CN112461880A - Method for positioning and detecting surface conductive type passage of glass sealing structure - Google Patents
Method for positioning and detecting surface conductive type passage of glass sealing structure Download PDFInfo
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
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- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
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Abstract
The invention relates to a method for quickly and accurately positioning and detecting a conductive path on the surface of a glass sealing structure. The method is used for visually displaying and acquiring the information such as the position, the form, the size and the like of the conductive path on the surface of the glass sealing structure. In particular to application verification and service reliability evaluation of materials, electronic products and electromechanical products. The method is characterized in that incident charged particle beams with specific energy are used as a charge input source to uniformly and repeatedly scan the surface of a glass sealing structure to be detected at a specific scanning speed and a specific number of times, the difference of the conductivity characteristics is utilized to cause the difference of the accumulated charge amount and the strong degree of charge effect on the repulsion effect of the incident electron beams, and the acquired excitation signals of the incident charged particle beams generate the comprehensive contrast difference imaging of the conductivity degree and the micro-morphology of an insulating part and a conductive part, so that the method can be used for realizing the rapid and accurate positioning and detection of a conductive path on the surface of the glass sealing structure.
Description
Technical Field
The invention relates to a method for positioning and detecting a conductive path on the surface of a glass sealing structure. The method is used for visually displaying and acquiring the information of the position, the form, the size and the like of the conductive path on the surface of the glass insulator. The method is characterized in that incident charged particle beams with set energy are used as input sources to uniformly and repeatedly scan the surface of a glass sealing structure to be detected at a set scanning speed and a set number of times, the difference of the conductivity characteristics is utilized to cause the difference of the accumulated charge amount and the strong degree of charge effect on the repulsion effect of the incident electron beams, and the collected excitation signals of the incident charged particle beams generate the comprehensive contrast difference imaging of the conductivity degree and the micro-morphology of an insulating part and a conductive part, so that the method can be used for realizing the rapid and accurate positioning and detection of a conductive path on the surface of the glass sealing structure. In particular to application verification and service reliability evaluation of materials, electronic products and electromechanical products.
Background
A glass sealing structure (glass insulating sealing structure) is one of typical insulating sealing forms of components. The sealing material has the characteristics of high strength, good sealing property, good insulating property, good tolerance to high and low temperature use environments, damp and hot use environments and irradiation use environments, low vacuum volatilization, low pollution and the like, and is suitable for structural insulating sealing of components and parts used in a large range of temperature fluctuation, damp and hot environments and irradiation hangings. Numerous component and device production plants at home and abroad mainly use the glass sealing structure in component and device products with relatively severe service environment and higher requirements on strength, insulativity, volatility and environmental tolerance so as to improve the environmental tolerance and service reliability of corresponding component and device products. In the aerospace field, a plurality of components in the aerospace mechanisms such as NASA, ESA and the like and aerospace products in China all use glass sealing structures in large quantity.
In recent years, the problem of component failure caused by abnormal conductive paths of glass sealing structures frequently occurs in aerospace engineering, but the judgment of component failure adopting the glass sealing structures is mainly based on whether component use function is lost or product-level function tests (such as leakage rate, insulation resistance and breakdown voltage) meet the requirements of product execution standards, an accurate and rapid positioning test method for the abnormal conductive paths of the glass sealing structures is lacked, the failure mechanism is not favorably and deeply analyzed, accurate prevention or control measures are adopted, and hidden dangers exist in engineering application. Particularly, for a small-sized glass sealing structure of a component, suspected cracks and microcracks are in a micro-nano scale, a sealing position is a concave liquid surface structure with larger curvature, a common optical microscope is difficult to observe micro-nano scale defects of the structure, and whether the defects are related to a conductive path or not can not be judged even if the defects are observed; although the infrared microscope can form current on a conductive path by electrifying and further display the conductive path by using a resistance thermal effect, on one hand, because the glass sealing structure to be detected is an insulating material, the current of about 1nA can be obtained by adding extremely large voltage (for example, 1000V), the current is far lower than the milliampere-level current required for generating detectable thermal effect, the failure mechanism is easy to generate fundamental change by applying overlarge voltage (the normal working voltage of components is usually not more than 10V), and in addition, because the infrared signal detected by the infrared microscope is transmitted by a sample, the spatial resolution is only millimeter level or submillimeter level, and the micro-nanometer conductive path cannot be distinguished; although the common fluorescence penetration inspection method can find micro-cracks on the surface of the glass sealing structure, the penetrating fluid is turbid liquid, the fluorescent component of the penetrating fluid is micron-sized particles, the penetrating fluid cannot effectively penetrate into potential conductive defects of a micro-nano scale, and the displayed defects cannot be confirmed to be conductive paths; generally, a scanning electron microscope cannot directly observe the surface appearance of a non-conductive glass insulation sealing structure due to the charge effect of an insulation sample, and a metal (or carbon) conductive coating layer is sprayed on the surface of the insulation sealing structure, or a low vacuum mode is used to eliminate or improve the charge effect, the conductive coating layer can cover the original appearance of a conductive path on the surface of the glass insulation structure, and whether the conductive path is a real conductive path can not be confirmed even if the original appearance is observed in the low vacuum mode. Analysis shows that the traditional methods can not realize fast reading and accurate positioning and detection on the conductive path (especially the micro-nano conductive path) on the surface of the glass sealing structure, and can not meet the application verification and service reliability evaluation requirements of materials, electronic products and electromechanical products.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method adopts the mode of controlling the energy, beam intensity, scanning speed, scanning mode and scanning time of an incident focused charged particle beam, utilizes the charged particle beam as a charge input source, utilizes the difference of the intensity of a charge effect induced by the charged particle beam in an insulating part and a conductive part on the surface of the glass sealing structure by the controlled and uniform scanning, and uses a corresponding detector to collect an excitation signal of the incident charged ion beam to form a comprehensive contrast image of the conductivity degree and the micro-morphology, so that the information of the position, the shape, the size and the like of the conductive path on the surface of the glass insulator can be accurately, quickly and intuitively displayed and obtained, and the quick and accurate positioning and detection of the conductive path on the surface of the glass sealing structure can be further realized.
The technical solution of the invention is as follows:
a method for locating and detecting the conductive path on the surface of glass sealing structure features that the incident charged particle beam with a predefined energy is used as charge input source to scan the surface of glass sealing structure uniformly and repeatedly at predefined speed and times. The glass sealing structure (the main body is made of insulating materials) can accumulate charges due to a charge effect after being irradiated by charged particles, the more charges are accumulated due to better insulating property, a stronger electric field is formed to repel subsequent incident charged particles, and a relatively stronger signal (shown as higher brightness) can be formed in an incident charged particle excitation signal detector (such as a typical common secondary electron detector). The conductive path has a conductive characteristic that accumulated charges are quickly dissipated after being irradiated by charged particles, the repulsion effect on subsequent incident charged particles is relatively weak, and relatively weak signals (represented as low brightness) are formed in the incident charged particle excitation signal detector. Under the uniform charged particle irradiation field which can cover the whole glass sealing structure, the insulating area and the conducting area form a comprehensive contrast image which integrates the conducting capacity and the surface appearance due to the difference of the conducting capacity and the charge effect accumulated charge difference. By reasonably controlling the charged particle irradiation process, the information such as the position, the form, the size and the like of the conductive passage on the surface of the glass sealing structure can be visually, quickly and accurately displayed and obtained.
A method for locating and detecting a conductive path on a surface of a glass sealing structure, the method comprising the steps of:
(1) detecting the insulation resistance of the glass sealing structure by using a resistance detection instrument, wherein when the resistance value of the detected insulation resistance is lower than a set threshold value, the detected glass sealing structure is a sample to be detected, otherwise, the detected glass sealing structure does not need to be subjected to subsequent detection;
(2) clearing the surface shelter of the sample to be detected in the step (1), wherein the surface of the sample to be detected cannot be damaged in the process of removing the shelter;
(3) directly placing the sample to be tested in an evacuable state (the vacuum degree is equal to or better than 10)-3Pa) in a controlled charged particle beam device, a field emission scanning electron microscope is usually used, and the normal direction of a sample to be measured is parallel to the direction of an incident charged particle beam, then the working distance, the accelerating voltage and the beam intensity of the field emission scanning electron microscope are set, scanning is started and focusing is performed, and focusing is not performed in a glass sealing structure area due to the following reasons: the local charge effect can seriously affect the subsequent observation;
working distance requirements in a field emission scanning electron microscope: the working distance is set as large as possible, so that the minimum magnification of the equipment can cover the whole complete glass sealing structure area, the working distance is not easy to be too small, the too small working distance can cause the charge effect to be too strong and the charge distribution uniformity to be poor during scanning, and is not beneficial to displaying a clear and complete conductive path, and the working distance can be set to be 30 mm-50 mm for the field emission scanning electron microscope generally; the field emission scanning electron microscope has the advantages that proper accelerating voltage and beam intensity are selected, the charging effect is too strong due to too high accelerating voltage or too high beam, the clear and complete conductive path is not easy to appear, the accelerating voltage of the field emission scanning electron microscope is 5kV-15kV, and the beam is 100pA-400 pA.
The detector in the field emission scanning electron microscope is a secondary electron detector (SE 2);
(4) after focusing is clear in the step (3), adjusting the minimum magnification of the equipment, adjusting the scanning speed to be not more than 900ms per frame, and adjusting the contrast to be 20-45% and the brightness to be 40-60%;
(5) moving a sample to be detected to the central position of a view field, adjusting the magnification of equipment to enable the whole complete glass sealing structure of the sample to be detected to be positioned in the middle of the view field (namely the center of the whole complete glass sealing structure is superposed with the center of the view field as much as possible), and adjusting the scanning speed to be 900ms-5s per frame and the scanning frequency to be 5-30 times;
(6) acquiring comprehensive contrast images of the conductivity degree and the micro morphology to obtain information such as positions, forms and sizes of a plurality of conductive paths;
(7) amplifying the comprehensive contrast image at one position of the conductive path obtained in the step (6) by 500 times and 50000 times, and collecting the image so as to obtain information such as the form, the size and the like of the conductive path in the micro-nano scale;
(8) and (5) taking the sample to be detected out of the field emission scanning electron microscope, removing the charges accumulated on the surface by using an ion fan, repeating the steps (3) to (7), and obtaining the information such as the shape, the size and the like of the conducting path with the micro-nano scale at the position of the other conducting path.
Advantageous effects
(1) The invention provides a method for visually, accurately and quickly displaying the comprehensive contrast image of the conductive path part and the micro-topography characteristic on the surface of the glass sealing structure so as to realize quick and accurate positioning and detection of the conductive path on the surface of the glass sealing structure. The method adopts the mode of controlling the energy, beam intensity, scanning speed, scanning mode and scanning time of the incident focused charged particle beam, utilizes the charged particle beam as a charge input source, utilizes the difference of the intensity of the charge effect induced by the charged particle beam which is controlled and uniformly scanned on the insulating part and the conductive part of the surface of the glass sealing structure, and uses a corresponding detector to collect the excitation signal of the incident charged particle beam to form a comprehensive contrast image of the conductivity degree and the micro-morphology, so that the information of the position, the shape, the size and the like of a conductive path on the surface of the glass insulator can be accurately, quickly and intuitively displayed and obtained, and the quick and accurate positioning and detection of the conductive path on the surface of the glass sealing structure can be further.
(2) The invention relates to a method for quickly and accurately positioning and detecting a conductive path on the surface of a glass sealing structure. The method is used for visually displaying and acquiring the information such as the position, the form, the size and the like of the conductive path on the surface of the glass sealing structure. In particular to application verification and service reliability evaluation of materials, electronic products and electromechanical products. The method is characterized in that incident charged particle beams with specific energy are used as a charge input source to uniformly and repeatedly scan the surface of a glass sealing structure to be detected at a specific scanning speed and a specific number of times, the difference of the conductivity characteristics is utilized to cause the difference of the accumulated charge amount and the strong degree of charge effect on the repulsion effect of the incident electron beams, and the acquired excitation signals of the incident charged particle beams generate the comprehensive contrast difference imaging of the conductivity degree and the micro-morphology of an insulating part and a conductive part, so that the method can be used for realizing the rapid and accurate positioning and detection of a conductive path on the surface of the glass sealing structure.
Drawings
FIG. 1 is a conductive path diagram of the edge of a metal pin of a crystal oscillator;
fig. 2 is a diagram for enlarging the width dimension of the leading edge of the microcracked conductive path obtained by the conductive path.
Detailed Description
And (4) carrying out resistance detection on the glass sealing structure by using a universal meter, a high resistance instrument and other related equipment, and confirming that the glass sealing structure shows abnormal low resistance characteristics. Carefully removing the normal shelter from the surface to be measured of the glass sealing structure, and ensuring that the shelter is removed without causing additional damage to the surface to be measured. And placing the processed glass sealing structure sample in a charged particle beam irradiation system with an electric field accelerator and an electromagnetic lens. Adjusting the distance from a sample to an irradiation source to a proper distance, setting the accelerating voltage, the beam spot size and the beam current intensity of an irradiation system, setting the scanning direction, the scanning speed and the scanning time so that the used controlled focused charged particle beam can uniformly scan the whole surface of the glass sealing structure to be detected at a specific distance for a specific time and a specific number of times, and collecting the excitation signal of the incident charged particle beam by a corresponding detector in the process. And acquiring images after the set scanning time and scanning times are reached, and adjusting parameters such as contrast, brightness and the like of the images if necessary to complete the positioning of the conductive type passage and measure the characteristic parameters of the size. And based on the acquired surface acquisition image of the whole glass sealing structure to be detected, further amplifying the observation area to carry out further amplification observation and measurement on the conductive passage.
A method for accurately positioning a conductive path on the surface of a glass sealing structure comprises the following steps:
(1) and removing the normal shelter from the surface to be measured of the glass sealing structure without damaging the surface to be measured.
(2) An electric field accelerator is used to accelerate certain specific charged particles to specific energy, an electromagnetic lens is used to focus the charged particle beam to a specific beam spot size and control the charged particle beam to a specific beam intensity.
(3) And controlling the controlled charged particle beams to carry out scanning for a specific time and a specific number of times on the whole surface of the glass sealing structure to be detected at a specific distance uniformly by using an electromagnetic lens, wherein the whole surface is scanned for a specific time by using a corresponding detector, and an excitation signal of the incident charged particle beams is collected by using a corresponding detector in the process. In the process of controllably scanning the surface to be detected by the incident charged particle beams, charges are accumulated on the surface of the glass sealing structure to be detected due to the charge effect, and by utilizing the difference characteristic (namely the conductivity difference characteristic) of the insulating region and the conducting path region of the glass sealing structure to the accumulated charge dissipation effect, the accumulated charges on the part with strong insulating property are dissipated slowly, and the accumulated charges on the part with strong conducting property are dissipated quickly. The part with slower accumulated charge dissipation can generate stronger repulsion to the subsequent incident electron beam due to the charge effect, and further generate stronger reflection (repulsion) signals in the collected incident charged particle beam excitation signals, thereby realizing the conductive degree of the insulating part and the conductive part and the comprehensive contrast difference imaging of the micro-morphology, and visually displaying the conductive path part and the micro-morphology characteristics.
(4) And acquiring images after the set scanning time and scanning times are reached, and adjusting parameters such as contrast, brightness and the like of the images if necessary to complete the positioning of the conductive type passage and measure the characteristic parameters of the size.
(5) And based on the acquired surface acquisition image of the whole glass sealing structure to be detected, further amplifying the observation area to carry out further amplification observation and measurement on the conductive passage.
(6) It is generally recommended to use a field emission scanning electron microscope with continuously adjustable acceleration voltage and beam intensity, which is convenient to obtain, for carrying out positioning and detection according to the method.
Examples
A method for positioning and detecting a conductive path on the surface of a glass sealing structure comprises the following steps:
(1) the resistance of a glass sealing structure region of a certain crystal oscillator to the ground (to a shell) is measured by using a multimeter, the resistance is found to be 150M omega and is lower than the technical requirement of 300M omega, and the phenomenon of abnormal low resistance (electric conduction) is confirmed to exist.
(2) And confirming that no shielding object exists on the surface of the glass sealing structure to be detected.
(3) Directly placing the glass sealing structure to be tested in a certain type of field emission scanning electron microscope (the vacuum degree is better than 10)- 3Pa), experiments were performed using a controlled electron beam.
(4) The detector is selected to be a secondary electron detector (SE 2).
(5) The working distance was set at 31 mm.
(6) The accelerating voltage is 10kV and the beam current is 200 pA.
(7) The focusing is clear in the non-observation area of the shell.
(8) To the minimum magnification of the device.
(9) The scanning speed is set to 900ms per frame.
(10) Contrast was adjusted to 23.8% and brightness 50.6%.
(11) Moving the glass sealing structure to the central position area of the glass sealing structure with abnormal low resistance (conduction) in the observation area (1), and adjusting the magnification to enable the view field to cover the whole complete glass sealing structure area.
(12) The scanning speed was adjusted to 4.1s per frame, scanning 10 times.
(13) Acquiring a comprehensive contrast image of the conductivity and the micro morphology to obtain the position and form information of a conductive path: and the crystal oscillator is positioned at the edge of the metal pin of the crystal oscillator and is in the form of surface microcracks. The morphology is shown in FIG. 1. The off-white part of the glass sealing structure is a region with relatively good insulativity, the dissipation is slow after charges are accumulated, the charge effect is strong, and a subsequent incident electron beam is rejected and then is collected by a secondary electron detector to form a strong signal; dark areas, such as low-resistance conductive path areas marked by the figures, have relatively fast dissipation and relatively weak charge effect after accumulating charges, and secondary electron detectors collect relatively weak signals, so that comprehensive contrast images of conductivity and micro-morphology are formed.
(14) Further amplifying the position of the conductive path to 34770 times, and acquiring an image to obtain the width dimension information of the front edge of the microcrack conductive path: about 83 nm. The resolution of the method on the conductive path is better than 100 nm. The morphology is shown in FIG. 2.
By positioning the conductive path, the conductive reason (single factor or comprehensive factor such as cracking, pollutant, inclusion and the like) of the glass sealing structure can be determined, and further, the method can provide specific process improvement and control measure guidance for manufacturers or users and prevent similar fault phenomena of subsequent products.
Claims (8)
1. A method for locating and detecting a conductive path on a surface of a glass sealing structure, the method comprising the steps of:
(1) detecting the insulation resistance of the glass sealing structure by using a resistance detection instrument, wherein when the resistance value of the detected insulation resistance is lower than a set threshold value, the detected glass sealing structure is a sample to be detected, otherwise, the detected glass sealing structure does not need to be subjected to subsequent detection;
(2) clearing the surface shelter of the sample to be detected in the step (1), wherein the surface of the sample to be detected cannot be damaged in the process of removing the shelter;
(3) directly placing a sample to be tested in a vacuum-pumping controlled charged particle beam device for testing, wherein the normal direction of the sample to be tested is parallel to the direction of an incident charged particle beam, then setting the working distance, the accelerating voltage and the beam intensity of a field emission scanning electron microscope, starting to scan and focus, and not focusing in a glass sealing structure area during focusing;
(4) after focusing is clear in the step (3), adjusting to the minimum magnification of the equipment, wherein each frame of the scanning speed is not more than 900ms, and adjusting the contrast ratio to be 20% -45% and the brightness to be 40% -60%;
(5) moving a sample to be detected to the central position of a view field, adjusting the magnification of equipment to enable the whole complete glass sealing structure of the sample to be detected to be positioned in the middle of the view field, and adjusting the scanning speed to be 900ms-5s per frame and the scanning frequency to be 5-30 times;
(6) acquiring comprehensive contrast images of the conductivity degree and the micro morphology to obtain position information of a plurality of conductive paths;
(7) and (5) amplifying the comprehensive contrast image at one position of the conductive path obtained in the step (6) by 500-50000 times, and collecting the image to obtain the shape and size information of the conductive path with the micro-nano scale.
2. The method for locating and detecting the conduction type path on the surface of the glass sealing structure according to claim 1, wherein:
in the step (3), the vacuum degree of the vacuumizable controlled charged particle beam equipment is equal to or better than 10-3Pa。
3. A method for locating and detecting a surface conduction type path of a glass sealing structure according to claim 1 or 2, wherein: the evacuable controlled charged particle beam apparatus is a field emission scanning electron microscope.
4. The method for locating and detecting the conduction type path on the surface of the glass sealing structure according to claim 1, wherein:
in the step (3), the working distance of the field emission scanning electron microscope is 30-50 mm.
5. The method for locating and detecting the conduction type path on the surface of the glass sealing structure according to claim 1, wherein:
in the step (3), the accelerating voltage of the field emission scanning electron microscope is 5kV to 15kV, and the beam current is 100pA to 400 pA.
6. The method for locating and detecting the conduction type path on the surface of the glass sealing structure according to claim 1, wherein:
in the step (3), the detector in the field emission scanning electron microscope is a secondary electron detector SE 2.
7. The method for locating and detecting the conduction type path on the surface of the glass sealing structure according to claim 1, wherein:
in the step (5), the magnification of the equipment is adjusted to enable the whole complete glass sealing structure of the sample to be detected to be located in the middle of the view field even if the center of the whole complete glass sealing structure coincides with the center of the view field.
8. The method for locating and detecting the conduction type path on the surface of the glass sealing structure according to claim 1, wherein:
and (5) taking the sample to be detected out of the field emission scanning electron microscope, removing the charges accumulated on the surface by using an ion fan, repeating the steps (3) to (7), and obtaining the shape and size information of the conducting path with the micro-nano scale at the position of the other conducting path.
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|---|---|---|---|---|
| CN113917243A (en) * | 2021-10-09 | 2022-01-11 | 重庆师范大学 | High-precision optical electroscope device and system based on surface plasmon |
| CN113917243B (en) * | 2021-10-09 | 2023-07-25 | 重庆师范大学 | High-precision optical electroscope device and system based on surface plasmons |
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