CN109856042A - The overall corrosion resistance detection method of SLM shaped metal articles - Google Patents
The overall corrosion resistance detection method of SLM shaped metal articles Download PDFInfo
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- CN109856042A CN109856042A CN201910134269.1A CN201910134269A CN109856042A CN 109856042 A CN109856042 A CN 109856042A CN 201910134269 A CN201910134269 A CN 201910134269A CN 109856042 A CN109856042 A CN 109856042A
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Abstract
The present invention relates to a kind of overall corrosion resistance detection methods of SLM shaped metal articles, the sample of representative products Different Plane has been made in this method simultaneously in SLM forming process, then working electrode is respectively prepared in these samples and tests its polarization curve using electrochemical workstation, and then the corrosion resistance of SLM metal product entirety can be evaluated.For this method without destroying product, testing cost is low, takes a short time, each sample can inside more accurate reactor product Different Plane corrosion resistance, it is as a result more accurate and reliable, be particularly suitable for the non-destructive testing of small size and complicated shape product.
Description
Technical field
The present invention relates to non-destructive testing and technical field of metal anti-corrosion, and in particular to a kind of SLM shaped metal articles it is whole
Body corrosion resistance lossless detection method.
Background technique
Selective laser melting (Selective Laser Melting, SLM) is a kind of advanced increases material manufacturing technology,
The technology passes through the laser melted alloy powder of high-energy density, can obtain the metal product of various shape and purposes.In reality
In the application of border, the stainless steel products such as 40Cr13 of SLM production have mechanical performance good enough, and using traditional preparation methods
Molding similar product is compared, and mechanical performance quite or is slightly promoted, and is very suitable for industrial application.
Can the corrosion resistance of stainless steel be to evaluate its important indicator that be applied to actual production.Corrosion resistance
Depend primarily on the factors such as whether surface topography, phase composition and institutional framework uniform of material.Not using the preparation of SLM technology
Rust Steel material has biggish difference with using the molding congruent stainless steel material of traditional approach.Firstly, SLM using laser at
Type makes that structural constituent and phase composition is caused there are obvious cladding road to have more apparent inhomogeneities in product；Its
Secondary, there are holes and aperture for the stainless steel product of SLM preparation.Hole, phase composition and structural constituent are that influence stainless steel product is resistance to
The key factor of corrosion energy.Therefore, it is produced using the stainless steel product of SLM technology preparation and using the stainless steel of traditional approach preparation
Product corrosion resistance is different.Currently, the corrosion resisting property to such product still lacks systematic research, there is an urgent need to new assessments
Standard and detection method.
It mainly include at present salt spray test, ferric trichloride examination for the corrosion resisting property assessment of stainless steel product, detection method
It tests.For the product of SLM preparation, these test methods have both sides to limit to: on the one hand, these test methods all belong to
In destructive testing, needs to prepare certain size and a number of sample is detected.In view of the product of SLM preparation is usual
Size is smaller, and product, based on customizing, output is generally limited pieces even single-piece, therefore traditional corrosion resisting property is commented
Method is estimated for SLM stainless steel product and is not suitable for, and time cost and economic cost are higher, it is difficult to realize；On the other hand, it passes
The each position of sample obtained by controlling Preparation Method is often uniform, and the characteristics of SLM technique make product in Z-direction there are one
Fixed phase constituent and porosity difference, cause corrosion resistance in this direction also to be had any different.For single-piece SLM product, need
It to be tested multiple positions are separately sampled, comprehensive corrosion resistance assessment result can be obtained.
Inventor team discloses a kind of corrosion resistance test method (CN107121377A) not long ago, using leaching
There is both sides limitation in actual operation in bubble method.The cylindrical body that this method needs to prepare diameter 10mm height 5mm first tries
Sample, specimen size is larger, there is a problem of that sample preparation difficulty is larger for small size SLM product, especially internal tool
Suitable infusion method sample can not be prepared substantially by having the SLM product of labyrinth, cause assessment reliability insufficient.Secondly, leaching
Bubble method is difficult to provide the scientific explarnation of corrosion mechanism, is not easy to the corrosion resistance that later period improvement improves product.
Shu Mingyong et al. (CN108548775A) discloses a kind of enamel coating corrosion resistance test method, and this method is first
Electrode is made in enamel coating, then its polarization curve is tested using electrochemical methods in etchant solution, calculates corrosion
Current potential and corrosion electric current density, finally obtain corrosion rate.This method is similar with above-mentioned conventional method, also belongs to destructive examination
It tests, needs to prepare certain size and a number of sample in advance, between layers and non-uniform SLM stainless steel product
And it is not suitable for.
The present invention is further improved innovation on the basis of summarizing and absorbing aforementioned various method advantages, successfully has developed one
The new SLM shaped metal articles overall corrosion resistance lossless detection method of kind.
Summary of the invention
It is not suitable for molding metal product of SLM etc. it is an object of the invention to solving existing corrosion resistance detection method to ask
Topic, creative develops a kind of corrosion resistance comprehensive assessment detection method for being exclusively used in such product.This method can be in SLM
The corrosion-resistant detection sample that each selected layer is obtained while shaped metal articles, recycles it to measure the corrosion resistance of each layer
Can, and then obtain the corrosion resistance of entire SLM metal product.It to achieve the above object, is technical solution used by invention
It is as follows:
The overall corrosion resistance detection method of the molding metal product of SLM, specifically includes the following steps:
(a) three-dimensional structure for designing SLM metal product, is reserved a certain number of on the selected layer periphery of SLM metal product
Detect sample forming layer；
(b) SLM is formed, while the detection sample for obtaining metal product and being attached thereto；
(c) detection sample is connected with conducting wire after pretreatment, then insulation-encapsulated obtains detection sample working electrode；
(d) it will test sample working electrode, saturated calomel electrode, platinum electrode to be connected with electrochemical workstation, composition closure connects
All electrodes are placed in electrolyte solution by logical three-electrode system, obtain the polarization curve of detection sample, assess SLM gold accordingly
Belong to the corrosion resistance of product entirety.
Further, the selected layer includes the top layer, bottom and several middle layers of SLM metal product.
Further, the detection sample is rectangle or thin rounded flakes, with a thickness of 1-5mm.
Further, each selected layer at least forms 3 detection samples.
Further, the pretreatment includes cleaning, dry etc..
Further, using the upper surface for detecting sample as working face, pretreated detection sample bottom surface is connected the line to, so
Insulation package is carried out to detection sample with insulating materials afterwards, guarantees that upper surface (working face) is in exposed state, then to working face
It is polished.
Further, the electrolyte solution is specially the sodium-chloride water solution of mass fraction 1%-5%.
Further, the temperature of electrolyte solution is 20-40 DEG C, scanning range -1V to 1V when electro-chemical test, scanning speed
Rate 0.3mV/s-1.0mV/s.
Further, the material of the molding metal product of the SLM is martensitic stain less steel, ferritic stainless steel, Ovshinsky
Any one in the stainless steel products such as body stainless steel, austenite-ferrite (two-phase) stainless steel, precipitation-hardening stainless steel,
The typical trade mark includes Cr13 type, such as 20Cr13,30Cr13,40Cr13.
Further, obtain detection sample polarization curve after, look first at detection sample working face corrosion pore quantity and
Size, (corrosion hole is smaller and quantity is fewer, then its corrosion resistance is got over for the corrosion resistance of visual assessment SLM metal product
It is good)；Then the size and variation of corrosion potential and corrosion current in polarization curve, further accurate judgement SLM are compared in analysis
The corrosion resistance of metal product (it is smaller that corrosion potential gets over high corrosion electric current, shows that its corrosion resistance is stronger)；Last root
The corrosion resistance of SLM metal product is determined according to the passivation section in polarization curve.If not being passivated section, not will form
Passivating film shows that its corrosion resistance is poor；It is on the contrary then corrosion resistance is preferable.
Compared with prior art, the invention has the following advantages: (1) also obtains while SLM shaped metal articles
A series of anti-corrosion detection samples are arrived, the ingredient of these samples is identical as the ingredient of metal product in same plane, can be more
Accurately react the corrosion resistance of metal product at its place plane；(2) non-destructive testing, without destroying SLM in detection process
Molding metal product can significantly save testing cost, shorten detection time, accurately can detect and evaluate comprehensively SLM molding
The corrosion resistance of metal product；(3) detection specimen size is flexibly adjustable, significantly less than ruler required by traditional means of experiment
Very little, detection method is quick, evaluation index multiplicity, as a result more accurate and reliable.
Detailed description of the invention
Fig. 1 is the molding metal product of SLM of the present invention and detection spline structure schematic diagram；
Fig. 2 is the detection sample material object photo that the embodiment of the present invention 1 obtains；
Fig. 3 is the photo in kind after the detection sample connecting wire that the embodiment of the present invention 1 obtains；
Fig. 4 is the photo in kind that the detection sample that the embodiment of the present invention 1 obtains becomes working electrode after insulation-encapsulated；
Fig. 5 is the polarization curve comparison diagram that the embodiment of the present invention 1 obtains.
Specific embodiment
To make those of ordinary skill in the art fully understand technical solution of the present invention and beneficial effect, below in conjunction with specific
Embodiment is further described.
As shown in Figure 1, the three-dimensional data for detecting sample for designing stainless steel product first and being attached thereto.In Z axis (height
Or thickness direction) X-Y plane of coordinate highest point chooses that 1 group of sample is 3 (top surface) total, the X-Y plane for being 0 in Z axis coordinate
It is 3 (bottom surface) total to choose 1 group of sample.It can also be according to stainless steel product Z axis altitudes (thickness or height be larger), in Z axis
Several (such as 1-5) X-Y planes are equidistantly chosen in direction, and each plane increases by 1 group of corrosion-resistant detection sample.The length and width phase of sample
Together, with a thickness of 3mm.After designing, SLM molding is carried out by raw material of 40Cr13 powder of stainless steel, respectively obtains stainless steel product
Sample as shown in Figure 2 with several has marked the Z axis numerical value of each group sample working face.During this period using same
The sample of same size has been prepared with conventional casting methods for 40Cr13 material, as control.
The upper surface of every group of sample is set to working face, each group sample is cleaned by ultrasonic and is dried, with being about 30cm
Conducting wire be connected with the back side of each sample, and (as shown in Figure 3) is fixed with conductive tape.Then it is tested with multimeter true
It protects conducting wire and sample connectivity is good, then use A-B glue (epoxy resin) by sample wrapping and encapsulating, it is ensured that expose the work of sample
Face and the conducting wire other end, thus assembling obtains working electrode, as shown in Figure 4.
The working face of sample is polished and cleaned up.The sodium-chloride water solution that mass fraction is 3.5% is prepared, is used
Water-bath keeps constant temperature after being heated to 25 DEG C.The conductor wire end of sample is connect with electrochemical workstation, and ensures the work of sample
Face is immersed in sodium-chloride water solution, then respectively connect saturated calomel electrode and platinum electrode with electrochemical workstation, is formed
The three-electrode system of one closed communicating.It is scanned in the scanning range of -1V to 1V with the sweep speed of 0.33mV.Same
Electrochemical Scanning is carried out using control sample under the conditions of sample, acquired results are as shown in Figure 5.
In Fig. 5, it is slightly below using the stainless steel sample corrosion potential of SLM preparation and uses the stainless of conventional casting methods preparation
Steel curved beam, this illustrates that its corrosion resistance is relatively poor, but entirely different by the corrosion mechanism of the visible the two of polarization curve.Tradition
Cast stainless steel product is scanned across after corrosion potential the sample surfaces oxidation behind this section of section there are one section of passivation section
Film rupture, corrosion process aggravation；And SLM preparation stainless steel product there is no passivation section, self-corrosion start after always with one
A more stable rate is corroded, and the stainless steel sample for being primarily due to SLM preparation is at laser welding and stainless steel
Expect the compound corrosion process of itself.
Claims (10)
- The overall corrosion resistance detection method of 1.SLM shaped metal articles, which is characterized in that method includes the following steps:(a) three-dimensional structure for designing SLM metal product, reserves a certain number of detections on the selected layer periphery of SLM metal product Sample forming layer；(b) SLM is formed, while the detection sample for obtaining metal product and being attached thereto；(c) detection sample is connected with conducting wire after pretreatment, then insulation-encapsulated obtains detection sample working electrode；(d) sample working electrode, saturated calomel electrode, platinum electrode be will test to be connected with electrochemical workstation, form closed communicating All electrodes are placed in electrolyte solution by three-electrode system, obtain the polarization curve of detection sample, and comprehensive assessment SLM metal produces The corrosion resistance of product entirety.
- 2. detection method as described in claim 1, it is characterised in that: the selected layer includes the top layer of SLM metal product, bottom Layer and several middle layers.
- 3. detection method as described in claim 1, it is characterised in that: the detection sample be rectangle or thin rounded flakes, with a thickness of 1-5mm。
- 4. detection method as described in claim 1, it is characterised in that: each selected layer at least forms 3 detection samples.
- 5. detection method as described in claim 1, it is characterised in that: step (c) pretreatment includes cleaning, drying.
- 6. detection method as described in claim 1, it is characterised in that: to detect the upper surface of sample as working face in step (c), Pretreated detection sample bottom surface is connected the line to, insulation package then is carried out to detection sample with insulating materials, guarantees work Face is in exposed state, then polishes to it.
- 7. detection method as described in claim 1, it is characterised in that: step (d) electrolyte solution is mass fraction The sodium-chloride water solution of 1%-5%.
- 8. detection method as described in claim 1, it is characterised in that: the temperature of electrolyte solution when step (d) electro-chemical test Degree is 20-40 DEG C, scanning range -1V to 1V, sweep speed 0.3mV/s-1.0mV/s.
- 9. detection method as described in claim 1, it is characterised in that: the material of the SLM shaped metal articles is selected from geneva It is body stainless steel, ferritic stainless steel, austenitic stainless steel, austenite-ferrite stainless steel, any in precipitation-hardening stainless steel It is a kind of.
- 10. detection method as described in claim 1, it is characterised in that: first after step (d) obtains the polarization curve of detection sample The corrosion hole quantity and size of first observation detection sample working face, thus the corrosion resistance of visual assessment SLM metal product: rotten Borrosion hole hole is smaller and quantity is fewer, then its corrosion resistance is better；Then corrosion potential and corruption in polarization curve are compared in analysis Lose the size and variation of electric current, the corrosion resistance of further accurate judgement SLM metal product: corrosion potential gets over high corrosion electricity It flows smaller, shows that its corrosion resistance is stronger；The corrosion resistant of SLM metal product is finally determined according to the passivation section in polarization curve Corrosion energy: if not being passivated section, show that its corrosion resistance is poor；It is on the contrary then corrosion resistance is preferable.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112649353A (en) * | 2021-01-05 | 2021-04-13 | 广东龙丰精密铜管有限公司 | Method for testing formic acid corrosion resistance of TU copper pipe for air conditioning refrigeration |
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Application publication date: 20190607 |