramic part; Can comparative analysis drip molding colour-change reason, improve technique and improve drip molding quality.
Accompanying drawing explanation
Fig. 1 is Al 2o 3the clean building mortion schematic diagram of Laser Near of ceramic structures.
Fig. 2 (a) is composite ceramics matrix front view.
Fig. 2 (b) is composite ceramics matrix left view.
Fig. 2 (c) is composite ceramics matrix vertical view.
In figure: 1 solid continuous wave laser; 2 Transmission Fibers; 3 laser Machining heads; 4 laser focusing bundles; 5 drip moldings; 6 substrates; 7 powder feeders; 8 rare gas elementes; 9 machine operation panels; 10 computers.
Embodiment
In conjunction with the accompanying drawings and embodiments the present invention is further described.
Embodiment 1
As shown in Figure 1, high-purity Al 2o 3the clean building mortion schematic diagram of Laser Near of pottery (massfraction is 99.73%) structural part, embodiments of the invention require: black Al 2o 3thin-wall part (long 15mm, wide 1.5mm, high 8mm), concrete forming step is as follows:
(1) selecting as requested diameter is the subsphaeroidal Al of 20~110 μ m 2o 3ceramic powder, dry 4h at 100 ℃ in electrothermic type air dry oven;
(2) before processing by forming board 6(Ti-6Al-4V or pure Ti) with sand papering, and clean with alcohol;
(3) dried powder is put into powder feeder 7, the operating distance of adjusting the laser Machining head relative substrate of 3 lowermost end 6 surfaces is 9mm, makes powder stream focus in finished surface;
(4) adjust black Al 2o 3thin-wall part forming parameter: defocusing amount is 0mm, and laser power is 298W, and powder sending quantity is adjusted to 2.0g/min, Z axis lifting capacity is selected 0.15mm, and Z axis pulling speed is 1000mm/min, sweep velocity (V two ends=350mm/min, V in=300mm/min).
(5) open rare gas element 8, adjusting powder feeding air pressure is 0.2MPa, and flow is 5L/min, and protection air pressure is selected 0.1MPa, and flow is 15L/min.Start powder feeder 7 and laser apparatus 1 and carry Al 2o 3ceramic powder is shaped, and the path movement that laser Machining head 3 is programmed in advance according to machine operation panel 9 completes shaping.
Embodiment 2
As shown in Figure 1, high-purity Al 2o 3the clean building mortion schematic diagram of Laser Near of pottery (massfraction is 99.73%) structural part, embodiments of the invention require: shaping grey Al 2o 3thin-wall part (long 15mm, wide 2mm, high 15mm), concrete forming step is as follows:
(1) selecting as requested diameter is the subsphaeroidal Al of 20~110 μ m 2o 3ceramic powder, dry 4h at 100 ℃ in electrothermic type air dry oven;
(2) before processing by forming board 6(Ti-6Al-4V or pure Ti) with sand papering, and clean with alcohol;
(3) dried powder is put into powder feeder 7, the operating distance of adjusting the laser Machining head relative substrate of 3 lowermost end 6 surfaces is 9mm, makes powder stream focus in finished surface;
(4) adjust grey Al 2o 3thin-wall part forming parameter: defocusing amount is 9mm, and powder sending quantity is adjusted into 1.2g/min, Z axis pulling speed is 1000mm/min; 1st~6 layers of laser power are 566W, and sweep velocity is 1000mm/min, and Z axis lifting capacity is 0mm, and the 7th layer is finished to being shaped, and laser power is 454W, and sweep velocity is 500mm/min, and Z axis lifting capacity is 0.2mm;
(5) open rare gas element 8, adjusting powder feeding air pressure is 0.2MPa, and flow is 5L/min, and protection air pressure is selected 0.1MPa, and flow is 15L/min.Start powder feeder 7 and laser apparatus 1 and carry Al 2o 3ceramic powder is shaped, and the path movement that laser Machining head 3 is programmed in advance according to machine operation panel 9 completes shaping.
Embodiment 3
As shown in Figure 1, high-purity Al 2o 3the clean building mortion schematic diagram of Laser Near of pottery (massfraction is 99.73%) structural part, embodiments of the invention require: white Al is shaped 2o 3thin-wall part (long 15mm, wide 2mm, high 16mm), concrete forming step is as follows:
(1) selecting as requested diameter is the subsphaeroidal Al of 20~110 μ m 2o 3and ZrO 2ceramic powder, dry 4h at 100 ℃ in electrothermic type air dry oven;
(2) before processing by forming board 6(Ti-6Al-4V or pure Ti) with sand papering, and clean with alcohol;
(3) dried powder is put into powder feeder 7, the operating distance of adjusting the laser Machining head relative substrate of 3 lowermost end 6 surfaces is 9mm, makes powder stream focus in finished surface;
(4) the 1st layer of adjusting process parameter shaped ceramic matrix: defocusing amount is 9mm, and laser power is 566W, powder sending quantity Q zrO2and Q al2O3be adjusted into respectively 1.85g/min and 0.62g/min, sweep velocity is 500 mm/min;
(5) open rare gas element 8, adjusting powder feeding air pressure is 0.2MPa, and flow is 5L/min, and protection air pressure is selected 0.1MPa, and flow is 15L/min.Start powder feeder 7 and carry Al 2o 3and ZrO 2ceramic powder is shaped, and starts laser apparatus 1, and laser Machining head 3 is according to the path automated movement of programming in advance, and (long 22mm, wide 12mm, high 0.5mm) cladding layer is shaped on substrate 6;
(6) close laser apparatus, powder feeder and rare gas element;
(7) the 2nd to 6 layers of adjusting process parameter shaping bases: defocusing amount is 9mm, and laser power is 318W, powder sending quantity Q zrO2and Q al2O3be adjusted into respectively 1.85g/min and 0.62g/min, sweep velocity is 500mm/min, and Z axis lifting capacity is set to 0.3mm, and Z axis pulling speed is 1200mm/min;
(8) open rare gas element 8, adjusting powder feeding air pressure is 0.2MPa, and flow is 5L/min, and protection air pressure is selected 0.1MPa, and flow is 15L/min.Start powder feeder 7 and carry Al 2o 3and ZrO 2ceramic powder is shaped, and starts laser apparatus 1, the path automated movement that laser Machining head 3 is programmed in advance according to machine operation panel 9, shaped ceramic matrix (as Fig. 2) on substrate 6;
(9) close laser apparatus, powder feeder and rare gas element;
(10) adjust white Al 2o 3thin-wall part forming parameter: defocusing amount is 9mm, laser power is 454W, powder sending quantity Q al2O3be adjusted into 1.2g/min, Z axis pulling speed is 1200mm/min; The 1st layer of sweep velocity is 500mm/min, and Z axis lifting capacity is set to 0.15mm, and the 2nd, 3 layers of sweep velocity are 1200mm/min, and Z axis lifting capacity is set to 0.05mm;
(11) open rare gas element 8, adjusting powder feeding air pressure is 0.2MPa, and flow is 5L/min, and protection air pressure is selected 0.1MPa, and flow is 15L/min.Start powder feeder 7 and carry Al 2o 3and ZrO 2ceramic powder is shaped, and starts laser apparatus 1, the path that laser Machining head 3 is programmed in advance according to machine operation panel 9 thin-wall part that is shaped on composite ceramics matrix.

Claims (2)

1. a different colours Al 2o 3the Laser Near net-shape method of ceramic member, is characterized in that the method comprises following step:
A. selecting diameter is spherical high-purity Al of 20~100 μ m 2o 3and ZrO 2powder, carries out drying treatment; Adjust laser beam spot identical with the diameter of flow of powder focal position overlapping position; Described high-purity Al 2o 3massfraction is 99.73%;
B. selected parameter Z axle pulling speed is 1000~1200mm/min;
C. for distinct colors, adjusting process parameter is shaped ceramic part on matrix:
Black Al 2o 3exemplar: defocusing amount is 0mm, laser power is between 170~298W, and sweep velocity is 300~500mm/min, and it is 2.0~3.2g/min that powder sending quantity is selected interval, and Z axis lifting capacity is 0.15~0.2mm;
Grey Al 2o 3exemplar: defocusing amount is 8~9mm, it is 1.2~1.61g/min that powder sending quantity is selected interval, 1st~6 layers of laser power are between 520~566W, sweep velocity is 800~1000mm/min, Z axis lifting capacity is 0mm, and the 7th layer is finished to being shaped, and laser power is between 250~454W, sweep velocity is 200~500mm/min, and Z axis lifting capacity is 0.15~0.2mm;
White Al 2o 3exemplar: defocusing amount is 8~9mm, the white exemplar that is shaped needs preshaped ZrO 2and Al 2o 3composite ceramics matrix, its forming parameters is: laser power is between 318~466W, and sweep velocity is 400~500mm/min, powder sending quantity Q zrO2and Q al2O3selecting interval is respectively 1.85~2.1g/min and 0.6~0.62g/min, and Z axis lifting capacity is 0.15~0.3mm; White Al 2o 3exemplar forming parameters: laser power between 398~520W, powder sending quantity Q al2O3zone of reasonableness be 1.0~1.6g/min, Z axis lifting capacity is 0.05~0.15mm, the 1st layer of sweep velocity is 400~520mm/min, the 2nd, 3 layers of sweep velocity are 1100~1300mm/min, every three layers is a loop cycle;
D. adjusting powder feeding air pressure is 0.15~0.25MPa, and flow is 4~7L/min, and protection air pressure is 0.08~0.15MPa, and flow is 12~20L/min, starts powder feeder and laser apparatus, and laser head completes shaping according to the path movement of programming in advance.
2. Laser Near net-shape method according to claim 1, is characterized in that: described matrix is Ti-6Al-4V or pure Ti.
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CN104086184B (en) * 2014-06-25 2015-12-30 大连理工大学 The method of the clean shaped ceramic part of a kind of ultrasonic wave added Laser Near
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CN111362673B (en) * 2020-04-28 2023-10-10 新化县众一陶瓷有限公司 Preparation method of iron gray alumina wear-resistant ceramic

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