CN1649104A - Surface inactivating method for antimonite and its device - Google Patents
Surface inactivating method for antimonite and its device Download PDFInfo
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- CN1649104A CN1649104A CNA2004100932498A CN200410093249A CN1649104A CN 1649104 A CN1649104 A CN 1649104A CN A2004100932498 A CNA2004100932498 A CN A2004100932498A CN 200410093249 A CN200410093249 A CN 200410093249A CN 1649104 A CN1649104 A CN 1649104A
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Abstract
This invention relates to a surface sulfur passivation method for a new antimonide and its devices including surface preprocess before the passivation and the method which overcomes the rough surface formed by conventional surface erosion and gets a dense flat smooth surface and interface shape to guarantee successive rate and control of technology and effectively increases the response degree and detection rate of detectors. The invented antimonide neutral ammonium sulfide passivation technology has better passivation result than the traditional basic one.
Description
Technical field
The present invention relates to a kind of novel antimonide and the surface passivation method of device thereof, comprise surface preparation and surperficial sulfur passivation method or rather, belong to semi-conducting material and device technology field.
Background technology
The surface smoothness of semi-conducting material is the basis of follow-up extension and device technology.The humidifying chemical corrosion of base what oxidation dissolution mechanism is the critical process of preparation semiconductor device, often find the process repeatability difference after III-V Zu Antimonyization He Wu Longitude wet processing is handled and influence device performance, fail always for a long time to understand that the appearance of these experimental results increases, thereby cause the reverse characteristic of detector soft partially, and influence its photoelectric response characteristic.III-V family semi-conducting material generally has surface propertys such as recombination-rate surface height, surperficial Fermi surface pinning, become one of key factor that hinders the device development, this problem is to low-gap semiconductor material and the device bigger particularly cause of influence and the approach certainly that is situated between, therefore, become the long-term difficult problem that is not situated between and determines of III-V Antimonyization thing.
Photodetector surfaces exists high surface density of states and recombination-rate surface can cause the dark current and parasitic electric the giving prominence to serious of device.For in the semi-conducting material of low energy gap such as infrared antimonide, surface recombination is particularly outstanding and serious to the influence of device performance.Recent decades, people sought various passivating methods always, to reduce the III-V family semiconductor material surface density of states, removed surperficial pinning.Sandroff[C.J.Sandroff.R.N.Nottenburg in 1987, J.C.Bischoff, and R.Bhat, Appl.Phys.Lett.51., 33-35 (1987). " Dramatic enchancement in the gain of a GaAs/AlGaAsheterostructure bipolar transistor by surface chemical passivation " ,] the discovery Na of research group
2S9H
2After the O aqueous solution is handled the few district of high-speed electronic components AlGaAs/GaAs heterojunction bipolar transistor (HBT) base periphery, current gain has had great improvement, almost reach near Utopian current transfer, illustrate the recombination-rate surface of the GaAs that handles through sulfur passivation greatly reduce, the recombination-rate surface that photoluminescence spectrum (PL spectrum) and electrical property directly record has also confirmed this point.Subsequently, the sulfide passivation technology just becomes the focus of III-V semiconductor surface passivation research.[N.Yokoi, H.Andoh el al, Appl.Phys.Lett.64.2578 (1994). " Surface structure of (NH
4)
2S
x-treatedGaAs (100) in an atomic resolution ", Z.L.Yuan et al, Appl.Phys.Lett.71 (21), 3081 (1997). " Investigation of neutralized (NH
4)
2S solution passivation of GaAs (100) surface "; X.Y.Hou; W.Z.Cai; X.Wang et al.; Appl.Phys.Lett.60.2252 (1992). " Electrochemical surfur passivation of GaAs " ,] but mainly concentrate on GaAs sill and high-speed electronic components.Result of study shows that sulfur passivation can make the material electric property that improvement is largely arranged.
Well-known 2-5 μ m middle-infrared band is very important atmospheric window, the fingerprint characteristic spectral line of many gas molecules all drops on middle-infrared band, and the laser and the detector that work in this wave band have important application in atmosphere environment supervision, medical diagnosis and fields such as drug identification and anti-terrorism.And the GaSb sill is the preferred material of 2-3 μ m middle-infrared band photoelectric device, but compare with GaAs sill and high speed device, for in the semi-conducting material of low energy gap such as infrared antimonide, surface recombination is bigger to the influence of device performance, photodetector surfaces with its preparation exists high surface density of states and recombination-rate surface to cause that the dark current of device and parasitic capacitance increase, thereby cause the reverse characteristic of detector poor, and influence the very important photoelectric response characteristic of detector.Therefore, the research and the difficulty certainly that is situated between are very big, and documents and materials that can be for reference and basic parameter are also few.
Just since the importance of middle-infrared band photoelectric material and device and in low-gap semiconductor material and the existing surface of device such as infrared antimonide, the interface poor flatness, recombination rate and surface density of states height, photooxidation is strong, being situated between, certainly difficulty is big, about the surface treatment and the surface passivation of low-gap semiconductor material and device are reported few, just lacking from physical chemical mechanism theoretical and that experiment two aspects combine and carrying out deep research and analysis by what, therefore lack one clearly physical vision go to instruct the development of III-V family antimonide process for treating surface and passivating technique, be the long-term outstanding and unsolved crucial difficult problem of coming.For this reason, develop and a kind ofly improve the effective surface treatment method and the high efficiency passivating technique of III-V Zu Antimonyization thing semi-conducting material and device performance and reliability with what, understand fully cosmetic issue that wet processing brings and passivating process physical chemistry mechanism, find the approach of solution to become the task of top priority.
Summary of the invention
The object of the present invention is to provide a kind of surface passivation method that is used for antimonide and device thereof, comprise surface preparation and sulfur passivation method, method provided by the invention can be repeatably, stable wet corrosion technique and device technology provides smooth smooth surface, be a kind of reverse dark current of the GaInAsSb of reduction PIN detector, improving photoelectric properties provides effective De Bluntization method.Surface preparation provided by the invention and surface passivation method comprise three parts, i.e. the process for surface preparation of oxygen-free agent solution, the passivating method of neutral sulfuration ammonia solution and the physical and chemical process of antimonide sulfur passivation.
At first, the solution composition of describing the employed surface preparation of surface preparation is that potassium sodium tartrate solution concentration is the 0.4Mol/ liter, and concentration of hydrochloric acid solution is the 3.2Mol/ liter, and potassium sodium tartrate solution and hydrochloric acid solution were mixed in 1: 1 by volume.
Process for surface preparation is before the Antimonyization thing contains the solution wet etching of oxidant, slice, thin piece is immersed in the mixed solution of above-mentioned sodium potassium tartrate tetrahydrate and hydrochloric acid 4-8 minute, uses deionized water rinsing after the taking-up immediately, and high pure nitrogen dries up.Then, carrying out follow-up wet corrosion technique processing or other device technology immediately handles.Fig. 1 is that wet corrosion technique adopts before and after the surface preparation optimisation technique of the present invention, the surface and interface pattern comparison diagram of GaSb corrosion.Left figure is corrosion surface, the interface topography that does not adopt the surface preparation optimisation technique preceding, and right figure is corrosion surface, the interface topography that adopts after optimisation technique is managed on the present invention surface in advance.As can be seen, after adopting surface preparation optimisation technique of the present invention, the erosion profile of GaSb be much improved (seeing embodiment 1 and Fig. 1 for details).
Being configured to of the passivating solution that the passivation of described sulfuration ammonia is to use:
Alkaline solution: analyze the bright sulfur ammonia solution and mixed PH=9.5-11.5 in 1: 4 by volume with deionized water.
Neutral solution: in the solution after above-mentioned dilution, splashing into the hydrochloric acid of dilution 50%, and count the variation of monitoring pH value with PH, is 7 up to pH value.
To immerse behind deionized water rinsing in two kinds of passivating solutions that configure through antimonide after the surface preparation or its device InGaAsSb PIN detector and carry out Passivation Treatment, in the passivating process, the temperature of solution is held in 60 ℃ with the water-bath Faville.Utilize the 4145B semiconductor parameter instrument of Hewlett-Packard to test the I-V characteristic of detectors before and after the passivation, (see embodiment 2 for details) as shown in Figure 2.
The result shows, through (NH
4)
2After the S Passivation Treatment, the I-V of detector improves, and dark current reduces greatly, and neutral solution has obtained than the better effect of alkaline solution.In reverse biased be-during 1V, the dark current of untreated device is 7.3mA, after handling through alkaline solution, dark current drops to 4.7mA, and after handling through neutral solution, dark current is further reduced to 2.1mA.
Fig. 3 is the R of detector
0The relation of the A factor and passivation time, temperature are 60 ℃.R
0A is the resistance under the zero-bias and the product of detector photosensitive area, is the key parameter of decision detector quality.As can be seen from the figure, passivating process needs the long time to reach stable, and sulfur passivation reached optimum efficiency greatly after 60 minutes, for alkaline solution, and after transpassivation, the R of detector
0The A factor has improved 35 times, and after handling through neutral solution, R
0The A factor has improved about 60 times and (has seen embodiment 3 and Fig. 3 for details).
The I-V test result shows, neutral (NH
4)
2The S passivating dip can effectively reduce detector dark current, improves R
0The A factor is suitable for photoelectric properties such as responsiveness and the detectivity (seeing embodiment 3 tables 1 for details) of improving detector.
In order further to understand (NH
4)
2The passivation mechanisms of S is development sulfur passivation solution and the core that improves passivation effect, the invention provides X-ray electron Spectrum (XPS) test of the detector after the passivation, is intended to verify at passivating process (NH
4)
2Each component I n, Ga of the InGaAsSb of S atom and detector surface, Sb, As atomic bonding situation among the S.In the test, light source adopts AlK
aLine, the test spectrum adopts the calibration of C1s peak, and the position is 284.6eV.Test has obtained the spectral line of relevant Ga, Sb, In atom, because the content of As is lower, weak output signal does not obtain desirable curve.
Fig. 4 is measured Ga 3d xps energy spectrum figure.Curve is analyzed, after match, can be obtained 3 peak values.The corresponding Ga-As key in the peak of energy minimum, the corresponding Ga-Sb key in middle peak, the corresponding Ga-S key in the match peak of the right energy maximum.For Ga-As key and Ga-Sb key, energy position is 17.5eV and 18.8eV respectively.The peak position of the Ga-S key correspondence after the alkaline passivation solution-treated is 19.6eV, and the peak position of the Ga-S key correspondence after neutral passivating dip is handled is 20.1eV.Like this, corresponding to GaSb, the chemical shift of the Ga-S key that alkalescence and neutral solution are constituted after handling is respectively 0.8eV and 1.3eV, and neutral (NH is described
4)
2After the S passivation, S and Ga have constituted stronger chemical bond.
Fig. 5 is In 3d
5/2Xps energy spectrum figure.Obtain 3 peak values after curve analyzed.The corresponding In-As key in the peak of energy minimum, the corresponding In-Sb key in middle peak, the corresponding In-S key in the match peak of the right energy maximum.For In-As key and In-Sb key, energy position is 443.7eV and 444.2eV respectively.For the In-S key, same, through after the Passivation Treatment, neutral passivating dip has constituted stronger In-S key than alkaline solution, and its chemical shift is respectively 1.1eV and 0.3eV.
Fig. 6 is the Sb 3d and the XPS spectrum line at the very approaching O1s peak of energy position with it, and the ratio of the relative intensity by contrasting these 2 peaks changes, and can learn the effect that has situation and passivation of passivation rear surface oxide.The ratio at the Sb/O peak before the passivation is 0.65.Sb/O p-ratio through the alkaline passivation solution-treated becomes 0.86, and the Sb/O p-ratio after handling through neutral passivating dip is 1.21.The result shows, (NH
4)
2S can effectively remove the oxide layer on InGaAsSb surface, and after the neutral solution passivation, the S atom on surface has higher kurtosis, means more suspended chain by saturated, and surface state further reduces.
XPS tests and the analysis showed that (NH
4)
2S can remove the oxide layer of detector surface, and S replaces O, saturated dangling bonds, and become key with In with Ga.All show neutral (NH from the analysis of device detection and XPS
4)
2S solution is to the processing of InGaAsSb PIN detector, than traditional alkalescence (NH
4)
2S solution has been obtained better effect.
More than the Chemical Physics Processing mechanism of the passivation that proposes by the present invention of this result provided very and explained clearly, the surface preparation technology of the above-mentioned oxygen-free agent with the what antimonide of the present invention and vulcanize the rarely seen report of physical and chemical process of ammonia passivating technique and antimonide sulfur passivation with the neutrality of what InGaAsSb detector.The technology of the present invention has following characteristics: first, the surface preparation solution of oxygen-free agent has the good surface oxide layer of formation naturally of removing earlier, and do not introduce oxidation mechanism this moment, carry out follow-up wet etching that contains oxidant and device technology on this basis, the direct usefulness of having determined of being situated between effectively contains coarse, the nonlinear two large problems of the not gentle corrosion rate in interface of the surface topography that wet etching brought of oxidant.The second, provided clearly directly with coarse, the nonlinear Chemical Physics mechanism of the not gentle corrosion rate in interface of the surface topography that wet etching brought that contains oxidant.Be situated between and released result of the present invention.The 3rd, have good characteristic electron passivation, promptly the neutral solution passivating technique greatly reduces surface density of states and the recombination-rate surface of InGaAsSb.The 4th, provided the Chemical Physics mechanism of sulfur passivation process clearly, be situated between and released result of the present invention.The 4th, the InGaAsSb detector surface is through neutral (NH
4)
2After the S solution Passivation Treatment, the dark current of InGaAsSb PIN detector is reduced greatly, detectivity and responsiveness improve greatly and improve.Peak detection rate D
* λ pBy 4.8 * 10 before the passivation
9CmHz
1/2/ W brings up to 1.2 * 10 after the passivation
10CmHz
1/2/ W, responsiveness R
Bb *Bring up to 256V/W after the passivation by the 37V/W before the passivation.The 5th, provided the Chemical Physics mechanism of sulfur passivation process clearly, be situated between and released result of the present invention.
Description of drawings
Fig. 1 wet corrosion technique adopts before and after the surface preparation optimisation technique of the present invention, the surface and interface pattern contrast of GaSb corrosion.Corrosion depth: 0.7 μ m (amplifying 1000 times).
(a) adopt conventional surface preprocess method (b) to adopt process for surface preparation provided by the invention
I-V characteristic before and after the passivation of Fig. 2 InGaAsSb detector
(1): before the passivation (2): alkaline solution is handled (3): neutral solution is handled
The R of Fig. 3 InGaAsSb detector
0The relation of the A factor and passivation time
1: neutral solution handles 2: alkaline solution is handled
The xps energy spectrum figure of Fig. 4 Ga 3d: (a) alkaline solution, (b) neutral solution
Fig. 5 In 3d
5/2Xps energy spectrum figure: (a) alkaline solution, (b) neutral solution
The xps energy spectrum figure at Fig. 6 Sb 3d and O1s peak: (a) alkaline solution, (b) neutral solution
Fig. 4 to Fig. 6 abscissa is binding energy (ev), and ordinate is relative intensity (c/s).
Embodiment
Further specifying substantive distinguishing features of the present invention and advance below by chart in the literary composition and embodiment, but limit the present invention absolutely not, also is that the present invention is confined to embodiment absolutely not.
Embodiment 1: the antimonide surface preparation
Implementation step:
(1) potassium sodium tartrate solution concentration is 0.4Mol/L,
(2) concentration of hydrochloric acid solution is 3.2Mol/L.
(3) above-mentioned potassium sodium tartrate solution and hydrochloric acid solution were mixed in 1: 1 by volume.
(before 4) Zai Antimonyization things contain the solution wet etching of oxidant, slice, thin piece is immersed in several minutes (sodium potassium tartrate tetrahydrate 0.4Mol/L: hydrochloric acid 3.2Mol/L=1: 1) in the mixed solution of sodium potassium tartrate tetrahydrate and hydrochloric acid, take out and use deionized water rinsing fast, high pure nitrogen dries up.Carrying out follow-up wet corrosion technique processing or other device technology immediately handles.
The GaSb material is handled through implementation step (1)-(4), and Fig. 1 is that wet corrosion technique adopts before and after the surface preparation optimisation technique of the present invention, the surface and interface pattern comparison diagram of GaSb corrosion.Left figure is corrosion surface, the interface topography that does not adopt the surface preparation optimisation technique preceding, and right figure is corrosion surface, the interface topography that adopts after optimisation technique is managed on the present invention surface in advance.As can be seen, after adopting surface preparation optimisation technique of the present invention, the erosion profile of GaSb is much improved.
The sulfur passivation of embodiment 2:GaInAsSb PIN detector
Implementation step:
The detector flow
Scribing, cleavage
Press sonde method to survey device I-V properties, the photoelectric properties of test component.
The configuration of passivating solution: analyze the bright sulfur ammonia solution and mixes at 1: 4, in the solution after above-mentioned dilution, splash into 50% hydrochloric acid after the dilution, count with PH that to monitor pH value be 7 with deionized water.
To soak about 10s in the sodium potassium tartrate tetrahydrate/hcl corrosion liquid of device after 40 times of dilutions.
Take out device, immerse in the passivating solution that configures behind deionized water rinsing, the temperature of solution is held in 60 ℃ with the water-bath Faville, and passivation time was controlled at 40 minutes to 1 hour.
Device after the taking-up passivation, the I-V characteristic and the photoelectric properties of device after the test comparison passivation.
InGaAsSb PIN structural material utilizes the 4145B semiconductor parameter instrument of Hewlett-Packard to test the I-V characteristic of detectors before and after the passivation, as shown in Figure 2 after the rapid 1-7 of embodiment 1 handles.The result shows, through (NH
4)
2After the S Passivation Treatment, the I-V of detector improves, and dark current reduces greatly, and neutral solution has obtained than the better effect of alkaline solution.In reverse biased be-during 1V, the dark current of untreated device is 7.3mA, after handling through alkaline solution, dark current is reduced to 4.7mA, and after handling through neutral solution, dark current is further reduced to 2.1mA.
Embodiment 3:
InGaAsSb PIN structural material is through embodiment 2 described step 1-7, handles Fig. 3 and is through the neutral solution Passivation Treatment with through the R of the InGaAsSb of alkaline solution Passivation Treatment detector
0The relation of the A factor and passivation time is carried out the responsiveness and the detectivity test of detector then to this sample.Example is in table 1 as a result.
| Peak detection rate D * λp(cmHz 1/2/W) | Responsiveness is R bb *(V/W) | |
| Before the passivation | 4.2×10 9 | ?37 |
| After the alkaline solution passivation | 8.7×10 9 | ?191 |
| After the neutral solution passivation | 1.2×10 10 | ?256 |
Table 1 test result shows that the photoelectric properties of detector are improved after passivation, and neutral solution has obtained better effect.The I-V test result shows, neutral (NH
4)
2The S passivating dip can effectively reduce detector dark current, improves R
0The A factor is suitable for photoelectric properties such as responsiveness and the detectivity of improving detector.
Claims (7)
1, the surface passivation method of antimonide and device thereof is characterized in that it comprises two technical processs of passivation of surface preparation and sulfuration ammonia solution.
2, press the surface passivation method of described antimonide of claim 1 and device thereof, the solution composition that it is characterized in that described surface preparation is that the volume ratio of potassium sodium tartrate solution and hydrochloric acid solution is 1: 1, potassium sodium tartrate solution concentration is the 0.4mol/ liter, and concentration of hydrochloric acid solution is the 3.2mol/ liter; Processing method is that antimonide is immersed in the mixed solution 4-8 minute, takes out the back and dries up with deionized water rinsing, high purity nitrogen.
3,, it is characterized in that described sulfuration ammonia solution passivating dip or be alkaline solution, or be neutral solution by the surface passivation method of described antimonide of claim 1 and device thereof; Alkaline solution PH=9.5-11.5, it is that the sulfuration ammonia solution mixes by 1: 4 volume ratio with deionized water; Neutral solution PH=7, it is in described alkaline solution, splashes into that the hydrochloric acid of concentration diluted acid 50% generates; Passivation Treatment is that the antimonide detector after surface preparation immerses in the passivating dip, and temperature maintenance is at 60 ℃.
4,, it is characterized in that employed sulfuration ammonia is pure for analyzing by the surface passivation method of described antimonide of claim 3 and device thereof.
5, by the surface passivation method of described antimonide of claim 3 and device thereof, the temperature of passivating dip is held with the water-bath Faville when it is characterized in that passivation.
6, by the surface passivation method of claim 1,2 or 3 described antimonides and device thereof, it is characterized in that the dark current of S and InGaAsSb PIN detector is reduced to 2.1mA after the neutral passivating dip passivation, the peak detection rate brings up to 1.2 * 10
10CmHZ
1/2/ W, responsiveness is brought up to 256/W.
7, by the surface passivation method of claim 1,2 or 3 described antimonides and device thereof, it is characterized in that neutrality (NH
4) sulphur replaces oxygen after the S passivation, sulphur and gallium, sulphur and indium have constituted stronger chemical bond.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103578957A (en) * | 2013-11-01 | 2014-02-12 | 清华大学 | Substrate surface passivating method and semiconductor structure forming method |
| CN104143760A (en) * | 2013-05-10 | 2014-11-12 | 长春理工大学 | Surface passivation method used when InP-based semiconductor laser unit is prepared through ALD |
| CN105070655A (en) * | 2015-07-15 | 2015-11-18 | 中国电子科技集团公司第四十六研究所 | Method for passivating gallium antimonide wafer |
| CN106057663A (en) * | 2016-06-29 | 2016-10-26 | 北京华进创威电子有限公司 | Method for chemical passivation of surface of GaSb single crystal substrate |
| CN106784149A (en) * | 2016-12-28 | 2017-05-31 | 中国电子科技集团公司第十八研究所 | A kind of passivating method of III V II-VI group solar cell |
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2004
- 2004-12-17 CN CNA2004100932498A patent/CN1649104A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104143760A (en) * | 2013-05-10 | 2014-11-12 | 长春理工大学 | Surface passivation method used when InP-based semiconductor laser unit is prepared through ALD |
| CN103578957A (en) * | 2013-11-01 | 2014-02-12 | 清华大学 | Substrate surface passivating method and semiconductor structure forming method |
| CN105070655A (en) * | 2015-07-15 | 2015-11-18 | 中国电子科技集团公司第四十六研究所 | Method for passivating gallium antimonide wafer |
| CN106057663A (en) * | 2016-06-29 | 2016-10-26 | 北京华进创威电子有限公司 | Method for chemical passivation of surface of GaSb single crystal substrate |
| CN106784149A (en) * | 2016-12-28 | 2017-05-31 | 中国电子科技集团公司第十八研究所 | A kind of passivating method of III V II-VI group solar cell |
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