CN113176204B - Detection method and pretreatment method for interface bonding state of deposition unit and substrate - Google Patents
Detection method and pretreatment method for interface bonding state of deposition unit and substrate Download PDFInfo
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- CN113176204B CN113176204B CN202110484755.3A CN202110484755A CN113176204B CN 113176204 B CN113176204 B CN 113176204B CN 202110484755 A CN202110484755 A CN 202110484755A CN 113176204 B CN113176204 B CN 113176204B
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Abstract
The invention discloses a method for detecting the interface bonding state of a deposition unit and a substrate and a pretreatment method thereof, belonging to the technical field of interface bonding state detection. The pretreatment method comprises the following steps: the adhesive is coated on the deposition unit on the surface of the substrate, and the adhesive and at least part of the deposition unit are peeled from the surface of the substrate together under the action of external force, so that the peeling section is exposed for detection. The method can expose the combined fracture surface of the deposition unit and the surface of the substrate, and further can completely represent the most original, basic and important formation information of the coating. The corresponding detection method is simple to operate, low in cost and high in practicability, can quickly and accurately obtain the two-dimensional combination information of the deposition unit and the substrate interface, is complete and accurate in information quantity, and has important significance for the research of the spraying coating technology, the further improvement of the combination strength between the coating and the substrate interface and the optimization of the performance of the coating.
Description
Technical Field
The invention relates to the technical field of interface combination state detection, in particular to a method for detecting the interface combination state of a deposition unit and a substrate and a pretreatment method thereof.
Background
Spraying, such as gas atomization spraying, thermal spraying, cold spraying and the like, is a method for obtaining required surface properties (including corrosion resistance, wear resistance, oxidation resistance, high temperature resistance, electric conduction, heat conduction, magnetic conduction and the like) by preparing a coating on the surface of a part after surface treatment so as to change the shape, chemical components, tissue structure and stress state of the surface of the part. The service performance of the parts can be greatly improved only by preparing a layer of functional coating with the thickness of several micrometers to several millimeters on the surface of the body material, and the parts can be endowed with new functions which are not possessed by the parts.
The coating formation, such as thermal spraying, cold spraying and the like, is usually carried out by heating a certain linear or powdery material to a molten or semi-molten state (or directly accelerating in a solid state) by a flame, electric arc or plasma heat source, and depositing the material on the surface of the component through acceleration, collision and solidification in the form of a single deposition unit. So as to strengthen (such as wear resistance, corrosion resistance and the like), energize (electric conduction, heat conduction, magnetic conduction, optics and the like) or regenerate (perform size recovery on the oversize parts) the parts. The technology is widely applied to almost all industrial fields such as aerospace, aviation, metallurgy, machinery, papermaking, petrochemical industry, household appliances and the like.
The bonding strength between the coating and the part is an important evaluation index for abnormal coating quality, the performance, service safety and service life of equipment parts are directly influenced, the bonding strength between the coating and a substrate interface is further improved, the protective performance of the coating is optimized, and the service life of the coating is prolonged, so that the preparation of the coating faces an important challenge.
The coating is formed by stacking a large number of sprayed particles flying at high speed impacting a substrate layer by layer, and the research on the combination state of a single deposition unit is extremely important for optimizing the final combination performance of the whole coating. The behavior of the unit particles after colliding with the substrate is a topic of great concern to relevant scholars, and includes the influence of preparation conditions on the morphology of the particles of the deposition unit, the influence of the preheating temperature of the substrate on the morphology of the particles of the deposition unit, and the bonding state of the interface of the deposition unit and the substrate. Because the size of the deposition unit of the coating technology is too small and is only 1-500 micrometers, researchers mostly study and analyze the surface or section state of the deposition unit through observation of a scanning electron microscope, a magnifying glass and a transmission electron microscope, and no effective method is available for the two-dimensional combination state of the deposition unit and the surface of a part.
The two-dimensional combination state of the product unit and the surface of the part can directly reflect the combination state of the deposition unit and the surface of the part, whether element diffusion occurs on the coating and the part and whether effective combination is formed, and how the area ratio and the distribution of a diffusion combination area are important information for the combination research of the deposition unit and the surface of the part and also important information basis for the research of related coatings and performance optimization, and the information has a substantial effect on the combination strength optimization of the coating and the surface of the part. But the lack of two-dimensional combination information acquisition of the deposition unit and the surface of the part seriously affects the performance of related work.
In view of this, the invention is particularly proposed.
Disclosure of Invention
One of the objectives of the present invention is to provide a pretreatment method for detecting the bonding state of a deposition unit and a substrate interface, which can expose the bonding fracture surface of the deposition unit and the substrate surface, and is favorable for rapidly and accurately obtaining two-dimensional bonding information of the deposition unit and the substrate interface.
The second objective of the present invention is to provide a method for detecting the bonding state between the deposition unit and the substrate interface, which can obtain the two-dimensional bonding information between the deposition unit and the substrate interface.
The application can be realized as follows:
in a first aspect, the present application provides a pretreatment method for detecting a bonding state of a deposition unit and a substrate interface, comprising the following steps: the adhesive is coated on the deposition unit on the surface of the substrate, and the adhesive and at least part of the deposition unit are peeled from the surface of the substrate together through the action of external force, so that the peeling section is exposed for detection.
In an alternative embodiment, when there is a void between the deposition unit and the substrate, before applying the external force, the method further comprises performing a post-treatment on the substrate coated with the adhesive and the deposition unit to allow the adhesive to penetrate and fill the void between the deposition unit and the substrate.
In alternative embodiments, the means of post-treatment comprises at least one of heating, incubation, and sonication.
In an alternative embodiment, the adhesive comprises at least one of FM1000 glue and E7 glue.
In an alternative embodiment, the deposition unit is formed by spraying the spray material onto the substrate surface.
In an alternative embodiment, the pre-treatment of the substrate is further included prior to the covering of the deposition unit.
In an alternative embodiment, the pre-treatment comprises at least one of sand blasting, polishing, mechanical grinding, laser engraving, preheating, and cleaning.
In an optional embodiment, the pretreatment method further comprises: the coupling member is attached to a surface of the adhesive on a side facing away from the deposition unit, and a bonding force between the coupling member and the adhesive is greater than a bonding force between the adhesive and the deposition unit.
In a second aspect, the present application further provides a method for detecting a bonding state of a deposition unit and a substrate interface, including: applying an external force to the sample obtained by the pretreatment method to peel the adhesive and at least part of the deposition units from the surface of the substrate together to expose a peel section, and detecting the peel section.
In an alternative embodiment, detecting includes detecting two-dimensional binding information of an interface between the stripped deposition cell and the substrate.
In an alternative embodiment, the detection means comprises at least one of a scanning electron microscope, a scanning energy spectrum, a microscope, a magnifying glass, and a transmission electron microscope.
The beneficial effect of this application includes:
the adhesive is coated on the deposition units on the surface of the substrate, so that the adhesive and at least part of the deposition units are peeled off from the surface of the substrate together under the action of external force, the combined fracture surface of the deposition units and the surface of the substrate is exposed, and the most original, most basic and most important formation information of the coating can be completely characterized. The corresponding detection method is simple to operate, low in cost and high in practicability, and compared with the traditional method for observing the bonding state of the interface of the deposition unit by using the surface or the cross section, the method can quickly and accurately obtain the two-dimensional bonding information of the interface of the deposition unit and the substrate, has complete and accurate information quantity, and has important significance for the research of the spraying coating technology, the further improvement of the bonding strength between the coating/substrate interface and the optimization of the performance of the coating.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic flow diagram of a process for preparing a release member and a release process according to the present application;
FIG. 2 is a two-dimensional bonding topography of the interface of a pure nickel deposition unit and an aluminum substrate in a release member of example 1 of the present application;
FIG. 3 is a surface topography of the interface bond between the pure nickel deposition unit and the aluminum substrate in the release member of example 1 of the present application;
FIG. 4 is a cross-sectional view of the interface bonding between the pure nickel deposition unit and the aluminum substrate in the release member of example 1 of the present application;
FIG. 5 is a two-dimensional bond profile of the interface of a pure copper deposition unit and a stainless steel substrate in a release member of example 2 of the present application;
FIG. 6 is a surface topography of the interfacial bonding of a pure copper deposition unit and a stainless steel substrate in a release member of example 2 of the present application;
FIG. 7 is a cross-sectional profile of the interfacial bonding of a pure copper deposition unit and a stainless steel substrate in a release member of example 2 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following describes a method for detecting the bonding state of the interface between the deposition unit and the substrate and a pretreatment method thereof.
The application provides a pretreatment method for detecting the interface bonding state of a deposition unit and a substrate, which comprises the following steps: the deposition unit on the surface of the substrate is covered with the adhesive, and the adhesive and at least part of the deposition unit (preferably a plurality of independent deposition units) are peeled from the surface of the substrate together through the action of external force, so that the peeling section is exposed for detection.
The above expressions are to be understood as: in the case of peeling, a part of the deposition units may be peeled from the surface of the substrate, or all the deposition units may be peeled from the surface of the substrate.
In an alternative embodiment, the substrate may be pretreated prior to covering the deposition unit.
By reference, the pretreatment may include, for example, at least one of sand blasting, polishing, mechanical grinding, laser engraving, preheating, and cleaning. Substrates of different surface states can be obtained by sandblasting, polishing, mechanical grinding and laser engraving. The cleaning (acetone or alcohol) can remove various pollutants such as oil stain, dust and the like, and the surface of the substrate can be kept in a clean state.
In the present application, the deposition unit is obtained by spraying a spray material on the surface of the substrate. Preferably, the substrate is fixed during deposition without jitter, displacement, etc.
The spray material may be, by reference, any sprayable material such as ceramic, metal or rubber, and may be in the form of any sprayable form such as powder, wire or liquid.
The spraying process can be any spraying process such as gas atomization spraying, thermal spraying, cold spraying or liquid material spraying. Reference may be made in particular to electric arc spraying, plasma spraying, flame spraying, supersonic spraying or gas dynamic spraying, etc.
In the spraying process, the deposition state of a single deposition unit and the combination mode of the deposition unit and a substrate can be completely observed and analyzed by regulating and controlling process parameters such as powder feeding speed, heating power, accelerating power, gas flow, spraying distance, spraying bottom crossing or gun walking speed in any combination.
It should be noted that, in the present application, the deposition units may be only 1 layer, or may be multiple layers, that is, the surface of the original substrate may be covered with at least 2 layers of deposition units, different deposition units are obtained by spraying different spraying materials, each deposition unit is in a mutually independent bonding state, and each deposition unit does not interfere with each other.
When the interface combination information between the layer 1 deposition unit and the layer 2 deposition unit is researched in the direction from close to the substrate to far from the substrate, the layer 1 deposition unit can be regarded as a 'substrate', the layer 2 deposition unit and the following deposition units can be regarded as deposition units deposited on the surface of the layer 1 deposition unit, and in the process, the layer 2 deposition unit and the rest deposition units far from the layer 1 deposition unit are maintained in an integrated state in the stripping process. The interface between the remaining deposition units binds information and so on.
It should be noted that the above-mentioned "deposition unit is located between the substrate and the adhesive" covers the following three cases: firstly, the surface deposition of base member has the deposition unit layer, and the adhesive covers the surface that deviates from the one side of base member in the deposition unit, and at this moment, do not contact each other between adhesive and the base member. Secondly, a deposition unit is deposited on part of the surface of the substrate, while the deposition unit is not deposited on the rest part of the surface, and the adhesive is not only attached to the surface of the deposition unit, but also covers the surface of the substrate on which the deposition unit is not deposited. Thirdly, deposition units are deposited on the surface of the substrate, but pores are formed between the deposition units and the substrate, and the adhesive is attached to the surface of the deposition units.
Accordingly, in the first case, the bonding force between the adhesive and the deposition unit is at least greater than the bonding force between a portion of the deposition unit and the substrate. In the second and third cases, the bonding force between the adhesive and the deposition unit is greater than the bonding force between the adhesive and the substrate, and the bonding force between at least some of the deposition units and the substrate is less than or equal to the bonding force between the adhesive and the substrate.
When a gap exists between the deposition unit and the substrate (corresponding to the third condition), before the external force is applied, the method further comprises the step of performing post-treatment on the substrate coated with the adhesive and the deposition unit so that the adhesive permeates into and fills the gap between the deposition unit and the substrate, so that the adhesive is favorably and fully contacted with the surface of the deposition unit, the subsequent stripping is favorably performed, and the more intuitive and accurate information of the cross-section bonding state is obtained.
In alternative embodiments, the post-treatment may include at least one of heating, incubation, and sonication, for example.
Herein, the adhesive is a high bonding strength adhesive, and may include at least one of FM1000 glue, E7 glue, and 502, for example.
Further, the pretreatment method further comprises: and the surface of the side of the adhesive, which is far away from the deposition unit, is connected with the mating part, the bonding force between the mating part and the adhesive is greater than the bonding force between the adhesive and the deposition unit, and external force is applied to the mating part.
The above-mentioned mating parts can be workpieces of any material and any size, and only need to meet the requirements of corresponding drawing mechanical properties. The entirety of the substrate, the deposition unit, the adhesive, and the coupling member is referred to as a "release member".
Correspondingly, the application also provides a method for detecting the interface bonding state of the deposition unit and the substrate, which comprises the steps of applying external force to the sample obtained by the pretreatment method so as to peel the adhesive and at least part of the deposition unit from the surface of the substrate together to expose a peeling section, and then detecting the peeling section.
Specifically, the substrate and the mating member of the stripping member are simultaneously applied with opposite forces until the adhesive (adhesive layer, high-strength adhesive layer) is separated from the substrate, at which time, a large number of deposition units are stripped from the substrate surface along with the adhesive layer, and the stripping section between the stripped deposition unit and the substrate is completely exposed. The preparation process of the stripping member and the flow chart of the stripping process are shown in FIG. 1.
In an alternative embodiment, the above cross-sectional structure detection comprises detecting two-dimensional binding information of an interface between the deposition unit and the substrate. The detection means may comprise, for example, at least one of a scanning electron microscope, a scanning electron spectrometer, a microscope, a magnifying glass, and a transmission electron microscope.
In the method, the fracture morphology of the deposition unit/matrix can be obtained simply, at low cost and in large quantity by utilizing the stripping technology of the deposition unit, and the combination information of the deposition unit can be directly represented in the micron-scale (preferred) and nano-scale sizes.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for detecting the interface bonding state of a spray deposition unit, which comprises the following steps:
the surface of the aluminum substrate of 100X 100mm is subjected to polishing pretreatment to obtain a smooth and flat surface state of the part.
The aluminum-based matrix is fixed on the spraying table, so that adverse factors such as shaking and displacement are avoided in the preparation process of the deposition unit.
The surface of the aluminum matrix is cleaned by acetone or alcohol to remove various pollutants such as oil stain, dust and the like, so that the surface of the aluminum matrix is kept clean.
And preparing a pure nickel deposition unit on the surface of the aluminum matrix by using low-temperature high-speed spraying. Wherein the technological conditions of the supersonic flame spraying comprise that the spraying distance is 60mm, and the powder feeding rate is 0.5 g/min; the fuel flow rate is 5L/h, and the pressure is 2 MPa; the flow rate of oxygen is 20L/h, and the pressure is 3 MPa; the flow rate of the argon gas is 5L/h, and the pressure is 0.7 MPa.
And coating a layer of high bonding strength FM1000 adhesive on the surface of the pure nickel deposition unit, and adhering a 100X 100mm stainless steel mating part on the surface of the adhesive to finish the preparation of the pure nickel deposition unit/aluminum substrate stripping part.
An opposing force was applied to the aluminum substrate and stainless steel mating part of the deposition unit release member until the FM1000 adhesive separated from the aluminum substrate. Thereby peeling a large number of pure nickel deposition units from the surface of the substrate along with the FM1000 adhesive layer and then exposing the deposition unit/substrate peel profile.
The examination of the interface bonding state between the WC-12Co deposition unit and the aluminum matrix was carried out by observing the peeling cross-section between the pure nickel deposition unit (Ni particles) and the aluminum matrix using a scanning electron microscope, and the results are shown in FIG. 2, which shows: the center of the particle of the deposition unit is smooth and has no obvious abnormality. Obvious ring-mounted metallurgical bonding fracture zones are distributed around the deposition unit, and an obvious dimple structure is presented. Analysis results show that under the process condition, the center of the deposition unit and the substrate cannot form effective combination, and the effective combination area of the whole area does not exceed 50%.
In addition, the surface morphology and the cross-sectional morphology of the spray deposition unit of the stripping member are detected by using the existing combined interface observation means (scanning electron microscope, SEM), and the results are shown in fig. 3 and 4 respectively, which show that: the surface appearance can only observe the surfaces of the deposition unit and the substrate, and the information of the bonding interface between the deposition unit and the substrate cannot be obtained. The cross section appearance can only observe the one-dimensional appearance between the deposition unit and the substrate, and the combination information of the deposition unit and the substrate surface cannot be comprehensively reflected; meanwhile, a sample prepared by cutting and polishing cannot confirm that the section appearance is at a specific position of the deposition unit, so that the guidance significance of related information on interface combination analysis is extremely limited.
Example 2
The embodiment provides a method for detecting the interface bonding state of a spray deposition unit, which comprises the following steps:
the surface of a stainless steel substrate having a diameter of 25.6mm and a length of 100mm was subjected to a sand blast pretreatment to obtain a surface state of a part having a roughness Ra of 5 μm.
The stainless steel substrate is fixed on the spraying table, so that adverse factors such as shaking and displacement are avoided in the preparation process of the deposition unit.
The surface of the stainless steel substrate is cleaned by alcohol to remove various pollutants such as oil stain, dust and the like, so that the surface of the stainless steel substrate is kept in a clean state.
And preparing a pure copper deposition unit on the surface of the stainless steel substrate by utilizing gas dynamic spraying. Wherein, the technological conditions of the gas dynamic spraying comprise that the spraying distance is 50mm, and the powder feeding speed is 2 g/min; the working gas is air, the gas pressure is 3MPa, the gas temperature is 300 ℃, and the moving speed of the spray gun is 200 mm/min.
Coating a layer of high-bonding-strength E7 adhesive on the surface of the pure copper deposition unit, and adhering a 45# steel mating part with the diameter of 25.6mm and the length of 100mm to the end face of the adhesive to finish the preparation of the pure copper deposition unit/stainless steel substrate stripping part.
An opposing force was applied to the stainless steel substrate and the 45# steel mating part of the deposition unit release member until the E7 adhesive separated from the stainless steel substrate. Thereby peeling off a large number of pure copper deposition units from the surface of the substrate along with the E7 adhesive layer, and then exposing the peeling section of the pure copper deposition units/stainless steel substrate.
The detection of the interface bonding state of the pure copper deposition unit and the stainless steel substrate is completed by scanning and observing the stripping section of the pure copper deposition unit and the stainless steel substrate by using electron microscope elements, and the result is shown in figure 5, which shows that: the main body of the combination between the deposition unit and the particles is divided into three areas, namely a central original area, a ring-mounted metallurgical combination fracture dimple structure area surrounding the center and an unbonded area at the outermost periphery, and the information of the whole combination interface is complete and clear.
In addition, the surface morphology and the cross-sectional morphology of the spray deposition unit of the stripping member are detected by a scanning electron microscope method commonly adopted in the prior art, and the results are respectively shown in fig. 6 and 7, which show that: the surface appearance can only observe the surfaces of the deposition unit and the substrate, and the information of the bonding interface between the deposition unit and the substrate cannot be obtained. The cross-sectional morphology can only observe the one-dimensional morphology between the deposition unit and the substrate, and due to the material filling in the polishing process, the interface of the figure shows complete combination, but is actually false, does not reflect real combination information (combination information of the deposition unit and the substrate surface cannot be truly reflected), and is easy to mislead. Meanwhile, a sample prepared by cutting and polishing cannot confirm that the section appearance is at a specific position of the deposition unit, so that the guidance significance of related information on interface combination analysis is extremely limited.
In summary, the present application can completely characterize the most primitive, basic and important formation information of the coating by coating the surface of the substrate on which the deposition units are deposited with the adhesive, so that the adhesive and at least part of the deposition units are peeled off from the surface of the substrate together under the action of external force, thereby exposing the combined fracture surface of the deposition units and the surface of the substrate. The corresponding detection method is simple to operate, low in cost and high in practicability, and compared with the traditional method for observing the bonding state of the interface of the deposition unit by using the surface or the cross section, the method can quickly and accurately obtain the two-dimensional bonding information of the interface of the deposition unit and the substrate, has complete and accurate information quantity, and has important significance for the research of the spraying coating technology, the further improvement of the bonding strength between the coating/substrate interface and the optimization of the performance of the coating.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for detecting the bonding state of a spraying deposition unit and a substrate interface is characterized by comprising the following steps: applying an external force to the sample obtained by the pretreatment method to peel the adhesive and at least part of the deposition units from the surface of the substrate together to expose a peeling section, and then detecting the peeling section;
detecting two-dimensional binding information including detecting an interface between the deposition unit and the substrate being stripped;
the pretreatment method comprises the following steps: coating an adhesive on the deposition unit on the surface of the substrate;
the deposition unit and the substrate are provided with pores, and before external force is applied, the substrate covered with the adhesive and the deposition unit is subjected to post-treatment so that the adhesive can penetrate into and fill the pores between the deposition unit and the substrate; the post-treatment means includes at least one of heating, heat-retention, and ultrasound.
2. The method of claim 1, wherein the adhesive comprises at least one of FM1000 glue and E7 glue.
3. The detection method according to claim 1, wherein the deposition unit is formed by spraying a spray material on the surface of the substrate.
4. The method of claim 1, further comprising pre-treating the substrate prior to covering the deposition unit.
5. The inspection method of claim 4, wherein the pre-treatment comprises at least one of sand blasting, polishing, mechanical grinding, laser engraving, pre-heating, and cleaning.
6. The detection method according to claim 1, wherein the preprocessing method further includes: and a coupling member is connected to a surface of the adhesive on a side facing away from the deposition unit, and a bonding force between the coupling member and the adhesive is greater than a bonding force between the adhesive and the deposition unit.
7. The method of claim 1, wherein the detecting comprises at least one of scanning electron microscopy, energy spectroscopy, microscopy, magnifying glass, and transmission electron microscopy.
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| CN103528885A (en) * | 2013-09-26 | 2014-01-22 | 天津大学 | Method for testing elasticity moduli of coatings |
| CN205228938U (en) * | 2015-12-24 | 2016-05-11 | 河北工业大学 | Special fixture of accurate control hot spraying coating bonding strength test piece axiality |
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| CN110082194A (en) * | 2019-05-05 | 2019-08-02 | 中国人民解放军陆军装甲兵学院 | Coating material original position stretching observation method |
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| CN103528885A (en) * | 2013-09-26 | 2014-01-22 | 天津大学 | Method for testing elasticity moduli of coatings |
| CN205228938U (en) * | 2015-12-24 | 2016-05-11 | 河北工业大学 | Special fixture of accurate control hot spraying coating bonding strength test piece axiality |
| CN110031331A (en) * | 2019-03-07 | 2019-07-19 | 航天科工防御技术研究试验中心 | A kind of test sample, preparation method and the test method of thermal barrier coating bond strength |
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