CN1265210C - Microstrip particle detector and preparation method thereof - Google Patents
Microstrip particle detector and preparation method thereof Download PDFInfo
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- CN1265210C CN1265210C CN 200310109274 CN200310109274A CN1265210C CN 1265210 C CN1265210 C CN 1265210C CN 200310109274 CN200310109274 CN 200310109274 CN 200310109274 A CN200310109274 A CN 200310109274A CN 1265210 C CN1265210 C CN 1265210C
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Abstract
The present invention relates to a microstrip particle detector and a preparation method thereof. The microstrip particle detector of the present invention comprises a substrate, a surface coating on the substrate, a top electrode and a back electrode, wherein the substrate adopts [100] silicon wafers and the upper surface of the substrate is provided with the [100] oriented diamond film coating; the surface of the diamond film coating is provided with the top electrode which is formed by combining chromium and metal; the top electrode is etched into microstrip electrodes with 25 mu m of width and interval and each microstrip electrode is led out by a magnesium aluminum leading wire; the lower surface of the substrate is provided with the back electrode which is also the chromium metal composite electrode. The preparation method of the detector of the present invention comprises the steps of etching hydrogen plasma in situ, carburizing a silicon surface, nucleating, growing the surface of a diamond and steaming and coating the chromium metal composite electrode on the surface. The particle detector of the present invention has the advantage of low production cost and is favorable for industrial production. Each performance of the detector of the present invention is comparable with a detector grade natural diamond so that the detector of the present invention has a wide application foreground.
Description
Technical field
The present invention relates to a kind of is Microstrip particle detector of making of matrix material and preparation method thereof with oriented growth on the silicon chip (100) crystal face diamond thin.
Background technology
Semiconductor detector is a kind of novel nuclear radiation detection element that has obtained developing rapidly since the sixties in 20th century, and its feature is: the energy resolution height, and linear response is good, and pulse rise time is short, and is simple in structure, the detection efficiency height, operating voltage is low, and is easy to operate.After U.S. Bel's telecommunication telephone laboratory in 1949 utilized the germanium semiconductor particle detection first, this detector caused attracting attention of countries in the world at once.Rise the seventies, along with the preparation technology of silicon materials and updating of semiconductor planar technology, makes silicon detector obtain very fast development.Silicon detector is unique detector that wide power spectrum is analyzed simultaneously that is suitable for, and has therefore obtained using widely in the Detection Techniques of particle physics.But in strong radiation environment, silicon crystal lattice is vulnerable to radiation damage, and the leakage current of detector is increased, and performance descends.The intrinsic conductivity that is produced by thermal excitation increases by index with temperature in addition, because the energy gap of silicon is less, therefore the device by the silicon materials manufacturing is not suitable for being operated in the environment that is higher than 150 ℃.
Because adamantine many excellent properties, as: energy gap big (about 5.5eV), radiation intensity height, good chemistry and temperature stability etc. make it can replace silicon and work under maximum conditions.The natural diamond of detector grade costs an arm and a leg, recyclability is poor, has limited its application as radiation detector.In recent years, because the development of chemical vapour deposition technique (CVD), the quality and the application of artificially synthesizing diamond film are greatly improved.Can prepare the diamond thin of the almost Any shape of high-purity, low defect level at present, its character is aspect a lot of even be better than natural diamond.Recently, caused the researchers' in fields such as high-energy physics, heavy-ion physics, nuclear industry and radiation dose very big interest in the progress that aspect the diamond thin of chemical vapour deposition technique (CVD) technology growth " detector grade ", obtains.
What by the detection principle of detector as can be known, determine its performance quality is the power of the transport capability in electronics and hole in the material.The diamond thin of " detector grade " requires to have extremely strong charge transport ability.Yet because the diamond thin that conventional method makes is the polycrystalline of arbitrary orientation, the character that is shown is each different directions crystal grain character and coefficient average result such as impurity, defective.And because the inconsistency of orientation, a large amount of existence of defectives such as crystal boundary have hindered transporting of electric charge, therefore can't have the excellent properties of natural uni-crystal diamond.As the natural uni-crystal diamond thermal conductivity up to (20W/cmK), even and the polycrystalline diamond film purity of arbitrary orientation is very high, thermal conductivity is also lower, the performance that makes the polycrystal film detector is not as the detector of based single crystal material.In addition, random orientation diamond film surface flatness is not high, is unfavorable for that photomask surface electrode and signal draw.
Summary of the invention
One of purpose of the present invention be to provide a kind of on silicon chip the oriented growth diamond thin be the Microstrip particle detector that matrix material is made, by suitable treatment process, make diamond thin and electrode on this detector form Ohmic contact, thereby finally improve the combination property of diamond film/silicon composite substrate as Microstrip particle detector.
The preparation method of the particle detector that second purpose of the present invention is to provide above-mentioned.
For achieving the above object, the present invention adopts following technical scheme:
A kind of Microstrip particle detector of the present invention, comprise substrate and surface coating and top electrode and back electrode, it is characterized in that substrate adopts [100] silicon chip; Upper surface at this substrate is the diamond film coating layer of [100] crystal face; On the diamond film coating layer surface is top electrode, this top electrode is to be composited by the chromium gold, and be little strip electrode of 10～50 μ m through the wide and spacing of photoetching treatment slivering, every little strip electrode has magnesium aluminum wire to draw, what wherein be close to diamond film coating layer is chromium electrode, and on the network electrode is gold electrode; The lower surface of substrate is a back electrode, and this back electrode also is a chromium gold combination electrode, and wherein close substrate is chromium electrode, and under chromium electrode is gold electrode.
The thickness of substrate is 0.5mm, and area is 2 * 2cm
2The thickness of diamond film coating layer is 50～400 μ m; The thickness of chromium electrode is 50～100m in top electrode and the back electrode, and the thickness of gold electrode is 200～800nm.
The preparation method of Microstrip particle detector of the present invention is characterized in that, this method comprises the steps:
A. hydrogen plasma in situ etching: with backing material, promptly [100] silicon chip carries out surperficial ultrasonic cleaning earlier, and putting into frequency then is that 2.45GHz, power are the settling chamber of the microwave plasma CVD device (MPCVD) of 300kW; Employing hydrogen is reacting gas, carries out hydrogen gas plasma original position etching; Hydrogen flowing quantity is 100 standard ml/min, and the air pressure of settling chamber is 800～900 ℃ at 2.7kPa by substrate temperature in the controlled microwave power adjustments settling chamber at this moment, and etching time is 15～45 minutes;
B. silicon face carburizing: change reacting gas into hydrogen and methane blended gas, wherein the flow of hydrogen and methane is respectively 100 standard ml/min and 480 standard ml/min, hydrogen and methane enter the settling chamber after mixing, the air pressure of settling chamber is at 3.2kPa at this moment, underlayer temperature is constant, and carburizing time is 30 minutes;
C. nucleation process: in this process, reacting gas still is hydrogen and methane blended gas, and wherein the flow of hydrogen and methane is respectively 100 standard ml/min and 480 standard ml/min, and hydrogen and methane enter the settling chamber after mixing, and the air pressure of settling chamber is at 3.2kPa; Underlayer temperature is reduced to 800 ℃, on substrate, add simultaneously-100～-200V dc negative bias voltage and make backing material have negative surface potential; Best nucleation time is 30 minutes;
D. diamond film growth process: at first reacting gas still is hydrogen and methane blended gas, and regulating methane flow is 100 standard ml/min, and hydrogen flowing quantity is constant, and substrate temperature is controlled at 810 ℃, and biasing is realized the growth of diamond thin; Close the methane gas switch then, only feed hydrogen, utilize hydrogen plasma that crystal grain is carried out etching; Carry out so repeatedly 8 times, wherein each cyclic process duration is 8 hours, and the time scale of film growth phase and hydrogen plasma etching phase is 6: 2;
E. surperficial evaporation chromium gold combination electrode: with the upper and lower surface of the above-mentioned sample that makes, carry out evaporation chromium gold combination electrode in LDG-2A ion beam sputtering instrument, wherein the thickness of chromium electrode is 50～100nm, and the thickness of gold electrode is 200～800nm; Adopt the MJB6 litho machine to diamond film limit chromium gold combination electrode then, promptly top electrode carries out photoetching, and the formation bar is wide to be little strip electrode of 10～50 μ m with spacing, and adopts MgAl silk lead-in wire; In annealing furnace, under the nitrogen atmosphere,, make the diamond thin Microstrip particle detector at last through 350～450 ℃ of annealing 10～30 minutes.
Because hydrogen plasma is orientated the corrasion of crystal grain much larger than the corrasion to [100] orientation crystal grain to non-[100], therefore in the methods of the invention, adopted cycling deposition technology, promptly in the grain growth process, feed control methane and hydrogen as reacting gas, realize the growth of diamond thin, close the methane gas switch subsequently, only feed hydrogen, utilize the corrasion of hydrogen plasma, carry out repeatedly so repeatedly crystal grain.By this method, can reduce the quantity of non-in the film [100] orientation crystal grain, [100] orientation crystal grain is then because more weak corrasion and preferential deposition as far as possible.Promptly under hydrionic corrasion, [100] orientation crystal grain is realized preferred growth, non-[100] orientation crystal grain since selection rule reduce gradually, when long [100] oriented growth of finally having realized diamond thin during to certain thickness of film.
In inducing nucleation process, the employing Dc bias is handled, promptly with the molybdenum sheet that goes in ring as positive electrode, quartz boat draws copper cash as negative electrode, on silicon substrate, add dc negative bias voltage, make backing material have negative surface potential, can reduce the surface potential of silicon substrate like this, the accelerated electron bombardment helps the oriented nucleation of texture and improves nucleation density.
The adhesion condition of considering adamas and gold electrode is not satisfactory, so before the gold evaporation electrode, need the chromium layer of the about 50～100nm of first evaporation one bed thickness, simultaneously, in order to realize Ohmic contact, after the intact electrode of evaporation, need to place nitrogen atmosphere to carry out annealing in process in sample.
Compare with prior art, the present invention has following remarkable advantage:
1. [100] oriented diamond film has solved the expensive problem that adopts the detector grade natural diamond and cause as the matrix material of preparation particle detector on silicon chip because the present invention adopts, and has reduced production cost, helps suitability for industrialized production.
2. because adamantine (100) crystal face has surface smoothness and lower defect concentration preferably, make height-oriented diamond thin (HOD) on the direction of growth, almost show the character of monocrystalline.Thereby the charge delivery capability that has overcome the existence of arbitrary orientation adamas is poor, thermal conductivity is low and surface smoothness is low, is unfavorable for the problem that photomask surface electrode lotus signal is drawn.
3. the collection owing to signal in the m-d-m detector is coaxial, so the performance of height-oriented diamond thin on the charge-trapping direction also shows similar and performance monocrystalline, thereby helps the transmission of electric charge.
In sum, every performance of particle detector of the present invention can compare favourably with the detector grade natural diamond fully.Thereby be with a wide range of applications.
Description of drawings
Fig. 1 is the structural representation of a kind of particle detector of the present invention
Fig. 2 is the vertical view of Fig. 1 example
Embodiment
Embodiment one: earlier referring to Fig. 1 and Fig. 2, the concrete processing step of this preparation of product is as follows:
A. hydrogen gas plasma original position etching: with area is 2 * 2cm
2, thick [100] silicon chip for 0.5mm is through acetone, HF acid (25%) and deionized water with after containing three ultrasonic cleaning of acetone suspending liquid of diamond dust, putting into frequency is that 2.45GHz, power are the settling chamber of the microwave plasma CVD device (MPCVD) of 3000kW; Employing hydrogen is reacting gas, carries out hydrogen gas plasma original position etching; Hydrogen flowing quantity is 100 standard ml/min, this moment the settling chamber air pressure at 2.7kPa, the annealing temperature by substrate in the controlled microwave power adjustments settling chamber is 815 ℃, best etching time is 30 minutes;
B. silicon face carburizing: change reacting gas into hydrogen and methane blended gas, wherein the flow of hydrogen and methane is respectively 100 standard ml/min and 480 standard ml/min, hydrogen and methane enter the settling chamber after mixing, the air pressure of settling chamber is at 3.2kPa at this moment, underlayer temperature is constant, and best carburizing time is 30 minutes;
C. nucleation process: in this process, reacting gas still is hydrogen and methane blended gas, and wherein the flow of hydrogen and methane is respectively 100 standard ml/min and 480 standard ml/min, and hydrogen and methane enter the settling chamber after mixing, and the air pressure of settling chamber is at 3.2kPa; Underlayer temperature is reduced to 800 ℃, on substrate, add simultaneously-150V dc negative bias voltage and make backing material have negative surface potential; Best nucleation time is 30 minutes;
D. diamond film growth process: at first reacting gas still is hydrogen and methane blended gas, and regulating methane flow is 100 standard ml/min, and hydrogen flowing quantity is constant, and substrate temperature is controlled at 810 ℃, and biasing is realized the growth of diamond thin; Close the methane gas switch then, only feed hydrogen, utilize hydrogen plasma that crystal grain is carried out etching; Carry out so repeatedly 8 times, wherein each cyclic process duration is 8 hours, and the time scale of film growth phase and hydrogen plasma etching phase is 6: 2; At this moment, the thickness of diamond thin is 100 μ m;
E. surperficial evaporation chromium gold combination electrode: with the upper and lower surface of the above-mentioned sample that makes, carry out evaporation chromium gold combination electrode in LDG-2A ion beam sputtering instrument, wherein the thickness of chromium electrode is 50nm, and the thickness of gold electrode is 800nm; Adopt the MJB6 litho machine to diamond film limit chromium gold combination electrode then, promptly top electrode carries out photoetching, and the formation bar is wide to be little strip electrode of 25 μ m with spacing, and adopts MgAl silk lead-in wire; In annealing furnace, under the nitrogen atmosphere,, make the diamond thin Microstrip particle detector at last through 400 ℃ of annealing 10 minutes.
With the above-mentioned diamond thin Microstrip particle detector that makes, adopt the microcomputer multichannel spectrometer test its
241α particle spectrum response characteristic (impressed voltage 200V) under the irradiation of Am source (characteristic energy 5.5MeV).Test result shows: after collecting in the 180s time, energy is that the spectrum peak at 289.6eV place is narrow, and halfwidth is 0.294eV, and energy resolution is 0.1%.Signal peak obviously separates with the bottom noise, has excellent signal to noise ratio (S/N ratio).This detector is tested time resolution characteristics under the x-ray irradiation that it is 40keV at energy, and test result shows: explorer response speed is fast, and the rise time is 3ns.
Embodiment two: present embodiment is undertaken by the same step of embodiment one preparation technology, and different is:
In the growth course of diamond thin, the cycle index of film growth phase and hydrogen plasma etching phase is 32 times, each cyclic process duration is 8 hours, and the time scale of film growth phase and hydrogen plasma etching phase is 6: 2, and this moment, the thickness of diamond thin was 400 μ m;
In surperficial evaporation chromium gold combination electrode process, the thickness 100nm of chromium electrode, the thickness of gold electrode are 200nm; Adopt the MJB6 litho machine to diamond film limit chromium gold combination electrode then, promptly top electrode carries out photoetching, and the formation bar is wide to be little strip electrode of 50 μ m with spacing, and adopts MgAl silk lead-in wire; In annealing furnace, under the nitrogen atmosphere,, make the diamond thin Microstrip particle detector at last through 400 ℃ of annealing 10 minutes.
Claims (3)
1. a Microstrip particle detector comprises substrate (1) and surface coating (2) thereof and top electrode (3) and back electrode (4), it is characterized in that, substrate (1) adopts [100] silicon chip; Upper surface at this substrate (1) is the diamond film coating layer (2) of [100] crystal face; On diamond film coating layer (2) surface is top electrode (3), this top electrode (3) is to be composited by the chromium gold, and be little strip electrode of 10～50 μ m through the wide and spacing of photoetching treatment slivering, every little strip electrode has magnesium aluminum wire to draw, what wherein be close to diamond film coating layer (2) is chromium electrode, and on the network electrode is gold electrode; The lower surface of substrate (1) is back electrode (4), and this back electrode (4) also is a chromium gold combination electrode, and wherein close substrate (1) is chromium electrode, and under chromium electrode is gold electrode.
2. Microstrip particle detector according to claim 1 is characterized in that, the thickness of substrate (1) is 0.5mm, and area is 2 * 2cm
2The thickness of diamond film coating layer (2) is 50～400 μ m; Top electrode (3) is 50～100nm with the thickness of the middle chromium electrode of back electrode (4), and the thickness of gold electrode is 200～800nm.
3. a preparation method who is used for claim 1 or 2 described Microstrip particle detectors is characterized in that this method comprises the steps:
A. hydrogen plasma in situ etching: with backing material, promptly [100] silicon chip carries out surperficial ultrasonic cleaning earlier, and putting into frequency then is that 2.45GHz, power are the settling chamber of the microwave plasma CVD device (MPCVD) of 3000kW; Employing hydrogen is reacting gas, carries out hydrogen gas plasma original position etching; Hydrogen flowing quantity is 100 standard ml/min, and the air pressure of settling chamber is 800～900 ℃ at 2.7kPa by substrate temperature in the controlled microwave power adjustments settling chamber at this moment, and etching time is 15～45 minutes;
B. silicon face carburizing: change reacting gas into hydrogen and methane blended gas, wherein the flow of hydrogen and methane is respectively 100 standard ml/min and 480 standard ml/min, hydrogen and methane enter the settling chamber after mixing, the air pressure of settling chamber is at 3.2kPa at this moment, underlayer temperature is constant, and carburizing time is 30 minutes;
C. nucleation process: in this process, reacting gas still is hydrogen and methane blended gas, and wherein the flow of hydrogen and methane is respectively 100 standard ml/min and 480 standard ml/min, and hydrogen and methane enter the settling chamber after mixing, and the air pressure of settling chamber is at 3.2kPa; Underlayer temperature is reduced to 800 ℃, on substrate, add simultaneously-100～-200V dc negative bias voltage and make backing material have negative surface potential; Nucleation time is 30 minutes;
D. diamond film growth process: at first reacting gas still is hydrogen and methane blended gas, and regulating methane flow is 100 standard ml/min, and hydrogen flowing quantity is constant, and substrate temperature is controlled at 810 ℃, and biasing is realized the growth of diamond thin; Close the methane gas switch then, only feed hydrogen, utilize hydrogen plasma that crystal grain is carried out etching; Carry out so repeatedly 8 times, wherein each cyclic process duration is 8 hours, and the time scale of film growth phase and hydrogen plasma etching phase is 6: 2;
E. surperficial evaporation chromium gold combination electrode: with the upper and lower surface of the above-mentioned sample that makes, carry out evaporation chromium gold combination electrode in LDG-2A ion beam sputtering instrument, wherein the thickness of chromium electrode is 50～100nm, and the thickness of gold electrode is 200～800nm; Adopt the MJB6 litho machine to diamond film limit chromium gold combination electrode then, promptly top electrode carries out photoetching, and the formation bar is wide to be little strip electrode of 10～50 μ m with spacing, and adopts MgAl silk lead-in wire; In annealing furnace, under the nitrogen atmosphere,, make the diamond thin Microstrip particle detector at last through 350～450 ℃ of annealing 10～30 minutes.
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| CN1328598C (en) * | 2005-01-26 | 2007-07-25 | 上海大学 | Method for preparing coplanar grid anode tellurium-zinc-cadmium detector |
| CN106024862B (en) * | 2016-06-28 | 2019-06-25 | 上海大学 | A kind of preparation method of the diamond thin with electrode/GaN hetero-junctions |
| CN114709271B (en) * | 2022-03-18 | 2024-07-23 | 中国科学院微电子研究所 | Microstrip detector and preparation method thereof |
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