CN1286351C - A manufacturing method of microstrip gas compartment detector substrate - Google Patents
A manufacturing method of microstrip gas compartment detector substrate Download PDFInfo
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- CN1286351C CN1286351C CN 200410016257 CN200410016257A CN1286351C CN 1286351 C CN1286351 C CN 1286351C CN 200410016257 CN200410016257 CN 200410016257 CN 200410016257 A CN200410016257 A CN 200410016257A CN 1286351 C CN1286351 C CN 1286351C
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- substrate
- base plate
- gas chamber
- hydrogen
- diamond film
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Abstract
The present invention relates to a manufacturing method for a base plate of a detector of a microstrip gas chamber, which is made of an upper deposition CVD diamond film of a silicon base sheet by adopting a heating wire chemical gas phase deposition method. An n-shaped (100) single crystal silicon base sheet is firstly pretreated, and then, the n-shaped (100) single crystal silicon base sheet is placed in a vacuum reaction chamber of a heating wire chemical gas phase deposition device which is filled with ethanol and hydrogen gas of reaction gases. A base plate blank is made through four processes of the cleanness of hydrogen plasma, carbonation, biasing enhancing nucleation and growth. The base plate blank is polished by using a laser method and treated in a cleaning mode to make a base plate. A diamond film base plate with high quality and low surface roughness is obtained by the present invention through two ways of controlling the preferential growth of diamond crystal particles and adopting a laser polishing method, and a large charge accumulation effect of a current detector and the instability of a base plate can be overcome. The diamond film base plate is an ideal base plate of a detector of a microstrip gas chamber. The present invention has the advantages of simple preparation technique, low cost, strong practicability, no poison and no harm.
Description
Technical field
The present invention relates to the manufacture method of a kind of micro-strip gas chamber (MSGC) detector substrate, it is to be made by chemical vapor deposition (CVD) diamond film on the silicon chip.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 cation acquisition 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 count 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 unsteadiness of substrate under High-Field that in the snowslide amplification process, produces, dead time and little detector performances such as damage decline of bringing gas gain to reduce, discharge and cause 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 volume resistivity is 10 under the room temperature
9~ 10
12During Ω cm scope, the cation 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 (Nucl.Instr.Meth.A364 (1995) 287) with suitable resistivity, but in order to reduce Order Scattering, substrate thickness should be at a hundreds of μ m, but is difficult to obtain so thin S8900 glass.Adopt evaporation semiconductor or means such as little conducting material, ion injection that substrate is carried out surface modification and obtain stable micro-strip gas chamber substrate.Though the work of this respect has obtained result preferably, but still not ideal enough.
The best of micro-strip gas chamber substrate requires: room temperature resistivity 10
9~ 10
12Ω cm; The electron conductive type material; A substrate thickness hundreds of μ m; High dielectric strength and capability of resistance to radiation etc.The material that can satisfy these requirements simultaneously is considerably less, and the adamantine premium properties of the development of chemical vapor deposition (CVD) technology and CVD makes it become best selection undoubtedly, and its resistivity can
10003 2002.4
10
7~ 10
16Ω cm is adjustable on a large scale, premium properties such as high radiation preventing intensity and physical and chemical stability, and it is a kind of good electron conductive type thin-film material.The character of CVD diamond film is as shown in table 1:
Table 1. diamond film character
| Dielectric strength | The forbidden band is wide | Dielectric constant | Hole mobility | Thermal conductivity | Hardness |
| ~10 7V/cm | ~5.5eV | ~5.7 | ~1500cm 2/Vs | ~20W/cm·K | ~10000Kg/mm 2 |
Summary of the invention
The manufacture method that the purpose of this invention is to provide the micro-strip gas chamber detector substrate of the little and substrate good stability of a kind of electric charge accumulation effect.
The present invention realizes by following steps:
A kind of manufacture method of micro-strip gas chamber detector substrate, it is to be made by chemistry for gas phase depositing diamond film on the silicon chip.The manufacturing of main employing hot filament CVD the method is characterized in that to have following processing step:
A. using n type (100) monocrystalline silicon piece is substrate, and following preliminary treatment is carried out on its surface: ultrasonic cleaning-acetone adds the bortz powder ultrasonic cleaning-oven dry of micron dimension diameter in acetone ultrasonic cleaning-10% hydrogen fluoride solution;
B. the vacuum reaction chamber that pretreated substrate is put into the hot-wire chemical gas-phase deposition device is sent into reacting gas ethanol and hydrogen after vacuumizing decompression, make its reaction; Reaction pressure stabilizes to 3～5Kpa; The mol ratio of ethanol and hydrogen is 0.005～0.08; Make the substrate blank through hydrogen plasma cleaning, carbonization, bias voltage enhancing nucleation and four processes of growing then;
C. adopt laser method that meticulous polishing is carried out on the blank surface, promptly with the ArF laser at 90 ° at wavelength 190～266nm, power 80～200mJ, laser beam incident angle from perpendicular to the thickness direction of diamond thin to its polishing 5～15min;
D. earlier through the acetone clean, again at saturated K
2CrO
7With dense H
2SO
4Handle 5～10min in the mixed solution, at NH
4OH and H
2O
2Boil 5～10min in the mixed liquor, remove surperficial graphite composition; After washed with de-ionized water, dry again, get final product the micro-strip gas chamber detector substrate formed by depositing diamond film on the silicon chip.
The bias voltage of the manufacture method of above-mentioned micro-strip gas chamber detector substrate is enhanced to the deposition parameter that adopts in the nuclear process: pressure is 3.5Kpa, and the mol ratio of ethanol and hydrogen is 0.05, and bias voltage is-200V that temperature is 850 ℃.
Micro-strip gas chamber substrate performance is the most critical parameters of detector steady operation, and the adamantine premium properties of CVD satisfies the best requirement of micro-strip gas chamber substrate fully.Condition by control heated filament CVD method growing diamond film can deposit the large area film that meets the demands on silicon chip.Should be pointed out that especially that the general diamond film that deposits with heat wire method is because surface roughness and graphite composition are more, and be not suitable for directly making little strip electrode by photoetching technique in the above, need carry out critical technical finesse to obtain to have the diamond film of excellent surface performance (as fineness, resistivity) and thickness.In conjunction with above characteristics, technical scheme of the present invention has adopted on (100) monocrystalline silicon piece deposition CVD diamond thin, and makes the substrate of micro-strip gas chamber detector grade through reprocessing such as laser polishing.
Characteristics of the present invention are to adopt hot filament CVD depositing diamond film on (100) monocrystalline silicon substrate, and through after the critical technical finesse, prepare micro-strip gas chamber detector CVD diamond thin substrate.Be reactant with ethanol and hydrogen in the inventive method, under the vacuum decompression condition, make the thick diamond film of deposition＞0.3mm on the indoor silicon chip of deposition reaction.
In order effectively to address the above problem, the present invention obtains the CVD diamond of high-quality, low surface roughness: a. control of growing by two kinds of approach: by the deposition parameter in substrate selection and preliminary treatment and the control CVD process, promote the preferred orientation of diamond crystals, obtain consistent, that appear level and smooth crystal face (100) face as far as possible diamond thin; B. adopt the laser polishing method that the CVD diamond is carried out surperficial retrofit, and carry out clean, remove surperficial graphite composition.
The CVD diamond of the present invention's preparation satisfies the requirement of micro-strip gas chamber to substrate, is the optimal selection of substrate.Area 2.5cm * 2.5cm can satisfy the requirement of making the large tracts of land micro-strip gas chamber.This material has good radiation resistance and physical and chemical stability, resistivity under the room temperature ~ 5.2 * 10
11Ω cm, and can be by technological parameters such as control growing conditions 10
7~ 10
16Ω cm is adjustable on a large scale, satisfies the requirement of detector to the substrate resistance rate; Dielectric strength ~ 7 * 10
6V/cm can make detector steady operation under high electric field strength; Dielectric constant 6.2 ~ 10 (under the 1MHz 7.5), dielectric loss are 0.005 ~ 0.026 (under the 1MHz 0.011), and this improves signal to noise ratio and have very big attraction time response for detector.(100) diamond thin is mainly by sp
3Hydridization becomes to be grouped into, but also has defectives such as non-diamond composition such as a small amount of amorphous carbon, graphite and crystal boundary, and they have certain sp
2And sp
1The hydridization composition has determined the electrical properties of film, and electronics provides the conduction charge carrier on the π key, is a kind of good electron conductivity type thin-film material therefore, can improve the stability of detector substrate and reduce the positive charge build-up effect.After reprocessings such as laser polishing, surface roughness drops to 50nm, can satisfy the making of detector chip fully.Under identical chip manufacturing and detector performance test condition, CVD Buddha's warrior attendant masonry micro-strip gas chamber substrate is significantly improved than the performance of D263 glass substrate, can see Table 2.
The micro-strip gas chamber performance of two kinds of different substrates of table 2. relatively
In addition, simple, with low cost, the wide application, practical, nontoxic of manufacture craft of the present invention.
Description of drawings
Fig. 1 makes the vapor phase growing apparatus structural representation of diamond film for the present invention.
Each digital code is expressed as follows among the figure:
1. reative cell, 2. gas, 3. ethanol, 4. thermostat, 5. tungsten filament, 6. substrate, 7. sample bench, 8. thermocouple, 9. vacuum pump, 10. pressure-reducing valve, 11 mass flowmenters, 12. mass flowmenters, 13. temperature controller, 14. barometers, 15. valves, 16. bell jars, 17. cold cut water, 18. biasing devices
Embodiment
Embodiment one
Resistivity is that the 0.5mm of 4 ~ 7 Ω cm thick (100) monocrystalline silicon piece is respectively after acetone, 10% hydrogen fluoride, acetone+bortz powder ultrasonic cleaning and oven dry, put (see figure 1) on the sample bench 7 in the reative cell 1 into, the tungsten filament 5 that it is 0.4mm that its top is provided with 16 diameters is as heating source, its power output is adjustable continuously, maximum power is 1000W, and adopting ethanol and hydrogen is reactant.Analysis pure hydrogens in the hydrogen cylinder 2 have two output branch roads, and gas transmission branch road is that hydrogen passes through mass flowmenter 11 and directly feeds cvd reactive chambers 1, and to control its flow be 100ml/min; Another gas transmission branch road is that hydrogen is by bubbling bottle 3 and take out with the analysis straight alcohol in this bottle and enter cvd reactive chamber 1 through mass flowmenter.The bubbling bottle of analyzing straight alcohol is housed places the thermostat 4 of frozen water mixed liquor to keep temperature constant.It is 2ml/min that this branch road is controlled its flow.Be connected with a vacuum pump 9 and pressure-reducing valve 10 in the bottom of cvd reactive chamber 1, can vacuumize decompression, and it is stable to keep reative cell 1 internal gas pressure, it is 4.2kPa that barometer 14 records its reaction pressure, and deposition power is stabilized in 450W.Thermocouple 8 is embedded in below the substrate 6, and recording its temperature is 800 ℃.In addition, by temperature controller 13 substrate temperature is stabilized in ± 10 ℃, the standoff distance of tungsten filament and substrate 6 remains on about 8mm.The CVD diamond film deposition has the four-stage process, i.e. hydrogen plasma cleaning, carbonization, bias voltage strengthen nucleation and growth.Wherein, at nucleation stage, apply-the 200V bias voltage by 18 pairs of substrates; At growth phase, every growing diamond membrane was closed the branch road that carries ethanol after 2 hours, and making does not have carbon source in the reative cell and stop growing, and atomic hydrogen carries out 0.5 hour etching to film, and then opens the branch road that carries ethanol, carries out diamond film growth.Hydrogen plasma cleaning in heated filament CVD diamond deposition, carbonization, bias voltage strengthen the major parameter such as the following table 3 of the nucleation and four processes of growing.
Table 3.HFCVD diamond deposition parameters
| Parameter | Hydrogen plasma cleans | Carbonization | Nucleation (bias voltage enhancing) | Growth (cycling deposition) |
| Power (W) | 450 | 600 | 450 | 450 |
| Pressure (kPa) | 4.2 | 4.8 | 3.5 | 4.2 |
| Gas mole ratio | H 2 | C 2H 5OH/H 2＝0.02 | C 2H 5OH/H 2＝0.05 | C 2H 5OH/H 2＝0.005 |
| Bias voltage (V) | -200 | |||
| Temperature (℃) | 800 | 950 | 850 | 800 |
| Time (h) | 0.5 | 1 | 0.25 | 2 |
Through 15 hours deposition reaction, can obtain ~ (100) oriented diamond film blank that 10 μ m are thick.The ArF laser that adopts 90 ° of wavelength 193nm, power 100mJ, pulse repetition frequency 20Hz, laser beam incident angle then from perpendicular to the thickness direction of diamond thin to its meticulous polishing 10min, make surface roughness be reduced to 50nm.Diamond thin after the polishing is after the acetone clean, at saturated K
2CrO
7With H
2SO
4Handle 10min in the boiling mixed solution, then at NH
4OH and H
2O
2Boil 10min in the mixed liquor, remove surperficial graphite composition, promptly get the micro-strip gas chamber substrate.Utilize modern advanced microelectronic processing technology, on the CVD cvd diamond substrate, make the micro-strip gas chamber graphics chip by lithography, and make complete micro-strip gas chamber detector by gold ball bonding and encapsulation.Utilize rearmounted electronic system to carry out detector data collection and processing, 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 100mCcm
-1
Claims (3)
1. the manufacture method of a micro-strip gas chamber detector substrate, it is to be made by chemistry for gas phase depositing diamond film on the silicon chip, mainly adopts the hot filament CVD manufacturing, this substrate manufacturing is characterised in that to have following processing step:
A. using n type (100) monocrystalline silicon piece is substrate, and following preliminary treatment is carried out on its surface: ultrasonic cleaning-acetone adds the bortz powder ultrasonic cleaning-oven dry of micron dimension diameter in acetone ultrasonic cleaning-10% hydrogen fluoride solution;
B. the vacuum reaction chamber that pretreated substrate is put into the hot-wire chemical gas-phase deposition device is sent into reacting gas ethanol and hydrogen after vacuumizing decompression, make its reaction; Reaction pressure stabilizes to 3～5Kpa; The mol ratio of ethanol and hydrogen is 0.005～0.08; Make the substrate blank through hydrogen plasma cleaning, carbonization, bias voltage enhancing nucleation and four processes of growing then;
C. adopt laser method that meticulous polishing is carried out on the blank surface, promptly with the ArF laser at 90 ° at wavelength 190～266nm, power 80～200mJ, laser beam incident angle from perpendicular to the thickness direction of diamond thin to its polishing 5～15min;
D. earlier through the acetone clean, again at saturated K
2CrO
7With dense H
2SO
4Handle 5～10min in the mixed solution, at NH
4OH and H
2O
2Boil 5～10min in the mixed liquor, remove surperficial graphite composition; After washed with de-ionized water, dry again, get final product the micro-strip gas chamber detector substrate formed by depositing diamond film on the silicon chip.
2. press the manufacture method of the described micro-strip gas chamber detector substrate of claim 1, it is characterized in that described bias voltage is enhanced to the deposition parameter that adopts in the nuclear process: pressure is 3.5Kpa, the mol ratio of ethanol and hydrogen is 0.05, and bias voltage is-200V that temperature is 850 ℃.
3. press the manufacture method of the described micro-strip gas chamber detector substrate of claim 1, it is characterized in that described growth course adopts the cycling deposition method of growth-etching-growth, promptly discontinuity stops carbon source in growth course, carries out hydrogen plasma etching diamond film.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410016257 CN1286351C (en) | 2004-02-12 | 2004-02-12 | A manufacturing method of microstrip gas compartment detector substrate |
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|---|---|---|---|
| CN 200410016257 CN1286351C (en) | 2004-02-12 | 2004-02-12 | A manufacturing method of microstrip gas compartment detector substrate |
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| CN1286351C true CN1286351C (en) | 2006-11-22 |
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ID=34351780
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1302890C (en) * | 2005-03-18 | 2007-03-07 | 北京工业大学 | Polishing method and device for sphere high quality large area diamond thick film |
| CN100409460C (en) * | 2006-06-27 | 2008-08-06 | 上海大学 | Method for preparing detector in ultraviolet light |
| CN100432287C (en) * | 2006-07-21 | 2008-11-12 | 上海大学 | Process for preparing diamond film under strong magnetic field |
| CN101393852B (en) * | 2008-11-11 | 2010-04-14 | 武汉工程大学 | Method for cleaning semiconductor wafer |
| CN103757600A (en) * | 2014-01-06 | 2014-04-30 | 上海交通大学 | Method for preparing silicon-doped micro-nano composite diamond film through chemical vapor deposition (CVD) |
| CN104498892A (en) * | 2014-12-12 | 2015-04-08 | 中国科学院重庆绿色智能技术研究院 | Method for preparing graphene film through low-temperature fixed-point nucleating |
| CN108823551A (en) * | 2018-07-05 | 2018-11-16 | 四川纳涂科技有限公司 | A kind of matrix self-cleaning method in cvd diamond deposition process |
| US20220184743A1 (en) * | 2019-04-05 | 2022-06-16 | Tokyo Electron Limited | Substrate processing system and substrate processing method |
| CN110079786A (en) * | 2019-06-03 | 2019-08-02 | 杭州睿清环保科技有限公司 | It is used to prepare the device of the hot wall HF CVD of large-area diamond film |
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