CN113072393A - Method for inhibiting secondary electron emission coefficient of dielectric material - Google Patents

Method for inhibiting secondary electron emission coefficient of dielectric material Download PDF

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CN113072393A
CN113072393A CN202110350644.3A CN202110350644A CN113072393A CN 113072393 A CN113072393 A CN 113072393A CN 202110350644 A CN202110350644 A CN 202110350644A CN 113072393 A CN113072393 A CN 113072393A
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dielectric material
secondary electron
electron emission
emission coefficient
irradiation
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向锋
洪小飞
顾腾
刘潇帅
董亦鹏
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Xian Jiaotong University
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    • G01MEASURING; TESTING
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    • G01N23/22Investigating 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 by measuring secondary emission from the material
    • G01N23/225Investigating 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 by measuring secondary emission from the material using electron or ion
    • G01N23/2251Investigating 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 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/22Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance
    • G01N27/221Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating capacitance by investigating the dielectric properties
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/07Investigating materials by wave or particle radiation secondary emission
    • G01N2223/09Investigating materials by wave or particle radiation secondary emission exo-electron emission

Abstract

The invention discloses a method for inhibiting secondary electron emission coefficient of a dielectric material, which selects a ceramic sample and a polymer sample as research objects and utilizes gamma rays to carry out irradiation treatment on the samples. Experiments prove that the resistivity of the dielectric material is reduced along with the increase of the irradiation dose, the maximum value of the secondary electron emission coefficient is reduced, and the secondary electron emission coefficient of the dielectric material is inhibited to a certain extent. Compared with the processes of surface corrosion, photoetching, chemical methods and the like, the method for reducing the secondary electron emission coefficient of the dielectric material by irradiation has the advantages of universality, simple process, low cost, simplicity and convenience in operation and the like.

Description

Method for inhibiting secondary electron emission coefficient of dielectric material
Technical Field
The invention relates to a micro-discharge effect of a microwave device in a spacecraft, which is used for inhibiting a secondary electron emission coefficient on the surface of a dielectric material.
Background
When the microwave device is operated in a high frequency or high power state, a discharge phenomenon occurs, which is a microdischarge effect. Since the microdischarge phenomenon is often accompanied by the generation and emission of secondary electrons, it is also referred to as a secondary electron multiplication effect. The microdischarge effect is a special effect that affects the space vehicle payload and reliable operation in orbit, and can cause the accumulation of charges on the surface of the dielectric material. When the electric charge is accumulated to a certain degree, the electric discharge can cause the failure of various components of the spacecraft, especially power devices. The influence of micro-discharge is very extensive, and the slight influence includes the reduction of the dielectric property of the device (including the increase of dielectric loss, the reduction of high voltage resistance and the like), and the serious influence can cause the loss of the function of the device and can not ensure the normal operation of the spacecraft. The micro-discharge effect mainly comprises three processes of generating secondary electrons in the material, moving the secondary electrons to the surface in an electric field and escaping the secondary electrons from the surface. With the continuous deep exploration of the outer space and the increasing power of space spacecraft components, the subsequent requirement on the suppression of the micro-discharge effect of a high-power device is also increased.
Due to the existence of various radiations and rays in the space, the surface of the spacecraft in the space is electrified, and the surface reaches a balance value after being charged and discharged. This equilibrium value is related not only to the incident particles but also to the secondary electron emission, back scattering, caused by the particles after incidence. The secondary current and the back scattering current are not only related to various parameters of incident particles, but also related to the characteristics of the material (such as the roughness, the conductivity and the like of the surface) and the surface potential of the spacecraft. The secondary electron emission phenomenon will affect the speed of charging and discharging on the surface of the spacecraft and the final equilibrium potential of the charging and discharging. The charging and discharging effect on the surface of the spacecraft can generate electromagnetic pulses with high voltage and large current, so that the functions of components or assemblies in the spacecraft are disordered, the communication and instruction transmission between the ground and the in-orbit spacecraft are influenced, and the spacecraft cannot be overturned to lose efficacy and be scrapped in severe cases. Therefore, the surface secondary electron emission coefficient of the dielectric material needs to be suppressed, and the traditional process flow for suppressing the surface secondary electron emission coefficient of the dielectric material is very complex, poor in applicability, relatively high in cost and needs to spend a large amount of manpower and material resources.
Disclosure of Invention
The invention provides a method for inhibiting the secondary electron emission coefficient of a dielectric material, which can obviously inhibit the secondary electron emission coefficient on the surface of the dielectric material.
In order to achieve the purpose, the method for inhibiting the secondary electron emission coefficient of the dielectric material provided by the invention is used for irradiating the dielectric material to reduce the secondary electron emission coefficient of the dielectric material, and the irradiation dose is less than or equal to 2.09 MGy.
Further, the method comprises the following steps:
placing the dielectric material in an environment with 23 +/-2 ℃ and 50 +/-5% RH for at least 24 hours;
and irradiating the medium material until the total irradiation dose reaches the set irradiation dose.
Furthermore, the average radiation dose rate of the medium material is 3KGy/h, and the daily average irradiation time is 10 h.
Furthermore, when the medium material is irradiated, the distance between the radioactive source and the medium material is 30 cm.
Further, if the exposure time of the dielectric material in the wet air exceeds 30 minutes, the dielectric material is dried and then placed in an environment with 23 +/-2 ℃ and 50 +/-5% RH.
Further, the process of drying the medium material is as follows: drying in an air circulation oven at 105+5 ℃/-2 ℃.
Further, the drying time is 2 hours.
Further, the dielectric material is irradiated with gamma rays.
Compared with the prior art, the invention has at least the following beneficial technical effects:
experiments prove that the resistivity of the dielectric material is reduced along with the increase of the irradiation dose, the maximum value of the secondary electron emission coefficient is reduced, and the secondary electron emission coefficient of the dielectric material is inhibited to a certain extent. Compared with the surface corrosion, photoetching, chemical methods and other processes, the method for inhibiting the secondary electron emission coefficient of the dielectric material by irradiation has the advantages of universality, simple process flow, greatly reduced cost, simplicity and convenience in operation and the like, and the most important point is that the secondary electron emission coefficient of the dielectric material can be effectively inhibited, and the technical application of the dielectric microwave device on the aerospace can be greatly promoted.
From an analysis of the secondary electron emission process, there are two possible mechanisms for the effect of resistivity on the emission coefficient. For insulating materials such as polymers, the high resistivity means that there are few freely moving particles inside the material. The secondary electrons absorb energy and take a certain distance in the process of reaching the surface after being excited in the material. Which in motion will collide with particles inside the material. As the resistivity of the material decreases, the number of freely movable particles within the material begins to increase. The probability of collision between secondary electrons and particles during the escape process is high, the energy of the secondary electrons is reduced in both elastic collision and inelastic collision, and when the secondary electrons reach the surface of the material, if the energy lost by collision during the moving process is high, the residual energy of the secondary electrons is not enough to overcome the limit of the surface of the material to escape, so that the mechanism can reduce the emission coefficient of the secondary electrons.
Furthermore, the average radiation dose rate of the sample is 3KGy/h, the daily average irradiation time is 10h, the optimal radiation dose rate can be quickly found out, and therefore the sample can be fully irradiated.
Furthermore, gamma rays have higher energy and stronger penetrating power, and have great advantages over high-energy electrons and protons in terms of total dose effect in a simulated space radiation environment, so that the gamma rays are utilized to irradiate the dielectric material.
Drawings
FIG. 1a shows Al at different irradiation doses 203Secondary electron emission coefficient measurement results;
FIG. 1b shows Al at different irradiation doses203A resistivity measurement;
FIG. 2a shows Zr at different irradiation doses0.8Sn0.2TiO4Secondary electron emission coefficient measurement results;
FIG. 2b shows Zr at different irradiation doses0.8Sn0.2TiO4A resistivity measurement;
FIG. 3a shows 0.95MgTiO at different irradiation doses3-0.05CaTiO3Secondary electron emission coefficient measurement results;
FIG. 3b shows 0.95MgTiO at different irradiation doses3-0.05CaTiO3A resistivity measurement;
FIG. 4a shows BaO-Ln at different irradiation doses2O3-TiO2Secondary electron emission coefficient measurement results;
FIG. 4b shows BaO-Ln at different irradiation doses2O3-TiO2A resistivity measurement;
FIG. 5a shows the measurement results of the secondary electron emission coefficient of hydrocarbon under different irradiation doses;
FIG. 5b is a graph showing the effect on the overall performance of a hydrocarbon material at different irradiation doses;
FIG. 6a shows the measurement results of the secondary electron emission coefficient of the epoxy resin under different irradiation doses;
FIG. 6b is a graph showing the effect of the overall performance of the epoxy resin at different irradiation doses;
FIG. 7a shows the measurement results of the secondary electron emission coefficient of polyimide under different irradiation doses;
FIG. 7b is a graph showing the effect of the overall performance of polyimides at different irradiation doses;
fig. 8 is a material irradiation environment.
Detailed Description
In order to make the objects and technical solutions of the present invention clearer and easier to understand. The present invention will be described in further detail with reference to the following drawings and examples, wherein the specific examples are provided for illustrative purposes only and are not intended to limit the present invention.
In the description of the present invention, it should be understood that the terms "mounted," "connected," and "connected" are used in a broad sense, and may be, for example, 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.
A method for inhibiting secondary electron emission coefficient of a dielectric material is characterized in that irradiation experiments are carried out on the dielectric material through different irradiation doses, and the situation that the secondary electron emission coefficient of the surface of the dielectric material is reduced along with the increase of the irradiation dose can be found through comparison. The method specifically comprises the following steps:
step 1, pre-treating the sample in an environment with the temperature of 23 +/-2 ℃ and the relative humidity of 50 +/-5% for at least 24 hours. If the sample is exposed to humid air for more than 30 minutes, it should be first dried in an air circulation oven at 105+ 5/2 ℃ for two hours, leaving the sample dry, and then pre-treated under the conditions described above;
the ray sources used for the irradiation experiment at present mainly comprise three types, namely gamma rays, X rays, electron beams and the like, and the 60Co gamma rays have the advantages of higher energy and stronger penetrating power and have great advantages over high-energy electrons and protons in the aspect of simulating the total dose effect in a space radiation environment. In the experiment, a 60Co gamma ray source of a northwest nuclear test base is adopted to carry out irradiation treatment on the medium material, the average radiation dose rate of a sample is 3KGy/h, the daily average irradiation time is 10h, and the total radiation dose reaching 2MGy is about 80 working days. The irradiation dose was measured using a dosimeter of the germany PTW union Webline type.
And 3, placing the sample in a plane of 30cm multiplied by 30cm, and finally determining the average radiation dose rate of the sample to be 3KGy/h by measuring the radiation dose rate of five points in the plane as shown in FIG. 8. The irradiation mechanism is limited to work in working days, the daily average irradiation time is 10 hours, and the total radiation dose reaching 2MGy is about 80 working days. The existing irradiation doses (unit: MGy) are: 0. seven dosages, such as 0.379, 0.716, 1.136, 1.596, 1.826 and 2.09.
A method for inhibiting secondary electron emission coefficient of a dielectric material by irradiation comprises the following steps:
s1: all samples are flaky samples with flat, smooth and defect-free surfaces;
s2: the procurement source, size and purity of the material are shown in table 1;
s3: and (3) carrying out irradiation treatment on the medium material, wherein the average radiation dose rate of the sample is 3KGy/h, the daily average irradiation time is 10h, and the total radiation dose reaching 2MGy is about 80 working days.
And irradiating the same material with different doses to measure the secondary electron emission coefficients of the dielectric material under different irradiation doses.
In S1, the sample comprises a ceramic group and a polymer group, wherein the ceramic group is Al2O3、0.95MgTiO3-0.05CaTiO3、Zr0.8Sn0.2TiO4And BaO-Sm2O3-TiO2The polymer group is epoxy, polyimide and hydrocarbon materials.
TABLE 1 sample information
Figure BDA0003002017090000051
The method for measuring the secondary emission system of the sample comprises the following steps:
1. the secondary electron current pulse of the dielectric material is changed along with time, and the influence process of charging on secondary electron emission can be dynamically shown by adopting a pulse method for measurement. According to the characteristics of the secondary electron current pulse of the dielectric material, the secondary electron emission coefficient of the dielectric material is calculated by adopting SEY-Vs/Vp in combination with the definition of the secondary electron emission coefficient, wherein SEY is the secondary electron emission coefficient, Vs is the maximum value of the secondary electron current pulse, and Vp is the amplitude of the incident electron current pulse.
2. When the sample reaches the test condition, after the electron gun is set, the current Amplifier is connected (the Amplifier Gain is generally set to 10)6). And starting the test, adjusting the incidence time of the electron gun to be 5 mu s, and moving the sample position after testing one point each time to ensure that the testing position is not at the same point each time. The displacement is measured twice and is at least larger than 1mm, and finally, data can be read by giving a pulse.
3. For polymeric materials, the main parameters tested are: testing from 50V acceleration voltage to 3000V acceleration voltage, measuring every 50V near 200V, and measuring the maximum value of the secondary electron current pulse and the amplitude of the incident electron current pulse; taking a point every 100V after 400V to 1000V; the maximum value of the secondary electron current pulse and the amplitude of the incident electron current pulse were measured every 200V in the range of 1000V to 3000V. And testing for three times at each accelerating voltage, and taking an arithmetic mean value to calculate the secondary electron emission coefficient.
4. For ceramic materials, the main parameters tested were: the test was carried out from 30V acceleration voltage to 3000V acceleration voltage, and measurements were carried out every 50V around 200V. One dot per 100V after 500V to 1000V. The maximum value of the secondary electron current pulse and the amplitude of the incident electron current pulse were measured every 1000V in the range of 1000V to 3000V. And testing for three times at each accelerating voltage, and taking an arithmetic mean value to calculate the secondary electron emission coefficient. Meanwhile, before pressurization each time, the sample needs to be displaced, and the displacement needs to ensure that electron beam focal spots emitted by the electron guns for two times do not overlap. By means of a plurality of actual measurements, it is now established that the distance traveled by each sample is about 1.5 mm.
Analysis of test results
As can be seen from fig. 1 a: irradiated Al in the range of 0 to 3000V2O3And non-irradiated Al2O3Compared with the prior art, the secondary electron emission coefficient has an obvious descending trend; fromAs can be seen in fig. 1 b: the larger the irradiation dose is, the Al 203The smaller the resistivity of (a);
as can be seen from fig. 2 a: zr irradiated in the interval of 0-3000V0.8Sn0.2TiO4And non-irradiated Zr0.8Sn0.2TiO4Compared with the prior art, the secondary electron emission coefficient has an obvious descending trend; as can be seen from fig. 2 b: the larger the irradiation dose is, the more Zr0.8Sn0.2TiO4The smaller the resistivity of (a);
as can be seen from fig. 3 a: irradiated 0.95MgTiO within the range of 0-3000V3-0.05CaTiO3And 0.95MgTiO which is not irradiated3-0.05CaTiO3Compared with the prior art, the secondary electron emission coefficient has an obvious descending trend; as can be seen from fig. 3 b: the larger the irradiation dose is, the more the irradiation dose is, the 0.95MgTiO3-0.05CaTiO3The smaller the resistivity of (a);
as can be seen from fig. 4 a: irradiated BaO-Ln in the range of 0 to 3000V2O3-TiO2And non-irradiated BaO-Ln2O3-TiO2Compared with the prior art, the secondary electron emission coefficient has an obvious descending trend; as can be seen from fig. 4 b: the larger the irradiation dose is, the BaO-Ln2O3-TiO2The smaller the resistivity of (a);
as can be seen from fig. 5 a: in the range of 0 to 3000V, the secondary electron emission coefficient of the irradiated hydrocarbon has an obvious descending trend compared with the secondary electron emission coefficient of the irradiated hydrocarbon; as can be seen from fig. 5 b: the larger the irradiation dose is, the smaller the resistivity and the maximum secondary electron emission coefficient of the hydrocarbon are, and the larger the relative dielectric constant is;
as can be seen from fig. 6 a: in the range of 0 to 3000V, the secondary electron emission coefficient of the irradiated epoxy resin has an obvious descending trend compared with that of the non-irradiated epoxy resin; as can be seen from fig. 6 b: the larger the irradiation dose is, the smaller the resistivity and the maximum secondary electron emission coefficient of the epoxy resin are, and the larger the relative dielectric constant is;
as can be seen from fig. 7 a: in the range of 0 to 3000V, the secondary electron emission coefficient of the irradiated polyimide is smaller than that of the polyimide without irradiation, and the secondary electron emission coefficient has an obvious descending trend; as can be seen from fig. 7 b: the larger the irradiation dose, the smaller the resistivity and the maximum secondary electron emission coefficient of polyimide, and the larger the relative dielectric constant.
There are many factors that influence the secondary electron emission coefficient. The effect of irradiation on a material is all-round, either as a change in the appearance of the material or as a change in internal properties. Therefore, the relationship between the irradiation and the secondary electron emission coefficient needs to be researched, and a middle bridge needs to be searched. The secondary electron emission coefficients of the ceramic group and the polymer group after irradiation were measured.
The acceleration voltage tested from 50V to 3000V constructed the complete secondary electron emission characteristic curve. As can be seen from the curves, the emission coefficients of the ceramic and polymer groups remain overall for the characteristics of the composite characteristic curve after irradiation. As the irradiation dose increases, the peak of the characteristic curve decreases.
From an analysis of the secondary electron emission process, there are two possible mechanisms for the effect of resistivity on the emission coefficient. For insulating materials such as polymers, the high resistivity means that there are few freely moving particles inside the material. The secondary electrons absorb energy and take a certain distance in the process of reaching the surface after being excited in the material. Which in motion will collide with particles inside the material. As the resistivity of the material decreases, the number of freely movable particles within the material begins to increase. The probability of collision with the particle during escape of the secondary electron is high, and the energy of the secondary electron is reduced by both elastic collision and inelastic collision. When the secondary electrons reach the material surface, if the energy lost by collision during the movement is large, the residual energy of the secondary electrons is not enough to overcome the limit of the material surface to escape. Therefore, this mechanism will reduce the secondary electron emission coefficient.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (8)

1. A method for inhibiting the secondary electron emission coefficient of a dielectric material is characterized in that the dielectric material is irradiated to reduce the secondary electron emission coefficient of the dielectric material, and the irradiation dose is less than or equal to 2.09 MGy.
2. A method for suppressing the secondary electron emission coefficient of a dielectric material as recited in claim 1, comprising the steps of:
placing the dielectric material in an environment with 23 +/-2 ℃ and 50 +/-5% RH for at least 24 hours;
and irradiating the medium material until the total irradiation dose reaches the set irradiation dose.
3. The method according to claim 2, wherein the average radiation dose rate of the dielectric material is 3KGy/h, and the daily average irradiation time is 10 h.
4. The method of claim 2, wherein the distance between the radiation source and the dielectric material is 30cm when the dielectric material is irradiated.
5. The method of claim 2, wherein if the dielectric material is exposed to humid air for more than 30 minutes, the dielectric material is dried and then placed in an environment of 23 ± 2 ℃ and 50 ± 5% RH.
6. The method for suppressing the secondary electron emission coefficient of a dielectric material as claimed in claim 5, wherein the drying process of the dielectric material comprises: drying in an air circulation oven at 105+5 ℃/-2 ℃.
7. The method of claim 6, wherein the drying time is 2 hours.
8. A method of suppressing the secondary electron emission coefficient of a dielectric material as recited in claim 1 or 2, wherein the dielectric material is irradiated with gamma rays.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111270249A (en) * 2020-03-24 2020-06-12 西安交通大学 Aluminum-based material and surface treatment method for reducing secondary electron emission coefficient
CN111748769A (en) * 2020-06-03 2020-10-09 西安空间无线电技术研究所 Method for reducing secondary electron emission coefficient of silver surface high-energy area
CN112281141A (en) * 2020-09-25 2021-01-29 西安空间无线电技术研究所 Method for inhibiting secondary electron emission coefficient of medium surface based on controllable carbon nano coating

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CN111270249A (en) * 2020-03-24 2020-06-12 西安交通大学 Aluminum-based material and surface treatment method for reducing secondary electron emission coefficient
CN111748769A (en) * 2020-06-03 2020-10-09 西安空间无线电技术研究所 Method for reducing secondary electron emission coefficient of silver surface high-energy area
CN112281141A (en) * 2020-09-25 2021-01-29 西安空间无线电技术研究所 Method for inhibiting secondary electron emission coefficient of medium surface based on controllable carbon nano coating

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