CN109916941B - 3D printing separation detection method for premixed powder - Google Patents
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Abstract
The invention discloses a 3D printing separation detection method for premixed powder, which adopts an acrylic plate with a release film when powder is collected, and is matched with a double-sided adhesive tape and a colorless and transparent epoxy resin adhesive, so that the problem that a detection result is interfered by surface sample wrinkles during sampling is solved, the mixed powder layer is sampled and subjected to element energy spectrum surface scanning, the actual proportion of the mixed powder is calculated according to an energy spectrum color chart obtained by scanning, and whether the powder is separated or not is judged according to the actual proportion. The invention can effectively solve the technical problem that the 3D printing separation of premixed powder with the same color, similar apparent density and similar particle size cannot be detected, ensures the component proportion of the material, and has simple operation and easy implementation.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to a 3D printing separation detection method for premixed powder.
Background
With the continuous rising of energy and power requirements in China, the extreme development of service conditions of major equipment becomes a trend. The functional gradient material is characterized in that the material components and the macroscopic performance of the functional gradient material are in continuous and uniform gradient change in spatial position, overcomes the defects of stress concentration and microcracks of the traditional composite material, and can meet the requirements of different parts of major equipment on different performances.
The laser 3D printing realizes the gradient change of material performance by controlling the mass ratio of the premixed powder, and is an important method for preparing the functionally gradient material. However, due to different powder qualities and particle diameters, the premixed powder is separated under high-speed jetting of laser 3D printing, which causes deviation of material components, resulting in reduced material use performance and failure to meet design requirements. Therefore, whether the mixed powder is separated after being sprayed at a high speed by the 3D printing nozzle or not is detected and judged, the premise of accurately controlling the powder quality ratio is provided, and the key point for ensuring the performance of the functional gradient material is provided.
Therefore, the research on the powder separation detection is carried out by the scientific and technical workers at home and abroad. Chinese patent publication No. CN105486705B provides a method for quantitatively analyzing components of a powder mixture, which obtains scores of a powder to be measured and each standard powder through an X-ray diffraction spectrum of the standard powder, establishes a score map, and obtains a mass percentage of the powder according to a lever law formula for absorption coefficient correction.
At present, accurate detection of 3D printing premixed powder with the same color, similar apparent density and similar particle size cannot be realized.
Disclosure of Invention
The invention aims to provide a 3D printing separation detection method for premixed powder, which solves the problem that 3D printing separation of premixed powder with the same color, similar apparent density and similar particle size cannot be detected, and is simple to operate and easy to implement.
In order to solve the technical problem, the invention provides a premixed powder 3D printing separation detection method, which comprises the following steps:
uniformly mixing the powder a and the powder b according to a preset proportion k to obtain mixed powder, and filling the mixed powder into a powder feeding hopper of a 3D printer; wherein the predetermined ratio k is greater than 0;
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 epoxy resin adhesive layer are sequentially arranged on the release film;
step three, opening the powder feeding hopper, keeping the laser beam closed, enabling a 3D printing laser nozzle to spray powder towards the acrylic plate and move to obtain the acrylic plate covering the mixed powder layer, and then standing and cooling until the liquid epoxy resin glue is solidified;
step four, marking a 1 cm-1 cm sample area on the release film on the acrylic plate by using a cutting machine, uniformly uncovering and tearing off the release film in the sample area from the acrylic plate by using a tool tip to obtain a sample with a smooth mixed powder layer;
step five, pasting the sample on a sample substrate of a scanning electron microscope, and after spraying gold, scanning the surface of the sample by using the scanning electron microscope to obtain an energy spectrum color chart;
analyzing and testing the energy spectrum color chart, counting and calculating the average diameter of the powder a and the powder b in the energy spectrum color chart by using graph measurement software, and calculating to obtain the actual ratio eta of the powder a to the powder b:
where ρ isaApparent density of powder a, pbIs the bulk density of the powder b,
the average diameter of the powder a in each diameter range on the energy spectrum color chart is represented respectively; m1 and M2 … … Mn respectively represent the number of particles of the powder a in each diameter range,
respectively representing the average diameter of the powder b in each diameter range on the energy spectrum color chart, respectively representing the number of the particles of the powder b in each diameter range by N1 and N2 … … Nn, and eta is the actual mixture ratio of the mixed powder;
step seven, judging the size of eta, if the eta belongs to [ k-0.05, k +0.05], enabling the mixed powder not to be separated after being sprayed by a 3D printing laser nozzle; on the contrary, the mixed powder is separated.
Preferably, in the third step, the laser nozzle performs s-shaped reciprocating motion.
Preferably, in the first step, the powder a and the powder b are mixed for 30-60min using a ball mill to be uniformly mixed.
Preferably, the image measurement software is Digmizer.
Preferably, in the second step, a double-sided adhesive layer and a liquid epoxy resin adhesive layer are sequentially arranged on the release film, and the method specifically comprises the following steps:
sticking a double-sided adhesive layer on the release film;
and uniformly coating a colorless and transparent liquid epoxy resin adhesive layer on the double-sided adhesive layer, wherein the thickness of the liquid epoxy resin adhesive layer is less than or equal to 1 mm.
Preferably, in the third step, the perpendicular distance between the 3D printing laser nozzle and the surface of the acrylic plate is not more than 20 cm.
Preferably, in step five, the element spectral surface scanning only scans the elements with the highest content, and the magnification of the spectral color map is not more than 200 times.
The invention has the beneficial effects that:
1. the invention provides a 3D printing separation detection method for premixed powder, which is characterized in that an acrylic plate with a release film, a double-sided adhesive tape and an epoxy resin adhesive are adopted during powder collection, mixed powder is collected through the epoxy resin adhesive, then the release film is uncovered, and a sample with a mixed powder layer is obtained, so that the powder sample is rapidly collected, and the method is convenient and practical.
2. According to the invention, the acrylic plate with the release film is used, and the flatness of the release film on the acrylic plate is high, so that a mixed powder layer collected at the later stage is flat, and the experimental result is more accurate.
3. The method is suitable for 3D printing separation detection of premixed powder with the same color, similar apparent density and similar particle size, and can quickly judge whether the premixed powder is separated, so that the component proportion of the functional gradient material is ensured, and later adjustment is facilitated.
4. According to the invention, the premixed powder is directly bonded and solidified on the epoxy resin adhesive, the actual mass ratio of the heterogeneous mixed powder is accurately calculated by scanning analysis of the scanning electron microscope element energy spectrum and combining with powder particle image recognition and measurement, and whether the powder is separated or not is judged according to the actual mass ratio, so that the method is simple.
5. The invention has low requirement on the quality of the service of the detection personnel, and has simple operation and easy implementation.
Drawings
FIG. 1 is a schematic view of the powder collection of the present invention;
FIG. 2 is a schematic diagram showing the morphology of pre-mixed powders of the present invention having the same color, similar bulk density and similar particle size after spraying;
FIG. 3 is a schematic plan scan of the elemental spectra of the premixed powders of the present invention. Wherein 10 is one powder and 11 is the other powder.
The reference numbers in the figures illustrate: 1. powder feeding hopper, 2, powder pipe, 3, coaxial optical internal powder feeding laser head, 4, epoxy resin glue, 5, double faced adhesive tape, 6, acrylic plate, 7, powder feeding track, 8, workbench, 9 and mixed powder.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
The invention discloses a 3D printing separation detection method for premixed powder, which comprises the following steps:
uniformly mixing the powder a and the powder b according to a preset proportion k to obtain mixed powder, and filling the mixed powder into a powder feeding hopper of a 3D printer; wherein the predetermined ratio k is greater than 0, and the powder a and the powder b are two different powders;
in this step, the powder a and the powder b are mixed using a ball mill for 30 to 60min to be uniformly mixed.
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 epoxy resin adhesive layer are sequentially arranged on the release film;
in this step, set gradually double-sided adhesive layer and liquid epoxy glue film on leaving the type membrane, specifically include:
sticking a double-sided adhesive layer on the release film;
and uniformly coating a colorless and transparent liquid epoxy resin adhesive layer on the double-sided adhesive layer, wherein the thickness of the liquid epoxy resin adhesive layer is less than or equal to 1 mm.
Step three, opening the powder feeding hopper, keeping the laser beam closed, enabling a 3D printing laser nozzle to spray powder towards the acrylic plate and move to obtain the acrylic plate covering the mixed powder layer, and then standing and cooling until the liquid epoxy resin glue is solidified;
in the step, the laser nozzle does s-shaped reciprocating motion.
In the step, the vertical distance between the 3D printing laser nozzle and the surface of the acrylic plate is not more than 20 cm.
In this step, the two powders are not melted together in the laser beam off state, which facilitates subsequent observation.
Step four, marking a 1 cm-1 cm sample area on the release film on the acrylic plate by using a cutting machine, uniformly uncovering and tearing off the release film in the sample area from the acrylic plate by using a tool tip to obtain a sample with a smooth mixed powder layer;
step five, pasting the sample on a sample substrate of a scanning electron microscope, and after spraying gold, scanning the surface of the sample by using the scanning electron microscope to obtain an energy spectrum color chart;
in the step, the element energy spectrum surface scanning only scans the elements with the highest content, and the magnification of the energy spectrum color chart is not more than 200 times.
Analyzing and testing the energy spectrum color chart, and enabling powder particles of the energy spectrum color chart to be equivalent to a spherical shape, wherein spherical equivalent statistics is conducted on incomplete powder at the edge of the image, and the method specifically comprises the following steps: if the area of the powder at the edge of the image in the image sheet exceeds 1/2, the powder is marked as 1 powder; if the area in the picture is more than 1/4 and less than 1/2, the number of the powder is marked as 0.5; if the area in the picture is less than 1/4, marking as 0 powder;
counting and calculating the average diameter of the powder a and the powder b in the energy spectrum color chart by using a graph measurement software, and calculating to obtain the actual ratio eta of the powder a to the powder b:
where ρ isaApparent density of powder a, pbIs the bulk density of the powder b,
respectively represent energyThe average diameter of the powder a in each diameter range on the spectrum color chart; m1 and M2 … … Mn respectively represent the number of particles of the powder a in each diameter range,
respectively representing the average diameter of the powder b in each diameter range on the energy spectrum color chart, respectively representing the number of the particles of the powder b in each diameter range by N1 and N2 … … Nn, and eta is the actual mixture ratio of the mixed powder;
in this step, the image measurement software is Digmizer or other measurement software.
Step seven, judging the size of eta, if the eta belongs to [ k-0.05, k +0.05], enabling the mixed powder not to be separated after being sprayed by a 3D printing laser nozzle; on the contrary, the mixed powder is separated.
In the invention, the diameter D of a laser spot emitted by the laser nozzle is less than or equal to 10 mm.
Aiming at the Ni-Fe functional gradient material at the supporting position of the rotor IN the cylinder body of the million kilowatt nuclear turbine produced by Shanghai electric group Shanghai steam turbine plant, the method provided by the invention is applied, the material a is selected to be IN625 nickel powder, the material b is selected to be 304L iron powder, and when the design mass ratio k is 1:1, whether the premixed powder is separated after being sprayed by a 3D printing laser head is judged.
The method for separating and detecting the premixed powder is applied, please refer to the attached figures 1, 2 and 3, and the specific steps are as follows:
1) respectively weighing IN625 nickel powder and 304L iron powder by an electronic balance with the precision of 0.01g according to the mass ratio of 1:1 (500 g each), then respectively cleaning and drying the powder by using an ultrasonic cleaner and a drying box, then putting the weighed, cleaned and dried two kinds of powder into a ball mill for mixing for 60 minutes, and taking out and putting the powder into a hopper 1 of a 3D printing powder feeder after the powder mixing is finished;
2) fixing an acrylic plate 6 with a release film on a 3D printing workbench 8, adhering a double-sided adhesive tape 5 on the surface of a thin plate 6, then pouring colorless and transparent epoxy resin A adhesive and B adhesive into a 240ml transparent disposable plastic cup (the plastic cup does not chemically react with epoxy resin) according to the proportion of 2:1, uniformly mixing the two adhesives by using a stirring rod, tearing off the surface layer of the double-sided adhesive tape, uniformly coating epoxy resin 4 on the surface of the double-sided adhesive tape by using a flat brush with the width of 5mm, and controlling the thickness of the adhesive not to exceed 1 mm;
3) programming an industrial mechanical arm provided with a 3D printing laser nozzle 3, setting the length L of a moving track 7 to be 0.5m, adjusting the powder feeding rate to be 8g/min, the scanning speed to be 8mm/s, setting the vertical distance (the spraying distance) between the laser nozzle and the surface of an acrylic plate to be 18.5mm (not more than 20mm) as shown in figure 1, then opening an argon and powder feeder hopper 1, keeping a laser beam closed, moving the laser beam according to the preset track 7 to be 0.5m, spraying mixed powder 9 onto the acrylic plate 6 adhered with epoxy resin glue 4 through a powder pipe 2, and then placing the acrylic sheet 6 adhered with the powder in a shade for drying as shown in figure 2 until the liquid epoxy resin glue 4 is completely cured;
4) aiming at the mixed powder adhered on the acrylic plate 6, a cutting machine matched with a cutter is used for cutting 1cm to 1cm, and then the release film below the powder is uniformly uncovered and torn off from the acrylic plate by a cutter tip, so that the release film is ensured not to wrinkle in the process;
5) pasting the bottom surface of the release film adhered with the mixed powder on a sample substrate of a scanning electron microscope, placing the release film on an E-1010 gold spraying instrument for spraying gold for 3-4 minutes, placing the release film into the scanning electron microscope for surface scanning energy spectrum analysis to obtain a main element energy spectrum color chart, and determining the powder particle category in the color chart, wherein the specific steps are as follows:
5.1) correcting parameters such as voltage value, magnification factor, focusing, astigmatism, brightness, contrast and the like, observing and photographing the area to be measured in the powder sample by 100 times (not more than 200 times), and storing pictures;
5.2) eliminating the interference of Au, Cr, Mn and other elements, selecting Fe and Ni as main elements, marking the Fe element as green and the Ni element as blue. Finally, determining 304L of iron powder 10 and IN625 nickel powder 11 particles, and storing a spectral surface color scanning map;
6) respectively counting the number of two powder particles in the energy spectrum color chart, measuring the diameters of the two powder particles in the color chart by using measurement software, calculating the average diameter of the two powder particles, and calculating the actual mixture ratio of the mixed powder to be 0.904, wherein the specific steps are as follows:
6.1) as shown in FIG. 3, the powder particles of the energy spectrum color chart are equivalent to be spherical, wherein, the spherical equivalent statistics is carried out on the incomplete powder at the edge of the image, specifically: if the area of the powder at the edge of the image in the image sheet exceeds 1/2, the powder is marked as 1 powder; if the area in the picture is more than 1/4 and less than 1/2, the number of the powder is marked as 0.5; if the area in the map is less than 1/4, neglecting and marking as 0;
6.2) opening Digimizer measurement software, clicking a spectral surface scanning map, and setting a reference scale mu; selecting a length tool, and selecting 304L powder 10 with red line measurement counting as L1 and L2 … L5 respectively IN the ranges of 0-20 μm, 20-40 μm, 40-60 μm, 60-80 μm and more than 80 μm and selecting S1 and S2 … S5 respectively IN the range of 0-20 μm, 20-40 μm, 40-60 μm, 60-80 μm and more than 80 μm and selecting yellow line measurement counting IN625 powder 11 according to the powder counting principle of the step 6.1); therefore, the actual particle diameters of the 304L iron powder 10 and the IN625 nickel powder 11 are:
wherein A isiIs 304L of iron powder particle diameter, BiThe IN625 nickel powder particle diameter;
6.3) counting the number of the two powders in the ranges of 0-20 μ M, 20-40 μ M, 40-60 μ M, 60-80 μ M and more than 80 μ M, respectively, and recording as M1, M2 … M5, N1 and N2 … N5, and calculating the average value of the powder diameter in each range
And
6.4) the mass of the 304L powder and the IN625 powder was calculated from the mass formula and the average value obtained IN step 6.3), and the mass percentages of the two powders were calculated as shown IN Table 1.
Wherein rho a and rho b respectively represent the loose packing densities of a metal powder and b metal powder; eta is the actual proportion of the mixed powder; the mass ratio of nickel powder to iron powder is calculated in Table 1.
TABLE 1
7)
It indicates that the mixed powder is separated after being sprayed by the 3D printing laser head.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (7)
1. A premixed powder 3D printing separation detection method is characterized by comprising the following steps:
uniformly mixing the powder a and the powder b according to a preset proportion k to obtain mixed powder, and filling the mixed powder into a powder feeding hopper of a 3D printer; wherein the predetermined ratio k is greater than 0;
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 epoxy resin adhesive layer are sequentially arranged on the release film;
step three, opening the powder feeding hopper, keeping the laser beam closed, enabling a 3D printing laser nozzle to spray powder towards the acrylic plate and move to obtain the acrylic plate covering the mixed powder layer, and then standing and cooling until the liquid epoxy resin glue is solidified;
step four, marking a 1 cm-1 cm sample area on the release film on the acrylic plate by using a cutting machine, uniformly uncovering and tearing off the release film in the sample area from the acrylic plate by using a tool tip to obtain a sample with a smooth mixed powder layer;
step five, pasting the sample on a sample substrate of a scanning electron microscope, and after spraying gold, scanning the surface of the sample by using the scanning electron microscope to obtain an energy spectrum color chart;
analyzing and testing the energy spectrum color chart, counting and calculating the average diameter of the powder a and the powder b in the energy spectrum color chart by using graph measurement software, and calculating to obtain the actual ratio eta of the powder a to the powder b:
where ρ isaApparent density of powder a, pbIs the bulk density of the powder b,
the average diameter of the powder a in each diameter range on the energy spectrum color chart is represented respectively; m1 and M2 … … Mn respectively represent the number of particles of the powder a in each diameter range,
respectively representing the average diameter of the powder b in each diameter range on the energy spectrum color chart, respectively representing the number of the particles of the powder b in each diameter range by N1 and N2 … … Nn, and eta is the actual mixture ratio of the mixed powder;
step seven, judging the size of eta, if the eta belongs to [ k-0.05, k +0.05], enabling the mixed powder not to be separated after being sprayed by a 3D printing laser nozzle; on the contrary, the mixed powder is separated.
2. The premixed powder 3D printing separation detection method as claimed in claim 1, wherein the laser nozzle performs s-shaped reciprocating motion in step three.
3. The premixed powder 3D printing separation detecting method as claimed in claim 1, wherein in the first step, the powder a and the powder b are mixed for 30-60min using a ball mill to be uniformly mixed.
4. The premixed powder 3D printing separation detection method of claim 1 wherein the graphic measurement software is Digmizer.
5. The premixed powder 3D printing separation detection method according to claim 1, wherein in the second step, a double-sided adhesive layer and a liquid epoxy resin adhesive layer are sequentially disposed on the release film, and specifically comprises:
sticking a double-sided adhesive layer on the release film;
and uniformly coating a colorless and transparent liquid epoxy resin adhesive layer on the double-sided adhesive layer, wherein the thickness of the liquid epoxy resin adhesive layer is less than or equal to 1 mm.
6. The premixed powder 3D printing separation detection method of claim 1, wherein in step three, the perpendicular distance between the 3D printing laser nozzle and the surface of the acrylic plate is not more than 20 cm.
7. The premixed powder 3D printing separation detection method of claim 1, wherein in step five, the elemental energy spectrum surface scan scans only the elements with the highest content, and the magnification of the energy spectrum color chart is not more than 200 times.
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