CN111366598A - A 3D printing mixed powder ratio measurement method - Google Patents

A 3D printing mixed powder ratio measurement method Download PDF

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CN111366598A
CN111366598A CN202010280789.6A CN202010280789A CN111366598A CN 111366598 A CN111366598 A CN 111366598A CN 202010280789 A CN202010280789 A CN 202010280789A CN 111366598 A CN111366598 A CN 111366598A
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王呈栋
张克栋
胡友迅
李盈盈
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Abstract

本发明公开了一种3D打印混合粉末配比实测方法，包括以下步骤：混合粉末收集与制样；确定粉末A和B成分差异最大的主元素；在同一视场下，对两种主元素进行着色，分别拍摄能谱图照片和实物彩照；导入图像处理软件，用“色彩范围”功能拾取主元素着色像素点；用“记录测量”功能获取着色像素总面积，据此计算确定混合粉末配比。本发明能有效解决颜色相同、松装密度相近、颗粒大小相似的3D打印混合粉末配比测试的难题，相比传统的粉末颗粒逐一测量法，本发明所述的方法速度快、效率高、误差小，操作简单，易于实施。

Figure 202010280789

The invention discloses a method for measuring the proportion of mixed powders for 3D printing, comprising the following steps: collecting and preparing samples of the mixed powders; determining the main element with the largest difference in the composition of powders A and B; under the same field of view, measuring the two main elements For coloring, take the photo of the energy spectrum and the color photo of the real object respectively; import the image processing software, use the "color range" function to pick up the coloring pixels of the main elements; use the "record measurement" function to obtain the total area of the colored pixels, and calculate and determine the mixed powder ratio based on this . The present invention can effectively solve the problem of the proportion test of 3D printing mixed powders with the same color, similar bulk density and similar particle size. Small, simple to operate and easy to implement.

Figure 202010280789

Description

一种3D打印混合粉末配比实测方法A 3D printing mixed powder ratio measurement method

技术领域technical field

本发明涉及3D打印技术领域，具体涉及一种3D打印混合粉末配比实测方法。The invention relates to the technical field of 3D printing, in particular to a method for measuring the proportion of mixed powders for 3D printing.

背景技术Background technique

功能梯度材料是由两种或多种材料复合且成分和结构呈连续梯度变化的一种新型复合材料，其材料组分和宏观性能在空间位置上呈连续、均匀梯度变化的特征，克服了传统复合材料因不同相界面之间引起的应力集中与微裂纹缺陷，可满足航天、能源、生物医学领域结构件的不同部位对材料使用性能的差异化需求。激光沉积(3D打印)，通过控制混合粉末质量比以实现材料性能梯度变化，是制备功能梯度材料的重要方法。然而，当采用粉末质量、颗粒直径不同时，混合粉末经送粉管高速喷射后会发生分离，造成材料成分偏差，致使材料使用性能下降，无法满足设计要求。因此，如何快速、精准地测得混合粉末的实际质量配比，是实现粉末分离调控，保障功能梯度材料成分准确的前提与基础。Functionally graded material is a new type of composite material composed of two or more materials with continuous gradient changes in composition and structure. Due to the stress concentration and microcrack defects caused by different phase interfaces, composite materials can meet the differentiated requirements of different parts of the structure in the aerospace, energy, and biomedical fields for the performance of the material. Laser deposition (3D printing), by controlling the mass ratio of mixed powders to achieve gradient changes in material properties, is an important method for preparing functionally graded materials. However, when the powder quality and particle diameter are different, the mixed powder will be separated after being sprayed at a high speed by the powder feeding tube, resulting in deviation of material composition, resulting in a decline in the performance of the material, which cannot meet the design requirements. Therefore, how to quickly and accurately measure the actual mass ratio of mixed powders is the premise and basis for realizing powder separation and regulation and ensuring the accuracy of functionally graded materials.

近年来，工程人员逐渐认识到混合粉末成分配比的精准检测的重要性，广泛开展粉末配比检测方法与装置的研究。公开号为CN105486705B的中国发明专利提供了一种定量分析粉末混合物成分的方法，通过X光衍射谱分析得到粉末分值及吸收系数，进而建立杠杆定律公式测得粉末质量配比；公开号为CN109916941A的中国发明专利提出了一种预混合粉末3D打印分离检测方法，通过图像测量系统Digimizer对能谱彩图中的粉末颗粒直径进行逐一测量，换算体积求和后，计算得到混合粉末质量配比；在此基础上，公开号为CN109746447A的中国发明专利提出一种预混合粉末分离调控方法，实现了对粉末分离的精准调控。上述专利中提出的粉末成分与配比测试方法，需要对粉末颗粒进行逐一测量，测试工作量大，且计算过程过于复杂，对技术人员的数学水平要求较高。In recent years, engineers have gradually realized the importance of accurate detection of the composition ratio of mixed powders, and have carried out extensive research on powder ratio detection methods and devices. The Chinese invention patent with the publication number CN105486705B provides a method for quantitatively analyzing the composition of powder mixtures. The powder score and absorption coefficient are obtained through X-ray diffraction analysis, and then a lever law formula is established to measure the powder mass ratio; the publication number is CN109916941A The Chinese invention patent of the company proposes a pre-mixed powder 3D printing separation and detection method. The image measurement system Digimizer measures the diameter of the powder particles in the energy spectrum color map one by one, and after the conversion volume is summed, the mass ratio of the mixed powder is calculated; On this basis, the Chinese invention patent publication number CN109746447A proposes a premixed powder separation control method, which realizes precise control of powder separation. The powder composition and proportioning test method proposed in the above-mentioned patent requires the powder particles to be measured one by one, the test workload is large, and the calculation process is too complicated, which requires a high level of mathematics for technicians.

随着人工智能技术的快速崛起，研发与工程人员逐渐意识到运用计算机图像识别方法来解决工程问题。公开号为CN110658040A的中国发明专利提出一种金属球形粉末标准样品的制备方法，运用图像统计软件完成粉末颗粒粒度统计；公开号为CN110335257A的中国发明专利提出一种图像色彩检测方法及移动终端，能够识别出图像数据颜色基调信息；公开号为CN107068589B的中国发明专利提出一种基于图像识别的晶粒挑选系统及方法，通过蓝膜，将标准晶粒的图像分解成像素点,并记录每个像素点的灰阶标准值，实现晶粒挑选；公开号为CN110853017A的中国发明专利提出了一种粉末颗粒图像中圆颗粒数量的统计方法，通过提取图像中的联通域，结合中心漂移算法实现对图像中形状不规则、大小不一、重叠情况的粉末颗粒的数量和大小进行统计。然而，上述方法不是需要额外的硬件，就是计算过于复杂，实际操作难度极大。针对颜色相同、松装密度相近，颗粒大小相似的混合粉末，尚缺乏简单、快速、有效的混合粉末配比实测方法。With the rapid rise of artificial intelligence technology, R&D and engineering personnel have gradually realized the use of computer image recognition methods to solve engineering problems. The Chinese invention patent with publication number CN110658040A proposes a method for preparing a standard sample of metal spherical powder, which uses image statistics software to complete powder particle size statistics; the Chinese invention patent with publication number CN110335257A proposes an image color detection method and a mobile terminal, which can The color tone information of the image data is identified; the Chinese invention patent with the publication number CN107068589B proposes a grain selection system and method based on image recognition, through the blue film, the image of the standard grain is decomposed into pixel points, and each pixel is recorded. The grayscale standard value of the point is used to achieve grain selection; the Chinese invention patent publication number CN110853017A proposes a statistical method for the number of circular particles in a powder particle image. The number and size of powder particles with irregular shapes, different sizes and overlapping conditions are counted. However, the above method either requires additional hardware, or the calculation is too complicated and the actual operation is extremely difficult. For mixed powders with the same color, similar bulk density and similar particle size, there is still a lack of a simple, fast and effective method for measuring the proportion of mixed powders.

发明内容SUMMARY OF THE INVENTION

本发明要解决的技术问题是提供一种3D打印混合粉末配比实测方法，其能有效解决颜色相同、松装密度相近、颗粒大小相似的3D打印混合粉末配比测试的难题，速度快，效率高。The technical problem to be solved by the present invention is to provide a method for measuring the proportion of 3D printing mixed powder, which can effectively solve the problem of measuring the proportion of 3D printing mixed powder with the same color, similar bulk density and similar particle size, with high speed and efficiency. high.

为了解决上述技术问题，本发明提供了一种3D打印混合粉末配比实测方法，包括以下步骤：In order to solve the above technical problems, the present invention provides a method for measuring the proportion of mixed powders for 3D printing, which includes the following steps:

步骤一、获取具有混合粉末的样品，其中混合粉末包括粉末A和粉末B；Step 1. Obtain a sample with mixed powder, wherein the mixed powder includes powder A and powder B;

步骤二、选定粉末A和粉末B的化学成分差异最大的元素EA和EB,其中，元素EA为粉末A的主元素，元素EB为粉末B的主元素；Step 2, select the elements E A and E B with the largest chemical composition difference between powder A and powder B, wherein, element E A is the main element of powder A, and element E B is the main element of powder B;

步骤三、通过扫描电子显微镜对样品表面的元素能谱面扫描，在能谱分析仪附带的软件界面，设置元素EA为第一颜色，设置元素EB为第二颜色，所述第一颜色和第二颜色为两种不同颜色的三元色；Step 3: Scan the element energy spectrum on the surface of the sample with a scanning electron microscope. On the software interface attached to the energy spectrum analyzer, set the element E A as the first color, and set the element E B as the second color, and the first color and the second color is a triad of two different colors;

步骤四、获取同一视场下样品中元素EA的能谱照片Fig.A、样品中元素EB的能谱照Fig.B和彩色照片图Fig.C，其中，所述彩色照片图Fig.C同时对元素EA和元素EB着色；Step 4: Obtain the energy spectrum photo of element EA in the sample Fig.A , the energy spectrum photo of element E B in the sample Fig.B and the color photo map Fig.C under the same field of view, wherein the color photo is Fig. C simultaneously colors element E A and element E B ;

步骤五、判断彩色照片图Fig.C中的粉尘颗粒是否完全着色，若是，则进入步骤六；若否，则调整扫描电子显微镜的拍摄位置，选取临近区域重复步骤四，直至Fig.C中的粉末颗粒完全着色；Step 5. Determine whether the dust particles in the color photo in Fig.C are completely colored. If so, go to Step 6; The powder particles are fully colored;

步骤六、通过图像处理软件对能谱照片Fig.A进行处理，获取能谱照片Fig.A中元素EA的像素总面积SA，具体包括：Step 6: Process the energy spectrum photo Fig.A by image processing software to obtain the total pixel area S A of the element EA in the energy spectrum photo Fig.A , which specifically includes:

S61、若粉末B中不含有元素EA，则拾取并选中能谱照片Fig.A中着色区域，直至所有非背景色被选中，利用图像处理软件中的“记录测量”功能，获取着色区域的像素总面积SA；S61. If the powder B does not contain the element E A , pick and select the colored area in the energy spectrum photo Fig.A until all non-background colors are selected, and use the "record measurement" function in the image processing software to obtain the coloring area. Total pixel area S A ;

S62、若粉末B中含有元素EA，则拾取并选中能谱照片Fig.A中所有着色区域，之后根据彩色照片图Fig.C中元素EB对应粉末颗粒位置剔除能谱照片Fig.A中干扰像素，利用图像处理软件中的“记录测量”功能，获取剔除干扰像素后的着色区域的像素总面积SA；S62. If the powder B contains element E A , pick and select all the colored areas in the energy spectrum photo Fig.A, and then remove the energy spectrum photo Fig.A according to the position of the powder particle corresponding to the element E B in the color photo image Fig.C Interfering pixels, use the "record measurement" function in the image processing software to obtain the total pixel area S A of the coloring area after eliminating the interference pixels;

步骤七、通过图像处理软件对能谱照片Fig.B进行处理，获取能谱照片Fig.B中元素EB的像素总面积SB，具体包括：Step 7: Process the energy spectrum photo Fig.B by image processing software to obtain the total pixel area S B of the element E B in the energy spectrum photo Fig.B, which specifically includes:

S71、若粉末A中不含有元素EB，则拾取并选中能谱照片Fig.B中着色区域，直至所有非背景色被选中，利用图像处理软件中的“记录测量”功能，获取着色区域的像素总面积SB；S71. If the powder A does not contain the element E B , pick and select the colored area in the energy spectrum photo Fig.B until all non-background colors are selected, and use the "record measurement" function in the image processing software to obtain the coloring area. total pixel area S B ;

S72、若粉末A中含有元素EB，则拾取并选中能谱照片Fig.B中所有着色区域，之后根据彩色照片图Fig.C中元素EA对应粉末颗粒位置剔除能谱照片Fig.B中干扰像素，利用图像处理软件中的“记录测量”功能，获取剔除干扰像素后的着色区域的像素总面积SB；S72. If the powder A contains element E B , pick and select all the colored areas in the energy spectrum photo Fig.B, and then remove the energy spectrum photo Fig.B according to the position of the powder particle corresponding to the element E A in the color photo image Fig.C Interfering pixels, use the "record measurement" function in the image processing software to obtain the total pixel area S B of the coloring area after eliminating the interference pixels;

步骤八、计算获得混合粉末的实测配比η；Step 8, calculate and obtain the measured ratio η of mixed powder;

Figure BDA0002446495720000041
Figure BDA0002446495720000041

其中，ρA为粉末A的松装密度，ρB为粉末B的松装密度，mA为粉末A的总质量，mB为粉末B的总质量，nA为Fig.C中粉末A的颗粒个数，nB为Fig.C中粉末B的颗粒个数，

Figure BDA0002446495720000042
为粉末A的制造厂商提供的粉末颗粒平均直径，
Figure BDA0002446495720000043
为粉末B的制造厂商提供的粉末颗粒平均直径，μ为像素比例尺，
Figure BDA0002446495720000044
Figure BDA0002446495720000045
Among them, ρ A is the bulk density of powder A, ρ B is the bulk density of powder B, m A is the total mass of powder A, m B is the total mass of powder B, and n A is the total mass of powder A in Fig.C Number of particles, n B is the number of particles of powder B in Fig.C,
Figure BDA0002446495720000042
Average diameter of powder particles provided to the manufacturer of Powder A,
Figure BDA0002446495720000043
The average diameter of powder particles provided by the manufacturer of powder B, μ is the pixel scale,
Figure BDA0002446495720000044
Figure BDA0002446495720000045

作为优选的，S61中，运用颜色取样“吸管+”拾取能谱照片Fig.A中着色区域。Preferably, in S61, use the color sampling "Pipe+" to pick up the colored area in the energy spectrum photo Fig.A.

作为优选的，S62中，运用颜色取样“吸管-”拾取剔除能谱照片Fig.A中干扰像素。Preferably, in S62, the color sampling "pipe-" is used to pick out the disturbing pixels in the energy spectrum photo Fig.A.

作为优选的，步骤一具体包括：As preferably, step one specifically includes:

S11、在3D打印机的工作台上固定亚克力板，所述亚克力板的上表面自带离型膜，在所述离型膜上依次设置双面胶层和液态环脂胶层；S11. Fix an acrylic plate on the worktable of the 3D printer, the upper surface of the acrylic plate is provided with a release film, and a double-sided adhesive layer and a liquid cycloaliphatic adhesive layer are arranged on the release film in sequence;

S12、将混合粉末装入3D打印机的送粉料斗，打开所述送粉料斗，保持激光束关闭，3D打印激光喷头朝所述亚克力板喷射粉末，获得覆盖混合粉末层的亚克力板，之后静置冷却直至所述液态环氧树脂胶固化；S12. Load the mixed powder into the powder feeding hopper of the 3D printer, open the powder feeding hopper, keep the laser beam turned off, and spray the powder with the 3D printing laser nozzle to the acrylic plate to obtain an acrylic plate covering the mixed powder layer, and then let it stand cooling until the liquid epoxy resin is cured;

S13、对亚克力板上粘附的混合粉末层取样、清洗与烘干，获得样品。S13, sampling, cleaning and drying the mixed powder layer adhering to the acrylic plate to obtain a sample.

作为优选的，S12中所述3D打印激光喷头为同轴送粉式。Preferably, the 3D printing laser nozzle in S12 is a coaxial powder feeding type.

作为优选的，所述图像处理软件为Photoshop。Preferably, the image processing software is Photoshop.

作为优选的，所述图像处理软件为FlauntR。Preferably, the image processing software is FlauntR.

作为优选的，所述步骤六中的能谱照片Fig.A为png无损压缩格式图片。Preferably, the energy spectrum photo Fig.A in the step 6 is a png lossless compression format picture.

作为优选的，所述步骤七中的能谱照片Fig.B为png无损压缩格式图片。Preferably, the energy spectrum photo Fig.B in the step 7 is a picture in png lossless compression format.

作为优选的，S71中，运用颜色取样“吸管+”拾取能谱照片Fig.B中着色区域；S72中，运用颜色取样“吸管-”拾取剔除能谱照片Fig.B中干扰像素。Preferably, in S71, use the color sampling "Pipe+" to pick up the colored area in the energy spectrum photo Fig.B; in S72, use the color sampling "Pipe-" to pick and remove the interference pixels in the energy spectrum photo Fig.B.

本发明的有益效果：Beneficial effects of the present invention:

1、本发明提供了一种3D打印混合粉末配比实测方法，能有效解决颜色相同、松装密度相近、颗粒大小相似的3D打印混合粉末配比测试的难题，相比传统的粉末颗粒逐一测量法，本发明所述的方法速度快、效率高、误差5％以内。1. The present invention provides a method for measuring the proportion of 3D printing mixed powder, which can effectively solve the problem of measuring the proportion of 3D printing mixed powder with the same color, similar bulk density and similar particle size. Compared with the traditional powder particle measurement one by one The method of the present invention is fast, efficient, and has an error within 5%.

2、本发明对检测人员业务素质要求不高，操作简单，易于实施。2. The present invention does not have high requirements on the professional quality of testing personnel, and is simple to operate and easy to implement.

附图说明Description of drawings

图1为本发明实施例的流程示意图；1 is a schematic flowchart of an embodiment of the present invention;

图2为本发明实施例的粉末收集示意图；Fig. 2 is the powder collection schematic diagram of the embodiment of the present invention;

图3为本发明的混合粉末元素能谱面扫示意图。FIG. 3 is a schematic diagram of the elemental energy spectrum scan of the mixed powder of the present invention.

图中标号说明：1、送粉料斗；2、粉管；3、同轴光内送粉激光头；4、环氧树脂胶；5、双面胶；6、亚克力板；7、送粉轨迹；8、工作台；9、混合粉末；10、粉末B像素集；11、粉末A像素集；12、粉末A的干扰像素；13、元素EA的能谱照片；14、混合粉末实物彩色照片；15、元素EB的能谱照片。Description of the labels in the figure: 1. Powder feeding hopper; 2. Powder tube; 3. Coaxial optical inner powder feeding laser head; 4. Epoxy resin glue; 5. Double-sided tape; 6. Acrylic plate; 7. Powder feeding track 8. Workbench; 9. Mixed powder; 10. Powder B pixel set; 11. Powder A pixel set; 12. Interference pixel of powder A; 13. Energy spectrum photo of element E A ; 14. Color photo of mixed powder ; 15. Energy spectrum photo of element E B.

具体实施方式Detailed ways

下面结合附图和具体实施例对本发明作进一步说明，以使本领域的技术人员可以更好地理解本发明并能予以实施，但所举实施例不作为对本发明的限定。The present invention will be further described below with reference to the accompanying drawings and specific embodiments, so that those skilled in the art can better understand the present invention and implement it, but the embodiments are not intended to limit the present invention.

本发明公开了3D打印混合粉末配比实测方法，包括以下步骤：The invention discloses a method for measuring the proportion of 3D printing mixed powder, comprising the following steps:

步骤一、获取具有混合粉末的样品，其中混合粉末包括粉末A和粉末B：Step 1. Obtain a sample with mixed powder, wherein the mixed powder includes powder A and powder B:

S11、在3D打印机的工作台上固定亚克力板，所述亚克力板的上表面自带离型膜，在所述离型膜上依次设置双面胶层和液态环脂胶层；S11. Fix an acrylic plate on the worktable of the 3D printer, the upper surface of the acrylic plate is provided with a release film, and a double-sided adhesive layer and a liquid cycloaliphatic adhesive layer are arranged on the release film in sequence;

S12、将混合粉末装入3D打印机的送粉料斗，打开所述送粉料斗，保持激光束关闭，3D打印激光喷头朝所述亚克力板喷射粉末，获得覆盖混合粉末层的亚克力板，之后静置冷却直至所述液态环氧树脂胶固化，其中，3D打印激光喷头为同轴送粉式。S12. Load the mixed powder into the powder feeding hopper of the 3D printer, open the powder feeding hopper, keep the laser beam turned off, and spray the powder with the 3D printing laser nozzle to the acrylic plate to obtain an acrylic plate covering the mixed powder layer, and then let it stand Cool until the liquid epoxy resin is solidified, wherein the 3D printing laser nozzle is a coaxial powder feeding type.

S13、对亚克力板上粘附的混合粉末层取样、清洗与烘干，获得样品。S13, sampling, cleaning and drying the mixed powder layer adhering to the acrylic plate to obtain a sample.

步骤二、选定粉末A和粉末B的化学成分差异最大的元素EA和EB,其中，元素EA为粉末A的主元素，元素EB为粉末B的主元素。Step 2: Selecting elements E A and E B with the largest chemical composition difference between powder A and powder B, wherein element E A is the main element of powder A, and element E B is the main element of powder B.

步骤三、通过扫描电子显微镜对样品表面的元素能谱面扫描，在能谱分析仪附带的软件界面，设置元素EA为第一颜色，设置元素EB为第二颜色，所述第一颜色和第二颜色为两种不同颜色的三元色。三元色为RGB三色，如此，方便图像处理软件区分两种元素，也便于提取着色颗粒，便于与背景区域区分。Step 3: Scan the element energy spectrum on the surface of the sample with a scanning electron microscope. On the software interface attached to the energy spectrum analyzer, set the element E A as the first color, and set the element E B as the second color, and the first color and the second color is a triad of two different colors. The three primary colors are RGB three colors. In this way, it is convenient for image processing software to distinguish two elements, and it is also easy to extract colored particles, which is easy to distinguish from the background area.

步骤四、获取同一视场下样品中元素EA的能谱照片Fig.A、样品中元素EB的能谱照Fig.B和彩色照片图Fig.C，其中，所述彩色照片图Fig.C同时对元素EA和元素EB着色。Step 4: Obtain the energy spectrum photo of element EA in the sample Fig.A , the energy spectrum photo of element E B in the sample Fig.B and the color photo map Fig.C under the same field of view, wherein the color photo is Fig. C colors both element E A and element E B.

步骤五、判断彩色照片图Fig.C中的粉尘颗粒是否完全着色，若是，则进入步骤六；若否，则调整扫描电子显微镜的拍摄位置，选取临近区域重复步骤四，直至Fig.C中的粉末颗粒完全着色。Step 5. Determine whether the dust particles in the color photo in Fig.C are completely colored. If so, go to Step 6; Powder particles are fully pigmented.

步骤六、通过图像处理软件对能谱照片Fig.A进行处理，获取能谱照片Fig.A中元素EA的像素总面积SA，具体包括：Step 6: Process the energy spectrum photo Fig.A by image processing software to obtain the total pixel area S A of the element EA in the energy spectrum photo Fig.A , which specifically includes:

S61、若粉末B中不含有元素EA，则拾取并选中能谱照片Fig.A中着色区域，直至所有非背景色被选中，利用图像处理软件中的“记录测量”功能，获取着色区域的像素总面积SA；S61. If the powder B does not contain the element E A , pick and select the colored area in the energy spectrum photo Fig.A until all non-background colors are selected, and use the "record measurement" function in the image processing software to obtain the coloring area. Total pixel area S A ;

S62、若粉末B中含有元素EA，则拾取并选中能谱照片Fig.A中所有着色区域，之后根据彩色照片图Fig.C中元素EB对应粉末颗粒位置剔除能谱照片Fig.A中干扰像素，利用图像处理软件中的“记录测量”功能，获取剔除干扰像素后的着色区域的像素总面积SA。S62. If the powder B contains element E A , pick and select all the colored areas in the energy spectrum photo Fig.A, and then remove the energy spectrum photo Fig.A according to the position of the powder particle corresponding to the element E B in the color photo image Fig.C For interference pixels, use the "record measurement" function in the image processing software to obtain the total pixel area S A of the colored area after eliminating the interference pixels.

步骤七、通过图像处理软件对能谱照片Fig.B进行处理，获取能谱照片Fig.B中元素EB的像素总面积SB，具体包括：Step 7: Process the energy spectrum photo Fig.B by image processing software to obtain the total pixel area S B of the element E B in the energy spectrum photo Fig.B, which specifically includes:

S71、若粉末A中不含有元素EB，则拾取并选中能谱照片Fig.B中着色区域，直至所有非背景色被选中，利用图像处理软件中的“记录测量”功能，获取着色区域的像素总面积SB；S71. If the powder A does not contain the element E B , pick and select the colored area in the energy spectrum photo Fig.B until all non-background colors are selected, and use the "record measurement" function in the image processing software to obtain the coloring area. total pixel area S B ;

S72、若粉末A中含有元素EB，则拾取并选中能谱照片Fig.B中所有着色区域，之后根据彩色照片图Fig.C中元素EA对应粉末颗粒位置剔除能谱照片Fig.B中干扰像素，利用图像处理软件中的“记录测量”功能，获取剔除干扰像素后的着色区域的像素总面积SB。S72. If the powder A contains element E B , pick and select all the colored areas in the energy spectrum photo Fig.B, and then remove the energy spectrum photo Fig.B according to the position of the powder particle corresponding to the element E A in the color photo image Fig.C For interfering pixels, use the "record measurement" function in the image processing software to obtain the total pixel area S B of the colored area after removing the interfering pixels.

步骤八、计算获得混合粉末的实测配比η；Step 8, calculate and obtain the measured ratio η of mixed powder;

Figure BDA0002446495720000081
Figure BDA0002446495720000081

其中，ρA为粉末A的松装密度，ρB为粉末B的松装密度，mA为粉末A的总质量，mB为粉末B的总质量，nA为Fig.C中粉末A的颗粒个数，nB为Fig.C中粉末B的颗粒个数，

Figure BDA0002446495720000082
为粉末A的制造厂商提供的粉末颗粒平均直径，
Figure BDA0002446495720000083
为粉末B的制造厂商提供的粉末颗粒平均直径，μ为像素比例尺，
Figure BDA0002446495720000084
Figure BDA0002446495720000085
Among them, ρ A is the bulk density of powder A, ρ B is the bulk density of powder B, m A is the total mass of powder A, m B is the total mass of powder B, and n A is the total mass of powder A in Fig.C Number of particles, n B is the number of particles of powder B in Fig.C,
Figure BDA0002446495720000082
Average diameter of powder particles provided to the manufacturer of Powder A,
Figure BDA0002446495720000083
The average diameter of powder particles provided by the manufacturer of powder B, μ is the pixel scale,
Figure BDA0002446495720000084
Figure BDA0002446495720000085

S61中，运用颜色取样“吸管+”拾取能谱照片Fig.A中着色区域；S62中，运用颜色取样“吸管-”拾取剔除能谱照片Fig.A中干扰像素。S71中，运用颜色取样“吸管+”拾取能谱照片Fig.B中着色区域；S72中，运用颜色取样“吸管-”拾取剔除能谱照片Fig.B中干扰像素。In S61, use the color sampling "Pipe+" to pick up the colored area in the energy spectrum photo Fig.A; in S62, use the color sampling "Pipe-" to pick out the interference pixels in the energy spectrum photo Fig.A. In S71, use the color sampling "Pipe+" to pick up the colored area in the energy spectrum photo Fig.B; in S72, use the color sampling "Pipe-" to pick out the interference pixels in the energy spectrum photo Fig.B.

图像处理软件为Photoshop或FlauntR。The image processing software is Photoshop or FlauntR.

步骤六中的能谱照片Fig.A为png无损压缩格式图片。The energy spectrum photo in step 6, Fig.A, is a png image in lossless compression format.

步骤七中的能谱照片Fig.B为png无损压缩格式图片。The energy spectrum photo in Step 7, Fig.B, is a png image in lossless compression format.

实施例1Example 1

针对上海电气集团上海汽轮机厂生产的百万千瓦核电汽轮机缸体中分面转子支撑处的Ni-Fe功能梯度材料，采用激光沉积工艺制备，即原材料粉末A为IN625镍粉，粉末B为304L铁粉、按设计质量比1：3称重混合，现需测量3D打印喷射后的实际粉末配比。Aiming at the Ni-Fe functionally graded material at the faceted rotor support in the cylinder block of the million-kilowatt nuclear power steam turbine produced by Shanghai Electric Group Shanghai Steam Turbine Plant, the laser deposition process was used to prepare it, that is, the raw material powder A was IN625 nickel powder, and the powder B was 304L iron. The powder is weighed and mixed according to the designed mass ratio of 1:3. Now it is necessary to measure the actual powder ratio after 3D printing spraying.

应用本发明提供的一种3D打印混合粉末配比实测方法，具体流程如图1所示，操作如下：Applying a method for measuring the proportion of mixed powders for 3D printing provided by the present invention, the specific process is shown in Figure 1, and the operations are as follows:

1)将自带离型膜的亚克力板6固定在3D打印工作台8上，在亚克力板6表面粘贴双面胶5，随后将无色、透明环氧树脂A胶与B胶按2:1的比例倒入240ml透明的一次性塑料杯中(该塑料杯不会与环氧树脂4发生化学反应)，用搅拌棒将两种胶混合均匀，撕掉双面胶5表层，用宽度为5mm的扁刷将环氧树脂胶4均匀涂抹在双面胶表面，控制环氧树脂4的厚度不超1mm；1) Fix the acrylic board 6 with its own release film on the 3D printing table 8, paste the double-sided tape 5 on the surface of the acrylic board 6, and then put the colorless and transparent epoxy resin A glue and B glue in a ratio of 2:1 Pour the proportion of the adhesive into a 240ml transparent disposable plastic cup (the plastic cup will not chemically react with epoxy resin 4), mix the two glues evenly with a stirring rod, tear off the surface layer of the double-sided adhesive tape 5, and use a width of 5mm. Apply the epoxy resin glue 4 evenly on the surface of the double-sided tape with the flat brush, and control the thickness of the epoxy resin 4 to not exceed 1mm;

2)对装有同轴光内送粉激光头3的工业机械臂编程，如图2所示，设定移动轨迹7的长度L为0.5m，调整送粉率为8g/min，扫描速度为8mm/s，激光喷头与亚克力板6表面垂直距离(喷射距离)为18.5mm，随后打开氩气与送粉料斗1，保持激光束关闭，按预设轨迹7移动0.5m，混合粉末9经粉管2喷射到粘有环氧树脂胶4的亚克力板6上，再将粘有混合粉末层的亚克力板6放在阴凉处干燥，直至液态环氧树脂胶4完全固化；2) Program the industrial robotic arm equipped with the coaxial optical inner powder feeding laser head 3, as shown in Figure 2, set the length L of the moving track 7 to 0.5m, adjust the powder feeding rate to 8g/min, and the scanning speed to be 8mm/s, the vertical distance (spray distance) between the laser nozzle and the surface of the acrylic plate 6 is 18.5mm, then turn on the argon gas and the powder feeding hopper 1, keep the laser beam closed, move 0.5m according to the preset trajectory 7, and mix the powder 9 through the powder The tube 2 is sprayed onto the acrylic sheet 6 with the epoxy resin glue 4, and then the acrylic sheet 6 with the mixed powder layer is placed in a cool place to dry until the liquid epoxy resin glue 4 is completely cured;

3)针对含有粉末的亚克力板6，用裁剪机配套刀具刻划出1cm*1cm大小,再用刀尖将粉末下方的离型膜从亚克力板6上均匀揭开并撕下，确保在此过程中离型膜不发生褶皱，获取检测样品，随后对其喷金处理，并使用导电胶与铜片固定，放入扫描电子显微镜真空仓。3) For the acrylic sheet 6 containing powder, use the cutter supporting the cutting machine to cut out the size of 1cm*1cm, and then use the tip of the knife to evenly lift and tear off the release film under the powder from the acrylic sheet 6 to ensure that during this process The release film is not wrinkled, the test sample is obtained, and then it is sprayed with gold, fixed with conductive glue and copper sheet, and placed in the vacuum chamber of scanning electron microscope.

表1Table 1

Figure BDA0002446495720000091
Figure BDA0002446495720000091

表1为粉末A和粉末B出厂附带的化学元素成分表。根据表1，选定粉末A的主元素EA为Ni，粉末B的主元素EB为Fe，利用扫描电子显微镜(扫描电子显微镜的型号为德国蔡司EVO18或日立JSM-7800F)对样品粉末表面进行元素能谱面扫描，在能谱分析仪附带软件界面，设置元素Ni为蓝色，元素Fe为绿色。在同一个视场下，分别拾取并拍摄混合粉末中元素Ni的能谱照片13，元素Fe的能谱照片15，以及同时存在元素Ni和Fe的实物彩色照片14；Table 1 is the chemical element composition table attached to Powder A and Powder B. According to Table 1, the main element E A of powder A is selected to be Ni, and the main element E B of powder B is Fe. The surface of the sample powder is analyzed by scanning electron microscope (the model of the scanning electron microscope is German Zeiss EVO18 or Hitachi JSM-7800F). Perform element energy spectrum scan, in the software interface attached to the energy spectrum analyzer, set the element Ni as blue and the element Fe as green. Under the same field of view, pick up and take the energy spectrum photo 13 of element Ni in the mixed powder, the energy spectrum photo 15 of element Fe, and the physical color photo 14 of both elements Ni and Fe;

4)判断混合粉末实物彩色照片14中的粉末颗粒是否完全着色，此时，所有粉末颗粒已完全着色，故进入下一步骤；4) Judging whether the powder particles in the mixed powder real color photo 14 are completely colored, at this time, all powder particles have been completely colored, so enter the next step;

5)将主元素为Ni的能谱照片13导入图像处理软件Photoshop CS6，调整照片至100％大小，点击主菜单“选择”，开启用图像处理软件“色彩范围”模块，设置颜色容差为100％，用颜色取样吸管，拾取并选中能谱照片中着色颗粒，由于粉末B含有10.1％的镍元素，则运用颜色取样“吸管+”进行多次叠加拾取，直至所有非背景色被选中后，观察彩图14中元素Ni对应粉末颗粒位置，然后再用“吸管-”工具拾取粉末A的干扰像素12对应位置RGB值，排除此类干扰像素；5) Import the energy spectrum photo 13 whose main element is Ni into the image processing software Photoshop CS6, adjust the size of the photo to 100%, click the main menu "Select", open the "Color Range" module of the image processing software, and set the color tolerance to 100 %, use the color sampling pipette to pick and select the colored particles in the energy spectrum photo. Since powder B contains 10.1% nickel element, use the color sampling "Pipe +" to superimpose multiple picks until all non-background colors are selected. Observe the position of the powder particles corresponding to the element Ni in the color picture 14, and then use the "Pipe-" tool to pick up the RGB value of the position corresponding to the interference pixel 12 of powder A, and eliminate such interference pixels;

6)利用图像处理软件Photoshop CS6主菜单“图像”模块中的“分析”、“记录测量”功能，获取步骤五的照片13中Ni元素像素总面积SA为6436；6) Utilize "analyze", "record measurement" function in image processing software Photoshop CS6 main menu "image" module to obtain Ni element pixel total area S A in the photo 13 of step 5 is 6436;

7)将主元素为Fe的能谱照片15导入图像处理软件Photoshop CS6，重复步骤5)和步骤6)，获取能谱照片15中Fe元素的像素总面积SB为21640；7) the main element is that the energy spectrum photo 15 of Fe is imported into the image processing software Photoshop CS6, repeating step 5) and step 6), and obtaining the total pixel area S B of Fe element in the energy spectrum photo 15 is 21640;

8)根据公式，代入表2所示的粉末A和粉末B的松装密度及平均颗粒直径，计算混合粉末的实测配比η为0.299；8) According to the formula, substitute the bulk density and average particle diameter of powder A and powder B shown in Table 2, and calculate the measured ratio η of the mixed powder to be 0.299;

表2Table 2

Figure BDA0002446495720000101
Figure BDA0002446495720000101

Figure BDA0002446495720000102
Figure BDA0002446495720000102

为了验证上述测试方法的效果，我们运用图像测量软件Digimizer逐一测量混合粉末实物彩色照片14中的粉末颗粒直径，换算体积求和后，计算得到混合粉末质量配比为0.312，与本实施例中得到的实测配比0.299进行比对，误差仅为4.3％。而显而易见，本发明中的测试方法比使用测量软件Digimizer逐一测量混合粉末实物彩色照片14中的粉末颗粒直径的方式快速便捷多，能够减少人力，提高工作效率。In order to verify the effect of the above test method, we use the image measurement software Digimizer to measure the diameter of the powder particles in the color photo 14 of the real mixed powder one by one. After converting the volume and summing up, the calculated mass ratio of the mixed powder is 0.312, which is the same as that obtained in this example. The measured ratio of 0.299 is compared, and the error is only 4.3%. Obviously, the testing method in the present invention is much faster and more convenient than using the measurement software Digimizer to measure the powder particle diameter in the color photo 14 of the actual mixed powder, which can reduce manpower and improve work efficiency.

结果表明，本发明所述的一种3D打印混合粉末配比实测方法有效，结果准确，效率高。The results show that the method for measuring the proportion of mixed powders for 3D printing in the present invention is effective, with accurate results and high efficiency.

以上所述实施例仅是为充分说明本发明而所举的较佳的实施例，本发明的保护范围不限于此。本技术领域的技术人员在本发明基础上所作的等同替代或变换，均在本发明的保护范围之内。本发明的保护范围以权利要求书为准。The above-mentioned embodiments are only preferred embodiments for fully illustrating the present invention, and the protection scope of the present invention is not limited thereto. Equivalent substitutions or transformations made by those skilled in the art on the basis of the present invention are all within the protection scope of the present invention. The protection scope of the present invention is subject to the claims.

Claims (10)

1. The actual measurement method for the ratio of the 3D printing mixed powder is characterized by comprising the following steps of:
step one, obtaining a sample with mixed powder, wherein the mixed powder comprises powder A and powder B;
step two, selecting the element E with the largest difference of chemical compositions of the powder A and the powder BAAnd EBWherein, element EAIs the main element of the powder A, element EBIs the main element of powder B;
step three, scanning the element energy spectrum surface of the sample surface through a scanning electron microscope, and setting an element E on a software interface attached to the energy spectrum analyzerAFor a first color, element E is setBA second color, the first color and the second color being three primary colors of two different colors;
step four, obtaining element E in the sample under the same view fieldAFIG. A shows the spectrum of the sampleBIn the spectrum fig. b and in the color picture fig. c, wherein the color picture fig. c simultaneously corresponds to the element EAAnd element EBColoring;
step five, judging whether the dust particles in the color photo figure FIG. C are completely colored, if so, entering step six; if not, adjusting the shooting position of the scanning electron microscope, selecting a neighboring area, and repeating the step four until the powder particles in the fig. C are completely colored;
step six, processing the energy spectrum photo fig. A through image processing software to obtain an element E in the energy spectrum photo fig. AATotal pixel area SAThe method specifically comprises the following steps:
s61, if powder B does not contain element EAPicking up and selecting the colored area in the energy spectrum photo fig. a until all non-background colors are selected, and utilizing record measurement in the image processing softwareFunction of obtaining the total area S of pixels of a colored regionA；
S62, if powder B contains element EAAll the colored areas in the energy spectrum fig. a are picked up and selected, after which the element E in the color photograph fig. c is taken as the basisBInterference pixels in the spectral photo Fig.A are removed corresponding to the positions of the powder particles, and the total pixel area S of the coloring area after the interference pixels are removed is obtained by utilizing the recording and measuring function in the image processing softwareA；
Step seven, processing the energy spectrum photo fig. B through image processing software to obtain an element E in the energy spectrum photo fig. BBTotal pixel area SBThe method specifically comprises the following steps:
s71, if powder A does not contain element EBPicking up and selecting the coloring area in the energy spectrum photo fig. B until all non-background colors are selected, and acquiring the total pixel area S of the coloring area by utilizing the recording measurement function in the image processing softwareB；
S72, if powder A contains element EBThen all the colored areas in the energy spectrum fig. b are picked up and selected, after which the element E in the colour photograph fig. c is taken as the basisAInterference pixels in the spectral photo Fig.B are removed corresponding to the positions of the powder particles, and the total pixel area S of the coloring area after the interference pixels are removed is obtained by utilizing the recording and measuring function in the image processing softwareB；
Step eight, calculating to obtain an actually measured mixture ratio η of the mixed powder;
Figure FDA0002446495710000021
where ρ isAApparent density of powder A, pBIs the apparent density of powder B, mAIs the total mass of powder A, mBIs the total mass of powder B, nANumber of particles of powder A in FIG. C, nBThe number of particles of powder B in fig. c,
Figure FDA0002446495710000022
is prepared from flourThe manufacturer of powder a provides the average diameter of the powder particles,
Figure FDA0002446495710000023
the average diameter of the powder particles, μ being the pixel scale,
Figure FDA0002446495710000024
Figure FDA0002446495710000025
2. the method for actually measuring the mixture ratio of the 3D printed mixed powder according to claim 1, wherein in S61, a color sampling pipette + is used to pick up a coloring area in a spectrum photo Fig.A.
3. The method for actually measuring the mixture ratio of the 3D printed mixed powder according to claim 1, wherein in S62, interference pixels in the spectrum photo Fig.A are picked and removed by using a color sampling straw- ".
4. The 3D printing mixed powder ratio actual measurement method according to claim 1, wherein the first step specifically comprises:
s11, fixing an acrylic plate on a workbench of the 3D printer, wherein a release film is arranged on the upper surface of the acrylic plate, and a double-sided adhesive layer and a liquid-state cycloaliphatic adhesive layer are sequentially arranged on the release film;
s12, loading the mixed powder into a powder feeding hopper of a 3D printer, opening the powder feeding hopper, keeping a laser beam closed, enabling a 3D printing laser nozzle to spray the powder towards the acrylic plate to obtain the acrylic plate covering the mixed powder layer, and then standing and cooling until the liquid epoxy resin glue is solidified;
and S13, sampling, cleaning and drying the mixed powder layer adhered to the acrylic plate to obtain a sample.
5. The method for actually measuring the mixture ratio of the 3D printing mixed powder according to claim 4, wherein in S12, the 3D printing laser nozzle is of a coaxial powder feeding type.
6. The 3D printing mixed powder ratio actual measurement method according to claim 1, wherein the image processing software is Photoshop.
7. The 3D printing mixed powder ratio actual measurement method according to claim 1, wherein the image processing software is FlauntR.
8. The 3D printing mixed powder ratio actual measurement method according to claim 1, wherein the energy spectrum photo FIG. A in the sixth step is a png lossless compression format picture.
9. The 3D printing mixed powder ratio actual measurement method according to claim 1, wherein the energy spectrum photo FIG. B in the seventh step is a png lossless compression format picture.
10. The method for actually measuring the mixture ratio of the 3D printed mixed powder according to claim 1, wherein in S71, a coloring area in a spectrum photo Fig.B is picked up by using a color sampling pipette +; in S72, a color sampling pipette is used to pick up and remove interfering pixels in the spectral photo fig.
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