CN1133761C - Open pipe tellurium cadmium mercury epitaxial material heat treatment method - Google Patents

Open pipe tellurium cadmium mercury epitaxial material heat treatment method Download PDF

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CN1133761C
CN1133761C CNB011319240A CN01131924A CN1133761C CN 1133761 C CN1133761 C CN 1133761C CN B011319240 A CNB011319240 A CN B011319240A CN 01131924 A CN01131924 A CN 01131924A CN 1133761 C CN1133761 C CN 1133761C
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hgte
graphite
heat
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CN1354287A (en
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杨建荣
陈新强
黄根生
何力
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Shanghai Institute of Technical Physics of CAS
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Abstract

The present invention discloses an open pipe tellurium-mercury source heat treatment method for tellurium-cadmium-mercury epitaxial materials. A stable mercury vapor pressure needed by heat treatment is provided by using the structure of a graphite box, the graphite box can be realized by improving a rheotaxial graphite boat, and an open pipe process provides an approach for the bulk production of materials. The successful rate of hole conduction type heat treatment which is carried out by using the process can reach 100%, the hole concentration under the temperature of 77K can be freely controlled within the range of 5*10<15> to 5*10<16>cm<-3>, and meanwhile the dislocation on material surfaces in the heat treatment process does not generate value adding effects; additionally, ingredients of materials and integrity of surface topography are also well kept.

Description

Open pipe tellurium cadmium mercury epitaxial material heat treatment method
Technical field
The present invention relates to monocrystalline or have the post-processing technology of the even polycrystalline compounds material of a fixed structure, especially for the open pipe tellurium cadmium mercury epitaxial material P type heat treating method of making extensive focal plane array detector.
Background technology
Hg-Cd-Te material P type heat treatment technics has very long history, through to the research of Hg-Cd-Te material solid and gas phasor, it is found that the mercury vacancy concentration of material and thermal treatment temp and mercury are pressed with the pass, and from experimentally having confirmed the corresponding relation between them.Being used for Te-Cd-Hg body material hot treatment technology the earliest is that mercury source and sample are split at two of the quartz ampoule of vacuum sealing, controls the temperature of mercury source and sample respectively by process furnace, and keeps time enough and reach thermal equilibrium by the mercury room in the material.As H.R.Vydyanath at J.Electrochem., Soc., in 128 (1981) 2609 to Hg 0.8Cd 0.2Comparatively comprehensively research has been done in the thermal treatment of Te body material P type, and R.Vydyanath also uses Hg source heat treatment technics (200～300 ℃) under lower temperature to obtain the tellurium cadmium mercury epitaxial material of low acceptor concentration in J.Appl.Phys.65 (8) (1989) 3080.
Along with the development of epitaxy technology, thin-film material has obtained application more and more widely.Be to obtain big area component uniform HgCdTe thin-film material, people's researchdevelopment liquid phase epitaxial technique (LPE), molecular beam epitaxy technique (MBE) and deposition of metal organic epitaxy technology (MOCVD).But these three kinds of technology all can not directly provide device needed 5～50 * 10 15Cm -3Tellurium cadmium mercury epitaxial material, epitaxial material all need to adjust to the required electrical parameter of focal plane device through Overheating Treatment.
Yet, traditional Hg source heat treatment technics applies to the epitaxial material processing two weak points, the one, this technology is very big to the influence of extension material surface, this causes heat treated success ratio lower, the 2nd, it is very difficult that the heat treatment technics of employing quartz ampoule is heat-treated the large size epitaxial material, and, along with the increase of size, heat treated cost sharply increases, and can't satisfy the demand of preparation tellurium cadmium mercury epitaxial material in enormous quantities.For this reason, in recent years, developed the multiple heat treating method that is exclusively used in epitaxial material again, the P type thermal treatment process of vacuum heat treatment has been proposed to carry out with ZnS or CdTe tectum at the LPE material as the LETI of France, as G.L.DESTEFANIS, J.Crystal Growth, 86,700 (1988), this method and production technology thereof patent " Intrinsic P-type HgCdTe using CdTe capping layer " (US6114738) and patent " Method of producing intrinsic P-type HgCdTe using CdTe cappinglayer " (US6030853).The vacuum heat treatment process of molecular beam epitaxial TeCdHg material that patent " vacuum heat treatment process of molecular beam epitaxial TeCdHg material " (ZL98 1 11054.1) provides a kind of sample surfaces not stain.These heat treating methods all can make the hole of material get a desired effect effectively.But, further discover, there is certain lattice mismatch between the ZnS that uses in this heat treating method or CdTe tectum and the Hg-Cd-Te material, mismatch on this lattice can produce misfit dislocation on the surface of epitaxial material in heat treatment process, and the generation of dislocation will cause the degeneration of PN junction performance.Patent " hole conduction tellurium-cadimium-mercury epitaxy material heat treatment process and device " (ZL96 1 16340.2) also provides a kind of method of utilizing quartz ampoule P type low-temperature heat treatment, this method can access P-type material, but shortcoming is to use the heat treatment technics of stopped pipe type, can't heat-treat large size and material in enormous quantities, in addition, the carrier concentration of the P-type material of this method acquisition has bigger discreteness.
Summary of the invention
Problem according to above-mentioned prior art existence, the present invention proposes a kind ofly can be applied in batches P type heat-treating methods of big area tellurium cadmium mercury epitaxial material, this method can obtain the certain P type tellurium cadmium mercury epitaxial material of concentration effectively, does not produce dislocation simultaneously in heat treatment process again.The technical scheme of this method is:
A. tellurium cadmium mercury epitaxial material that epitaxy technique is obtained and heat treatment source HgTe powder are placed on respectively in the material cavity and powder cavity in the graphite box body, these two cavitys communicate by a groove, with the graphite lid two cavitys, a groove are covered then, the graphite box is placed in the silica tube in the open pipe formula heat treatment system, under the mobile rare gas element, as hydrogen, nitrogen or argon gas, heat-treat at a certain temperature.
Said graphite box also comprises with pushing away sets up the graphite boat of placing HgTe powder cavity on the graphite boat that uses in the boat rheotaxy, like this behind mercury cadmium telluride rheotaxial material growth ending, need not material is taken out, only needing that HgTe powder cavity is added the HgTe powder can heat-treat, and the HgTe powder both can add before the material growth, also can behind the material growth ending, add, difference only is that both are under identical heat-treat condition, the hole of the material that obtains is different, its reason is in the rheotaxy process, and the HgTe powder exists certain Hg to leak.
B. thermal treatment temp is in 210 ℃ to 290 ℃ scopes, makes that the hole of tellurium cadmium mercury epitaxial material under the 77K temperature is corresponding to be adjusted at 5 * 10 15To 5 * 10 16Cm -3Between.
Tellurium cadmium mercury epitaxial material through the aforesaid method processing, the result shows the heat treated success ratio 100% of P type, statistics to the part test result shows, the standard deviation of P type electrical parameter value is less than 30%, and the P type carrier concentration of epitaxial material can be controlled in 5 * 10 with the hole concentration under the tellurium cadmium mercury epitaxial material 77K temperature by changing thermal treatment temp 15To 5 * 10 16Cm -3, this electric property index is suitable for the application of N-on-P structure HgCdTe infrared focal plane device.With the dislocation corrosion agent testing identity of Hg-Cd-Te material, there is not stress dislocation in the epitaxial material surface.
The present invention is the open pipe formula, that is, silica tube is tightly connected by nitrile rubber " O " type circle and vacuum system, and realizes HgTe source Hg-Cd-Te material thermal treatment under the mobile rare gas element.Its principle of work is with stopped pipe type, that is, the mercury source Effect of annealing of silica tube vacuum sealing is similar, all be the concentration of adjusting the mercury room, but the mode that realizes is different.The annealing of mercury source is the dividing potential drop by control mercury, and adjust the mercury atom in the Hg-Cd-Te material and the partial potential of reference point defective by the exchange of mercury atom between gas phase and the solid phase and diffusion, thereby reach the purpose of adjusting mercury vacancy concentration in the material, in this process, mercury is pressed by control mercury source temperature and is realized, is the balance mercury vapour pressure under this temperature.And the mercury vapour pressure in the open pipe formula HgTe source Hg-Cd-Te material thermal treatment is evaporated by the HgTe powder and is provided, in addition, what also there is a spot of leakage in slit between graphite box body and the graphite cover plate, mercury vapour pressure around the actual sample will be determined by the amount of HgTe powder and the size of leakage, by control to the amount of HgTe powder source, mercury vapour pressure under certain thermal treatment temp is constant basically, and experimental result has confirmed this point.The HgTe powder source that adopts of the present invention in addition, for Hg-Cd-Te material provides certain tellurium vapour pressure, the existence of tellurium vapour pressure has prevented the evaporation of Hg-Cd-Te material surface tellurium atom, this is useful to the surface integrity that keeps material, material surface quality after this art breading is without any variation, and after heat treatment material does not change by parameters such as wavelength yet.
Beneficial effect of the present invention has been to provide the heat treating method of the tellurium cadmium mercury epitaxial material that is not subjected to the sample surfaces contamination, after with this method tellurium cadmium mercury epitaxial material being heat-treated, the electrical parameter of material produces a desired effect, and the success ratio of obtaining P-type material reaches 100%; This technology can also keep the surface integrity of material and good surface topography, and after heat treatment the composition parameter of material does not change yet; The spatially uniform of material electrical parameter can satisfy the requirement of device reliability, owing to adopt the heat treated mode of open pipe formula, the present invention can satisfy the material requirement of mass production.
Description of drawings
Fig. 1 is the synoptic diagram of graphite box structure in the embodiment of the invention 1, and a is a longitudinal sectional drawing, and b is a transverse cross-sectional view;
Fig. 2 is for having the structural representation of the rheotaxy graphite boat of placing HgTe powder cavity in the embodiment of the invention 2;
Fig. 3 is the structural representation of tellurium cadmium mercury epitaxial material thermal treatment unit among the present invention;
Fig. 4 is the relation curve of Hg-Cd-Te material mercury vacancy concentration among the present invention and thermal treatment temp T;
Fig. 5 is the longitudinal uniformity figure of the Te-Cd-Hg P-type material electrical property of the present invention's acquisition;
Fig. 6 is the situation of material surface dislocation before and after the P type thermal treatment of the present invention, (a) be the pattern photo of Hg-Cd-Te material thermal treatment front surface dislocation etch pit, (b) be the pattern photo of Hg-Cd-Te material, (c) adopt the pattern photo of CdTe tectum vacuum heat treatment rear surface dislocation etch pit for Hg-Cd-Te material through thermal treatment of the present invention rear surface dislocation etch pit.
Embodiment
Embodiment 1
1) making of graphite box
The present invention has utilized current graphite material to have high-purity, high-compactness and easy machining characteristics, and graphite box 1 is closed by graphite box body 101 and graphite and covers 102 and form, and structure as shown in Figure 1.In the graphite box body, have two cavitys, the centre has a groove 106 that two cavitys are communicated, a cavity is for placing epitaxial material cavity 104, its degree of depth is slightly larger than thickness of sample, another cavity is for placing HgTe powder cavity 105, its degree of depth is determined according to the amount of required placement HgTe powder, less than 1 micron polishing paper that these two mirror polish are bright at graphite box body and the contacted one side of graphite lid with granularity, can play sealing effectiveness preferably when it is in contact with one another, the size requirements of graphite lid can all cover groove of two cavitys.The graphite box that processes need follow these steps to clean before using:
A. chloroazotic acid is poured in the beaker, graphite member is put into chloroazotic acid, about heating chloroazotic acid to 50 ℃, soaks 30 minutes;
B. outwell chloroazotic acid, use the above washed with de-ionized water of 10M Ω 10 minutes;
C. continue in deionized water, to soak, change water every day sooner or later, change water 2 times at every turn, heat water to boiling point earlier after for the first time changing water, so repeat 5 days;
D. detect the pH value and the electric conductivity of water before graphite member takes out, when the pH value be 7 and conductivity values can take out graphite member when constant;
E. put into after the graphite member of Qu Chuing dries up in the nitrogen operation box stream hydrogen stove 600 ℃ the baking 8 hours stand-by.
2) heat treating method:
Thermal treatment process is divided following 6 steps:
(a) epitaxial material takes out in the nitrogen operation box, takes out the back and directly in the nitrogen operation box it is placed in the material cavity 104 in the graphite box, does not do any cleaning as far as possible, avoids the contamination to sample surfaces;
(b) polycrystalline or monocrystalline HgTe material are being processed into powder through in the agate powder millstone of purifying treatment, size is advisable less than 2mm, the amount of HgTe powder is got every square centimeter 1～2 gram by the epitaxial material area and is advisable, mercury vapour pressure when what of amount will be to thermal treatment is influential, the big young pathbreaker of mercury vapour pressure influences the concentration in mercury room in the epitaxial material, therefore, it is to guarantee that thermal treatment process forms the basis of the mercury vacancy concentration of constant basis in epitaxial material that the amount of HgTe powder is carried out strict control, in the present embodiment, the sample that we adopt is 3 * 2cm 2Liquid-phase epitaxial material, the amount of HgTe powder are 6.05 ± 0.05 grams;
(c) pour the HgTe powder into powder cavity 105 after, attention may be gone to the outer HgTe powder of cavity and remove clean, influence stopping property in order to avoid be clipped between graphite box body and the graphite lid, then, graphite lid 102 is covered tightly on the graphite box body with graphite screw 103;
(d) silica tube 2 is opened behind nitrogen, graphite box 1 is connected with system sealing after putting into silica tube again, sealing is by rotation stainless steel clamping nut 6 extruding stainless steel briquettings 7, by briquetting 7 extruding nitrile rubber O type circles 8, make and realize sealing between silica tube 2 and the stainless steel pipes 5, adopt mechanical pump that silica tube 2 is evacuated to 10 -1More than the Pa, pour the hydrogen of crossing through the palladium tube purifying then, flow is 100～500 milliliters of per minutes;
(e) heat treatment furnace 3 is heated to predefined temperature, behind the temperature-stable, the silica tube 2 that graphite box 1 is housed is put into heat treatment furnace, with the actual thermal treatment temp of thermopair 4 monitorings that places graphite box bottom, if any deviation, adjusted by changing desired temperature;
When (f) thermal treatment finishes silica tube is withdrawed from heat treatment furnace, in air, be cooled to room temperature.
Embodiment 2
Present embodiment is to utilize to improve to push away the heat treating method that the graphite boat that uses in the boat rheotaxy is implemented the present invention's proposition, the structure of graphite boat is seen Fig. 2,1-1 is the graphite boat body, 1-2 is the graphite boat cover plate, 1-3 is the graphite screw, and 1-4 is the epitaxial material cavity, and 1-5 is a HgTe powder cavity, 1-6 is a graphite slider, and 1-7 is a through hole.When the liquid-phase epitaxial material growth ending, the HgTe powder is joined among the powder cavity 1-5, perhaps before the epitaxial material growth, the HgTe powder is joined among the powder cavity 1-5, behind the epitaxial material growth ending, by pulling slide block 1-6 cavity 1-5 that places the HgTe powder and the cavity 1-4 that places epitaxial material are connected by through hole 1-7, epitaxial material need not take out and can connect graphite boat and heat-treat together like this, thereby has prevented the contamination of environment to epitaxial material to greatest extent.Its heat treating method is the same.Hg vapour pressure when the difference that the HgTe powder is put into and put into before extension after extension finishes only is both thermal treatments is different, and its reason is in the rheotaxy process, and the HgTe powder exists certain Hg to leak.
The heat-treat condition of embodiment 1,2:
Heat-treat condition needs according to Hg-Cd-Te material component and device the requirement of P-type material carrier concentration to be set, and general element manufacturing requires carrier concentration is controlled at 5 * 10 15Cm -3～5 * 10 16Cm -3, Fig. 4 provided component at thickness between 0.22～0.23 in long wave tellurium cadmium mercury epitaxial material P type carrier concentration between 10～15 microns and the mutual relationship between the thermal treatment temp.Heat treatment time choose relation such as table 1 with thermal treatment temp.
Table 1. thermal treatment temp and time relation
Thermal treatment temp (℃) 225 235 250 280
Heat treatment time (hour) 29 hours 16 hours 8 hours 6 hours
By adjusting heat treated temperature, the present invention can effectively control and adjust the carrier concentration of P-type material, and thermal treatment temp is controlled in 210 ℃ to the 290 ℃ scopes, and the hole concentration under the tellurium cadmium mercury epitaxial material 77K temperature can be controlled in 5 * 10 15To 5 * 10 16Cm -3, Fig. 5 is the experimental result of the relation of the thermal treatment temp of long wave tellurium cadmium mercury epitaxial material and P type carrier concentration, this controllability is crucial for selecting best device parameters.
Table 2 is medium short wave tellurium cadmium mercury epitaxial material material electrical parameter under the 77K temperature after thermal treatment under 250 ℃ of 8 hours conditions.Different with the source thermal treatment of pure mercury, the present invention is except obtaining suitable electrical parameter, owing to adopt the HgTe powder source, for Hg-Cd-Te material provides certain tellurium vapour pressure, the existence of tellurium vapour pressure has prevented the evaporation of Hg-Cd-Te material surface tellurium atom, this is useful to the surface integrity that keeps material, and the material surface quality after this art breading is without any variation, and after heat treatment material does not change by parameters such as wavelength yet.
Table 2. medium short wave tellurium cadmium mercury epitaxial material after thermal treatment under 250 ℃ of 8 hours conditions material at the electrical parameter of 77K temperature
Epitaxial material numbering material component thickness (μ m) is ear concentration (cm suddenly -3) Hall coefficient (cm 2/ Vs)
LPES82 0.326 12.9 1.2E16 357
LPES91 0.44 10.0 4.67E15 235
The repeatability of material electrical property and spatially uniform are to weigh material property whether to satisfy the basic index that element manufacturing requires, table 3 is the situation of same composition tellurium cadmium mercury epitaxial material material electrical property after 225 ℃ of thermal treatment in 29 hours, the thermal treatment process of using the present invention to provide is carried out the thermal treatment of P type, its parameter index is very approaching under the material component situation identical with heat-treat condition, and this shows that also material has goodish repeatability.The results are shown in Figure 5 by what some samples are carried out vertical distribution that surface chemistry corrosion stripping layer comes the experimental material electrical property, the distribution along the longitudinal of material electrical property also is uniformly, can satisfy the requirement of device reliability fully.
Fig. 6 is for carrying out the situation of P type thermal treatment front and back material surface dislocation with the present invention, the dislocation corrosion agent is a Schaake solution, and its chemical ingredients and proportioning are CrO 38mg: 20ml H 2O: 5ml HCl, etching condition be 20 ℃ 150 seconds, point is a misfit dislocation among the figure, be the dislocation of passing through a little louder from substrate, can see that value-added situation does not appear in the dislocation in the material of thermal treatment front and back, and the material surface after CdTe tectum vacuum heat treatment can produce a large amount of misfit dislocations.Manufactured experimently out 1024 * 1 LONG WAVE INFRARED focus planardetector with the P-type material that this technology obtains, and realized the imaging of staring the room temperature target.
The situation epitaxial material numbering material component thickness (μ m) of table 3. same composition tellurium cadmium mercury epitaxial material material electrical property after 225 ℃ of thermal treatment in 29 hours is ear concentration (cm suddenly -3) Hall coefficient (cm 2/ Vs)
283 0.226 20.0 8.76E15 701
286 0.228 13.8 7.76E15 677
288 0.227 12.9 7.64E15 719
289 0.227 12.2 7.76E15 708
298 0.226 15.0 8.22E15 740

Claims (2)

1. the heat treating method of an open pipe tellurium cadmium mercury epitaxial material is characterized in that:
A. tellurium cadmium mercury epitaxial material that epitaxy technique is obtained and heat treatment source HgTe powder are placed on having in the material cavity (104) and powder cavity (105) that a groove (106) communicates in the graphite box body (101) respectively, use graphite lid (102) that two cavitys, a groove are covered then, graphite box (1) is placed in the silica tube (2) in the open pipe formula heat treatment system, under the mobile rare gas element, as hydrogen, nitrogen or argon gas, heat-treat at a certain temperature;
Said graphite box also comprises pushing away sets up the graphite boat of placing HgTe powder cavity on the graphite boat that uses in the boat rheotaxy, like this behind mercury cadmium telluride rheotaxial material growth ending, need not material is taken out, only needing that HgTe powder cavity is added the HgTe powder can heat-treat, and the HgTe powder both can add before the material growth, also can add behind the material growth ending, difference only is both under identical heat-treat condition, and the hole of the material that obtains is different;
B. thermal treatment temp is in 210 ℃ to 290 ℃ scopes, makes that the hole of tellurium cadmium mercury epitaxial material under the 77K temperature is corresponding to be adjusted at 5 * 10 15To 5 * 10 16Cm -3Between.
2. according to the heat treating method of claim 1 open pipe tellurium cadmium mercury epitaxial material, it is characterized in that: the amount of said heat treatment source HgTe powder is got every square centimeter 1～2 gram by the epitaxial material area and is advisable.
CNB011319240A 2001-10-16 2001-10-16 Open pipe tellurium cadmium mercury epitaxial material heat treatment method Expired - Fee Related CN1133761C (en)

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