阅读说明：本技术 一种大曲率微小件表面多层金属薄膜的无损检测方法 (Nondestructive testing method for multilayer metal films on surface of large-curvature small part ) 是由 罗晋如 龚星宇 邓林 全琪 蔡吉庆 李云 王曦 于 2021-06-03 设计创作，主要内容包括：本发明公开一种大曲率微小件表面多层金属薄膜的无损检测方法,包括以下步骤：S1：采用同步辐射X射线微束技术对样品进行检测；S2：采用切入射方法获得表面金属膜层的衍射信号,通过转动样品,使样品与入射X射线相切,入射X射线与样品表面夹角趋近于0°,进而获得表面金属膜层的衍射信号；S3：采用掠入射方法获得中间金属膜层的衍射信号,通过转动样品,使样品中间层与入射X射线形成夹角,夹角小于5°,进而获得中间层金属薄膜镀层的衍射信号；S4：采用透射方法对衍射信号进行校准,此时转动样品,使X射线水平穿透2层复合镀层,从而获得2套衍射信号以辅助校准；采用具有高亮度的同步辐射光源和同步辐射微束技术获得微米级的空间分辨率。(The invention discloses a nondestructive testing method for a multilayer metal film on the surface of a large-curvature micro part, which comprises the following steps: s1: detecting the sample by adopting a synchrotron radiation X-ray microbeam technology; s2: obtaining a diffraction signal of the surface metal film layer by adopting a tangential incidence method, rotating the sample to enable the sample to be tangential to incident X-rays, wherein an included angle between the incident X-rays and the surface of the sample approaches to 0 degree, and further obtaining the diffraction signal of the surface metal film layer; s3: obtaining a diffraction signal of the middle metal film layer by adopting a grazing incidence method, and rotating the sample to enable the middle layer of the sample and incident X-rays to form an included angle which is smaller than 5 degrees, so as to obtain a diffraction signal of the middle metal film coating; s4: calibrating the diffraction signal by adopting a transmission method, rotating the sample at the moment, and enabling X-rays to horizontally penetrate through the 2 layers of composite coatings, thereby obtaining 2 sets of diffraction signals to assist in calibration; the synchronous radiation light source with high brightness and the synchronous radiation micro-beam technology are adopted to obtain the micron-scale spatial resolution.)

1. A nondestructive testing method for a multilayer metal film on the surface of a large-curvature tiny piece is characterized by comprising the following steps:

s1: detecting the sample by adopting a synchrotron radiation X-ray microbeam technology;

s2: obtaining a diffraction signal of the surface metal film layer by adopting a tangential incidence method, rotating the sample to enable the sample to be tangential to incident X-rays, wherein an included angle between the incident X-rays and the surface of the sample approaches to 0 degree, and further obtaining the diffraction signal of the surface metal film layer;

s3: obtaining a diffraction signal of the middle metal film layer by adopting a grazing incidence method, and rotating the sample to enable the middle layer of the sample and incident X-rays to form an included angle which is smaller than 5 degrees, so as to obtain a diffraction signal of the middle metal film coating;

s4: the diffraction signal is calibrated by a transmission method, and at the moment, the sample is rotated to enable X-rays to horizontally penetrate through the 2 layers of composite coatings, so that 2 sets of diffraction signals are obtained to assist in calibration.

2. The method of claim 1, wherein the diffraction light source of step S1 detects the sample by using synchrotron X-ray microbeam, the energy of the beam is 20KeV after crystal selection, and the beam spot size of the chip slit is about 1X1 μm.

3. The method of claim 1, wherein in step S3, the sample is rotated to the maximum absorption point of the middle metal film, and the diffraction signal is obtained by a small-angle grazing method.

4. The method for nondestructive testing of a plurality of metal films on the surface of a large-curvature tiny component according to claim 1, wherein the surface of the sample is provided with a large-curvature curved surface, and the surface of the sample is plated with at least two metal films with nanometer thickness.

5. The method for nondestructive inspection of a multilayer metal film on a surface of a large-curvature small part according to claim 1, wherein the sample is a quartz-based large-curvature small-part gyroscope, and the surface of the quartz substrate is layered with a metal gold film and a metal titanium film each having a thickness of 200 nm and 10 nm.

6. The method for non-destructive testing of a plurality of layers of metal films on the surface of a small part with large curvature as claimed in claim 1, wherein in step S1, the type of probe used is Mar165, and the size of the probe pixel is 75 μm.

Technical Field

The invention relates to the field of nondestructive detection of the interior of metal, in particular to a nondestructive detection method for a multilayer metal film on the surface of a large-curvature micro part.

Background

The surface of a precise micro member such as a high-precision gyroscope and the like is often required to be plated with a plurality of layers of dissimilar metal films, the structure or orientation of the film layer may be different under the influence of the difference of substrate materials, the shape of the member and the plating process, and the thickness, orientation and structure of the film layer may be different along with the difference of distribution positions on the member, which are important factors influencing the performance and service life of the film. Therefore, nondestructive detection of the surface multilayer film structure and strain distribution is the key for monitoring the film quality and regulating and controlling the coating process.

At present, laser ultrasonic detection, neutron diffraction, X-ray diffraction, synchronous irradiation technology and the like are commonly used for nondestructive detection of metal film coatings. The laser ultrasonic detection is that when a laser beam with modulated intensity is emitted into a closed medium space, acoustic waves can be generated, nondestructive evaluation on the material properties is achieved through detection of the waves, the method can be used for detection of ultrathin materials and research on material microstructures, and the position of defects, the thickness of solid materials, surface residual stress, temperature and the like can be accurately determined. The characteristics of no coupling agent, non-contact, high sensitivity and the like enable the sensor to be used for detection, nano material measurement, composite material component evaluation and the like in severe environments such as high temperature and radiation. However, due to low photoacoustic energy conversion efficiency and low ultrasound acceptance sensitivity, theoretical and experimental research is not deep, and the application capability of the material to opaque metal materials is limited. Neutron diffraction has very strong penetration capacity, can provide information of depth from 100 micrometers below a surface layer to several centimeters or even tens of centimeters with millimeter-scale spatial resolution, can extend to the deep part of a structural component to obtain internal structural information, and can be widely applied to the fields of welding structures, composite materials and other multiphase materials, plastic deformation components and materials, near-surface stress and the like at present. The X-ray diffraction technology is the most commonly used nondestructive detection method for acquiring the incident signal of the crystal lattice in the material to judge the information such as the internal structure, the crystal lattice strain, the crystal lattice stress and the like of the metal, and has smaller diffraction volume and spatial resolution compared with the neutron diffraction technology. However, for the surface multilayer structure nano film of the gyroscope with the large curvature micro structure part with the complex shape, the thickness of the surface film layer is only nano magnitude, and the flux of the conventional experimental X-ray source is not enough to obtain enough diffraction information with large peak-to-back ratio for analysis, so that the detection is difficult to be carried out by using a common X-ray diffractometer or a residual stress meter, the high-brightness X-ray can be obtained by using the synchrotron radiation technology to meet the detection requirement, but the large shape curvature and the micro size structure characteristic of the gyroscope have the requirement of high spatial resolution for the detection, so that the X-ray source with high brightness and small beam spot must be used. Therefore, there is a need for a nondestructive testing method for a multilayer metal thin film on the surface of a small large-curvature part, which can solve the above problems.

Disclosure of Invention

The invention aims to provide a nondestructive testing method for a multilayer metal film on the surface of a large-curvature micro-part, which adopts a synchrotron radiation light source with high brightness to overcome the problem of insufficient flux of a conventional X-ray source, and simultaneously adopts a synchrotron radiation micro-beam technology to obtain micron-sized spatial resolution, thereby providing a solution for the problem of nondestructive testing caused by the large-shape curvature and micro-size structural characteristics of a gyroscope.

The embodiment of the invention is realized by the following steps:

a nondestructive testing method for a multilayer metal film on the surface of a large-curvature tiny piece comprises the following steps:

s1: detecting the sample by adopting a synchrotron radiation X-ray microbeam technology;

s2: obtaining a diffraction signal of the surface metal film layer by adopting a tangential incidence method, rotating the sample to enable the sample to be tangential to incident X-rays, wherein an included angle between the incident X-rays and the surface of the sample approaches to 0 degree, and further obtaining the diffraction signal of the surface metal film layer;

s3: obtaining a diffraction signal of the middle metal film layer by adopting a grazing incidence method, and rotating the sample to enable the middle layer of the sample and incident X-rays to form an included angle which is smaller than 5 degrees, so as to obtain a diffraction signal of the middle metal film coating;

s4: the diffraction signal is calibrated by a transmission method, and at the moment, the sample is rotated to enable X-rays to horizontally penetrate through the 2 layers of composite coatings, so that 2 sets of diffraction signals are obtained to assist in calibration. The synchrotron radiation light source with high brightness and high collimation is selected as a diffraction medium, so that high brightness and high spatial resolution which are difficult to reach by a conventional X-ray diffractometer or a residual stress meter can be obtained, and a solution is provided for the problem of nondestructive detection of the internal structure of the surface multilayer metal film of the gyroscope with large-shape curvature and micro-size structural characteristics. The structure and the grain strain of each layer of the quartz-based gyroscope plated with the hundred-nanometer-level gold film and the ten-nanometer-level titanium film are effectively detected and analyzed, and the uniformity of a plating layer is qualitatively analyzed; the problem of insufficient flux of a conventional X-ray source is solved by adopting a synchrotron radiation light source with high brightness, and meanwhile, the problem of nondestructive detection caused by the large-shape curvature and micro-size structural features of a gyroscope is solved by adopting a synchrotron radiation microbeam technology to obtain micron-sized spatial resolution.

Preferably, the diffraction light source in step S1 detects the sample by using synchrotron radiation X-ray microbeam, the energy of the light beam is 20KeV after crystal selection, and the beam spot size card slit is about 1X1 microns.

Preferably, in step S3, the sample is rotated to the maximum absorption point of the intermediate metal film, and the diffraction signal is obtained by a small-angle grazing incidence method.

Preferably, the surface of the sample is provided with a curved surface with large curvature, and the surface is plated with at least two layers of metal films with nanometer thickness.

Preferably, the sample is a large-curvature micro-component gyroscope with a quartz substrate, and a metal gold film and a metal titanium film with the thicknesses of 200 nanometers and 10 nanometers are respectively plated on the surface of the quartz substrate in a layered mode.

Preferably, in step S1, the probe type used is Mar165, and the detection pixel size is 75 μm.

Due to the adoption of the technical scheme, the invention has the beneficial effects that: the invention relates to a nondestructive testing method for a multilayer metal film on the surface of a large-curvature tiny piece, which comprises the following steps of: s1: detecting the sample by adopting a synchrotron radiation X-ray microbeam technology; s2: obtaining a diffraction signal of the surface metal film layer by adopting a tangential incidence method, rotating the sample to enable the sample to be tangential to incident X-rays, wherein an included angle between the incident X-rays and the surface of the sample approaches to 0 degree, and further obtaining the diffraction signal of the surface metal film layer; s3: obtaining a diffraction signal of the middle metal film layer by adopting a grazing incidence method, and rotating the sample to enable the middle layer of the sample and incident X-rays to form an included angle which is smaller than 5 degrees, so as to obtain a diffraction signal of the middle metal film coating; s4: the diffraction signal is calibrated by a transmission method, and at the moment, the sample is rotated to enable X-rays to horizontally penetrate through the 2 layers of composite coatings, so that 2 sets of diffraction signals are obtained to assist in calibration. The synchrotron radiation light source with high brightness and high collimation is selected as a diffraction medium, so that high brightness and high spatial resolution which are difficult to reach by a conventional X-ray diffractometer or a residual stress meter can be obtained, and a solution is provided for the problem of nondestructive detection of the internal structure of the surface multilayer metal film of the gyroscope with large-shape curvature and micro-size structural characteristics. The structure and the grain strain of each layer of the quartz-based gyroscope plated with the hundred-nanometer-level gold film and the ten-nanometer-level titanium film are effectively detected and analyzed, and the uniformity of a plating layer is qualitatively analyzed; the problem of insufficient flux of a conventional X-ray source is solved by adopting a synchrotron radiation light source with high brightness, and meanwhile, the problem of nondestructive detection caused by the large-shape curvature and micro-size structural features of a gyroscope is solved by adopting a synchrotron radiation microbeam technology to obtain micron-sized spatial resolution.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings 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 diagram of the steps of the method of the present invention;

FIG. 2 is a schematic view of the position of a mark on a sample test point according to the present invention;

FIG. 3 is a schematic diagram of the optical path of the grazing incidence detection method for the intermediate plating layer in the present invention;

FIG. 4 is a schematic diagram of a transmission calibration optical path according to the present invention;

FIG. 5 is a graph of typical diffraction signatures and structural and stress analysis of a surface coating plated by the present invention;

FIG. 6 is a graph of typical diffraction signal patterns and structure and stress analysis of an intermediate coating plated by the present invention;

FIG. 7 is a diffraction pattern of a typical diffraction signal and calibration signal of the present invention;

FIG. 8 is a plot of the location of a sample test point in accordance with the present invention;

FIG. 9 is a graph of calculated data and analysis results of diffraction signals from a surface coating plated by the present invention;

FIG. 10 is a graph of data calculated and analysis results of diffraction signals from an intermediate coating applied by the present invention.

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 with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.

The following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.

Furthermore, the terms "horizontal", "vertical", "suspended", and the like do not imply that the components are required to be absolutely horizontal or suspended, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.

In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

Since the discovery of synchrotron radiation in 1947, a total of three generations of developments have been made, and the first generation synchrotron radiation device is a synchrotron shared with high-energy physical experiments and mainly used for high-resolution X-ray diffraction, X-ray spectroscopy, X-ray absorption spectrum, structural analysis of small crystals, small-angle scattering, and microscopy. The second generation synchrotron radiation is mainly a magnet focusing structure proposed in 1976 to obtain high synchrotron brightness with low electron beam emittance, which is reduced to 50-150nm. The third generation of synchrotron radiation changes the straight line section design of the storage ring, and more plug-ins are installed, so that a larger brightness ratio is obtained, the divergence of light beams is greatly reduced, and the size of light spots is reduced. Compared with the traditional experimental characterization technology and method, the synchrotron radiation light source has the advantages of brightness, collimation and stability which are far higher than those of the experimental light source, wide band coverage, high polarization, pulse time structure and the like. The high flux and high collimation of the synchrotron radiation light source provide possibility for reducing the size of a focal spot to a micron order so as to obtain micron-scale spatial resolution, and the resolution can be improved from a few microns to a submicron or even nanometer level by the light source provided by a third generation synchrotron radiation device and adopting methods such as slit or micropore beam limiting and the like to obtain an X-ray microbeam technology, so that the structure, element components and the like of a tiny sample or a sample with a microcell structure can be analyzed, and the synchrotron radiation light source has the advantages of high sensitivity, high spatial resolution, no damage to the sample, capability of analyzing a thick sample, capability of measuring under atmosphere and water environment and the like. Commonly used microbeam research methods include: the method can obtain the structure (such as crystal structure, texture, strain, etc.), the spatial distribution of chemical components and chemical valence of a sample, can detect the distribution of the surface and the interior of an object, and can be used for the tomography of element distribution and structure distribution. For example, Biermann et al, have measured the X diffraction peak distribution of {400} and {300} type single crystal Ni-based superalloy turbine blades using synchrotron radiation microbeam X-ray diffraction technique, and have obtained some new results different from conventional X-ray diffraction. Therefore, in the invention, aiming at the difficult problem of nondestructive detection of the multilayer metal film on the surface of the large-curvature tiny piece, the synchronous radiation microbeam is adopted to develop the detection method for the uniformity, the structure and the grain strain distribution of the multilayer metal film with the nanometer-level thickness.

Example 1: referring to fig. 1 to 10, a nondestructive testing method for a multi-layer metal film on a surface of a large-curvature micro element in the present embodiment includes the following steps: s1: detecting the sample by adopting a synchrotron radiation X-ray microbeam technology; s2: obtaining a diffraction signal of the surface metal film layer by adopting a tangential incidence method, rotating the sample to enable the sample to be tangential to incident X-rays, wherein an included angle between the incident X-rays and the surface of the sample approaches to 0 degree, and further obtaining the diffraction signal of the surface metal film layer; s3: obtaining a diffraction signal of the middle metal film layer by adopting a grazing incidence method, and rotating the sample to enable the middle layer of the sample and incident X-rays to form an included angle which is smaller than 5 degrees, so as to obtain a diffraction signal of the middle metal film coating; s4: the diffraction signal is calibrated by a transmission method, and at the moment, the sample is rotated to enable X-rays to horizontally penetrate through the 2 layers of composite coatings, so that 2 sets of diffraction signals are obtained to assist in calibration. The synchrotron radiation light source with high brightness and high collimation is selected as a diffraction medium, so that high brightness and high spatial resolution which are difficult to reach by a conventional X-ray diffractometer or a residual stress meter can be obtained, and a solution is provided for the problem of nondestructive detection of the internal structure of the surface multilayer metal film of the gyroscope with large-shape curvature and micro-size structural characteristics. The structure and the grain strain of each layer of the quartz-based gyroscope plated with the hundred-nanometer-level gold film and the ten-nanometer-level titanium film are effectively detected and analyzed, and the uniformity of a plating layer is qualitatively analyzed; the problem of insufficient flux of a conventional X-ray source is solved by adopting a synchrotron radiation light source with high brightness, and meanwhile, the problem of nondestructive detection caused by the large-shape curvature and micro-size structural features of a gyroscope is solved by adopting a synchrotron radiation microbeam technology to obtain micron-sized spatial resolution.

Example 2: the diffraction light source in step S1 of this embodiment detects the sample by using synchrotron radiation X-ray microbeam, the energy of the beam is 20KeV after crystal selection, and the beam spot size card slit is about 1X1 microns. In step S3, the sample is rotated to the maximum absorption point of the intermediate metal thin film, and a diffraction signal is obtained by a small-angle grazing incidence method. The surface of the sample of the embodiment is provided with a curved surface with large curvature, and the surface is plated with at least two layers of metal films with nanometer thickness. The sample of this example is a large-curvature micro-component gyroscope with a quartz substrate, and a metal gold film and a metal titanium film with thicknesses of 200 nm and 10 nm are layered on the surface of the quartz substrate. In step S1, the probe type used is Mar165, and the detection pixel size is 75 μm.

Example 3: in the embodiment, the diffraction signal is obtained from the tangential incidence direction of the light beam passing through the surface of the surface metal film coating, and the optical path of the surface coating detection tangential incidence method is shown in fig. 3, and the angle between the incident X-ray and the surface of the sample is almost 0 °. The typical diffraction signal pattern and structure of the obtained surface coating and the stress analysis result are shown in fig. 6. The result shows that the titanium or the amorphous layer or the plating layer is incomplete, diffraction spots can be obtained only at the position close to the plane base, and the complex diffraction spots show that the grain size of the titanium film at the base is below micron, but the orientation is more obvious.

Example 4: in this embodiment, a grazing incidence method is used to obtain a diffraction signal of the intermediate metal film layer, a small-angle grazing incidence method is used to obtain a diffraction signal at the position where the absorption of the intermediate metal film plating layer is maximum, the light path of the intermediate plating layer detection grazing incidence method is shown in fig. 4, and the included angle between the incident X-ray and the sample surface is small and is within 5 °. The typical diffraction signal pattern and structure of the obtained intermediate coating and the analysis result of stress are shown in fig. 7. Analysis results show that most of the strain distribution of the middle gold plating layer is uniform, and the material content is non-uniform, which indicates that the thickness of the film layer is possibly not uniform; the complex diffraction spots show that the number of crystal grains participating in diffraction is small, the gold film is also a nano crystal with the size below micron, the gold film has strong preferred orientation, and diffraction spot signals can be obtained at all test positions.

Example 5: in the embodiment, a transmission method is adopted, so that X-rays penetrate through the 2 layers of composite coatings to obtain 2 sets of diffraction signals to assist calibration, and a sample and incident X-rays are horizontally placed to ensure that X-rays can penetrate through the 2 layers of composite coatings. The optical path of the transmission method is shown in fig. 5. FIG. 8 is a typical diffraction signature of a transmission calibration signal for a component of the invention. Wherein, the further X-ray fluorescence analysis check result of the surface metal film coating shows that the surface has no titanium signal, which indicates that the surface coating is incomplete; the result of further X-ray fluorescence analysis of the intermediate metal film coating indicates that the gold element exists, which indicates the integrity of the film.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by 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.