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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
diamond
delivery
energy window
growth
window
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201410011479.9A
Other languages
Chinese (zh)
Other versions
CN103779154A (en
Inventor
丁明清
李莉莉
杜英华
胡银富
蔡军
冯进军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CETC 12 Research Institute
Original Assignee
CETC 12 Research Institute
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CETC 12 Research Institute filed Critical CETC 12 Research Institute
Priority to CN201410011479.9A priority Critical patent/CN103779154B/en
Publication of CN103779154A publication Critical patent/CN103779154A/en
Application granted granted Critical
Publication of CN103779154B publication Critical patent/CN103779154B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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

A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof
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.
CN201410011479.9A 2014-01-10 2014-01-10 A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof Active CN103779154B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410011479.9A CN103779154B (en) 2014-01-10 2014-01-10 A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410011479.9A CN103779154B (en) 2014-01-10 2014-01-10 A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof

Publications (2)

Publication Number Publication Date
CN103779154A CN103779154A (en) 2014-05-07
CN103779154B true CN103779154B (en) 2016-03-30

Family

ID=50571289

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410011479.9A Active CN103779154B (en) 2014-01-10 2014-01-10 A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof

Country Status (1)

Country Link
CN (1) CN103779154B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010043347A (en) * 2008-08-18 2010-02-25 Kyushu Univ Ultra nanocrystal diamond film laminate and its method for manufacturing

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Also Published As

Publication number Publication date
CN103779154A (en) 2014-05-07

Similar Documents

Publication Publication Date Title
CN103779154B (en) A kind of diamond delivery of energy window of terahertz wave band vacuum device and manufacture method thereof
CN103236390A (en) Diamond energy transmission window for short millimeter wave traveling tubes and manufacturing method of diamond energy transmission window
CN102102220B (en) Preparation method of graphene on diamond (111) surface
US8318268B2 (en) AA stacked graphene-diamond hybrid material by high temperature treatment of diamond and the fabrication method thereof
CN106848016A (en) The preparation method of the porous DBR of GaN base
Yang et al. Low-temperature growth of ZnO nanorods in anodic aluminum oxide on Si substrate by atomic layer deposition
US10066317B2 (en) Method for manufacturing a single crystal diamond
US8970329B2 (en) Component having a multipactor-inhibiting carbon nanofilm thereon, apparatus including the component, and methods of manufacturing and using the component
CN105506575A (en) Manufacturing equipment and method of low temperature nanometer/ultrananocrystalline diamond film
CN211947216U (en) Microwave plasma chemical vapor deposition device
CN105244249B (en) A kind of graphene film carbon nano-tube film flexible composite and preparation method and application
CN109097741A (en) A kind of CsPbBr3The preparation method of film
CN103193224A (en) Method for preparing graphene film on nonmetallic substrate at low temperature
CN114086126B (en) Monocrystalline solar cell film material and preparation method thereof
Sahu et al. Effect of plasma parameters on characteristics of silicon nitride film deposited by single and dual frequency plasma enhanced chemical vapor deposition
CN101768741A (en) High-performance multi-layered membrane structure-borne noise surface wave device and preparation method thereof
CN110416039B (en) Energy transmission window sheet for terahertz waveband vacuum device and preparation method thereof
CN106011784A (en) Method for preparing alpha-phase molybdenum carbide crystals through microwave plasma enhanced chemical vapor deposition
CN101323971A (en) Method for preparing high quality ZnO film using cushioning layer
JP2020073433A (en) Substrate including silicon layer and diamond layer having silicon-diamond interface optically finished (or closed)
Li et al. Effect of temperature on the properties of Al: ZnO films deposited by magnetron sputtering with inborn surface texture
CN103388130B (en) The preparation method of ECR-PEMOCVD low temperature depositing InN film on ZnO buffer/diamond thin/Si multi-layer film structure substrate
KR101272995B1 (en) Method of graphene growing and graphene size adjusting
CN102094178A (en) Method for preparing high-performance surface acoustic wave device with multilayer film structure
CN111676450A (en) Hexagonal boron nitride thick film based on ion beam sputtering deposition and preparation method and application thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant