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CN100432025C - Metal/ ceramic laser sintering product post-processing method - Google Patents

Metal/ ceramic laser sintering product post-processing method Download PDF

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CN100432025C
CN100432025C CNB2006101252221A CN200610125222A CN100432025C CN 100432025 C CN100432025 C CN 100432025C CN B2006101252221 A CNB2006101252221 A CN B2006101252221A CN 200610125222 A CN200610125222 A CN 200610125222A CN 100432025 C CN100432025 C CN 100432025C
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silicone rubber
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CN1970503A (en
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史玉升
黄树槐
刘锦辉
张晶
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Huazhong University of Science and Technology
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Abstract

本发明公开了一种金属/陶瓷激光烧结制件的后处理方法。先对待处理的金属/陶瓷激光烧结制件进行脱脂处理和高温烧结;再将高温烧结后的制件附上包套,再放入冷等静压炉,进行加压处理;附包套的方法为:将制件浸入硅橡胶溶液中,在表面均匀附着一层液体后,进行加热烘干处理,使液体在制件表面形成封闭的保护膜;最后对近净成形得到的零件进行后续加工,使零件几何尺寸和形状符合要求。本发明将快速成形技术中的选择性激光烧结(SLS)技术与冷等静压(CIP)技术结合起来,可以成形复杂形状结构、高性能的制件。采用SLS技术,可以成形复杂形状结构的制件,特别是具有复杂的曲面和内部有孔的制件。

Figure 200610125222

The invention discloses a post-processing method for a metal/ceramic laser sintered product. First degrease and high-temperature sinter the metal/ceramic laser sintered parts to be treated; then attach the high-temperature sintered parts to a sheath, and then put them into a cold isostatic pressing furnace for pressure treatment; the method of attaching a sheath It is: immerse the part in the silicone rubber solution, and after a layer of liquid is evenly attached to the surface, heat and dry it to make the liquid form a closed protective film on the surface of the part; finally, carry out subsequent processing on the part obtained by the near-net shape. Make the part geometry and shape meet the requirements. The invention combines the selective laser sintering (SLS) technology and the cold isostatic pressing (CIP) technology in the rapid prototyping technology, and can form complex shape structures and high-performance parts. Using SLS technology, parts with complex shapes and structures can be formed, especially those with complex curved surfaces and internal holes.

Figure 200610125222

Description

一种金属/陶瓷激光烧结制件的后处理方法 A post-processing method for metal/ceramic laser sintered parts

技术领域 technical field

本发明属于快速成形技术领域,具体为一种金属/陶瓷激光烧结制件的后处理方法。The invention belongs to the technical field of rapid prototyping, in particular to a post-processing method for metal/ceramic laser sintered parts.

背景技术 Background technique

选择性激光烧结(SLS)技术是近年来发展非常迅速的一种快速成形技术,它采用激光有选择地分层烧结固体粉末,并使烧结成形的固化层叠加,生成所需形状的制件,可以成形金属、陶瓷、高分子材料等多种粉末材料。SLS技术具有加工周期短、可以成形复杂形状结构的制件、材料利用率高(可达100%)、成本低等优点。利用SLS技术成形金属/陶瓷制件时,需加入熔点较低的高分子粉末材料作为粘结剂,得到的SLS原型件依次通过脱脂和高温烧结除去粘结剂,并使金属/陶瓷颗粒之间建立初步的连接。高温烧结后,原型件已具有一定的机械性能,但内部还有很多孔隙,致密度较低,机械性能还不能完全达到使用要求,必须把这种多孔的制件致密化,提高其机械性能。Selective laser sintering (SLS) technology is a rapid prototyping technology that has developed very rapidly in recent years. It uses laser to selectively sinter solid powder in layers, and superimposes the solidified layers formed by sintering to generate parts of the desired shape. It can form a variety of powder materials such as metals, ceramics, and polymer materials. SLS technology has the advantages of short processing cycle, the ability to form parts with complex shapes and structures, high material utilization rate (up to 100%), and low cost. When using SLS technology to form metal/ceramic parts, it is necessary to add polymer powder materials with a lower melting point as a binder. Establish an initial connection. After high-temperature sintering, the prototype has certain mechanical properties, but there are still many pores inside, the density is low, and the mechanical properties cannot fully meet the requirements for use. This porous part must be densified to improve its mechanical properties.

冷等静压(CIP)技术通过施加外来压力,使粉末颗粒发生位移、变形或碎裂,缩短颗粒间的距离,扩大粉末颗粒间的接触面积,增强颗粒间机械啮合的程度,具有压坯均匀性好、可以成形复杂形状的压坯、机加工量少、节省原料等优点。冷等静压技术具有的这些优点,可以用来对金属/陶瓷SLS制件进行后处理,提高制件的致密度和机械性能。Cold isostatic pressing (CIP) technology applies external pressure to cause displacement, deformation or fragmentation of powder particles, shortens the distance between particles, expands the contact area between powder particles, and enhances the degree of mechanical meshing between particles. It has the advantages of good performance, can form compacts of complex shapes, less machining, and saves raw materials. These advantages of cold isostatic pressing technology can be used to post-treat metal/ceramic SLS parts to improve the density and mechanical properties of the parts.

发明内容 Contents of the invention

本发明的目的在于提供一种金属/陶瓷激光烧结制件的后处理方法,该方法工艺过程简单易行、低耗高效。The object of the present invention is to provide a post-processing method for metal/ceramic laser sintered parts, the process of the method is simple, easy to implement, low in consumption and high in efficiency.

本发明提供的一种金属/陶瓷激光烧结制件的后处理方法,其步骤为:A post-processing method of a metal/ceramic laser sintered part provided by the invention, the steps are:

(1)对待处理的金属/陶瓷激光烧结制件进行脱脂处理和高温烧结;(1) Degreasing and high-temperature sintering of the metal/ceramic laser sintered parts to be processed;

(2)将高温烧结后的制件附上包套,再放入冷等静压炉,进行加压处理;附包套的方法如下:(2) Attach a sheath to the high-temperature sintered part, and then put it into a cold isostatic pressing furnace for pressure treatment; the method of attaching a sheath is as follows:

将制件浸入硅橡胶溶液中,在制件表面均匀附着一层液体后,对制件进行加热烘干处理,使液体在制件表面形成封闭的保护膜;Immerse the workpiece in the silicone rubber solution, and after a layer of liquid is uniformly attached to the surface of the workpiece, the workpiece is heated and dried to make the liquid form a closed protective film on the surface of the workpiece;

(3)对近净成形得到的零件进行后续加工,使零件几何尺寸和形状符合要求。(3) Subsequent processing is performed on the parts obtained by the near-net shape, so that the geometric size and shape of the parts meet the requirements.

本发明将快速成形技术中的选择性激光烧结(SLS)与冷等静压(CIP)技术结合起来,这种复合方法具备以下优点:The present invention combines selective laser sintering (SLS) in rapid prototyping technology with cold isostatic pressing (CIP) technology, and this composite method has the following advantages:

(1)采用SLS技术,可以成形复杂形状结构的制件,特别是具有复杂的曲面和内部有孔的制件。(1) Using SLS technology, parts with complex shapes and structures can be formed, especially parts with complex curved surfaces and internal holes.

(2)经冷等静压,制件可以获得均匀的致密度。(2) After cold isostatic pressing, the workpiece can obtain uniform density.

(3)因经高温烧结的SLS制件已经具有一定的密度和强度,冷等静压(CIP)的生产效率明显提高,可提高50%~90%。(3) Because the SLS parts sintered at high temperature already have a certain density and strength, the production efficiency of cold isostatic pressing (CIP) is significantly improved, which can be increased by 50% to 90%.

(4)冷等静压(HIP)过程采用的包套很简单,免去了设计包套带来的偏差。(4) The sheath used in the cold isostatic pressing (HIP) process is very simple, which eliminates the deviation caused by the design of the sheath.

(5)工艺过程简单易行,低耗高效。(5) The technological process is simple and easy, with low consumption and high efficiency.

附图说明 Description of drawings

图1为本发明金属/陶瓷制件的选择性激光-热等静压复合制造方法的工艺流程图,其中,图1(a)为激光扫描切片处粉末;图1(b)为激光选择性烧结成形的制件;图1(c)为经脱脂和高温烧结后的制件;图1(d)为冷等静压;图1(e)为最终制件。Fig. 1 is the process flow diagram of the selective laser-hot isostatic pressing composite manufacturing method of metal/ceramic parts of the present invention, and wherein, Fig. 1 (a) is the powder at the laser scanning section place; Fig. 1 (b) is laser selective Sintered parts; Fig. 1(c) is the part after degreasing and high temperature sintering; Fig. 1(d) is cold isostatic pressing; Fig. 1(e) is the final part.

具体实施方式 Detailed ways

下面结合附图和实例对本发明的具体过程作进一步详细的阐述:Below in conjunction with accompanying drawing and example concrete process of the present invention is described in further detail:

(1)对待处理的金属/陶瓷激光烧结制件(即SLS制件)进行脱脂处理和高温烧结,其目的是除去制件中的高分子粘结剂,同时使粉末颗粒之间建立联结,提高制件的致密度和强度。(1) Degreasing and high-temperature sintering of the metal/ceramic laser sintered parts to be treated (ie SLS parts), the purpose of which is to remove the polymer binder in the part, and at the same time establish a connection between the powder particles to improve Density and strength of parts.

(2)为高温烧结后的SLS制件附上包套后,即可放入冷等静压炉,进行加压处理。包套的设计方法如下:将制件浸入包套溶液中,在制件表面均匀附着一层液体后,对制件进行加热烘干处理,使液体在制件表面形成封闭的保护膜,在冷等静压时起包套的作用。这里的液体材料需具有如下特点:a)与金属/陶瓷有一定的润湿性,可以附着在制件表面,且经加热烘干可以固化形成封闭的保护膜;b)形成的保护膜具有很好的弹性和抗撕裂性,在冷等静压过程中不会破裂。(2) After attaching the sheath to the high-temperature sintered SLS part, it can be placed in a cold isostatic pressing furnace for pressure treatment. The design method of the sheath is as follows: the workpiece is immersed in the sheath solution, and after a layer of liquid is evenly attached to the surface of the workpiece, the workpiece is heated and dried to make the liquid form a closed protective film on the surface of the workpiece. It acts as a sheath during isostatic pressing. The liquid material here needs to have the following characteristics: a) It has certain wettability with metal/ceramics, can be attached to the surface of the workpiece, and can be cured to form a closed protective film after heating and drying; b) The formed protective film has a strong Good elasticity and tear resistance, will not break during cold isostatic pressing.

包套溶液采用硅橡胶溶液,其中硅橡胶与有机溶剂的体积比约为1∶(0.8-1.5),固化剂与硅橡胶溶液的体积百分比为1∶100-2∶100,其中,有机溶剂可以采用乙酸乙酯等可以将硅橡胶溶解的任一种有机溶剂,固化剂可以为室温脂肪胺固化剂或环氧树脂耐高温固化剂等常规的硅橡胶溶液所使用的固化剂。The coating solution adopts a silicone rubber solution, wherein the volume ratio of the silicone rubber to the organic solvent is about 1: (0.8-1.5), and the volume percentage of the curing agent to the silicone rubber solution is 1: 100-2: 100, wherein the organic solvent can be Use any organic solvent such as ethyl acetate that can dissolve the silicone rubber, and the curing agent can be the curing agent used in conventional silicone rubber solutions such as room temperature aliphatic amine curing agent or epoxy resin high temperature resistant curing agent.

(3)对近净成形得到的零件进行后续加工,如简单机加工或表面处理,使零件几何尺寸和形状完全满足要求。(3) Subsequent processing of parts obtained by near-net shape, such as simple machining or surface treatment, so that the geometric size and shape of the parts can fully meet the requirements.

金属/陶瓷激光烧结制件的制备可以采用现有技术,可以采用下述处理步骤进行:The preparation of metal/ceramic laser sintered parts can adopt the existing technology, and can adopt the following processing steps to carry out:

(1)采用三维造型软件设计出零件CAD三维模型,然后由切片软件处理后保存为STL文件,将STL文件的数据信息输送到SLS快速成形系统。(1) Use 3D modeling software to design the CAD 3D model of the part, then process it with the slicing software and save it as an STL file, and send the data information of the STL file to the SLS rapid prototyping system.

(2)送粉机构在工作平台上平铺一层约为0.02-0.2mm厚度的待加工粉末(粒径约为10-60μm)。(2) The powder feeding mechanism spreads a layer of powder to be processed (with a particle size of about 10-60 μm) with a thickness of about 0.02-0.2 mm on the working platform.

(3)采用激光功率大于等于50W的半导体泵浦YAG激光器、光纤激光器或CO2激光器,激光光斑为10-250μm,扫描间距为0.04-0.2mm,扫描速度为500-3000mm/s,对位于该层切片的粉末进行扫描烧结。(3) Diode-pumped YAG lasers, fiber lasers or CO2 lasers with a laser power greater than or equal to 50W are used. The laser spot is 10-250μm, the scanning distance is 0.04-0.2mm, and the scanning speed is 500-3000mm/s. Layer sliced powders were subjected to scanning sintering.

(4)重复上述步骤(2)-(3),直至制成所需形状的原型件。(4) Repeat the above steps (2)-(3) until the prototype of the desired shape is made.

本发明的实质是将冷等静压(CIP)技术应用到快速成形领域,对金属选择性激光烧结(SLS)制件进行后处理加工,可以提高制件的致密度和强度。同时冷等静压时包套设计简单易行,免去了设计包套所带来的偏差。因此,结合选择性激光烧结(SLS)技术和冷等静压(CIP)技术,可以成形复杂形状结构、高性能的零件。The essence of the present invention is to apply cold isostatic pressing (CIP) technology to the field of rapid prototyping, and perform post-processing on metal selective laser sintering (SLS) parts, which can improve the density and strength of the parts. At the same time, the design of the sheath during cold isostatic pressing is simple and easy, which avoids the deviation caused by the design of the sheath. Therefore, combining selective laser sintering (SLS) technology and cold isostatic pressing (CIP) technology, it is possible to form parts with complex shapes and structures and high performance.

实例1Example 1

(1)首先根据SLM制件经过热等静压后可能出现的变形情况,利用三维造型软件(如UG、Pro/E等)设计出零件热等静压前的CAD三维模型,然后由切片软件处理后保存为STL文件,将STL文件的数据信息输送到SLM快速成形系统。(1) First, according to the possible deformation of SLM parts after hot isostatic pressing, use 3D modeling software (such as UG, Pro/E, etc.) to design the CAD 3D model of the part before hot isostatic pressing, and then use the slicing software After processing, it is saved as an STL file, and the data information of the STL file is sent to the SLM rapid prototyping system.

(2)送粉机构在工作平台上平铺一层约为0.1mm厚的已添加粘结剂的不锈钢粉末(粒径约为20μm),粘结剂为环氧树脂,含量约4%。(2) The powder feeding mechanism spreads a layer of stainless steel powder (particle size about 20 μm) with a thickness of about 0.1 mm on the working platform. The binder is epoxy resin with a content of about 4%.

(3)采用激光功率大于等于50W的半导体泵浦YAG激光器或光纤激光器,激光光斑直径约为50μm,扫描速度约为2000mm/s,扫描间距约为0.1mm,对位于该层切片粉末进行扫描。(3) Use a diode-pumped YAG laser or fiber laser with a laser power greater than or equal to 50W. The laser spot diameter is about 50μm, the scanning speed is about 2000mm/s, and the scanning distance is about 0.1mm. Scan the sliced powder located in this layer.

(4)重复上述步骤(2)-(3),直至制成一个整体的、形状符合需求的SLS制件。(4) Repeat the above steps (2)-(3) until a whole SLS part with the required shape is produced.

(5)将SLS制件转移到真空脱脂炉,抽真空,设定脱脂工艺路线为:在室温下经1小时升温至200℃,1.5小时升温至400℃,2.5小时升温至460℃,2小时升温至750℃,1小时升温至950℃,保温半小时后随炉冷却至室温,出炉。(5) Transfer the SLS parts to the vacuum degreasing furnace, vacuumize, and set the degreasing process route as follows: at room temperature, the temperature is raised to 200°C in 1 hour, the temperature is raised to 400°C in 1.5 hours, the temperature is raised to 460°C in 2.5 hours, and 2 hours Raise the temperature to 750°C, then raise the temperature to 950°C in 1 hour, keep warm for half an hour, then cool to room temperature with the furnace, and take it out of the furnace.

(6)将SLS制件转移到真空烧结炉,抽真空,设定工艺路线为:室温下经1小时升温至1100℃,保温3小时,然后半小时升温至1200℃,保温2小时,冷却到室温出炉。(6) Transfer the SLS parts to a vacuum sintering furnace, vacuumize, and set the process route as follows: at room temperature, heat up to 1100°C for 1 hour, hold for 3 hours, then heat up to 1200°C for half an hour, hold for 2 hours, and cool to Bake at room temperature.

(7)将高温烧结后的SLS制件浸入硅橡胶溶液中,使制件表面附着一层硅橡胶,转移制件至烘干炉,30℃~40℃下烘7~9小时,使硅橡胶在制件表面形成一层保护膜。其中,硅橡胶溶液的成分为:室温脂肪胺固化剂的体积分数为1.5%,硅橡胶与乙酸乙酯的体积比为1∶1。(7) Immerse the SLS parts after high-temperature sintering in the silicone rubber solution, so that a layer of silicone rubber is attached to the surface of the parts, transfer the parts to the drying oven, and bake them at 30 ° C to 40 ° C for 7 to 9 hours to make the silicone rubber Form a protective film on the surface of the workpiece. Wherein, the composition of the silicone rubber solution is: the volume fraction of the fatty amine curing agent at room temperature is 1.5%, and the volume ratio of the silicone rubber to ethyl acetate is 1:1.

(8)检查保护膜是否封闭。若不是完全封闭,重复步骤(7),直至制件表面形成一层完全封闭的保护膜。(8) Check whether the protective film is closed. If it is not completely closed, repeat step (7) until a fully closed protective film is formed on the surface of the workpiece.

(9)将表面已附着封闭保护膜的的制件转移至冷等静压炉,以煤油和汽油等混合液态油为介质,快速加压至2GPa,保压5min。在压力的作用下,SLS制件致密度和机械性能大大提高,且几何尺寸和形状都基本符合要求。(9) Transfer the workpiece with a closed protective film attached to the surface to a cold isostatic pressing furnace, use mixed liquid oil such as kerosene and gasoline as the medium, quickly pressurize to 2GPa, and keep the pressure for 5min. Under the action of pressure, the density and mechanical properties of SLS parts are greatly improved, and the geometric size and shape basically meet the requirements.

(10)最后,对近净成形得到的零件进行后续加工,使零件几何尺寸和形状完全满足要求。(10) Finally, follow-up processing is carried out on the parts obtained by the near net shape, so that the geometric size and shape of the parts fully meet the requirements.

实例2Example 2

(1)首先根据SLM制件经过热等静压后可能出现的变形情况,利用三维造型软件(如UG、Pro/E等)设计出零件热等静压前的CAD三维模型,然后由切片软件处理后保存为STL文件,将STL文件的数据信息输送到SLM快速成形系统。(1) First, according to the possible deformation of SLM parts after hot isostatic pressing, use 3D modeling software (such as UG, Pro/E, etc.) to design the CAD 3D model of the part before hot isostatic pressing, and then use the slicing software After processing, it is saved as an STL file, and the data information of the STL file is sent to the SLM rapid prototyping system.

(2)送粉机构在工作平台上平铺一层约为0.1mm厚的已添加粘结剂的陶瓷粉末(主要成分为氧化铝,粒径约为80μm),粘结剂为环氧树脂,含量约5%。(2) The powder feeding mechanism spreads a layer of ceramic powder with a thickness of about 0.1 mm on the working platform (the main component is alumina, the particle size is about 80 μm), and the binder is epoxy resin. The content is about 5%.

(3)采用激光功率大于等于50W的半导体泵浦YAG激光器或光纤激光器,激光光斑约为50μm,扫描速度约为2000mm/s,扫描间距约为0.1mm,对位于该层切片粉末进行扫描。(3) Use a diode-pumped YAG laser or fiber laser with a laser power greater than or equal to 50W. The laser spot is about 50μm, the scanning speed is about 2000mm/s, and the scanning distance is about 0.1mm. Scan the sliced powder located in this layer.

(4)重复上述步骤(2)-(3),直至制成一个整体的、形状符合需求的SLS制件。(4) Repeat the above steps (2)-(3) until a whole SLS part with the required shape is produced.

(5)将SLS制件转移到真空炉,抽真空,进行脱脂和高温烧结处理。设定脱脂工艺路线为:在室温下经1小时升温至200℃,1小时升温至450℃,1小时升温至550℃,3小时升温至1400℃,保温6小时后随炉冷却至室温,出炉。(5) Transfer the SLS parts to a vacuum furnace, vacuumize, degrease and sinter at high temperature. The degreasing process route is set as follows: heat up to 200°C for 1 hour at room temperature, 450°C for 1 hour, 550°C for 1 hour, and 1400°C for 3 hours, and then cool to room temperature with the furnace after 6 hours of heat preservation. .

(6)将高温烧结后的SLS制件浸入硅溶胶溶液中,使制件表面附着一层硅溶胶,转移制件至烘干炉,80℃~100℃下烘7~9小时,使硅橡胶在制件表面形成一层保护膜。其中,硅橡胶溶液的成分为:环氧树脂耐高温固化剂的体积分数为1.5%,硅橡胶与乙酸乙酯的体积比为1∶1。(6) Immerse the SLS parts after high-temperature sintering in the silica sol solution, so that a layer of silica sol is attached to the surface of the parts, transfer the parts to the drying oven, and bake them at 80 ° C to 100 ° C for 7 to 9 hours to make the silicone rubber Form a protective film on the surface of the workpiece. Wherein, the composition of the silicone rubber solution is: the volume fraction of epoxy resin high temperature resistant curing agent is 1.5%, and the volume ratio of silicone rubber to ethyl acetate is 1:1.

(7)检查保护膜是否封闭。若不是完全封闭,重复步骤(7),直至制件表面形成一层完全封闭的保护膜。(7) Check whether the protective film is closed. If it is not completely closed, repeat step (7) until a fully closed protective film is formed on the surface of the workpiece.

(8)将表面已附着封闭保护膜的的制件转移至冷等静压炉,以煤油和汽油等混合液态油为介质,快速加压至3GPa,保压6min。在压力的作用下,SLS制件致密度和机械性能大大提高,且几何尺寸和形状都基本符合要求。(8) Transfer the workpiece with a closed protective film attached to the surface to a cold isostatic pressing furnace, use mixed liquid oil such as kerosene and gasoline as the medium, quickly pressurize to 3GPa, and keep the pressure for 6 minutes. Under the action of pressure, the density and mechanical properties of SLS parts are greatly improved, and the geometric size and shape basically meet the requirements.

(9)最后,对近净成形得到的零件进行后续加工,使零件几何尺寸和形状完全满足要求。(9) Finally, follow-up processing is carried out on the parts obtained by the near-net shape, so that the geometric size and shape of the parts fully meet the requirements.

Claims (2)

1, a kind of post-treating method of metal/ceramic laser sintering product, its step comprises:
(1) pending metal/ceramic laser sintering product is carried out skimming treatment and high temperature sintering;
(2) product behind the high temperature sintering is enclosed jacket, put into the isostatic cool pressing stove again, carry out pressure treatment; The method of attached jacket is as follows:
Product is immersed in the silicone rubber solution, after one deck liquid is evenly adhered on the product surface, product is carried out heating, drying handle, make liquid form the protective membrane of sealing on the product surface;
(3) part that near-net-shape is obtained carries out following process, and the part geometry size and dimension is met the requirements.
2, post-treating method according to claim 1 is characterized in that: in the silicone rubber solution, wherein silicon rubber is 1 with the volume of organic solvent ratio: 0.8-1 in the step (2): 1.5, and the volume percent of solidifying agent and silicone rubber solution is 1: 100-2: 100.
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