CN101924160B - Infrared photovoltage detector in In203/PbTe heterojunction and preparation method thereof - Google Patents

Infrared photovoltage detector in In203/PbTe heterojunction and preparation method thereof Download PDF

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CN101924160B
CN101924160B CN2010102280564A CN201010228056A CN101924160B CN 101924160 B CN101924160 B CN 101924160B CN 2010102280564 A CN2010102280564 A CN 2010102280564A CN 201010228056 A CN201010228056 A CN 201010228056A CN 101924160 B CN101924160 B CN 101924160B
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pbte
electrode
heterojunction
mid
vapor deposition
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CN101924160A (en
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吴惠桢
魏晓东
蔡春锋
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention provides a technique for manufacturing an infrared photovoltage detector in In203/PbTe heterojunction. The method comprises the following steps of: with CdZnTe as the substrate, growing a p-type PbTe semiconductor single crystal film on the substrate by using a molecular beam epitaxy (MBE) device, growing an n-type In203 polycrystal film on the p-type PbTe semiconductor single crystal film by using a magnetic control sputtering device to form pn junction; and with ZnS as an insulation protective layer, forming an electrode window through a standard photoetching process, ICP dry etching In2O3, wet etching ZnS and evaporating the In film electrode, and manufacturing pn junction photovoltage detector chip through back side reduction and gold wire lead, wherein the spectral response is in the 2-5mum of middle-infrared band, and the chip has faster response speed and higher responsiveness.

Description

In 2O 3/ PbTe heterojunction mid-infrared light volt type detector and preparation method thereof
Technical field
The present invention relates to heterojunction semiconductor photovoltaic detector of a kind of middle-infrared band response and preparation method thereof, more particularly, is a kind of In 2O 3/ PbTe heterojunction mid-infrared light volt type detector and preparation method thereof.
Background technology
In recent years, along with the traction of system applies, Infrared Detectors is as the core component of infrared machine system, and its research, exploitation and even production more and more receive publicity.Infrared Detectors is the device that the infrared radiation signal with incident is transformed into signal of telecommunication output, and in Infrared Detectors, photovoltaic detector is of greatest concern a kind of.Semiconductor produces electron hole pair after absorbing the enough big photon of energy, and under the effect of internal electric field, electronics and hole be respectively to two polar motions, thus on the both sides, interface the generation photovoltage.The detector that utilizes this photovoltaic effect to process is exactly a photovoltaic detector.
PbTe is a kind of important narrow gap semiconductor mid-infrared light electric material, has quantum efficiency height, highly sensitive, advantage such as device noise is low with the middle Infrared Detectors of this material.As far back as early 1930s; Belonging to the similar IV-VI semi-conductive PbS of family is a kind of infrared photoconductive detector by the development of German's early start; Be used for the infrared communication machine in the World War II; The missile-borne fuse of " rattle snake " infrared guidance and the detection of a target of U.S.'s current year's production also are to use this detector, and are still using till now always.Photovoltaic detector based on IV-VI family semi-conducting material has quicker response and more superior performance than photoconductive detector.
Chinese patent 200810060092.7 disclose a kind of in the CdTe substrate molecular beam epitaxial method prepare the method for IV-VI family semiconductor single crystal thin film.PbTe is that IV-VI family is semi-conductive a kind of, and the band gap of PbTe is narrower than PbS, the mid-infrared light that detectable wavelength is longer.
Summary of the invention
The objective of the invention is to solve problem set forth above, providing a kind of is base with Chinese patent 200810060092.7 prepared non-impurity-doped PbTe semiconductor single crystal thin films, growth In 2O 3Thin layer constitutes a kind of heterojunction photovoltaic detector of effectively surveying for the light of middle-infrared band.
Technical scheme of the present invention is such:
A kind of In 2O 3/ PbTe heterojunction mid-infrared light volt type detector, with CdZnTe as substrate, growth p-type PbTe monocrystal thin films in substrate, growth n-type In on the PbTe monocrystal thin films 2O 3Polycrystal film forms heterojunction, also comprises insulating protective layer, electrode.
Use ZnS as insulating protective layer.
Described electrode is the In membrane electrode.
Also comprise the spun gold lead-in wire, utilize conductive silver glue spun gold lead-in wire and electrode bonding.
A kind of In 2O 3The preparation method of/PbTe heterojunction mid-infrared light volt type detector is in the CdZnTe substrate, utilizes molecular beam epitaxy (MBE) the method undoped p-type PbTe monocrystal thin films of growing, and utilizes the magnetically controlled sputter method n-type In that on the PbTe monocrystal thin films, grows 2O 3Polycrystal film forms heterojunction, adopts vacuum deposition method vapor deposition ZnS as insulating protective layer, adopts vacuum deposition method vapor deposition In film to do electrode.
Step of preparation process is following:
1) the CdZnTe substrate is prepared;
2) MBE growth PbTe monocrystal thin films;
3) magnetron sputtering growth In 2O 3Polycrystal film;
4) epitaxial wafer cleans;
5) photoetching table top;
6) ICP dry etching table top;
7) vapor deposition ZnS film;
8) photoetching graph window;
9) ZnS wet etching;
10) photoetching electrode window through ray;
11) vapor deposition In electrode;
12) peel off;
13) photoetching thickening electrode window through ray;
14) vapor deposition adds thick electrode;
15) peel off;
16) thinning back side;
17) spun gold lead-in wire and electrode bonding;
18) Dewar packaging and testing.
Use ICP dry etch process etching In 2O 3Form table top, etching gas is selected Cl for use 2/ H 2/ CH 4=7: 10: 8,20 ℃ of temperature, pressure 3.5mTorr, RE power 200W, ICP power 300W.
Use the In film as upper/lower electrode, metal In and In 2O 3All satisfy the good Ohmic contact characteristic with PbTe.
Beneficial effect of the present invention is following:
Under low temperature environment (>=200K), this detector is sensitive to the light reaction of middle-infrared band, responsiveness is big.
Description of drawings
Fig. 1 is growth PbTe film, In in the CdZnTe substrate 2O 3Form the sectional view of heterojunction behind the film;
Fig. 2 is the sample in cross section figure behind the photoetching table top;
Fig. 3 is the sample in cross section figure behind the ICP dry etching table top;
Fig. 4 is the sample in cross section figure behind the vapor deposition ZnS film;
Fig. 5 is the photoetching graph window, the sample in cross section figure behind the wet etching ZnS;
Fig. 6 be vapor deposition In electrode and peel off after sample in cross section figure;
Fig. 7 be vapor deposition add thick electrode and peel off after sample in cross section figure;
Among the figure: the 1st, substrate, the 2nd, PbTe monocrystal thin films, the 3rd, In 2O 3Polycrystal film, the 4th, insulating protective layer, the 5th, electrode, the 6th, add thick electrode, the 7th, photoresist.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are further elaborated:
In 2O 3/ PbTe heterojunction mid-infrared light volt type detector, with CdZnTe as substrate 1, growth p-type PbTe monocrystal thin films 2 in substrate 1, growth n-type In on PbTe monocrystal thin films 2 2O 3 Polycrystal film 3 forms heterojunction, also comprises insulating protective layer 4, electrode 5.
Use ZnS as insulating protective layer 4.
Described electrode 5 is an In membrane electrode 5.
Also comprise the spun gold lead-in wire, utilize conductive silver glue spun gold lead-in wire and electrode 5 bondings.
In 2O 3The preparation method of/PbTe heterojunction mid-infrared light volt type detector is in CdZnTe substrate 1, utilizes molecular beam epitaxy (MBE) the method undoped p-type PbTe monocrystal thin films 2 of growing, and utilizes the magnetically controlled sputter method n-type In that on PbTe monocrystal thin films 2, grows 2O 3 Polycrystal film 3 forms heterojunction, adopts vacuum deposition method vapor deposition ZnS as insulating protective layer 4, adopts vacuum deposition method vapor deposition In film to do electrode 5.
Concrete step of preparation process is following:
1) CdZnTe substrate 1 is prepared
CdZnTe single crystal substrates 1 is bought by market, and crystal orientation < 111 >, Zn content is 4%, before epitaxial growth film, handle through chemical polishing and high-temperature degassing earlier.
2) MBE growth p-type PbTe monocrystal thin films 2
In CdZnTe substrate 1, adopt molecular beam epitaxial method growth p-type PbTe monocrystal thin films 2, through regulating the line ratio with control growing temperature, VI/IV family, acquisition p-type PbTe monocrystal thin films 2, film thickness～2um, carrier concentration～5 * 10 17Cm -3, carrier mobility～700cm 2/ Vs.
3) magnetron sputtering growth n-type In 2O 3 Polycrystal film 3
On PbTe monocrystal thin films 2 with radio frequency magnetron sputtering method growth n-type In 2O 3 Polycrystal film 3, through the control growing temperature, the air pressure n-type In of sputtering power and sputter gas 2O 3 Polycrystal film 3, two-layer n-type In successively grows 2O 3: the film thickness～500nm that grows earlier, carrier concentration～5 * 10 18Cm -3, carrier mobility～5cm 2/ Vs regrowth film thickness～200nm, carrier concentration～5 * 10 19Cm -3, carrier mobility～15cm 2/ Vs.Ready epitaxial slice structure is seen Fig. 1.
4) epitaxial wafer cleans
Epitaxial wafer is successively soaked 5 minutes 2 times with carbon tetrachloride, and acetone soaks 5 minutes 3 times, soaked in absolute ethyl alcohol 5 minutes 3 times, and deionized water rinsing 3 minutes, nitrogen dries up.
5) photoetching table top
Cleaned epitaxial wafer is put into 120 ℃ of baking ovens 30 minutes, remove the slice, thin piece surface moisture.Take out epitaxial wafer, cooled off 3～5 minutes.Even glue uses ultraviolet eurymeric photoresist 7, and condition is 6000r/min, the even 40 seconds glue time.Putting into 80 ℃ of baking ovens behind the even glue carries out drying by the fire timing 20 minutes before the photoetching.Photoetching, 40 seconds time for exposure, exposure intensity is determined by mask aligner.Develop after the photoetching, the proportioning of developer solution and water is 1: 1, developing time 35 seconds at once.Nitrogen dries up, and put into 120 ℃ of baking ovens and carry out drying by the fire after the photoetching, timing 20 minutes, purpose is for post bake, improves the adhesiveness of photoresist 7 and substrate, optimizes the corrosion edge.Sample in cross section figure after the completion photoetching process sees Fig. 2.
6) ICP dry etching table top
Should carry out mesa etch immediately behind the post bake.Use ICP dry etch process etching table top, concrete parameter is: Cl 2/ H 2/ CH 4=7: 10: 8,20 ℃ of temperature, pressure 3.5mTorr, RE power 200W, ICP power 300W, etch period 5min30s.Etch thicknesses 850～900nm.After etching is accomplished, place 50 ℃ of acetone under the water bath condition to soak about 2 hours in sample, take out afterwards, place in the culture dish that fills acetone, gently wipe away sample surfaces, remove the photoresist 7 of carbonization with cotton.The sample in cross section figure that accomplishes after the above technology sees Fig. 3.
7) vapor deposition ZnS film
Use thermal evaporation technology vapor deposition ZnS film, vapor deposition air pressure is 5 * 10 -3Pa, the vapor deposition electric current is about 140A, about 40 seconds of vapor deposition time, uses the real-time monitoring film thickness of crystal oscillator appearance in the evaporate process.Vapor deposition ZnS insulating protective layer 4250～300nm sees Fig. 4.
8) photoetching graph window
With the standard cleaning that the epitaxial wafer of the good ZnS insulating barrier of vapor deposition passes through acetone-absolute ethyl alcohol-deionized water, nitrogen dries up, and puts into 120 ℃ of baking ovens 30 minutes.Take out epitaxial wafer, cooled off 3～5 minutes.Even glue uses ultraviolet eurymeric photoresist 7, and condition is 6000r/min, the even 40 seconds glue time.Putting into 80 ℃ of baking ovens behind the even glue carries out drying by the fire timing 20 minutes before the photoetching.Photoetching, 40 seconds time for exposure, exposure intensity is determined by mask aligner.Develop after the photoetching, the proportioning of developer solution and water is 1: 1, developing time 35 seconds at once.Nitrogen dries up, and puts into 120 ℃ of baking ovens and carries out back baking post bake, timing 20 minutes.
9) ZnS wet etching
Should corrode immediately behind the post bake.Sample is dipped in reaction 4-5 second in 37% concentrated hydrochloric acid, and deionized water rinsing is clean, and nitrogen dries up, and device window forms.Sample is placed acetone 2 times, each 10 minutes, remove photoresist 7, absolute ethyl alcohol cleans 2 times, and deionized water rinsing is clean, and nitrogen dries up.Sample in cross section figure after the corrosion sees Fig. 5.
10) photoetching electrode 5 windows
Cleaned sample is put into 120 ℃ of baking ovens 30 minutes, remove moisture.Take out epitaxial wafer, cooled off 3～5 minutes.Even glue uses ultraviolet eurymeric photoresist 7, and condition is 3500r/min, the even 40 seconds glue time.Putting into 80 ℃ of baking ovens behind the even glue carries out drying by the fire timing 20 minutes before the photoetching.Photoetching, 60 seconds time for exposure, exposure intensity is determined by mask aligner.Develop after the photoetching, the proportioning of developer solution and water is 1: 1, developing time 40 seconds at once.Nitrogen dries up, and does not carry out back baking post bake.
11) vapor deposition In electrode 5
Use thermal evaporation technology vapor deposition In electrode 5, in the vapor deposition boat, put into 3 In grains, vapor deposition air pressure is 5 * 10 -3Pa, the vapor deposition electric current is about 100A, uses the real-time monitoring film thickness of crystal oscillator appearance in the evaporate process, and 3 In grains evaporate fully, In thickness 200～250nm.
12) peel off
Sample is soaked in 50 ℃ of acetone under the water bath condition, and soak time is about 3 hours.Take out afterwards, place in the culture dish that fills acetone, use cotton gently to wipe away material surface, the In film of vapor deposition on photoresist 7 wiped away.Take out epitaxial wafer, alcohol wash 3 times, each 5 minutes, deionized water rinsing 3 minutes, nitrogen dries up.The sample in cross section figure that peels off after the completion sees Fig. 6.
13) photoetching adds thick electrode 6 windows
Processing step is identical with step 10) photoetching electrode 5 windows, photoetching.
14) vapor deposition adds thick electrode 6
Processing step is identical with step 11) vapor deposition In electrode 5, vapor deposition In thickness 200～250nm.
15) peel off
Processing step is peeled off identical with step 12).Sample in cross section figure after the completion sees Fig. 7.
16) thinning back side
Use the paraffin bonding die, cooling is placed on attenuate on the attenuate machine, and attenuate is used Al 2O 3Powder.Take off sample after accomplishing attenuate, be placed on earlier in the carbon tetrachloride of heat 3 times, each 10 minutes, in the acetone of heat 3 times, each 10 minutes, absolute ethyl alcohol cleaned, and deionized water rinsing is clean, and nitrogen dries up.
17) spun gold lead-in wire and electrode 5 bondings
Utilize conductive silver glue with spun gold lead-in wire and electrode 5 bondings, placed 120 ℃ of baking ovens 15 minutes, conductive silver glue is solidified.
18) Dewar packaging and testing
With the chip Dewar bottle of packing into, the spun gold lead-in wire on the electrode 5 is welded on the pin of Dewar bottle with indium, and mechanical pump vacuumized 2 hours, poured into liquid nitrogen, test chip performance under cryogenic conditions.
Above-described only is preferred implementation of the present invention; Should be pointed out that for the heavy those of ordinary skill in present technique field, under the prerequisite that does not break away from core technology characteristic of the present invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.

Claims (7)

1. In 2O 3/ PbTe heterojunction mid-infrared light volt type detector is characterized in that: as substrate (1), go up growth p-type PbTe monocrystal thin films (2) in substrate (1) with CdZnTe, go up growth n-type In at PbTe monocrystal thin films (2) 2O 3Polycrystal film (3) forms heterojunction, also comprises insulating protective layer (4), electrode (5).
2. In according to claim 1 2O 3/ PbTe heterojunction mid-infrared light volt type detector is characterized in that, uses ZnS as insulating protective layer (4).
3. In according to claim 1 2O 3/ PbTe heterojunction mid-infrared light volt type detector is characterized in that described electrode (5) is In membrane electrode (5).
4. In according to claim 1 2O 3/ PbTe heterojunction mid-infrared light volt type detector is characterized in that, also comprises the spun gold lead-in wire, utilizes conductive silver glue with spun gold lead-in wire and electrode (5) bonding.
5. In 2O 3The preparation method of/PbTe heterojunction mid-infrared light volt type detector; It is characterized in that; Be in CdZnTe substrate (1), utilize molecular beam epitaxy (MBE) the method undoped p-type PbTe monocrystal thin films (2) of growing, utilize magnetically controlled sputter method to go up growth n-type In2O3 polycrystal film (3) and form heterojunction at PbTe monocrystal thin films (2); Adopt vacuum deposition method vapor deposition ZnS as insulating protective layer (4), adopt vacuum deposition method vapor deposition In film to do electrode (5).
6. the described In of claim 5 2O 3The preparation method of/PbTe heterojunction mid-infrared light volt type detector, step of preparation process is following:
1) CdZnTe substrate (1) is prepared;
2) MBE growth PbTe monocrystal thin films (2);
3) magnetron sputtering growth In 2O 3Polycrystal film (3);
4) epitaxial wafer cleans;
5) photoetching table top;
6) ICP dry etching table top;
7) vapor deposition ZnS film;
8) photoetching graph window;
9) ZnS wet etching;
10) photoetching electrode (5) window;
11) vapor deposition In electrode (5);
12) peel off;
13) photoetching adds thick electrode (6) window;
14) vapor deposition adds thick electrode (6);
15) peel off;
16) thinning back side;
17) spun gold lead-in wire and electrode (5) bonding;
18) Dewar packaging and testing.
7. In according to claim 6 2O 3The preparation method of/PbTe heterojunction mid-infrared light volt type detector is characterized in that: use ICP dry etch process etching In 2O 3Form table top, etching gas is selected Cl for use 2/ H 2/ CH 4=7: 10: 8,20 ℃ of temperature, pressure 3.5mTorr, RE power 200W, ICP power 300W.
CN2010102280564A 2010-07-16 2010-07-16 Infrared photovoltage detector in In203/PbTe heterojunction and preparation method thereof Expired - Fee Related CN101924160B (en)

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CN106935513B (en) * 2017-02-26 2019-08-13 桂林理工大学 A kind of preparation method of Te/PbTe hetero-junctions nano thin-film

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CN101478007A (en) * 2009-01-22 2009-07-08 浙江大学 Infrared detector in PbTe semi-conductor photoconduction and manufacturing process thereof

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