CN1557758A - Method for making composite substrate of microstrip gas-compartment detector - Google Patents

Method for making composite substrate of microstrip gas-compartment detector Download PDF

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CN1557758A
CN1557758A CNA2004100162604A CN200410016260A CN1557758A CN 1557758 A CN1557758 A CN 1557758A CN A2004100162604 A CNA2004100162604 A CN A2004100162604A CN 200410016260 A CN200410016260 A CN 200410016260A CN 1557758 A CN1557758 A CN 1557758A
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substrate
base plate
composite base
gas chamber
micro
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CN1259269C (en
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夏义本
王林军
张明龙
杨莹
汪琳
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The process of making composite substrate for micro stripe gas chamber detector is one RF plasma aided chemically vapor deposition process to deposit diamond-like film onto D263 glass. Optical glass D263 via pre-treatment is first deposited inside high vacuum reaction chamber and then annealed in a nitrogen atmosphere furnace to produce composite substrate. By means of applying bios, increasing magnetic field and annealing treatment, the present invention obtain high quality composite diamond-like/D263 glass substrate. The present invention overcomes the stress between the film and the substrate, lower combining force and other problems, and has less detector charge accumulating effect and high substrate stability.

Description

A kind of manufacture method of micro-strip gas chamber detector composite base plate
Technical field
The present invention relates to the manufacture method of a kind of micro-strip gas chamber (MSGC) detector composite base plate, it is to be made by D263 deposition on glass quasi-diamond (DLC) film.Belong to thin film vapor deposition technology, detector and high energy physics and nuclear physics field.
Background technology
A.Oed was on the multiwire proportional chamber basis in 1988, a kind of novel position sensitive detector is proposed---micro-strip gas chamber (Microstrip Gas Chamber, MSGC), because strip width and spacing is little, good uniformity, make the positive ion collection time very short, can satisfy under high counting rate and work, demonstrate advantages such as high spatial resolution and temporal resolution, obtain Preliminary Applications experimentally, become the candidate of high-energy physics experiment middle high-resolution of new generation and high counting rate track detector, and developing and be used for the X-ray imaging detector.Though micro-strip gas chamber has shown very excellent performance, but some problems have also been found under study for action, mainly be positive charge build-up effect and the unstable of substrate under High-Field that in the snowslide amplification process, produces, bring gas gain reduce, discharge dead time of causing and little to damage etc. and to cause detector performance to descend thus.
The positive charge build-up effect is the main problem that the particularly high counting rate detector of gas detector faces, and the substrate performance is the index of decision micro-strip gas chamber performance most critical.The micro-strip gas chamber substrate is generally selected insulation or little conducting material for use, as plastics, glass, quartz etc.Studies show that: adopting the low-resistivity substrate is a kind of effective ways of avoiding the positive charge accumulation, and body resistivity is 10 under the room temperature 9~ 10 12During Ω cm scope, the positive ion that substrate surface is offset can reach 10 6Mm -2s -1(Nucl.Instr.Meth.A 400 (1997) 233)).As the micro-strip gas chamber substrate, 20 ℃ of following resistivity are 10 9~ 10 12Best between Ω cm.People have found the highly stable glass substrate of a kind of Schott of crying S8900, it is the N-semiconductor glass with suitable resistivity, but in order to reduce Order Scattering, substrate thickness should be greater than a hundreds of μ m, but is difficult to obtain so thin S8900 glass.Adopt evaporation semi-conductor or little conducting material, means such as ion implantation substrate to be carried out surface modification obtain stable micro-strip gas chamber substrate, the work of this respect has obtained result preferably.
(Diamond-like Carbon, DLC) film has many premium propertiess similar with diamond (as table 1.) to quasi-diamond, and easier depositing large-area, has the film of optics flat surface.The best that its performance can satisfy the micro-strip gas chamber substrate fully requires: room temperature resistivity 10 9~ 10 12Ω cm; The electron conductive type material; High dielectric strength and capability of resistance to radiation etc.
Table 1. diamond-film-like electric property
Resistivity Dielectric strength The forbidden band is wide Specific inductivity Thermal conductivity
10 9~10 12Ω·cm ~10 7V/cm 2~3eV 4~9 0.7~1W/cm·K
Summary of the invention
The purpose of this invention is to provide that a kind of electric charge accumulation effect is little, substrate good stability and compatible good micro-strip gas chamber detector composite base plate.
The present invention realizes by following steps:
The manufacture method of a kind of micro-strip gas chamber (MSGC) detector composite base plate, it is to be made by D263 deposition on glass quasi-diamond (DLC) film.Main employing radio-frequency plasma auxiliary chemical vapor deposition method is made, and the method is characterized in that to have following processing step:
A. the opticglass D263 with thick 0.5mm makes substrate, cleans 10min in acetone, deionized water for ultrasonic successively, oven dry;
B. pretreated substrate is put into the vacuum reaction chamber of radio-frequency plasma assistant chemical vapor deposition device behind pumping high vacuum, send into reactant gases methane and argon gas, reaction pressure is stabilized in 0.5 ~ 5pa, and methane flow is 10 ~ 60ml/min, and argon flow amount is 50 ~ 200ml/min.The reaction self-bias is stabilized in 950V, substrate DC bias-50 ~-300V, underlayer temperature is controlled at below 80 ℃ by recirculated cooling water; Obtaining the quasi-diamond film thickness behind deposition reaction 2 ~ 5h is the composite base plate blank of 0.5 ~ 2.0 μ m;
C. the composite base plate blank is put into the nitrogen atmosphere stove, 200 ~ 450 ℃ of following anneal 15 ~ 60 minutes, get final product micro-strip gas chamber detector composite base plate.
Micro-strip gas chamber substrate performance is the most critical parameters of detector steady operation, and the premium properties of diamond-film-like/D263 glass satisfies the best requirement of micro-strip gas chamber substrate fully.But in deposition on glass quasi-diamond membrane process, because sedimentary energy and underlayer temperature are lower, film and substrate, thin-film memory are met water or solvent and are come off easily in bigger unrelieved stress.If without appropriate technical finesse, also can stress and bonding force problem and be not suitable for making the micro-strip gas chamber chip thereon.
In order effectively to address the above problem, the present invention is when depositing diamond-like (DLC) film, to substrate apply-50 ~-bias voltage of 300V and increase magnetic field and come active ion is selected, and raising energy of plasma, thereby the effect of increase and substrate makes sticking power strengthen and deposit high-quality film.This method is to carry out simultaneously with the CVD deposition process, and can not introduce other impurity, can the performance of material not had a negative impact, and is simple to operation.The important means that another kind of the present invention improves diamond-film-like sticking power is: the sample behind the deposit film is put into the nitrogen atmosphere stove, annealed 15 ~ 60 minutes down at 200 ~ 450 ℃, can obviously improve the sticking power and the surface finish of quasi-diamond (DLC) film, can not make film generation greying simultaneously.This is that annealing has reduced hydrogen richness in the film because having a large amount of c h bonds, hydrogen in film is to cause film to have the major cause of stress, thereby stress is reduced and improves adhesive force and intensity.
Diamond-film-like/D263 glass the composite base plate of the present invention's preparation has good radiation resistance and physical and chemical stability, resistivity under the room temperature ~ 10 10Ω cm, and 10 9~ 10 12Ω cm scope is adjustable, satisfies the optimal resistivity requirement of detector substrate.Breakdown electric field 3.2 * 10 6V/cm can make detector be operated under the high voltage, obtains high gas gain.Dielectric coefficient 2.3 under the 1MHz, and dielectric loss is 1.7 * 10 -3, help to improve the detector signal to noise ratio.Diamond-film-like is mainly by sp 2And sp 3Two kinds of one-tenth of hydridization are grouped into sp in the film 3Hydridization is sp 2More than 100 times of hydridization is mainly the diamond composition, wherein sp 2The π bonding electron of hydridization has determined the film electric property, so it is a kind of electron conductive type material, can improve the stability of detector, reduces electric charge accumulation effect.Surface average roughness is 4.25nm, and the ultrasonic several hrs of washing does not have any obscission in water or acetone solvent, can satisfy the manufacturing conditions of detector chip fully.
Under identical chip manufacturing and detector performance test condition, diamond-film-like/D263 glass is made the micro-strip gas chamber composite base plate and is significantly improved than D263 glass properties, sees Table 2.
The micro-strip gas chamber performance of two kinds of different substrates of table 2. relatively
In addition, the present invention is compatible mutually with present widely used micro-strip gas chamber substrate and device making technics, and manufacture craft is simple, with low cost, fabrication cycle fast, wide application, practical.
Description of drawings
Fig. 1 is the structural representation of radio-frequency plasma assistant chemical vapor deposition device.
Each digital code is expressed as follows among the figure:
1. gas 2,3,4. target 7. negative electrode graphite target 8. permanent magnets 9. vacuum reaction chambers 10. radio frequency generatorss 11. recirculated cooling waters 12. direct-current biasinges 13. venting ports 14. reducing valve 15. vacuum pumps+molecular pump air-bleed system 16. vacuumometers on float typeflowmeter 5. inlet mouths 6. graphite
Embodiment
After now embodiments of the invention being described in.
Embodiment one
Use the opticglass D263 of thick 0.5mm, area 2cm * 2cm to make substrate, successively at acetone, deionized water ultrasonic cleaning 10min.After the oven dry substrate is put on the negative electrode graphite target 7 of vacuum reaction chamber 9 of radio-frequency plasma assistant chemical vapor deposition device (as Fig. 1), rf frequency is 13.56MHz, and adopting high-purity (99.99%) methane gas and high-purity (99.998%) argon gas is reactant.Two-way gas mixes through under meter dominant discharge separately and before entering reaction chamber respectively, and argon gas branch road dominant discharge is 60ml/min, and methane flow is 30ml/min.Be connected with vacuum pump+molecular pump air-bleed system 15 and reducing valve 14 below reaction chamber 9, can carry out the pumping high vacuum decompression, and it be stable to keep reaction chamber 9 internal gas pressures, it is 1~2Pa that vacuumometer 16 records its reaction pressure, and the reaction self-bias is stabilized in 950V.Underlayer temperature is controlled at below 80 ℃ by recirculated cooling water.Between substrate and plasma body, add a direct current reverse voltage-200V, permanent magnet 8 is arranged below the negative electrode graphite target 7, can select, thereby improve the quality of diamond-film-like greatly the activated atomic radical.Obtain the composite base plate blank of quasi-diamond film thickness behind the deposition reaction 3h for ~ 1.0 μ m.
Diamond-film-like/D263 glass composite base plate blank is put into the annealing furnace of nitrogen protection,, can obtain well behaved micro-strip gas chamber composite base plate 300 ℃ of following anneal 30 minutes.Utilize modern advanced microelectronic processing technology, on diamond-film-like/D263 composite base plate, make the micro-strip gas chamber graphics chip by lithography, and make complete micro-strip gas chamber by gold ball bonding and encapsulation.Utilize rearmounted electronic system to carry out detector data and gather and handle, but the information of analyzing radiation particle or ray just, and the counting rate ability of detector is greater than 10 6Mm -2S -1, the maximum electric charge of collecting reaches 100mC.cm -1

Claims (4)

1. the manufacture method of a micro-strip gas chamber (MSGC) detector composite base plate, it is to be made by D263 deposition on glass quasi-diamond (DLC) film.Main employing radio-frequency plasma auxiliary chemical vapor deposition method is made, and the method is characterized in that to have following processing step:
A. the opticglass D263 with thick 0.5mm makes substrate, cleans 10min in acetone, deionized water for ultrasonic successively, oven dry;
B. pretreated substrate is put into the vacuum reaction chamber of radio-frequency plasma assistant chemical vapor deposition device behind pumping high vacuum, send into reactant gases methane and argon gas, reaction pressure is stabilized in 0.5 ~ 5pa, and methane flow is 10 ~ 60ml/min, and argon flow amount is 50 ~ 200ml/min.The reaction self-bias is stabilized in 950V, substrate DC bias-50 ~-300V, underlayer temperature is controlled at below 80 ℃ by recirculated cooling water; Obtaining the quasi-diamond film thickness behind deposition reaction 2 ~ 5h is the composite base plate blank of 0.5 ~ 2.0 μ m;
C. the composite base plate blank is put into the nitrogen atmosphere stove, 200 ~ 450 ℃ of following anneal 15 ~ 60 minutes, get final product micro-strip gas chamber detector composite base plate.
2. the manufacture method of micro-strip gas chamber detector composite base plate according to claim 1 is characterized in that being equipped with magnetic field in the described radio-frequency plasma assistant chemical vapor deposition device, and substrate is applied negative bias is-200V.
3. by the manufacture method of the described micro-strip gas chamber detector of claim 1 composite base plate, it is characterized in that the temperature optimum is 300 ℃ in the described anneal, the time is 30 minutes.
4. by the manufacture method of the described micro-strip gas chamber detector of claim 1 composite base plate, it is characterized in that described quasi-diamond film thickness optimum is ~ 1.0 μ m.
CN 200410016260 2004-02-12 2004-02-12 Method for making composite substrate of microstrip gas-compartment detector Expired - Fee Related CN1259269C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831625A (en) * 2010-05-28 2010-09-15 江苏南晶红外光学仪器有限公司 Process for forming diamond-like carbon film on surface of infrared optical element
CN102330063A (en) * 2011-06-13 2012-01-25 星弧涂层科技(苏州工业园区)有限公司 Method for preparing DLC (Diamond-Like Carbon) coating with high visible light transmissivity
CN105152548A (en) * 2015-08-21 2015-12-16 浙江星星瑞金科技股份有限公司 Preparation method of diamond-like film glass

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831625A (en) * 2010-05-28 2010-09-15 江苏南晶红外光学仪器有限公司 Process for forming diamond-like carbon film on surface of infrared optical element
CN102330063A (en) * 2011-06-13 2012-01-25 星弧涂层科技(苏州工业园区)有限公司 Method for preparing DLC (Diamond-Like Carbon) coating with high visible light transmissivity
CN105152548A (en) * 2015-08-21 2015-12-16 浙江星星瑞金科技股份有限公司 Preparation method of diamond-like film glass
CN105152548B (en) * 2015-08-21 2017-07-21 浙江星星科技股份有限公司 A kind of preparation method of DLC film glass

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