CN116699247A - Medium material steady-state X-ray radiation induced conductivity tester - Google Patents
Medium material steady-state X-ray radiation induced conductivity tester Download PDFInfo
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- CN116699247A CN116699247A CN202310408767.7A CN202310408767A CN116699247A CN 116699247 A CN116699247 A CN 116699247A CN 202310408767 A CN202310408767 A CN 202310408767A CN 116699247 A CN116699247 A CN 116699247A
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- 230000005855 radiation Effects 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 63
- 239000003989 dielectric material Substances 0.000 claims abstract description 26
- 238000012545 processing Methods 0.000 claims abstract description 25
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- 238000005259 measurement Methods 0.000 abstract description 30
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- 239000010931 gold Substances 0.000 description 15
- 229910052737 gold Inorganic materials 0.000 description 15
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 14
- 239000004642 Polyimide Substances 0.000 description 11
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- 229920001721 polyimide Polymers 0.000 description 11
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 229910002482 Cu–Ni Inorganic materials 0.000 description 1
- 240000008086 Echinocereus enneacanthus Species 0.000 description 1
- 235000010837 Echinocereus enneacanthus subsp brevispinus Nutrition 0.000 description 1
- 235000006850 Echinocereus enneacanthus var dubius Nutrition 0.000 description 1
- 101100421299 Schizosaccharomyces pombe (strain 972 / ATCC 24843) set7 gene Proteins 0.000 description 1
- 229910020836 Sn-Ag Inorganic materials 0.000 description 1
- 229910020988 Sn—Ag Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
- G01R27/08—Measuring resistance by measuring both voltage and current
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R27/00—Arrangements for measuring resistance, reactance, impedance, or electric characteristics derived therefrom
- G01R27/02—Measuring real or complex resistance, reactance, impedance, or other two-pole characteristics derived therefrom, e.g. time constant
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The application discloses a medium material steady-state X-ray radiation induced conductivity tester, which comprises a vacuum box, wherein an X-ray source is further arranged outside the vacuum box, a sample clamping unit is further arranged inside the vacuum box, and the X-ray source can irradiate the sample clamping unit; the sample clamping unit is connected with a signal processing unit arranged outside the vacuum box, and the signal processing unit is also connected with an X-ray source; the steady-state X-ray radiation induction conductivity tester for the dielectric material can well generate continuous energy and monoenergetic X-rays and analyze and test the radiation induction conductivity of the dielectric material under the action of the X-rays; the device has good electromagnetic shielding performance and X-ray collimation shielding performance while realizing the measurement of the steady-state X-ray radiation induction conductivity of the semiconductor material, and can ensure that the X-rays emitted by an X-ray source only irradiate on a sample to be measured, thereby effectively eliminating the influence of the X-rays on a signal processing module.
Description
Technical Field
The application relates to the technical field of conductivity testing, in particular to a dielectric material steady-state X-ray radiation induced conductivity tester.
Background
With the development of space technology, a large number of aircraft electronic devices and systems are threatened by space radiation environments, and with the increase of spacecraft operating voltages, the probability of dielectric damage increases. The combination effect of high working voltage and high-energy particles influences the charge and discharge process of the medium, the damage probability of the material is improved, and higher requirements are put forward for the design of insulating materials and radiation structures. X-rays are typical space radiation environments and are widely applied to the research fields of cable X-ray radiation effect, electromagnetic pulse effect of an X-ray system and the like.
The X-ray is taken as a main component of strong ionizing radiation, and the phenomenon of surface and deep charging of a dielectric material caused by the X-ray can lead to the generation of radiation induced conductivity, so that the probability of surface flashover or body breakdown of the material is increased, and the service life of equipment is reduced. The phenomenon of reduced dielectric strength of dielectric materials has limited the further development of many electrical vacuum devices. Radiation-sensitive conductivity measurement is one of the important parameters for studying the radiation effect of a material.
The monoenergetic X-ray has wide application in scientific researches such as quantitative element determination, medical imaging radiography, radiation detector calibration and the like, and is inconvenient to develop related researches due to wide distribution of the emergent energy spectrum of the conventional X-ray tube. The method for generating the monoenergetic X-rays is quite a lot, but compared with other modes, the K fluorescence has the advantages of large dosage rate, good monochromaticity, simple device construction and the like, and is suitable for the research in a small laboratory. At present, a plurality of devices for generating monoenergetic X-rays based on the method exist at home and abroad.
However, the prior art lacks a special device for generating continuous energy and monoenergetic X-rays and analyzing and testing the radiation induction conductivity of the dielectric material under the action of the X-rays. Therefore, the radiation effect of the dielectric material under the action of X rays is studied, and the measurement of the radiation induced conductivity is of great significance.
Disclosure of Invention
Aiming at the defects existing in the prior art, the application aims to provide a steady-state X-ray radiation induction conductivity tester for a dielectric material, which solves the problem that special equipment for generating continuous energy and single-energy X-rays and analyzing and testing the radiation induction conductivity of the dielectric material under the action of the X-rays is not available in the prior art.
In order to solve the technical problems, the application adopts the following technical scheme: the medium material steady-state X-ray radiation induced conductivity tester comprises a vacuum box, wherein an X-ray source is further arranged outside the vacuum box, a sample clamping unit is further arranged inside the vacuum box, and the X-ray source can irradiate the sample clamping unit;
the sample clamping unit is connected with a signal processing unit arranged outside the vacuum box, and the signal processing unit is also connected with an X-ray source.
The application also has the following technical characteristics:
the sample clamping unit comprises a first sample clamping mechanism,
the first sample clamping mechanism is detachably arranged on the inner wall of the vacuum box and comprises a first fixing plate and a first stud for mounting the first fixing plate on the inner wall of the vacuum box;
the first sample clamping mechanism further comprises a mounting bracket detachably arranged in the vacuum box, and a collimating lead cylinder with two open ends is arranged on the mounting bracket;
x-rays emitted by the X-ray source can pass through the collimating lead cylinder to irradiate on the first fixed plate;
the first fixed plate is connected with the signal processing unit;
the vacuum box comprises a box body provided with a vacuum cavity and a cover plate matched with the box body;
the X-ray source is used for making X-rays incident on the sample clamping unit through a vacuum window arranged on the bottom plate of the box body;
a first side wall of the box body is provided with a test signal interface, one end of the test signal interface is connected with the sample clamping unit, the other end is connected with the signal processing module,
the sample clamping unit also comprises a second sample clamping mechanism;
the second sample clamping mechanism comprises a fluorescent target, wherein the fluorescent target is placed at an angle of 45 degrees with an incident light path of the X-ray source, and the fluorescent target is arranged on the incident light path of the X-ray source;
the second sample clamping mechanism further comprises a light filter, wherein the light filter is arranged in parallel with an incident light path of the X-ray source and is arranged on a light path of fluorescent X-rays generated after the X-ray source irradiates the fluorescent target;
the second sample clamping mechanism further comprises a shielding plate, the shielding plate is arranged on one side of the optical filter, which is opposite to the fluorescent target, a second fixing plate is arranged on one side of the shielding plate, which is opposite to the optical filter, and the second fixing plate is connected with the shielding plate through a second stud;
the second fixed plate is connected with the signal processing unit;
the first fixing plate comprises a bottom plate and two spring clamping pieces which are arranged on the bottom plate through guide rails, the two spring clamping pieces are respectively connected with a wire, the wire is connected with a connecting-out terminal arranged on the bottom plate,
the output terminal is used for connecting with a test signal interface;
the structure of the second fixing plate is the same as that of the first fixing plate;
the vacuum box is also provided with a vacuumizing device,
the vacuum pumping device comprises a dry pump and a molecular pump which are connected, and the molecular pump is connected with a vacuum flange arranged on the vacuum box through a four-way joint;
and the four-way valve is also connected with a vacuum gauge and a deflation valve.
The signal processing unit comprises a Pianpi meter and a high-voltage source which are connected with the test signal interface, wherein the Pianpi meter is connected with the high-voltage source, and the Pianpi meter is connected with the industrial personal computer;
the industrial personal computer is connected with an X-ray source.
Compared with the prior art, the application has the following technical effects:
the steady-state X-ray radiation induction conductivity tester for the dielectric material can well generate continuous energy and monoenergetic X-rays and analyze and test the radiation induction conductivity of the dielectric material under the action of the X-rays.
And (II) the steady-state X-ray radiation induction conductivity tester for the dielectric material ensures that the device has good electromagnetic shielding performance and X-ray collimation shielding performance while measuring the steady-state X-ray radiation induction conductivity of the dielectric material. The vacuum cavity and the vacuum cavity cover are made of aluminum and stainless steel respectively, and the sample card is connected with an external instrument wiring by a shielding wire, so that electromagnetic interference is prevented from affecting a measurement result. The arrangement of the collimation lead cylinder and the shielding plate can enable the X-rays emitted by the X-ray source to be irradiated on the sample to be detected, so that the influence of the X-rays on the signal processing module is effectively eliminated.
And (III) the device can realize radiation induction conductivity measurement under different bias voltages and X-ray dosage rates and radiation induction conductivity measurement under different energy monoenergetic X-ray radiation in one set of equipment by arranging the detachable first sample clamping mechanism and the detachable second sample clamping mechanism.
The medium material steady-state X-ray radiation induced conductivity tester is simple in structure, convenient to operate, safe, reliable and high in adaptability.
Drawings
FIG. 1 is a schematic view showing the overall structure of embodiment 1 of the present application;
FIG. 2 is a schematic diagram of a first mounting plate structure and a test circuit connection according to the present application;
FIG. 3 is a schematic view showing the overall structure of embodiment 2 of the present application;
FIG. 4 is a measurement flow chart of the present application;
FIG. 5 is a graph showing percent verification of radiant induction conductivity test deviations for alumina ceramic samples;
FIG. 6 is a graph of conductivity measurements of polyimide samples at different X-ray dose rates;
FIG. 7 is a plot of polyimide conductivity as a function of X-ray dose rate versus bias electric field;
FIG. 8 is a comparison of polyimide conductivity experimental results with simulated calculations;
FIG. 9 is an outgoing X-ray energy spectrum for different operating voltages of an X-ray tube;
FIG. 10 is an X-ray energy spectrum after treatment with a fluorescent target and a filter;
FIG. 10 (a) is an X-ray energy spectrum before filtering by a filter;
FIG. 10 (b) is an X-ray energy spectrum after filtering by a filter;
FIG. 11 shows the results of various X-ray energy conductivity measurements of polyimide materials;
FIG. 12 is a graph of radiation induced conductivity of polyimide material versus X-ray tube current and X-ray energy.
Meaning of the individual reference numerals in the drawings:
1-a vacuum box; a 2-X-ray source; a 3-signal processing unit; 4-a first sample clamping mechanism; the device comprises a 5-second sample clamping mechanism, a 6-vacuumizing device, a 7-sealing structure, an 8-sample, a 9-gold electrode, a 10-corrugated pipe, an 11-shielding cable, a 12-GPIB-USB communication line, a 13-USB communication line and a 14-optical clamp;
1-1 of a box body, 1-2 of a cover plate, 1-3 of a test signal interface and 1-4 of a vacuum flange;
3-1 Pian meter, 3-2 high-voltage source and 3-3 industrial personal computer;
4-1 of a first fixing plate, 4-2 of a first stud, 4-3 of a mounting bracket and 4-4 of a collimation lead cylinder;
4-1-1 bottom plate, 4-1-2 guide rail, 4-1-3 spring clip, 4-1-4 wire, 4-1-5 outlet terminal;
the fluorescent lamp comprises a 5-1 fluorescent target, a 5-2 optical filter, a 5-3 shielding plate, a 5-4 second fixing plate and a 5-5 second stud;
6-1 dry pump, 6-2 molecular pump, 6-3 four-way, 6-4 vacuum gauge, 6-5 air release valve;
the following examples illustrate the application in further detail.
Detailed Description
The following specific embodiments of the present application are provided, and it should be noted that the present application is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical scheme of the present application fall within the protection scope of the present application.
The terms "upper," "lower," "front," "rear," "top," "bottom," and the like are used herein to refer to an orientation or positional relationship for ease of description and simplicity of description only, and are not intended to indicate or imply that the devices or elements being referred to must be oriented, configured and operated in a particular orientation, with "inner," "outer" referring to the inner and outer sides of the corresponding component profiles, and the above terms are not to be construed as limiting the application.
In the present application, unless otherwise indicated, the terms "mounted," "connected," "secured," and the like are to be construed broadly and may be, for example, fixedly connected or detachably connected or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present application can be understood by those skilled in the art according to the specific circumstances.
All parts of the application, unless otherwise specified, are known in the art.
As shown in fig. 1, the embodiment provides a dielectric material steady-state X-ray radiation induction conductivity tester, which comprises a vacuum box 1, wherein an X-ray source 2 is further installed outside the vacuum box 1, a sample clamping unit is further installed inside the vacuum box 1, and the X-ray source 2 can irradiate the sample clamping unit;
the sample clamping unit is connected with a signal processing unit 3 arranged outside the vacuum box 1, and the signal processing unit 3 is also connected with an X-ray source 2;
the sample clamping unit comprises a first sample clamping mechanism 4,
the first sample clamping mechanism 4 is detachably arranged on the inner wall of the vacuum box 1 and comprises a first fixing plate 4-1 and a first stud 4-2 for mounting the first fixing plate 4-1 on the inner wall of the vacuum box 1;
the first sample clamping mechanism 4 also comprises a mounting bracket 4-3 which is detachably arranged in the vacuum box 1, and the mounting bracket 4-3 is provided with a collimation lead cylinder 4-4 with two open ends;
x-rays emitted by the X-ray source 2 can pass through the collimating lead drum 4-4 to irradiate the first fixing plate 4-1;
the first fixing plate 4-1 is connected with the signal processing unit 3;
the vacuum box 1 comprises a box body 1-1 provided with a vacuum cavity and a cover plate 1-2 matched with the box body;
the X-ray source 2 is used for making X-rays incident on the sample clamping unit through a vacuum window arranged on the bottom plate of the box body 1-1;
the first side wall of the box body 1-1 is provided with a test signal interface 1-3, one end of the test signal interface 1-3 is connected with the sample clamping unit, and the other end is connected with the signal processing unit 3.
The sample clamping unit also comprises a second sample clamping mechanism 5;
the second sample clamping mechanism 5 comprises a fluorescent target 5-1, wherein the fluorescent target 5-1 is placed at an angle of 45 degrees with an incident light path of the X-ray source 2, and the fluorescent target 5-1 is arranged on the incident light path of the X-ray source;
the second sample clamping mechanism 5 further comprises an optical filter 5-2, the optical filter 5-2 is arranged in parallel with an incident light path of the X-ray source 2, and the optical filter 5-2 is arranged on a light path of fluorescent X-rays generated after the X-ray source 2 irradiates the fluorescent target 5-1;
the second sample clamping mechanism 5 further comprises a shielding plate 5-3, the shielding plate 5-3 is arranged on one side of the optical filter 5-2, which is opposite to the fluorescent target 5-1, a second fixing plate 5-4 is arranged on one side of the shielding plate 5-3, which is opposite to the optical filter 5-2, and the second fixing plate 5-4 is connected with the shielding plate 5-3 through a second stud 5-5;
the second fixing plate 5-4 is connected with the signal processing unit 3;
the first fixing plate 4-1 comprises a bottom plate 4-1-1 and two spring clamping pieces 4-1-3 arranged on the bottom plate 4-1-1 through guide rails 4-1-2, wherein the number of the spring clamping pieces 4-1-3 is two, the guide rails 4-1-2 are respectively connected with a lead 4-1-4, the lead 4-1-4 is connected with a connecting-out terminal 4-1-5 arranged on the bottom plate 4-1,
the output terminals 4-1-5 are used for connecting the test signal interfaces 1-3;
the second fixing plate 5-4 has the same structure as the first fixing plate 4-1.
The vacuum box 1 is also provided with a vacuumizing device 6,
the vacuum pumping device 6 comprises a dry pump 6-1 and a molecular pump 6-2 which are connected, wherein the molecular pump 6-2 is connected with a vacuum flange 1-4 arranged on the vacuum box 1 through a four-way 6-3;
the four-way valve 6-3 is also connected with a vacuum gauge 6-4 and a deflation valve 6-5.
The signal processing unit 3 comprises a Pitay meter 3-1 and a high-voltage source 3-2 which are connected with the test signal interface 1-3, wherein the Pitay meter 3-1 is connected with the high-voltage source 3-2, and the Pitay meter 3-1 is connected with the industrial personal computer 3-3;
the industrial personal computer 3-3 is connected with the X-ray source 2;
the conductivity measurement of the application adopts a two-electrode structure of electrode-sample-electrode. The two spring clamping pieces 4-1-3 are fixed on the guide rail 4-1-2 of the bottom plate 4-1-1 in a positive-negative mode and are guaranteed to be in contact with the gold electrodes 9 on two sides of the sample 8, and correspondingly, a certain voltage is applied to the gold electrodes 9 through the high-voltage source 3-2 to generate an approximate uniform bias electric field, and the electric field strength E of the approximate uniform bias electric field is given by the formula (1).
Wherein E is the electric field intensity inside the sample, in units of: v cm -1 The method comprises the steps of carrying out a first treatment on the surface of the U is the voltage at two ends of the sample, unit: v, V; d is the thickness of the sample, unit: cm.
The LABVIEW software is installed on the industrial personal computer 3-3 and is used for real-time monitoring of radiation induction conductivity measurement and integrated control of the whole measurement process. The software comprises an X-ray tube control module, a parameter input module, a data acquisition and analysis module and a conductivity real-time monitoring module, and supports the control of the working state of the X-ray source 2, the input of testing initial conditions, the control of instruments and meters, the real-time transmission, calculation, display and storage of measured data, and the specific measurement flow of the software is shown in figure 4.
The X-ray tube control module is used for controlling the emission state of the X-ray source 2, is realized by embedding the control program of the X-ray source after being converted into Chinese into the LABVIEW program, and can change the energy spectrum distribution and intensity of the emergent X-rays by setting voltage and current respectively. Clicking the voltage enable and current enable buttons can apply set voltage and current values to the X-ray source 2, the voltage and the current are displayed in real time through a text window below, and clicking the lock can keep the state of the X-ray tube unchanged. Clicking on "X-ray enable" the X-ray source 2 will emit corresponding X-rays. The duration of X-ray emission by the X-ray source 2 can also be set by the following "on time" and "off time" input boxes.
The parameter input module is used for inputting parameters required by conductivity test, including bias voltage, sample thickness, electrode diameter, X-ray source voltage and current, sample number and test time. The software will perform the calculation of the conductivity in combination with the corresponding parameters.
The data acquisition and analysis module is used for acquiring the measurement data of the Pitaya table 3-1 from the GPIB-USB communication line 12, and carrying out calculation of conductivity by a two-electrode method in combination with the input parameters. Based on the definition of resistivity and its relation to conductivity, the software calculates the conductivity σ of sample 8 from the data read from each measurement, as shown in equation (2):
wherein σ is the conductivity of the sample, unit: omega shape -1 ·cm -1 The method comprises the steps of carrying out a first treatment on the surface of the ρ is the resistivity of the sample in units of: omega cm; u is the voltage at two ends of the sample, unit: v, V; i is the current through the sample in units of: a, A is as follows; r is the electrode radius, unit: cm; d is the thickness of the sample, unit: cm.
The conductivity real-time monitoring module is used for displaying the result of each measurement in the conductivity testing process, namely the current instantaneous conductivity. After the conductivity data is obtained through each calculation, a line graph of the instantaneous value of the conductivity along with time is drawn through a waveform chart so as to grasp the real-time change condition of the conductivity in the whole measurement process. After the test is completed, the software can save the conductivity data for this test as a text document of txt for later mapping and further processing.
Example 1:
the medium material steady-state X-ray radiation induced conductivity tester in the embodiment comprises a first sample clamping mechanism 4, an X-ray source 2, a collimation lead cylinder 4-4 and a mounting bracket 4-3, wherein a sample card 1 is used for fixing a sample 8 and two gold electrodes 9 for leading out the sample 8;
the X-ray source 2 can be set with working voltage of 0-70 kV, working current of 0-1000 mu A, maximum power of 12W and X-ray with 742mGy/s dosage rate under the maximum power;
the inner diameter of the collimation lead cylinder 4-4 is 20mm, so that the X-ray emitted by the X-ray source 2 can be collimated, the X-ray can only irradiate the sample 8, the influence of the X-ray on other circuit cables is eliminated, and the X-ray collimation shielding performance is realized;
the signal processing unit 3 mainly comprises a Jili 6485 Pi Ann table 3-1, a Stanford PS350 high-voltage source 3-2 and an industrial personal computer 3-3, wherein the industrial personal computer 3-3 is provided with on-line monitoring software;
the vacuum pumping device 6 mainly comprises a dry pump 6-1 and a molecular pump 6-2 which are connected, wherein the molecular pump 6-2 is connected with a vacuum flange 1-4 arranged on the vacuum box 1 through a four-way 6-3;
the four-way valve 6-3 is also connected with a vacuum gauge 6-4 and a deflation valve 6-5. The vacuum pump group is used for vacuumizing, and the interior of the cavity can reach about 10 -3 Vacuum environment of mBar.
Sample 8The material is KAPTON TM Polyimide medium material, which is a circular film with a diameter of 38mm and a thickness of 75 μm, wherein a sample 8 is arranged on a bottom plate 4-1-1, and the surfaces of two sides of the sample 8 are plated with circular gold electrodes 9 with a diameter of 36mm by an ion sputtering instrument, and the circular gold electrodes are used as nodes measured by a two-electrode method; the bottom plate 4-1-1 is of a double-layer structure, two layers of holes with a large hole and a small hole are respectively formed in the middle of the two layers, the diameter of the large hole is 38mm, the small hole is slightly smaller, a formed circular groove can fix the sample 8 in the hole, four fixing holes are formed around the circular groove, and the circular groove can be fixed through the stud 4-2; the spring clamping piece 4-1-3 can move towards the center of the sample 8 within the distance specified by the adjusting guide rail 4-1-2 so as to perform fine adjustment; the outgoing terminal 4-1-5 has two interfaces, and is connected with the adjusting guide rail 4-1-2 through the lead wires 4-1-4 in the bottom plate 4-1-1, so as to ensure the contact between the outgoing terminal 4-1-5 and the round gold electrode 9.
The hardware connection relation of the instrument is as follows: the front surface of the vacuum box 1 is provided with an opening and is connected with the X-ray source 2 through a sealing structure 7; the collimation lead cylinder 4-4 is fixed in the middle of the vacuum box 1 through the mounting bracket 4-3; a first fixing plate 4-1 in a first sample clamping mechanism 4 inside the vacuum box 1 is fixed on the cover plate 1-2 through a first stud 4-2;
the dry pump 6-1 is connected with the molecular pump 6-2 through a corrugated pipe 10 to form a vacuum pump group; the side surface of the vacuum box 1 is connected with a vacuum pump set through a vacuum flange 1-4, a four-way joint 6-3 and a corrugated pipe 10, and a vacuum gauge 6-4 and a deflation valve 6-5 are also connected to the four-way joint 6-3; the other side of the vacuum box 1 is provided with a test signal interface 1-3 for connecting the sample 8 in the vacuum box 1 with an external test circuit.
The electrical connection relation of the instrument is as follows: as shown in fig. 2, the PS350 high voltage source 3-2 and the two gold electrodes 9, 6485 picoampere meter 3-1 of the sample are connected in series to form a measurement loop, specifically, the two terminals led out are respectively connected to the positive polarity terminals of the PS350 high voltage source 3-2 and the 6485 picoampere meter 3-1, and the negative polarity terminals of the two instruments are connected together and connected with the ground wire; 6485 Pi An table 3-1 links to each other with industrial computer 3-3 through GPIB-USB data line 12, guarantees that the in-process of measuring can communicate smoothly.
The test flow of the instrument is as follows:
first, preparing a sample, and connecting all components of a placing instrument.
(1) Plating gold on two sides of the sample 8 by using an ion sputtering instrument, perforating a gold plating mould, wherein the power of the ion sputtering instrument is 18W, and the sputtering time of each side is 60s;
(2) The two spring clamping pieces 4-1-3 are fixed on the two guide rails 4-1-2 on the opposite sides of the bottom plate 4-1-1 in a positive-negative way through studs, the sample 8 is fixed in a circular groove in the middle of the bottom plate 4-1-1, the contact with gold electrodes 9 on the two sides of the sample 8 is ensured, and the bottom plate 4-1-1 is fixed on the cover plate 1-2 through the first studs 4-2 of four M2;
(3) Connecting the outgoing terminals 4-1-5 with the test signal interface 1-3 by using two high-voltage-resistant wires;
(4) A mounting bracket 4-3 and a collimation lead cylinder 4-4 are arranged in the vacuum box 1;
(5) Mounting the cover plate 1-2 on the vacuum box 1;
(6) An X-ray source 2 is mounted on the front side of the vacuum box 1.
And secondly, connecting a testing instrument with a communication line and vacuumizing.
(7) According to the electric connection relation, the shielding cable 11 is utilized to connect the test signal interface 1-3 with the high voltage source 3-2 and 6485 Piampere meter 3-1 of the test instrument PS 350;
(8) The GPIB-USB communication line 12 is used for connecting the 6485 Pi-an meter 3-1 and the industrial personal computer 3-3, so that the two can be communicated normally;
(9) The X-ray source 2 is connected with the industrial personal computer 3-3 by a USB communication line 13, so that the X-ray source and the industrial personal computer can normally communicate;
(10) The dry pump 6-1 is turned on. And observing the indication number of the vacuum gauge 6-4, and starting the molecular pump 6-2 when the air pressure in the vacuum box 1 is basically stable, and waiting for the air pressure in the cavity to be stable again.
And thirdly, starting to conduct conductivity test.
(11) Starting power supplies of a PS350 high-voltage source 3-1 and a 6485 Pi-ampere meter 3-1 of a testing instrument, starting LABVIEW testing software installed on an industrial personal computer, and inputting information such as bias voltage, sample size, sample number, testing date and the like of the current test into a software interface;
(12) The operating voltage of the X-ray source was preset to 50kV and the operating current to 25. Mu.A. Setting the bias voltage of a PS350 high-voltage source to be 600V, enabling high-voltage output, and generating a bias electric field of 8kV/mm in the sample;
(13) Clicking the "start" button on the test software initiates the software, starting the conductivity test. And observing a software interface conductivity curve graph, enabling the X-ray source 2 to generate X-rays with a certain dosage after the software interface conductivity curve graph tends to be stable, enabling the conductivity to be basically stable after about 35-60 minutes, closing the X-ray source 2, waiting for the conductivity to change to an initial level, closing test software, and closing the output of the PS350 high-voltage source 3-2. The software automatically stores the waveform data of the test;
(14) And (3) replacing a new sample 8 on the first sample clamping mechanism 4, and changing test conditions, which can comprise bias voltage, working voltage and current of the X-ray source 2, repeating the steps (11) - (13), and performing a new group of tests to realize radiation induction conductivity measurement under different bias voltages and dose rates.
Example 2:
as shown in fig. 3, the dielectric material steady-state X-ray radiation induced conductivity tester in the present embodiment includes a second sample clamping mechanism 5, an X-ray source 2, a fluorescent target 5-1, an optical filter 5-2, a shielding plate 5-3, and an optical clamp 14. The second sample clamping mechanism 5 is used for fixing a sample 8 and leading out two gold electrodes 9 of the sample 8; the X-ray source 2 can be set with working voltage of 0-70 kV, working current of 0-1000 mu A, maximum power of 12W and X-ray with 742mGy/s dosage rate under the maximum power; the fluorescent target 5-1 is matched with the optical filter 5-2, the material of the fluorescent target 5-1 is Cu/Nb/Sn (according to the required energy of the generated X-rays), the thickness is 0.3mm, the diameter is 80mm, the fluorescent target is used for generating fluorescent X-rays with specific energy, the material of the optical filter 5-2 is Ni/Zr/Ag, the thickness is 0.015/0.12/0.12mm, the diameter is 60mm, the fluorescent target is used for filtering out other clutters of the fluorescent X-rays, and the energy spectrum received by a sample is purified. The three fluorescent targets and filters combination were capable of generating monoenergetic X-rays with energies of 8.01/16.58/25.26keV, respectively. The X-ray shielding plate 5-3 is 8mm thick, the front size is 170 multiplied by 170mm, the diameter of the middle through hole is 38mm, and the X-ray emitted by the X-ray source 2 can be shielded and collimated, so that the X-ray only irradiates the sample 8, the influence of the X-ray on other circuit cables is eliminated, and the X-ray shielding plate has good collimation shielding performance; the signal transmission and acquisition module mainly comprises a 6485 Pi-ampere meter 3-1, a Stanford PS350 high-voltage source 3-1 and an industrial personal computer 3-3, wherein the industrial personal computer 3-3 is provided with on-line monitoring software, so that the input and configuration of experimental conditions, the real-time display of sample conductivity and the control of other instruments and meters are supported; the vacuum pumping device 6 mainly comprises a dry pump 6-1 and a molecular pump 6-2 which are connected, wherein the molecular pump 6-2 is connected with a vacuum flange 1-4 arranged on the vacuum box 1 through a four-way 6-3;
the four-way valve 6-3 is also connected with a vacuum gauge 6-4 and a deflation valve 6-5. The vacuum pump group is used for vacuumizing, and the interior of the cavity can reach about 10 -3 Vacuum environment of mBar.
The sample 8 was clamped in the same manner as in example 1.
The hardware connection relation of the instrument is as follows:
the front surface of the box body 1-1 is provided with a hole and is connected with an X-ray source 2 through a sealing structure 10; the fluorescent target 5-1 and the X-ray source 2 are placed at an angle of 45 degrees, so that rays are enabled to enter in an inclined direction of the angle, fluorescent X-rays are generated, the optical filter 5-2 and the fluorescent target 5-1 are placed at an angle of 45 degrees and parallel to an incident light path, and the emitted fluorescent X-rays can be received; the shielding plate 5-3 is placed behind the optical filter 5-2, and the first fixing plate 4-1 is fixed behind the shielding plate 5-3 in parallel; the fluorescent target 5-1, the optical filter 5-2 and the shielding plate 5-3 are fixed on the inner side of the box body 1-1 through an optical clamp 16;
the remaining connections and calculation methods are the same as in example 1.
The test flow of the instrument is as follows:
first, preparing a sample, connecting all components of a placing instrument and vacuumizing.
(1) Plating gold on two sides of the sample 8 by using an ion sputtering instrument, perforating a gold plating mould, wherein the power of the ion sputtering instrument is 18W, and the sputtering time of each side is 60s;
(2) The two spring clamping pieces 4-1-3 are fixed on the two guide rails 4-1-2 on the opposite sides of the bottom plate 4-1-1 in a positive-to-negative mode through studs, the sample 8 is fixed in a groove in the middle of the bottom plate 4-1-1, good contact with gold electrodes 9 on the two sides of the sample 8 is ensured, and the bottom plate 4-1-1 is fixed on the shielding plate 5-3 through the first studs 4-2 of four M2;
(3) Connecting the outgoing terminals 4-1-5 with the test signal interface 1-3 by using two high-voltage-resistant wires;
(4) Selecting a proper fluorescent target 5-1 and an optical filter 5-2 (Cu-Ni is a group, nb-Zr is a group and Sn-Ag is a group), fixing the materials by an optical clamp 16, placing an X-ray source 2 at an angle of 45 degrees with the fluorescent target 5-1, placing the optical filter 5-2 at an angle of 45 degrees with the fluorescent target 5-1 and parallel to an incident light path of X-rays, and placing a shielding plate 5-3 behind the optical filter 5-2;
(5) The cover plate 1-2 is arranged on the box body 1-1;
(6) An X-ray source 2 is mounted on the front surface of the case 1-1.
And secondly, connecting a testing instrument with a communication line and vacuumizing.
(7) According to the electric connection relation, the shielding cable 11 is utilized to connect the test signal interface 1-3 with the high voltage source 3-2 and 6485 Piampere meter 3-1 of the test instrument PS 350;
(8) The GPIB-USB communication line 12 is used for connecting the 6485 Pi-an meter 3-1 with the industrial personal computer, so that the two can normally communicate;
(9) The X-ray source 2 is connected with the industrial personal computer 3-3 by a USB communication line 13, so that the X-ray source and the industrial personal computer can normally communicate;
(10) The dry pump 6-1 is turned on. And observing the indication number of the vacuum gauge 6-4, and starting the molecular pump 6-2 after the air pressure in the box body 1-1 is basically stable, and waiting for the air pressure in the cavity to be stable again.
And thirdly, starting to conduct conductivity test.
(11) Starting power supplies of a PS350 high-voltage source 3-2 and a 6485 Pi-ampere meter 3-1 of a testing instrument, starting LABVIEW testing software installed on an industrial personal computer 3-3, and inputting information such as bias voltage, sample size, sample number, testing date and the like of the current test into a software interface;
(12) The operating voltage of the X-ray source 2 was set to 50kV and the operating current to 25 ua. Setting the bias voltage of the PS350 high-voltage source 3-2 to be 600V, enabling high-voltage output, and generating a bias electric field of 8kV/mm in the sample 8;
(13) Clicking the "start" button on the test software initiates the software, starting the conductivity test. And observing a software interface conductivity curve graph, enabling the X-ray source 2 to generate X-rays with a certain dosage after the software interface conductivity curve graph tends to be stable, enabling the conductivity to be basically stable after about 35-60 minutes, closing the X-ray source, waiting for the conductivity to change to an initial level, closing test software, and closing the PS350 high-voltage source 3-2 output. The software automatically stores the waveform data of the test;
(14) Changing a new sample 8 onto the sample card 1, changing test conditions, including bias voltage, working voltage and current of the X-ray source 2, repeating the steps (11) - (13), and performing a new set of tests to realize radiation induction conductivity measurement under different bias voltages and dose rates;
(15) And (3) replacing a new set of fluorescent targets 5-1 and optical filters 5-2, replacing a new sample 8, and repeating the steps (11) - (14) to measure the radiation induction conductivity under the radiation of different energy monoenergetic X rays.
Application example 1: this application example was performed using the apparatus of example 1:
1. dielectric material conductivity test deviation percentage verification
And continuously measuring the alumina ceramic sample with the same dielectric material for a plurality of times to realize the detection of the measurement deviation of the instrument test result. The same sample was repeatedly measured at one hour intervals, and the irradiation time period of the X-rays was also controlled to one hour, and the test results are shown in fig. 5. Since the sample has a certain fluctuation between the steady-state values of the conductivity measured by the system in four continuous measurements, the maximum deviation is 1×10 -13 Ω -1 cm -1 About 6% of the steady state measurement mean, the overall measurement bias of the system is about 6%.
2. Continuous energy X-ray test results and analysis of dielectric materials
FIG. 6 is a graph of the conductivity of polyimide samples at different X-ray dose rates tested at a bias voltage of 300V and a bias electric field of 4 kV/mm. The conductivity stabilized at 10 before the sample was irradiated -18 Ω -1 ·cm -1 On the order of magnitude, the conductivity of a sample will rise rapidly in about tens of seconds after it has been irradiated1-3 orders of magnitude, then reach respective stable values, all at 10 -15 Ω -1 ·cm -1 On the order of magnitude, after turning off the X-ray irradiation, the sample conductivity drops exponentially to the initial level within hundreds of seconds. And compared with the results of multiple tests, the instrument has the advantages of good measurement stability and repeatability and good measurement noise inhibition effect.
As shown in fig. 7, the average value of the conductivity stability time period under irradiation under each test condition was taken to obtain the relationship of the conductivity with the bias electric field under different X-ray dose rates. It can be seen that when a polyimide sample is irradiated to a steady state, its conductivity is linear with the bias electric field. Fig. 8 shows simulation calculation results of radiation induction conductivity of the sample under different bias electric field conditions, which can be well matched with experimental results, and can also prove that the accuracy of the measurement result of the instrument is better.
Application example 2: this application example was performed using the apparatus of example 2:
3. monochromizing effect of K fluorescence method on emergent X-ray
Fig. 9 shows the energy spectrum of the X-ray source 2 emitting X-rays under different operating voltages, wherein the energy spectrum distribution width can reach 70keV, and the characteristic peaks are mainly distributed in 8-12 keV energy segments.
FIG. 10 shows the results of spectral simulation of two positions before and after the filter has been filtered by different sets of fluorescent targets and filters. As can be seen from FIG. 10 (a), the energy spectrum of the K fluorescent X-ray has a certain single energy compared with the X-ray tube emission spectrum, and the main energy peak energies of the X-rays scattered by the three fluorescent targets are respectively 8.01keV, 16.58keV and 25.26keV. But the spectral lines are not pure enough. As can be seen from FIG. 10 (b), the filter filters out other spectral lines which are not relevant, and the monoenergetic of the emergent X-ray energy spectrum is greatly improved.
4. Single-energy X-ray test result and analysis of dielectric material
FIG. 11 shows the results of measurements of the conductivity of polyimide samples at different X-ray energies and X-ray tube currents. As can be seen from the graph, the conductivity of the polyimide can be stabilized at about @ before the X-rays are turned on, regardless of the experimental conditions set7～8)×10 -16 Ω -1 ·cm -1 . At the moment of X-ray turning on, the conductivity rises rapidly, then falls slowly until reaching a stable state, and the stable value is 10 -16 ～10 -15 Ω -1 ·cm -1 The range, the stable value is related to the current experimental conditions. The stability and repeatability of the measurement of the instrument are good and the effect of suppressing the measurement noise is also good by comparing the test results of multiple times.
Radiation induced conductivity is defined as the amount of change in conductivity of a material before and after irradiation. The change in average conductivity over a small period of time before and after X-ray shutdown was therefore taken as the radiation induced conductivity measured for this set of experiments and analyzed for its relationship to the X-ray tube current. As shown in FIG. 12, it is understood that the radiation induced conductivity of the polyimide sample was about 10 under the experimental conditions -16 Ω -1 ·cm -1 Magnitude. At all three X-ray energies, the radiation induced conductivity increases linearly with increasing X-ray tube current. The increase is most pronounced when the X-ray energy is 8keV, since the number of outgoing photons is relatively large.
While the application has been described with respect to the preferred embodiments, it is to be understood that the application is not limited thereto, but is intended to cover modifications and alternatives falling within the spirit and scope of the present application as disclosed by those skilled in the art without departing from the spirit and scope of the present application.
Claims (7)
1. The steady-state X-ray radiation induction conductivity tester for the dielectric material comprises a vacuum box (1) and is characterized in that an X-ray source (2) is further arranged outside the vacuum box (1), a sample clamping unit is further arranged inside the vacuum box (1), and the X-ray source (2) can irradiate the sample clamping unit;
the sample clamping unit is connected with a signal processing unit (3) arranged outside the vacuum box (1), and the signal processing unit (3) is also connected with the X-ray source (2).
2. The steady-state X-ray radiation induced conductivity tester for dielectric materials according to claim 1, wherein the sample clamping unit comprises a first sample clamping mechanism (4),
the first sample clamping mechanism (4) is detachably arranged on the inner wall of the vacuum box (1) and comprises a first fixing plate (4-1) and a first stud (4-2) for mounting the first fixing plate (4-1) on the inner wall of the vacuum box (1);
the first sample clamping mechanism (4) further comprises a mounting bracket (4-3) which is detachably arranged in the vacuum box (1), and a collimating lead cylinder (4-4) with two open ends is arranged on the mounting bracket (4-3);
x-rays emitted by the X-ray source (2) can pass through the collimating lead cylinder (4-4) to irradiate on the first fixed plate (4-1); the first fixing plate (4-1) is connected with the signal processing unit (3).
3. The steady-state X-ray radiation induced conductivity tester for dielectric materials according to claim 2, characterized in that the vacuum box (1) comprises a box body (1-1) provided with a vacuum cavity and a cover plate (1-2) matched with the box body;
the X-ray source (2) is used for making X-rays incident on the sample clamping unit through a vacuum window arranged on the bottom plate of the box body (1-1);
a first side wall of the box body (1-1) is provided with a test signal interface (1-3), one end of the test signal interface (1-3) is connected with the sample clamping unit, and the other end of the test signal interface is connected with the signal processing unit (3).
4. The steady-state X-ray radiation induced conductivity tester for dielectric materials according to claim 1, wherein said sample clamping unit further comprises a second sample clamping mechanism (5);
the second sample clamping mechanism (5) comprises a fluorescent target (5-1), the fluorescent target (5-1) is placed at an angle of 45 degrees with an incident light path of the X-ray source (2), and the fluorescent target (5-1) is arranged on the incident light path of the X-ray source;
the second sample clamping mechanism (5) further comprises an optical filter (5-2), the optical filter (5-2) is arranged in parallel with an incident light path of the X-ray source (2), and the optical filter (5-2) is arranged on a light path of fluorescent X-rays generated after the X-ray source (2) irradiates the fluorescent target (5-1);
the second sample clamping mechanism (5) further comprises a shielding plate (5-3), the shielding plate (5-3) is arranged on one side, opposite to the fluorescent target (5-1), of the optical filter (5-2), a second fixing plate (5-4) is arranged on one side, opposite to the optical filter (5-2), of the shielding plate (5-3), and the second fixing plate (5-4) is connected with the shielding plate (5-3) through a second stud (5-5);
the second fixing plate (5-4) is connected with the signal processing unit (3).
5. The steady state X-ray radiation induced conductivity tester for dielectric materials according to claim 2 or 4, characterized in that the first fixing plate (4-1) comprises a bottom plate (4-1-1) and two spring clips (4-1-3) mounted on the bottom plate (4-1-1) through guide rails (4-1-2), wherein the number of the spring clips (4-1-3) is two, the spring clips (4-1-3) are respectively connected with a wire (4-1-4), the wire (4-1-4) is connected with an outgoing terminal (4-1-5) arranged on the bottom plate (4-1-1),
the output terminal (4-1-5) is used for connecting with the test signal interface (1-3);
the structure of the second fixing plate (5-4) is the same as that of the first fixing plate (4-1).
6. The steady-state X-ray radiation induced conductivity tester for dielectric materials according to claim 1, wherein a vacuum pumping device (6) is also arranged on the vacuum box (1),
the vacuum pumping device (6) comprises a dry pump (6-1) and a molecular pump (6-2) which are connected, wherein the molecular pump (6-2) is connected with a vacuum flange (1-4) arranged on the vacuum box (1) through a four-way joint (6-3);
the four-way valve (6-3) is also connected with a vacuum gauge (6-4) and a deflation valve (6-5).
7. The steady-state X-ray radiation induced conductivity tester for dielectric materials according to claim 6, wherein the signal processing unit (3) comprises a Piano meter (3-1) connected with the test signal interface (1-3) and a high-voltage source (3-2), wherein the Piano meter (3-1) is connected with the industrial personal computer (3-3) and the Pi Anbiao (3-1) is connected with the high-voltage source (3-2);
the industrial personal computer (3-3) is connected with the X-ray source (2).
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