CN104532172A - Heat treatment method for eliminating tellurium-rich precipitate-phase defect in tellurium-zinc-cadmium material through two-step process - Google Patents
Heat treatment method for eliminating tellurium-rich precipitate-phase defect in tellurium-zinc-cadmium material through two-step process Download PDFInfo
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Abstract
The invention discloses a heat treatment method for eliminating a tellurium-rich precipitate-phase defect in a tellurium-zinc-cadmium material through a two-step process. The method comprises: firstly performing heat treatment on the tellurium-zinc-cadmium material in a tellurium-rich state, so as to discharge excessive tellurium atom in tellurium-rich precipitate-phase defect from a sample, then performing cadmium-rich heat treatment on the sample, so as to enable Cd atom to enter the liquid-state tellurium-rich precipitate phase, and reducing the dimension of the tellurium-rich precipitate-phase defect by utilizing the process of the liquid-state tellurium-rich precipitate phase being subjected to supersaturation epitaxy. A routine heat treatment method enables the peripheral material of the precipitate-phase defect to generate a large amount of misfit dislocations when helps to reduce the dimension of the tellurium-rich precipitate-phase defect. Compared with the routine heat treatment method, the disclosed method does not enable the peripheral material to generate stress and misfit dislocations because the tellurium atom content in the tellurium-rich precipitate phase is controlled during tellurium-rich heat treatment. The two-step heat treatment technology is capable of effectively improving the quality of the material, and satisfies application demands on the tellurium-zinc-cadmium material as a photoelectric device or a substrate material.
Description
Technical field
The present invention relates to a kind of Cdl-x_Znx_Te manufacturing process technology, be specifically related to the heat treating method that a kind of two-step approach eliminates rich tellurium precipitated phase defect in Cdl-x_Znx_Te.
Background technology
Cdl-x_Znx_Te is a kind of important semiconductor material, and it both can be used as the substrate of tellurium cadmium mercury epitaxial material, prepares and produces high performance infrared focal plane detector, also can be directly used in preparation and produce the gamma-ray high energy ray detector of induction.Infrared focal plane detector and gamma detector have a wide range of applications in spacer remote sensing, medical facilities, safety check and military equipment.
Compare with GaAs material with the Si material of widespread use, the Formation energy of Cdl-x_Znx_Te is very low, and thermal conductivity is very low again, and the tellurium zinc cadmium crystal ingot grown is mostly multiple grain material, and more or less containing rich tellurium or rich cadmium precipitated phase defect, defect concentration is 10
3~ 10
5cm
-3, size is between general 5 ~ 30 μm.Monocrystalline sheet material cuts out from large crystal grain, and the defect in material needs to be adjusted by thermal treatment process.Vydyanath
[1], Sen
[2]and Belas
[3]result of study Deng people all shows, utilize the thermal treatment process of rich cadmium state (crystal balanced each other with it is in the state of rich cadmium stoichiometric ratio) that the size of rich tellurium precipitated phase defect can be effectively reduced, but at us tellurium zinc cadmium rich tellurium precipitated phase defect heat-treated in the research process of elimination and find, rich cadmium thermal treatment is in reduction Cdl-x_Znx_Te while rich tellurium precipitated phase defect, serious dislocation multiplication effect (see Fig. 1) can be supervened in material around precipitated phase defect, as can be seen from the figure, through after heat treatment, rich tellurium precipitated phase defect significantly reduces, but around precipitated phase defect, there is a large amount of dislocations, its scope is roughly more than 5 to 10 times of precipitated phase defect, namely thermal treatment is while reduction precipitated phase defect size, the appearance in dislocation multiplication region also brings new infringement to quality of materials, it can cause the reduction of the minority carrier lifetime of material, finally cause the decline of detector performance.
Reference:
[1]H.R.Vydyanath，J.Ellsworth，J.J.Kennedy，et al.Recipe to minimize Teprecipitation in CdTe and(Cd，Zn)Te crystals[J].Journal of Vacuum Science&Technology B，1992，10:1476-1484
[2]S.Sen，C.S.Liang，D.R.Rhiger，et al.Reduction of CdZnTe substrate defectsand relation to epitaxial HgCdTe quality[J].J.Electron.Mater.1996，25:1188-1195
[3]E.Belas，M.Bugár，R.Grill，et al.Reduction of inclusions in(CdZn)Te andCdTe:In single crystals by post-growth annealing[J].J.Electron.Mater.2008，37:1212-1218
[4]Everson W J,Ard C K,Sepich J L,et al.Etch pit characterization of CdTe andCdZnTe substrates for use in Mercury Cadmium Telluride epitaxy[J].Journal ofElectronic Materials,1995,24(5):505-510
[5]J.H.GREENBERG,V.N.GUSKOV,M.FIEDERLE,et.al.,Experimental Studyof Non-Stoichiometry in Cd
1-xZn
xTe
1-δ，Journal of ELECTRONIC MATERIALS,33(6),2004:719-723
Summary of the invention
For rich cadmium thermal treatment, rich tellurium precipitated phase defect periphery material is produced to the problem of dislocation, the present invention proposes a kind of method that rich tellurium material is heat-treated in two steps, solve rich tellurium material and produce the value-added problem of dislocation while reduction precipitated phase defect size, thus more effectively promote the quality of rich tellurium material.Present method is first heat-treated rich tellurium Cdl-x_Znx_Te by rich tellurium state, Te atom excessive in rich tellurium precipitated phase is excluded from material, and then use rich cadmium state to heat-treat material, rich tellurium phase defect is made to enter hypersaturated state under the effect of Cd dividing potential drop, and then there is extension at material inwall (outside of defect area), not only reduce precipitated phase defect size but also do not produce the value-added object of dislocation to reach.The invention provides following technical scheme:
1. rich tellurium thermal treatment process
Research shows, under rich cadmium state, the rich tellurium liquid phase that rich tellurium precipitated phase defect is at high temperature formed is in hypersaturated state by entering of Cd atom, and then realizes extension on material inwall, and the size of defect area is reduced.The Te atomic quantity contained due to rich tellurium precipitated phase is generally all greater than the Te atomic quantity in same volume normal lens material, along with constantly entering of Cd atom, rich tellurium will be full of all freeboards mutually, but now still there is excessive Te atom, because the combination of Te atom and Cd atom can be very large, reaction can continue, the volume of defect area will exceed the volume of freeboard, thus cause defect area to produce internal stress, defect periphery material also will be subject to the effect of internal stress, and result causes the increment of defect periphery material Dislocations.Therefore, avoid rich cadmium thermal treatment around rich tellurium precipitated phase defect, produce dislocation increment, just must first excessive tellurium atom in rich tellurium precipitated phase defect be excluded from material.
Thermal treatment process is that the atom in material provides a hot environment that can move.At high temperature, the rich tellurium precipitated phase in rich tellurium material will make material be in rich tellurium state, and namely the stoichiometric ratio of material is in rich tellurium state, and the gaseous environment corresponding to the equilibrium vapor pressure of its correspondence is rich tellurium state (Te
2dividing potential drop is higher, and Cd dividing potential drop is lower), if the at this moment Te that provides of thermal treatment process
2dividing potential drop is lower than the equilibrium vapor pressure of material, and the Te atom in material will to gas phase diffusion, and the Cd dividing potential drop of heat treatment system is measured to materials chemistry and also will Cd atom be caused to do corresponding motion than the difference of corresponding equilibrium vapor pressure simultaneously.Because the spread coefficient unit of Cd atom is greater than Te atom, the Cd dividing potential drop that thermal treatment provides can not be too high, otherwise Cd atom is by the rich tellurium precipitated phase entered very soon in Cdl-x_Znx_Te (being now liquid phase), and make its supersaturation and extension occurs, too high Cd pressure can make the top layer of tellurium zinc cadmium proceed to rich cadmium state very soon simultaneously, the equilibrium vapor pressure of its Te atom is significantly reduced, and then to hinder in material Te atom to gas phase diffusion.As can be seen here, in order to eliminate Te atom excessive in rich tellurium precipitated phase defect, be required to be rich tellurium material and provide a lower gas phase Cd dividing potential drop, low Cd dividing potential drop will drop on the rich tellurium region of Cdl-x_Znx_Te dividing potential drop phasor, i.e. so-called rich tellurium thermal treatment.GREENBERG gives the phasor that Cdl-x_Znx_Te is in rich cadmium or rich tellurium state
[5], be in the Cd dividing potential drop P corresponding to Cdl-x_Znx_Te of positive stoichiometric ratio
cdwith the pass of material temperature T be,
Log P
cd(atm)=-12.255+0.01187T (DEG C) (1) Cd dividing potential drop and Cd source temperature T
cdrelation be then,
log P
Cd(atm)＝-5317/T
Cd(K)+5.119，T>594K (2)
Rich tellurium heat treated Cd temperature is typically chosen in the Cd source temperature be significantly less than corresponding to positive stoichiometric ratio, the balance Te now corresponding to gas phase
2dividing potential drop is higher, and this is disadvantageous to excessive Te atom in the rich tellurium material of eliminating.But in the rich tellurium thermal treatment process of reality, system does not provide higher Te
2dividing potential drop, is in fact in a kind of nonequilibrium situations that can not balance between heat treated gaseous environment and tellurium zinc cadmium solid phase.In order to slow down the destruction of this nonequilibrium situations to material surface crystalline structure, the powder of some amount in heat treatment system, can be placed, utilizing the Te atom that is evaporated in powder to provide a lower Te for heat treatment system
2dividing potential drop.With this understanding, the excessive Te atom in rich tellurium material will effectively to external diffusion, meanwhile, Cd atom enter and be not enough to defect area cause supersaturation extension and formed stress.The Te atomic quantity of discharging from material becomes positive correlation with thermal treatment temp, negative correlation is become with Cd source temperature, by selecting suitable heat-treat condition, the Te atomic quantity in rich tellurium precipitated phase can be controlled to slightly close to the quantity waiting Te atom in quantity space tellurium-zincium-cadmium crystal.If the Te atomic quantity in rich tellurium precipitated phase is by excessive discharge, after next step rich cadmium thermal treatment process, precipitated phase region will leave larger cavity.
2. rich cadmium thermal treatment process
After rich tellurium precipitated phase defect has excessive Te atom no longer, rich cadmium thermal treatment will be used to the precipitated phase defect reducing or eliminate in material.Rich cadmium thermal treatment is that material provides a higher Cd dividing potential drop, difference between it and the lower Cd equilibrium vapor pressure corresponding to material containing rich tellurium precipitated phase defect will cause gas phase Cd atom to enter Cdl-x_Znx_Te, Cd content in rich tellurium precipitated phase in liquid phase under high temperature is constantly increased gradually, until hypersaturated state, and then cause liquid precipitated phase in the plane of crystal generation extension of defect outside, the space of defect in material is diminished.Owing to there being the rich tellurium thermal treatment of the first step, rich tellurium precipitated phase has freely been converted into tellurium-zincium-cadmium crystal by the space occupied by defect, and this process no longer will produce internal stress, also just can not cause increasing considerably of dislocation in its periphery material again.Equally, the relative Cdl-x_Znx_Te of the rich heat treated gaseous environment of cadmium, also be a nonequilibrium situations, in order to slow down the destruction of this nonequilibrium situations to material surface crystalline structure, also can place the powder of some amount in heat treatment system, utilize the Te atom that is evaporated in powder to provide a lower Te for heat treatment system
2dividing potential drop.
3. the mode of thermal treatment process
Thermal treatment is undertaken in the independent controlled high-purity cavity of two sections of warm area temperature, and Fig. 2 is the schematic diagram of thermal treatment unit used herein.Heat treatment system is made up of well heater 1, thermal treatment cavity 2, specimen holder 3, sample 4, powder 5 and Cd source 6.Thermal treatment cavity can be airtight quartz ampoule, also can be to be placed on graphite cavity relatively airtight in silica tube cavity (thermal treatment process of open pipe mode).Sample is placed on the high-temperature zone of two-zone furnace, and Cd source is placed on cold zone, and the amount that Cd source is placed should ensure all can not be evaporated to gas in thermal treatment process, to ensure the control of Cd dividing potential drop by Cd source temperature of gas phase.The amount of powder decides the degree of depth of bill of material surface layer damage zone, and after thermal treatment, material surface can remove the size of thickness is the reference frame selecting powder how many.
Two-step approach thermal treatment process completes in same one-time process (be not namely down to room temperature, do not open cavity) by switching heat treated temperature condition, also can as required at twice thermal treatment process complete.
4. the selection of thermal treatment temp
The selection of thermal treatment temp should make Cd and Te atom have higher rate of migration in the material, experimental result shows, thermal treatment temp just can need make the migration amount of Cd and Te atom in a few time-of-week in material be enough to change composition and the volume of precipitated phase in Cdl-x_Znx_Te more than 550 DEG C.After thermal treatment temp is more than 900 DEG C, the dislocation desity of Cdl-x_Znx_Te increases starting, and therefore, the thermal treatment temp of two-step approach thermal treatment process should be selected between 550 DEG C to 900 DEG C.Adopt such thermal treatment temp, we adopt 550 DEG C, 800 DEG C and 900 DEG C of sample temperatures to carry out rich tellurium thermal treatment to cadmium zinc telluride crystal wafer (thickness is 1mm), and adopt 700 DEG C of sample temperatures to carry out the rich Cadmium treated of second step to material, rich cadmium precipitated phase size in result display material obviously reduces, and dislocation increment does not occur simultaneously in the periphery material of precipitated phase defect.
Two-step approach eliminate the heat treatment technics of rich tellurium precipitated phase defect in Cdl-x_Znx_Te be special one for reducing or eliminate the technology of rich tellurium precipitated phase defect in Cdl-x_Znx_Te, compare with conventional art, this technology can suppress the dislocation multiplication effect supervened around defect while reducing precipitated phase defect size.
Accompanying drawing explanation
Fig. 1 is containing the change of Cdl-x_Znx_Te System of Detecting Surface Defects For Material after rich cadmium thermal treatment of rich tellurium precipitated phase defect, and (a) is the surface topography of material before thermal treatment, and (b) is the material surface pattern after thermal treatment.The temperature condition of thermal treatment process is 650 DEG C/600 DEG C (sample temperature/Cd source temperatures), and heat treatment time is 72 hours, and material surface corrodes through Everson etching reagent
[5]
Fig. 2 two-step approach eliminates the heat treatment system schematic diagram of rich tellurium precipitated phase defect in Cdl-x_Znx_Te
Embodiment:
1. the preparation of heat treatment material
1) with transmission infrared microscopy, processed Cdl-x_Znx_Te is detected, classify by the type (rich tellurium and rich cadmium precipitated phase defect) of precipitated phase defect contained by material and size, the sample that each thermal treatment process should select precipitated phase defect size roughly the same, and sample is cleaned, cleaning way is as follows;
A) sample is put into trieline liquation and be heated to boiling, sample is taken out from liquation, reheat to boiling after changing trieline liquation, continuous more than 3 times or 3 times, after taking-up, put into methyl alcohol liquation cleaning more than 3 times or 3 times;
B) Br methyl alcohol liquation (concentration is 0.5% ~ 1%) is configured, sample is put into Br methyl alcohol liquation corrosion more than 10 seconds or 10 seconds, put into methyl alcohol liquation cleaning more than 3 times or 3 times after quick taking-up, then clean more than 3 times or 3 times in deionized water, after taking-up, use high-purity N
2it is stand-by after air-blowing is dry.
2) get the tellurium zinc cadmium polycrystal of some amount, by above-mentioned cleaning way cleaning rear clean agate utensil, process is shattered to bulk, obtain the powder that powder particle size is less than 1mm;
3) some purity is got for subsequent use higher than the Cd bar of 6N.
4) processing and heat treatment technique quartz ampoule or make high purity graphite sample box, degasification (removing the adsorbed gas that silica tube and graphite member material surface may exist) process need be carried out before quartz ampoule or heat treated sample box use at the temperature higher than heat treated sample temperature 100 DEG C.
2. load
1) sample 4 and powder 5 are loaded after specimen holder 3 and load ampoule or heat treated sample box 2, the amount of powder is determined by the control overflow of thermal treatment process effects on surface damage layer depth, puts into behind Cd source 6 that (vacuum tightness is less than 10 in vacuum
-4pa) under, ampoule entrance is melted rear enclosed, or closed by heat treated sample box with lid, the amount in Cd source should ensure that it is not all gasified in whole heat treatment process;
2) ampoule or heat treated sample box 2 are put into two-zone furnace 1, sample 4 and Cd source 6 lay respectively at high-temperature zone and the cold zone of two-zone furnace 1.As adopted the mode of heat treated sample box, need vacuumize (vacuum tightness is less than 10Pa) thermal treatment cavity 7, after vacuumizing end, putting into the N of flowing
2gas, again vacuumizes and puts into the H of flowing
2gas.
3. thermal treatment
1) by rich tellurium process of thermal treatment condition setting sample temperature and Cd source temperature, effective migration is there is in thermal treatment process in order to enable the atom in material, do not cause serious destruction to again the perfection of lattice of material surface simultaneously, the sample temperature of thermal treatment process generally should be greater than 550 DEG C, but can not more than 900 DEG C.The Cd source temperature that rich tellurium thermal treatment is selected will be starkly lower than the Cd source temperature (being generally less than more than 50 DEG C) calculated according to formula (1) and (2).According to selected thermal treatment temp, temperature setting is carried out to the heating unit of two sections of warm area stoves, temperature rise rate is located between 3 DEG C/min ~ 5 DEG C/min (making sample temperature and Cd source temperature reach set(ting)value) simultaneously, as adopted the open pipe thermal treatment process of heat treated sample box, the H that sample temperature will flow after reaching set(ting)value
2autogenous cutting is changed to the Ar gas of flowing;
2) after rich tellurium thermal treatment process reaches rich tellurium heat treatment time, by rich cadmium process of thermal treatment condition adjustment sample temperature and Cd source temperature.The range of choice of the sample temperature of rich cadmium thermal treatment process is also between 550 DEG C ~ 900 DEG C, and Cd temperature will apparently higher than according to formula (1) and 3) the Cd source temperature (generally also will exceed more than 50 DEG C) that calculates;
1., after heat treatment time reaches the heat treatment time of rich cadmium thermal treatment process setting, cut off the heating power supply of two sections of warm area stove heating units, make heat treated sample 4 and Cd source 6 furnace cooling;
2. after the temperature in heat treatment furnace is down to room temperature, take out quartz ampoule or heat treated sample box 2, and take out processed Cdl-x_Znx_Te.
4. the detection of Cdl-x_Znx_Te performance and the judgement of thermal effectiveness
1) Everson etching reagent is adopted to corrode Cdl-x_Znx_Te surface
[5].As observed the dislocation etch pit bunch group as shown in Fig. 1 (a) at material surface, then show that rich tellurium thermal treatment is abundant not, should suitably increase heat treatment time or increase heat treated sample temperature;
2) the precipitated phase defect in transmission infrared microscopy test material is adopted.As still observed micron-sized bulk defects in Cdl-x_Znx_Te, and there is not corrosion pit bunch group in material, then show that the Te atom got rid of from rich tellurium precipitated phase defect in rich tellurium heat treatment process is excessive.Now the rich tellurium heat treated time should suitably shorten (or the heat treated sample temperature of rich tellurium should suitably reduce); Or need suitably increase rich cadmium heat treatment time or increase the heat treated sample temperature of rich cadmium.By adjustment heat-treat condition, the Te atomic quantity in rich tellurium precipitated phase is controlled to the quantity close to waiting Te atom in quantity space tellurium-zincium-cadmium crystal;
3) X-ray diffractometer is adopted to measure the twin crystal peak width at half height of bill of material surface layer, and observe twin crystal peak width at half height removes degree of depth change with upper layer, the depth of material of twin crystal peak width at half height generation broadening is material surface damage layer thickness, in the scope making the surface damage layer of material control to allow at subsequent technique by the quantity adjusting heat treated sample temperature, Cd source temperature and powder.
Claims (1)
1. two-step approach eliminates a heat treating method for rich tellurium precipitated phase defect in Cdl-x_Znx_Te, it is characterized in that comprising the following steps:
1) first Cdl-x_Znx_Te is heat-treated under rich tellurium state, tellurium atom excessive in rich tellurium precipitated phase defect is discharged sample; Thermal treatment temp is between 550 DEG C to 900 DEG C, and the setting of Cd source temperature makes sample be in the state of rich tellurium, and the selection of heat treatment time is relevant with thickness of sample with the size of tellurium precipitated phase defect rich in treated material;
2) by rich cadmium thermal treatment process, sample is heat-treated again, Cd atom is made to enter liquid rich tellurium precipitated phase, utilize the process of liquid rich tellurium precipitated phase generation supersaturation extension to reduce the size of rich tellurium precipitated phase defect, and accomplish not produce stress and misfit dislocation to periphery material in heat treatment process; Sample temperature controls between 550 DEG C to 900 DEG C, and Cd source temperature is arranged on and makes sample be in rich cadmium state, and the selection of heat treatment time is relevant with thickness of sample with the size of tellurium precipitated phase defect rich in treated material;
3) the thermal treatment heat treatment technics that adopts a kind of Te dividing potential drop under-balanced state controlled, to reduce in heat treatment process gas phase nonequilibrium situations to the destruction of material surface layer crystal body structure; The Cd point of pressure-controlled that heat treated state is provided by Cd source, place powder in sample area simultaneously, by the quantity of control Cd source temperature and powder, make the Te dividing potential drop that heat treated gas phase remains certain, be in the degree of nonequilibrium situations to slow down in thermal treatment process Te atom in material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106435738A (en) * | 2016-09-20 | 2017-02-22 | 广东先导稀材股份有限公司 | Preparation method of cadmium zinc telluride polycrystals |
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| CN113410124A (en) * | 2020-10-26 | 2021-09-17 | 昆明物理研究所 | Method for controlling electrical property stability of gold-doped liquid phase epitaxy mercury cadmium telluride material |
| CN113410124B (en) * | 2020-10-26 | 2022-06-14 | 昆明物理研究所 | Method for controlling electrical property stability of gold-doped liquid phase epitaxy mercury cadmium telluride material |
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