CN103779154B - A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof - Google Patents
A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof Download PDFInfo
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- CN103779154B CN103779154B CN201410011479.9A CN201410011479A CN103779154B CN 103779154 B CN103779154 B CN 103779154B CN 201410011479 A CN201410011479 A CN 201410011479A CN 103779154 B CN103779154 B CN 103779154B
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Abstract
A kind of diamond delivery of energy window of Terahertz vacuum device and manufacture method thereof, belong to vacuum electron device field, this diamond delivery of energy window structure is, basecoat is super nanocrystalline diamond diaphragm, on this diaphragm basis, alternating growth one deck polycrystalline diamond flag, again one deck surpass nanocrystalline diamond diaphragm and one deck polycrystalline diamond flag more successively, i.e. the diamond delivery of energy window that is alternately arranged of two kinds of lattices.The preparation process of THz diamond delivery of energy window is, first use bortz powder that silicon chip surface is carried out the process of polishing forming core, carry out the alternating growth of super nanocrystalline and epitaxial diamond films with microwave plasma CVD equipment, remove the diamond that silicon chip obtains.Fracture strength and the vacuum seal performance of this delivery of energy window are better than polycrystalline diamond window, are applicable to THz vacuum device.
Description
Technical field
The invention belongs to vacuum electron device field, be specifically related to a kind of diamond delivery of energy window and manufacture method thereof of terahertz wave band vacuum device.
Background technology
Terahertz (referred to as THz) vacuum device has the advantages such as power is large, bandwidth, is widely applied in radar, guidance, tactics and strategic communicaton, electronic countermeasures, remote sensing, radiation measurement etc.Because the frequency of this vacuum device is relatively high, the size of parts is less, brings all difficulties to development, and the processing and manufacturing of the slow wave structure, attenuator and the microwave energy transmission window that particularly adopt in THz travelling wave tube is all the more so.Microwave energy transmission window is one of vitals in THz travelling wave tube.In order to make travelling wave tube energy steady operation, and provide good unit for electrical property parameters, delivery of energy window must have the features such as standing wave is low, loss is little, and should have enough structural strengths and vacuum seal performance.
For short millimeter wave, such as W-waveband travelling wave tube, there is series of problems in the sapphire window for delivery of energy.First, its dielectric constant (9.5) is higher.If window-frame wants to make WR10 standard waveguide mouth, the thickness of the sapphire window calculated according to dielectric constant and wavelength is less than 0.1mm, insufficient strength, is difficult to realize.In addition on the one hand, sapphire window is compared with diamond window, and lossy microwave is relatively large.And RF level high quality diamond material, being dielectric material the most excellent in known materials, having the characteristics such as low-k, low lossy microwave, high rigidity and high thermal conductivity, is microwave vacuum device, the delivery of energy window material that particularly short millimeter wave travelling wave tube is desirable.According to calculating, if window-frame makes WR10 standard waveguide mouth, the thickness of diamond window reaches 0.16 ~ 0.2mm, and this thickness can meet the real requirement of intensity.For this reason, we have developed short mm wave band travelling wave tube polycrystalline diamond stone window at the beginning of 2013, and have declared patent of invention (application number: 201310131910.9).But for THz vacuum device, along with the increase of frequency, device size reduces further, and the thickness of delivery of energy window drops to below 0.15mm, even tens microns.This is for polycrystalline diamond window, and first mechanical strength is inadequate, cannot carry out polishing, bring the intensity and vacuum seal performance problem that occur in use simultaneously.On the other hand, when grain size continues to be contracted to below polycrystalline, crystal grain is between several nanometer to tens nanometers, and the advantage of super nanocrystalline diamond is, compactness is good, and Resisting fractre intensity is high; Shortcoming is the amorphous carbon (sp2) containing about 5%, and it exists certain lossy microwave compared with polycrystalline.
The present invention utilizes the respective advantage of polycrystalline and super nanocrystalline diamond, by polycrystalline and super nanocrystalline two kinds of granularity alternating growths, have developed that both to have lossy microwave low, there is again the thin window sheet of enough mechanical strengths and vacuum seal performance, meet the user demand of the devices such as THz travelling wave tube.
Summary of the invention
The technical problem that the present invention solves is, for the polycrystalline diamond window used in prior art, enter one to THz wave band when frequency range to improve, intensity and the vacuum seal performance of its window can not meet the demands, in order to solve this difficulty, just need again to develop a kind of new delivery of energy window to meet intensity in delivery of energy process and vacuum seal performance problem.
The object of the invention is, a kind of diamond delivery of energy window and manufacture method thereof of terahertz wave band vacuum device is provided.
For realizing object of the present invention, the technical scheme taked is as follows, a kind of diamond delivery of energy window of THz vacuum device, basecoat is super nanocrystalline diamond diaphragm, on this diaphragm basis, alternating growth one deck polycrystalline diamond flag, again one deck surpass nanocrystalline diamond diaphragm and one deck polycrystalline diamond flag more successively, i.e. the diamond delivery of energy window that is alternately arranged of two kinds of lattices.
The thickness of described delivery of energy window can increase and decrease the number of plies of super nanocrystalline diamond film and the thickness of every layer adjusts.
A kind of manufacture method according to above-mentioned diamond delivery of energy window structure, adopt microwave plasma CVD equipment, first use bortz powder that silicon chip surface is carried out the process of polishing forming core, then microwave plasma CVD equipment is utilized to carry out the alternating growth of super nanocrystalline and epitaxial diamond films, etching away silicon chip obtains RF grade diamond material, then carry out grinding and polishing, be finally cut into the diamond delivery of energy window meeting design size and require by laser means.
The manufacture method of described diamond delivery of energy window, operates according to the following stated process step:
A. substrate silicon chip adopts bortz powder polishing forming core, and Enhancing Nucleation Density reaches>=and 10
10/ cm
2;
B. super nanocrystalline diamond growth: 1 ~ 6sccm methane, 100 ~ 200sccm argon gas and 1 ~ 20sccm hydrogen; Air pressure 5 ~ 12KPa, microwave power 1 ~ 2KW; Substrate temperature 750 ~ 850 DEG C;
C. epitaxial diamond films growth: 1 ~ 6sccm methane, 100 ~ 600sccm hydrogen; Air pressure 5 ~ 16KPa, microwave power 2 ~ 3KW; Substrate temperature 850 ~ 950 DEG C;
D. the growth of super nanocrystalline diamond film is repeated;
E. epitaxial diamond films growth is repeated;
F. terminate diamond film growth, close down gas and microwave source; Etching away silicon chip, prepares diamond window sheet material, then carries out according to the following steps:
G. grinding and polishing;
H. laser dicing.
The invention has the beneficial effects as follows, according to the super nanocrystalline and polycrystalline made by above-mentioned flow process be alternately arranged growth diamond window, overcome conventional synthesis technique to prepare the low and vacuum leakproofness of the fracture strength of polycrystalline diamond thin window sheet and can meet the defect that THz vacuum device requires, it is low that this delivery of energy window being alternately arranged growth had both had lossy microwave, there is again enough mechanical strengths and vacuum seal performance, meet the user demand of the devices such as THz travelling wave tube completely.
Accompanying drawing explanation
Fig. 1 is a kind of schematic diagram of diamond delivery of energy window of THz vacuum device;
Fig. 2 is the manufacturing flow chart of THz vacuum device diamond delivery of energy window.
Embodiment
With reference to Fig. 1, represent a kind of schematic diagram of diamond delivery of energy window of THz travelling wave tube.Represent in figure, this delivery of energy window is made up of two-layer super nanocrystalline diamond film 1 and two-layer epitaxial diamond films 2.In practicality, the adamantine number of plies and thickness design according to the gross thickness of window: if window is thinner or thicker, can increase or reduce the number of plies of super nanometer crystal film or the thickness of every layer.
With reference to Fig. 2, represent the manufacturing flow chart of THz vacuum device diamond delivery of energy window.The preparation of diamond delivery of energy window operates according to following steps:
A. substrate silicon chip adopts bortz powder polishing forming core, and Enhancing Nucleation Density reaches>=and 10
10/ cm
2;
B. super nanocrystalline diamond growth: 1 ~ 6sccm methane, 100 ~ 200sccm argon gas and 1 ~ 20sccm hydrogen; Air pressure 5 ~ 12KPa, microwave power 1 ~ 2KW; Substrate temperature 750 ~ 850 DEG C;
C. epitaxial diamond films growth: 1 ~ 6sccm methane, 100 ~ 600sccm hydrogen; Air pressure 5 ~ 16KPa, microwave power 2 ~ 3KW; Substrate temperature 850 ~ 950 DEG C;
D. the growth of super nanocrystalline diamond film is repeated;
E. epitaxial diamond films growth is repeated;
F. terminate diamond film growth, close down gas and microwave source; Etching away silicon chip, prepares diamond window sheet material, then carries out according to the following steps:
G. grinding and polishing;
H. laser dicing.
Claims (3)
1. the diamond delivery of energy window of a THz vacuum device, it is characterized in that, basecoat is super nanocrystalline diamond diaphragm, and on this diaphragm basis, alternating growth one deck polycrystalline diamond flag, again one deck surpass nanocrystalline diamond diaphragm and one deck polycrystalline diamond flag more successively.
2. diamond delivery of energy window according to claim 1, is characterized in that, the thickness of described delivery of energy window can increase and decrease the number of plies of super nanocrystalline diamond film and the thickness of every layer adjusts.
3., according to a manufacture method for diamond delivery of energy window structure described in claim 1, it is characterized in that, operate by the following stated process step:
A. substrate silicon chip adopts bortz powder polishing forming core, and Enhancing Nucleation Density reaches>=and 10
10/ cm
2;
B. super nanocrystalline diamond growth: 1 ~ 6sccm methane, 100 ~ 200sccm argon gas and 1 ~ 20sccm hydrogen; Air pressure 5 ~ 12KPa, microwave power 1 ~ 2KW; Substrate temperature 750 ~ 850 DEG C;
C. epitaxial diamond films growth: 1 ~ 6sccm methane, 100 ~ 600sccm hydrogen; Air pressure 5 ~ 16KPa, microwave power 2 ~ 3KW; Substrate temperature 850 ~ 950 DEG C;
D. the growth of super nanocrystalline diamond film is repeated;
E. epitaxial diamond films growth is repeated;
F. terminate diamond film growth, close down gas and microwave source; Etching away silicon chip, prepares diamond window sheet material, then carries out according to the following steps:
G. grinding and polishing;
H. laser dicing.
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CN105185677A (en) * | 2015-08-07 | 2015-12-23 | 南京三乐电子信息产业集团有限公司 | Millimeter wave traveling wave tube diamond energy transmission window and processing method |
CN110416039B (en) * | 2019-07-30 | 2021-08-10 | 中国电子科技集团公司第十二研究所 | Energy transmission window sheet for terahertz waveband vacuum device and preparation method thereof |
CN111286718A (en) * | 2020-03-20 | 2020-06-16 | 廊坊西波尔钻石技术有限公司 | Impact-resistant CVD diamond self-supporting material and manufacturing method thereof |
CN113794086B (en) * | 2021-09-14 | 2022-12-06 | 中国科学院物理研究所 | Terahertz generation device based on diamond film and generation method thereof |
CN114343572B (en) * | 2021-12-21 | 2023-03-31 | 中国人民解放军军事科学院国防科技创新研究院 | In-vivo biological nerve information detection method |
CN114775051B (en) * | 2022-04-15 | 2024-01-02 | 宁波杭州湾新材料研究院 | Small-size ultrathin single crystal diamond window for terahertz wave band and preparation method thereof |
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US6118358A (en) * | 1999-01-18 | 2000-09-12 | Crouch; David D. | High average-power microwave window with high thermal conductivity dielectric strips |
CN101830733A (en) * | 2009-03-13 | 2010-09-15 | 王兵 | Method for preparing ultra nanometer diamond coating of ceramic valve core |
CN102867716A (en) * | 2012-09-10 | 2013-01-09 | 中国电子科技集团公司第十二研究所 | Diamond-metal compound type clamping rod for travelling wave tube and manufacture method of diamond-metal compound type clamping rod |
CN103236390A (en) * | 2013-04-16 | 2013-08-07 | 中国电子科技集团公司第十二研究所 | Diamond energy transmission window for short millimeter wave traveling tubes and manufacturing method of diamond energy transmission window |
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JP2010043347A (en) * | 2008-08-18 | 2010-02-25 | Kyushu Univ | Ultra nanocrystal diamond film laminate and its method for manufacturing |
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US6118358A (en) * | 1999-01-18 | 2000-09-12 | Crouch; David D. | High average-power microwave window with high thermal conductivity dielectric strips |
CN101830733A (en) * | 2009-03-13 | 2010-09-15 | 王兵 | Method for preparing ultra nanometer diamond coating of ceramic valve core |
CN102867716A (en) * | 2012-09-10 | 2013-01-09 | 中国电子科技集团公司第十二研究所 | Diamond-metal compound type clamping rod for travelling wave tube and manufacture method of diamond-metal compound type clamping rod |
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