CN103305791A - Preparation process method for 6LiF/BC4 composite neutron conversion film for 4H-SiC-matrix neutron detector - Google Patents

Preparation process method for 6LiF/BC4 composite neutron conversion film for 4H-SiC-matrix neutron detector Download PDF

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CN103305791A
CN103305791A CN2013102529068A CN201310252906A CN103305791A CN 103305791 A CN103305791 A CN 103305791A CN 2013102529068 A CN2013102529068 A CN 2013102529068A CN 201310252906 A CN201310252906 A CN 201310252906A CN 103305791 A CN103305791 A CN 103305791A
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CN103305791B (en
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刘波
蒋勇
张彦坡
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Sichuan University
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Abstract

The invention discloses a preparation process method for a 6LiF/BC4 composite neutron conversion film for a 4H-SiC-matrix neutron detector. The preparation process method adopts a radiofrequency magnetron sputtering technology, and mainly comprises the following steps of: plating pre-treatment, bias re-sputtering cleaning, pre-sputtering cleaning, 6LiF/BC4 composite conversion film deposition, and the like, wherein the plating pre-treatment is ultrasonic cleaning by acetone and ethyl alcohol; the re-sputtering cleaning and the pre-sputtering cleaning aim at removing a 4H-SiC matrix and target impurities. The 6LiF/BC4 conversion film layer obtained by the preparation method disclosed by the invention is resistant to irradiation damage and high temperature, accurately controllable in thickness, excellent in bonding property with the 4H-SiC matrix, strong in preparation process repeatability, and easy for realization of industrial promotion. The neutron detector synthesised from the 6LiF/BC4 composite conversion film layer prepared by the preparation method and a semiconductor 4H-SiC device has the actual measurement effects of low noise, high neutron detection efficiency, high gamma inhibition property, and the like.

Description

4H-SiC base neutron detector is used 6LiF/ BC 4Compound neutron switching film process of preparing
Technical field
The invention belongs to the neutron detection technical applications, relate to a kind of for the high efficiency 4H-SiC base of the novel small volume of measuring oncoming neutron intensity neutron detector usefulness 6LiF/BC 4The complex conversion thin film preparation process.
Background technology
Based on the neutron spectrum measurement technical study work of Si device since the thirties in 20th century just, all Principle Methods to substantially clear and definite neutron spectrum measurement of nineteen sixty, after this, the research center of gravity is transferred to the gamma spectrometry scope of how widening, improves the detection efficiency of detector and improves the aspect such as energy resolution and obtains greater advance.Yet, owing to can't solve the anti-irradiance problems of detector all the time, to the nineties in last century, based on the research of the sandwich neutron detector of Si device and use and do not make progress.
In recent years along with the maturation of SiC material and manufacture craft, for make anti-irradiation, resistant to elevated temperatures SiC neutron detector has been established important foundation.Because the SiC detector can solve high temperature, the neutron energy of the extreme environments such as severe radiation and ionization meter problem, in military affairs, civil area performance significant role, the U.S., the countries such as Russia all successively actively develop SiC neutron detection and applied research and obtained very large effect sees document [E. V. Kalinina, N. B. Strokan, A. M. Ivanov. Performance of p – n 4H-SiC Film Nuclear Radiation Detectors for Operation at Elevated Temperatures (375 ℃), ISSN 1063-7850, Technical Physics Letters, 2008,34 (3): 210 – 212.], document [R. Ciolini, A. Di Fulvio, M. Piotto, A. Diligenti, F. d ' Errico. A feasibility study of a SiC sandwich neutron spectrometer. Radiation Measurements, 2011(46): 1634-1637.] and document [C.Manfredotti, A.Lo Giudice, F.Fasolo. SiC detectors for neutron monitoring. Nuclear Instruments and Methods in Physics Research A, 552 (2005) 131-137.].For example, U.S. Cree company is take the 4H-SiC crystal as matrix in recent years, developed high resolving power SiC semiconducter device (FWHM to 148Gd-α source is 41.5keV), and utilize this element manufacturing to become the SiC neutron detector, be applied on U.S. TRIGA heap and NIST (the National Institute of Standards and Technology) device and see document [Frank H.Ruddy, John G.Seidel, Haoqian Chen. High-resolution alpha-particle spectrometry using 4H silicon carbide semiconductor detectors. IEEE Nuclear Science Symposium Conference Record, N34-5, (2005) 1231-1235.].
In recent years, domestic minority unit (as 13 of electronics, electronics 55 etc.) also grasped low N doped 4 H-SiC element manufacturing technology, for important foundation stone has been established in the sandwich eds detector development of the SiC of anti-irradiation neutron, see document [Jia Renxu, Zhang Yimen, Zhang Yuming, Wang Yuehu. N-type 4H-SiC isoepitaxial growth [J] Acta Physica Sinica, 2008,57 (10): 6649-6652] and [Sun Guosheng, Ning Jin .4H-SiC isoepitaxial growth and the Ti/4H-SiC schottky diodes such as Gao Xin. the artificial lens journal, 2005,34 (6): 1006-1010].Compare with the Si device, the 4H-SiC device has clear superiority aspect quality of materials, element manufacturing and the cost of manufacture.The 4H-SiC device has energy gap large (Eg=3.26eV of 4H-SiC, the Eg=1.1eV of Si), crystal atoms is offed normal, and energy is large, the electron hole mobility is high, dark current is little, heat-conduction coefficient is large, hardness reaches greatly the voltage breakdown advantages of higher.
Yet, neutron detector conversion film thickness is larger on the detection efficiency impact of detector, conversion film is blocked up, energy was excessively low when reactant entered semi-conductor, change lepthymenia, reflection is not enough to produce enough charged particles and enters semi-conductor, and then cause electron-hole pair to lack, affect the detector detection efficiency and see document [D.S. McGregor, R.T. Klann, H.K. Gersch, Y.H. Yang. Thin-film-coated bulk GaAs detectors for thermal and fast neutron measurements. Nuclear Instruments and Methods in Physics Research A 466 (2001) 126-141.] and document [D.S. McGregor, J.T. Lindsay, C.C. Brannon, R.W. Olsen. Semi-Insulating Bulk GaAs Thermal Neutron Imaging Arrays. IEEE Transactions on Nuclear Science. VOL. 43, NO. 3:1357-1364. JUNE 1996].R. detection efficiency and the energy resolution of SiC device to alpha-particle measured in the Ciolini impact of neutron conversion layer thickness on detection efficiency of having adopted the analog calculation of M.C method.Studies show that: the SiC device performance of its development is relatively poor, optimum capacity resolving power to the alpha-particle of 5.5MeV only is 9%, detection efficiency lower (0.34-0.72), result of study has verified that further neutron conversion film layer thickness has material impact to the neutron detector detection efficiency and sees document [R. Ciolini, A. Di Fulvio, M. Piotto, A. Diligenti, F. d ' Errico. A feasibility study of a SiC sandwich neutron spectrometer. Radiation Measurements, 2011(46): 1634-1637.].
The previous individual layer that adopts 6LiF is as the neutron conversion layer, and the alpha-particle of generation is longer at the LiF medium range, and its theoretical and its thickness of experimental calculation is about 35 μ m, and along with the increase of conversion layer thickness, energy resolution degenerates, and then affects comparatively costliness of the detectivity of detector and price.There are some researches show, adopt BC 4As neutron conversion layer, BC 4In 10B has very large thermal cross section and content more than 75%, simultaneously good, the low price thickness of its stable chemical performance, thermal property can reduce greatly, residual compressive stress in the deposit film is conducive to improve interfacial combined function and sees document [single minister in ancient times, Ceng Jie, Jia Wenbao, black large thousand, Ling Yongsheng, Wei Yonghong, a spark. be coated with the modeling effort of boron MRPC thermal neutron detector performance. 2,013 43 (1): 66-70].Yet, producing residual tension when film is thicker so that the interfacial combined function variation, rete comes off.Therefore, this paper proposes the design of compound neutron conversion layer, namely deposits at the SiC matrix 6LiF/BC 4Rete both can reduce thicknesses of layers, improved the rete Interface adhesive strength, can also improve the resolution efficient of conversion layer simultaneously.The employing magnetron sputtering technique that the present invention proposes deposits at the 4H-SiC semiconductor detector 6LiF/BC 4Conversion film is task of the present invention place just.
Summary of the invention
Use for above-mentioned 4H-SiC semiconductor detector 6LiF and BC 4The existing deficiency of conversion film, purpose of the present invention aim to provide a kind of more simple, convenient and conversion film layer thickness and can accurately control, and the 4H-SiC base semiconductor neutron detector that parameter can be regulated and control and detection efficiency is higher is used 6LiF/BC 4The complex conversion membrane preparation method.
Basic thought of the present invention is: direct in-situ deposition design thickness on the 4H-SiC matrix that cleaned 6LiF/BC 4Compound coating, with reach by 6Li(n, α) 3H and 10B(n, α) 3H reacts to measure the information such as energy of oncoming neutron, improves the detection efficiency of detector.
4H-SiC base semiconductor neutron detector provided by the invention is used 6LiF/BC 4The complex conversion membrane preparation method mainly comprises following steps:
A, will be immersed in respectively as the monocrystalline 4H-SiC matrix of substrate material and carry out ultrasonic cleaning in acetone, the dehydrated alcohol, take out dried for standby after fully cleaning;
B, the monocrystalline 4H-SiC matrix after step a cleaned and as magnetic controlling target 6LiF target and BC 4Target is inserted respectively in the reaction magnetocontrol sputtering plated film vacuum oven, adopts the bias voltage reverse sputtering to clean and removes monocrystalline 4H-SiC matrix surface impurity, adopts pre-sputter clean to remove 6LiF target and BC 4The impurity of target material surface, bias voltage reverse sputtering clean and pre-sputter clean build-up of luminance gas is argon gas, and the flow of described argon gas is 150 ~ 200 Sccm, and the bias voltage reverse sputtering cleans and pre-sputter clean operation vacuum tightness is pounds per square inch absolute (psia) 1.0 ~ 3.0 Pa;
C, in reaction magnetocontrol sputtering plated film vacuum oven, after processing with the pre-sputter clean of step b 6The LiF target adopts magnetron sputtering deposition as magnetic controlling target at the cleaned monocrystalline 4H-SiC of step b bias voltage reverse sputtering matrix 6The LiF coating, magnetron sputtering deposition 6LiF coating build-up of luminance gas is argon gas, and argon flow amount is 150 ~ 250 Sccm, and magnetron sputtering deposition operation vacuum tightness is pounds per square inch absolute (psia) 0.40 ~ 0.50 Pa;
D, monocrystalline 4H-SiC matrix magnetron sputtering deposition 6The LiF coating is closed magnetic control to design thickness 6The LiF target; Keep obtaining at step c under original vacuum condition 6Deposit BC on the LiF coating 4Coating, used target are magnetic control BC 4Target, magnetron sputtering deposition BC 4Coating build-up of luminance gas is argon gas, and argon flow amount is 150 ~ 250 Sccm, and magnetron sputtering deposition operation vacuum tightness is pounds per square inch absolute (psia) 0.40 ~ 0.50 Pa;
E, magnetron sputtering deposition BC 4Coating is closed magnetic control BC to design thickness 4Target is closed build-up of luminance gas argon gas, the interior vacuum tightness of reaction magnetocontrol sputtering plated film vacuum oven is adjusted to is not less than 10 -3Come out of the stove behind the Pa naturally cooling, namely obtain 4H-SiC base neutron detector and use 6LiF/BC 4The complex conversion film.
In order to obtain better effect, the present invention can further take following technical measures, and following every technical measures can be taked separately, also capable of being combined taking, even take in the lump.
In technique scheme, sputter clean, sputtering sedimentation operation vacuum tightness can be considered to be not less than 10 by first reaction magnetocontrol sputtering plated film vacuum oven being evacuated to -3Pa makes sputter clean, sputtering sedimentation maintain the operation vacuum ranges after passing into build-up of luminance gas argon gas.
In technique scheme, be immersed in successively as the monocrystalline 4H-SiC matrix of substrate material that ultrasonic cleaning respectively is no less than 15 minutes in acetone, the dehydrated alcohol.
In technique scheme, as the magnetic control of magnetic controlling target 6The LiF target 6The Li concentration is 90%, BC 4Target is preferentially selected 10The B concentration is not less than 96% BC 4Target.
In technique scheme, when adopting the bias voltage reverse sputtering to clean matrix and adopt pre-sputter clean target, preferably keep the pumping speed valve to close, deposition 6LiF/BC 4During coating, keep the pumping speed valve to open.
In technique scheme, the power that the substrate bias reverse sputtering cleans can consider to be controlled at 80 W ~ 150 W scopes, and bias voltage can consider to be controlled at-400 V ~-500 V scopes, 6LiF target and BC 4The power of the pre-sputter clean of target can consider to be controlled at 80 W ~ 150 W scopes, and bias voltage can consider to be controlled at-100 V ~-200 V scopes.
In technique scheme, 6LiF target and BC 4The target as sputter deposition power can consider to be controlled at 80 W ~ 150 W scopes, and bias voltage can consider to be controlled at-50 V ~-80 V.
Of the present invention above-mentioned 6LiF/BC 4The compound film preparation processing method of changing, the operation of whole technological process is all implemented at normal temperatures.
Of the present invention finish be based on the contriver 4H-SiC semi-conductor is had that the broad stopband degree is large, crystal atoms is offed normal can be large, the deep understanding of radiation hardness, the performance such as high temperature resistant, energy resolution is high and voltage breakdown is high, substitute Si or Ge as the matrix of neutron detector with the 4H-SiC semi-conductor, adopt the reaction magnetocontrol sputtering technology to deposit at monocrystalline 4H-SiC matrix 6LiF/BC 4Compound coating prepares conversion film, and operation is simple, and conversion film layer thickness and preparation parameter are accurately controlled, can be thick at monocrystalline 4H-SiC matrix preparation 1.5 μ m in advance 6The LiF coating exists afterwards 6The thick BC of deposition 0.5 μ m on the LiF layer 4Rete, whole even film layer is fine and close.Provided by the invention depositing 6LiF/BC 4The 4H-SiC base neutron detector of complex conversion rete has the characteristics such as noise is little, volume is little, detection efficiency is high, anti-radiation damage, high temperature resistant and high γ inhibition.Overcome existing detector such as Au Si surface barrier detector and high purity germanium detector existing responsive to radiation injury, be subject to poor performance behind the strong irradiation, and high purity germanium detector must work under low temperature (liquid nitrogen) condition, use the problems such as inconvenience.
Description of drawings
Fig. 1 is that the present invention prepares 6LiF/BC 4Turn to turn to close again and change film cross section Electronic Speculum (SEM) scintigram.
Fig. 2 deposits 6LiF/BC 4The 4H-SiC base semiconductor neutron detector result of detection figure of complex conversion film.
Embodiment
Provide embodiments of the invention below in conjunction with description of drawings; and the present invention is described in further detail to pass through embodiment; it is important to point out; embodiment is only for the present invention is described further; can not be interpreted as limiting the scope of the invention; under the art skilled staff according to the foregoing invention content, the present invention is made some nonessential improvement and implementation is carried out in adjustment, should still belong to protection scope of the present invention.
Embodiment 1
The 4H-SiC base neutron detector of the present embodiment is used 6LiF/BC 4The complex conversion thin film preparation process is as follows:
A, substrate material 4H-SiC matrix is put into acetone, dehydrated alcohol successively carry out respectively 20 minutes ultrasonic cleaning, take out dried for standby after fully cleaning;
B, the monocrystalline 4H-SiC matrix after step a cleaned, 6The Li concentration is 90% 6The LiF target and 10The B concentration is 96% BC 4Target is inserted in the interior vacuum chamber of reaction magnetocontrol sputtering plated film vacuum oven, then is evacuated to 5.0 * 10 -4Pa adopts the bias voltage reverse sputtering to clean and removes impurity in the monocrystalline 4H-SiC matrix, and the power that reverse sputtering cleans is 120 W, and bias voltage is-500 V; Adopt pre-sputter clean to remove respectively 6LiF target and BC 4The impurity of target, the power of pre-sputter clean is 120 W, bias voltage is-100 V; Reverse sputtering cleans and pre-sputter clean build-up of luminance gas is argon gas, and the flow of argon gas is 180Sccm, and reverse sputtering cleans and pre-sputter clean operation vacuum tightness is pounds per square inch absolute (psia) 2.0 Pa; Reverse sputtering keeps the pumping speed valve to close when cleaning matrix with pre-sputter clean target.
After c, reverse sputtering clean and pre-sputter clean finishes, in same reaction magnetocontrol sputtering plated film vacuum oven, after processing with the pre-sputter clean of step b 6The LiF target adopts magnetron sputtering deposition as magnetic controlling target at the cleaned monocrystalline 4H-SiC of step b bias voltage reverse sputtering matrix 6LiF coating, sputter deposition power are 80 W, sputtering sedimentation 6LiF 4Coating build-up of luminance gas is argon gas, and argon flow amount is 180 Sccm, and sputtering sedimentation operation vacuum tightness is pounds per square inch absolute (psia) 0.45 Pa.Sputtering sedimentation 6Keep the pumping speed valve to open during the LiF coating operation.
D, monocrystalline 4H-SiC matrix sputtering sedimentation BC 4Coating is closed magnetic control to design thickness 1.5 μ m 6The LiF target keeps obtaining at step c under original vacuum condition 6Deposit BC on the LiF coating 4Coating, used target are magnetic control BC 4Target, magnetron sputtering deposition BC 4Coating build-up of luminance gas is argon gas, and argon flow amount is 180 Sccm, and magnetron sputtering deposition operation vacuum tightness is pounds per square inch absolute (psia) 0.45 Pa;
E, magnetron sputtering deposition BC 4Coating is closed magnetic control BC to design thickness 0.5 μ m 4Target is closed build-up of luminance gas argon gas, makes the vacuum tightness in the reaction magnetocontrol sputtering plated film vacuum oven be adjusted to 5.0 * 10 -4Come out of the stove after the Pa naturally cooling room temperature, namely obtain 4H-SiC base neutron detector and use 6LiF/BC 4The complex conversion film.
Fig. 1 is that the 4H-SiC base neutron detector that the present embodiment obtains is used 6LiF/BC 4The scanning electron microscope of complex conversion film (SEM) sectional view.By Electronic Speculum (SEM) scintigram as seen, 6The LiF coat-thickness is 1.5 μ m, BC 4Conversion film thickness is 0.5 μ m, can satisfy the controlled requirement of its thickness.Fig. 2 is for passing through 6Li(n, α) 3H and 10B (n, α) 3The α that the H reaction produces, 7Li particle spectrum figure, its energy are respectively 1.47 MeV and 0.840 MeV, and the two exit direction is opposite, by distinguish α, 7Li particle spectrum Accurate Determining oncoming neutron signal.
Embodiment 2
The 4H-SiC base neutron detector of the present embodiment is used 6LiF/BC 4The complex conversion thin film preparation process, substantially the same manner as Example 1, different places are that reaction magnetocontrol sputtering plated film vacuum oven is evacuated to 4.0 * 10 -4Pa, the power that reverse sputtering cleans is 100 W, bias voltage is-400 V; The power of pre-sputter clean is 100 W, and bias voltage is-100 V, and the flow of argon gas is 160 Sccm, and reverse sputtering cleans and pre-sputter clean operation vacuum tightness is pounds per square inch absolute (psia) 1.5 Pa.Sputter deposition power is 100 W, and argon flow amount is 150 Sccm, and sputtering sedimentation operation vacuum tightness is pounds per square inch absolute (psia) 0.43 Pa; BC 4The operating process of coating sputtering sedimentation is the operate continuously process.Sputtering sedimentation 6LiF/BC 4Coat-thickness is respectively 1.5 μ m and 0.5 μ m, and the vacuum tightness in the reaction magnetocontrol sputtering plated film vacuum oven is adjusted to 4.0 * 10 -4Come out of the stove after the Pa naturally cooling room temperature.
Embodiment 3
In deposition 6LiF/BC 4In the complex conversion membrane process, deposition 6LiF and BC 4Coat-thickness is also influential to the detector detection efficiency.The present embodiment 6LiF/BC 4It is all identical with embodiment 1 with other processing condition that conversion film prepares used filming equipment, and keep 6LiF/BC 42.0 μ m are controlled for complex conversion film total thickness, and are selected during deposition 6The LiF coat-thickness is 1.0 μ m, BC 4Coat-thickness is 1.0 μ m, and prepared conversion rete also can pass through 6Li(n, α) 3H and 10B (n, α) 3The α that the H reaction produces, 7Li, T particle spectrum test oncoming neutron signal improve detection efficiency.
Embodiment 4
In deposition 6LiF/BC 4In the complex conversion membrane process, deposition power is larger to conversion film thickness, uniformity coefficient and structure influence.The present embodiment 6LiF/BC 4It is all identical with embodiment 1 with other processing condition that conversion film prepares used filming equipment, and keep 6LiF/BC 42.0 μ m are controlled for complex conversion film total thickness, deposition 6LiF/BC 4Change deposition power during conversion film, as be chosen to be 50 W, 80 W and 120 W then can be to BC 4The regulation and control of conversion film sedimentation rate also can be satisfied the accurately controlled requirement of its thickness, and prepared conversion rete also can pass through 6Li(n, α) 3H and 10B (n, α) 3The α that the H reaction produces, 7Li, T particle spectrum test oncoming neutron signal.
Embodiment 5
In deposition 6LiF/BC 4In the complex conversion membrane process, the deposition bias voltage is larger to conversion film thickness, uniformity coefficient and structure influence.The present embodiment 6LiF/BC 4The used filming equipment of complex conversion film is all identical with embodiment 1 with other working conditions, and keeps 6LiF/BC 42.0 μ m are controlled for complex conversion film total thickness, deposition 6LiF/BC 4Change the deposition bias voltage during coating, as be chosen to be-20 V ,-50 V and-100 V then can be right respectively 6LiF/BC 4The regulation and control of conversion film sedimentation rate also can be satisfied the accurately controlled requirement of its thickness, and prepared conversion rete also can pass through 6Li(n, α) 3H and 10B (n, α) 3The α that the H reaction produces, 7Li, T particle spectrum test oncoming neutron signal.

Claims (8)

1. a 4H-SiC base semiconductor neutron detector is used 6LiF/ BC 4The complex conversion membrane preparation method is characterized in that mainly comprising following steps:
A, will be immersed in respectively as the monocrystalline 4H-SiC matrix of substrate material and carry out ultrasonic cleaning in acetone, the dehydrated alcohol, take out dried for standby after fully cleaning;
B, the monocrystalline 4H-SiC matrix after step a cleaned and as magnetic controlling target 6LiF target and BC 4Target is inserted respectively in the reaction magnetocontrol sputtering plated film vacuum oven, adopts the bias voltage reverse sputtering to clean and removes monocrystalline 4H-SiC matrix surface impurity, adopts pre-sputter clean to remove 6LiF target and BC 4The impurity of target material surface, bias voltage reverse sputtering clean and pre-sputter clean build-up of luminance gas is argon gas, and the flow of described argon gas is 150 ~ 200 Sccm, and the bias voltage reverse sputtering cleans and pre-sputter clean operation vacuum tightness is pounds per square inch absolute (psia) 1.0 ~ 3.0 Pa;
C, in reaction magnetocontrol sputtering plated film vacuum oven, after processing with the pre-sputter clean of step b 6The LiF target adopts magnetron sputtering deposition as magnetic controlling target at the cleaned monocrystalline 4H-SiC of step b bias voltage reverse sputtering matrix 6The LiF coating, magnetron sputtering deposition 6LiF coating build-up of luminance gas is argon gas, and argon flow amount is 150 ~ 250 Sccm, and magnetron sputtering deposition operation vacuum tightness is pounds per square inch absolute (psia) 0.40 ~ 0.50 Pa;
D, monocrystalline 4H-SiC matrix magnetron sputtering deposition 6The LiF coating is closed magnetic control to design thickness 6The LiF target; Keep obtaining at step c under original vacuum condition 6Deposit BC on the LiF coating 4Coating, used target are magnetic control BC 4Target, magnetron sputtering deposition BC 4Coating build-up of luminance gas is argon gas, and argon flow amount is 150 ~ 250 Sccm, and magnetron sputtering deposition operation vacuum tightness is pounds per square inch absolute (psia) 0.40 ~ 0.50 Pa;
E, magnetron sputtering deposition BC 4Coating is closed magnetic control BC to design thickness 4Target is closed build-up of luminance gas argon gas, the interior vacuum tightness of reaction magnetocontrol sputtering plated film vacuum oven is adjusted to is not less than 10 -3Come out of the stove behind the Pa naturally cooling, namely obtain 4H-SiC base neutron detector and use 6LiF/BC 4The complex conversion film.
2. 4H-SiC base semiconductor neutron detector according to claim 1 is used 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: be not less than 10 by reaction magnetocontrol sputtering plated film vacuum oven is evacuated to -3Pa makes sputter clean, sputtering sedimentation maintain the operation vacuum ranges after guaranteeing to pass into build-up of luminance gas argon gas.
3. 4H-SiC base semiconductor neutron detector according to claim 1 is used 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: be immersed in successively as the monocrystalline 4H-SiC matrix of substrate material and carry out ultrasonic cleaning in acetone, the dehydrated alcohol.
4. 4H-SiC base semiconductor neutron detector according to claim 3 is used 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: monocrystalline 4H-SiC matrix is immersed in respectively that ultrasonic cleaning respectively is no less than 15 minutes in acetone, the dehydrated alcohol.
5. 4H-SiC base semiconductor neutron detector according to claim 1 is used 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: described magnetic control 6The LiF target 6The Li concentration is 90%, magnetic control BC 4In the target 10The B concentration is not less than 96%.
According to claim 1 and 2 or described 4H-SiC base semiconductor neutron detector use 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: when adopting the bias voltage reverse sputtering to clean matrix and adopt pre-sputter clean target, keep the pumping speed valve to close, deposition 6LiF/BC 4During compound coating, keep the pumping speed valve to open.
7. 4H-SiC base semiconductor neutron detector according to claim 1 and 2 is used 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: the power that described substrate bias reverse sputtering cleans is 80 W ~ 150 W, and bias voltage is-400 V ~-500 V, and is described 6LiF target and BC 4The pre-sputter clean power of target is 80 W ~ 150 W, and bias voltage is-100 V ~-200 V.
8. 4H-SiC base semiconductor neutron detector according to claim 1 and 2 is used 6LiF/BC 4The complex conversion membrane preparation method is characterized in that: 6LiF target and BC 4The target material magnetic sputtering deposition power is 80 W ~ 150 W, and the deposition bias voltage is-50 V ~-80 V.
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CN108796447A (en) * 2018-05-29 2018-11-13 东华理工大学 A kind of large area thick film of GaN neutron detectors6LiF neutron conversion layer preparation methods
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Publication number Priority date Publication date Assignee Title
CN108796447A (en) * 2018-05-29 2018-11-13 东华理工大学 A kind of large area thick film of GaN neutron detectors6LiF neutron conversion layer preparation methods
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