CN104532172B - Two-step method eliminates the heat treatment method of rich tellurium precipitated phase defect in Cdl-x_Znx_Te - Google Patents
Two-step method eliminates the heat treatment method of rich tellurium precipitated phase defect in Cdl-x_Znx_Te Download PDFInfo
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Abstract
The invention discloses a kind of two-step method and eliminate the heat treatment method of rich tellurium precipitated phase defect in Cdl-x_Znx_Te, Cdl-x_Znx_Te is first placed under rich tellurium state and carries out heat treatment by the method, the tellurium atom of excess in rich tellurium precipitated phase defect is made to discharge from sample, with rich cadmium heat treatment, sample is processed the most again, make Cd atom enter the rich tellurium precipitated phase of liquid, utilize the process of the rich tellurium precipitated phase generation supersaturation extension of liquid to reduce the size of rich tellurium precipitated phase defect.Conventional heat treatment method is reducing the size of rich tellurium precipitated phase defect, can produce substantial amounts of misfit dislocation in the periphery material of precipitated phase defect simultaneously.By comparison, being under control in rich tellurium heat treatment process due to the tellurium atom content in rich tellurium precipitated phase in the inventive method, this process will not produce stress and misfit dislocation to periphery material.Two-step method heat treatment technics can be effectively improved the quality of material, meets the demand that Cdl-x_Znx_Te is applied as photoelectric device or backing material.
Description
Technical field
The present invention relates to a kind of Cdl-x_Znx_Te manufacturing process technology, be specifically related to a kind of two-step method and eliminate cadmium-zinc-teiluride material
The heat treatment method of rich tellurium precipitated phase defect in material.
Background technology
Cdl-x_Znx_Te is a kind of important semi-conducting material, and it both can be used as the lining of tellurium cadmium mercury epitaxial material
The end, prepare and produce high performance infrared focal plane detector, it is possible to be directly used in preparation and produce sensing γ
The high energy ray detector of ray.Infrared focal plane detector and gamma ray detector are in space remote sensing, medical treatment
Equipment, safety check and military equipment have a wide range of applications.
Comparing with GaAs material with wide variety of Si material, the Formation energy of Cdl-x_Znx_Te is the lowest,
Thermal conductivity is the lowest, and the cadmium-zinc-teiluride crystal ingot grown is mostly multiple grain material, and more or less contains richness
Tellurium or rich cadmium precipitated phase defect, defect concentration is 103~105cm-3, size is between general 5~30 μm.Single
Wafer material is to cut out from big crystal grain, and the defect in material needs to be carried out by Technology for Heating Processing
Adjust.Vydyanath[1], Sen[2]And Belas[3]Et al. result of study all show, utilize rich cadmium state (with
Its crystal balanced each other is in the state of rich cadmium stoichiometric proportion) Technology for Heating Processing can effectively reduce rich tellurium and sink
The size of shallow lake phase defect, but at us, cadmium-zinc-teiluride richness tellurium precipitated phase defect is carried out the research of heat treatment elimination
During find, rich cadmium heat treatment is in reducing Cdl-x_Znx_Te while rich tellurium precipitated phase defect, in precipitation
Material around phase defect can be supervened serious dislocation multiplication effect (see Fig. 1), permissible from figure
Finding out, through after heat treatment, rich tellurium precipitated phase defect is substantially reduced, but goes out around precipitated phase defect
Having showed substantial amounts of dislocation, its scope is about more than 5 to 10 times of precipitated phase defect, i.e. heat treatment and is subtracting
While little precipitated phase flaw size, the appearance in dislocation multiplication region also brings new damage to quality of materials
Evil, it can cause the reduction of the minority carrier lifetime of material, ultimately result in the decline of detector performance.
List of references:
[1] H.R.Vydyanath, J.Ellsworth, J.J.Kennedy, et al.Recipe to minimize Te
Precipitation 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 defects
And relation to epitaxial HgCdTe quality [J] .J.Electron.Mater.1996,25:
1188-1195
[3] E.Belas, M.Bug á r, R.Grill, et al.Reduction of inclusions in (CdZn) Te and
CdTe: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 and
CdZnTe substrates for use in Mercury Cadmium Telluride epitaxy[J].Journal of
Electronic Materials,1995,24(5):505-510
[5]J.H.GREENBERG,V.N.GUSKOV,M.FIEDERLE,et.al.,Experimental Study
of Non-Stoichiometry in Cd1-xZnxTe1-δ, Journal of ELECTRONIC MATERIALS,
33(6),2004:719-723
Summary of the invention
The problem that rich tellurium precipitated phase defect periphery material produces dislocation for rich cadmium heat treatment, the present invention proposes
A kind of rich tellurium material is undertaken in two steps heat-treating methods, solves rich tellurium material and lack reducing precipitated phase
Produce the value-added problem of dislocation while falling into size, thus more efficiently promote the quality of rich tellurium material.This
Method first carries out heat treatment by rich tellurium state to rich tellurium Cdl-x_Znx_Te, by the Te of excess in rich tellurium precipitated phase
Atom excludes from material, then re-uses rich cadmium state and material is carried out heat treatment, makes rich tellurium lack mutually
It is trapped under the effect of Cd dividing potential drop and enters hypersaturated state, and then in material inwall (outside of defect area)
There is extension, to reach not only to reduce precipitated phase flaw size but also do not produce the value-added purpose of dislocation.The present invention carries
Supply techniques below scheme:
1. rich tellurium Technology for Heating Processing
Research shows, under rich cadmium state, the entrance of Cd atom will make rich tellurium precipitated phase defect at high temperature
The rich tellurium liquid phase of lower formation is in hypersaturated state, and then realizes extension on material inwall, makes defect area
Size reduce.It is the most brilliant that the Te atomic quantity contained due to rich tellurium precipitated phase is typically greater than same volume
Te atomic quantity in body material, along with the continuous entrance of Cd atom, rich tellurium will be filled with all the most empty mutually
Between, but now still suffer from the Te atom of excess, because the combination of Te atom and Cd atom can be very big, instead
Should continue, the volume of defect area will exceed the volume of free space, thus cause defect area to produce
Raw internal stress, defect periphery material also will be acted on by internal stress, and result causes position in defect periphery material
Wrong increment.Therefore, rich cadmium heat treatment to be avoided to produce dislocation increment around rich tellurium precipitated phase defect, just
First the tellurium atom of excess in rich tellurium precipitated phase defect must be excluded from material.
Technology for Heating Processing is that the atom in material provides a hot environment that can move.At high temperature
Under, the rich tellurium precipitated phase in rich tellurium material will make material be in the stoichiometric proportion of rich tellurium state, i.e. material
Being in rich tellurium state, the gaseous environment corresponding to the equilibrium vapor pressure of its correspondence is rich tellurium state (Te2Dividing potential drop
Higher, Cd dividing potential drop is relatively low), if the Te that at this moment Technology for Heating Processing provides2Dividing potential drop is steamed less than the balance of material
Air pressure, the Te atom in material will be to gas phase diffusion, the Cd dividing potential drop of heat treatment system and materials chemistry simultaneously
Metering also will cause Cd atom to do corresponding motion than the difference of corresponding equilibrium vapor pressure.Owing to Cd is former
The diffusion coefficient unit of son is more than Te atom, and the Cd dividing potential drop that heat treatment provides can not be too high, otherwise Cd atom
The rich tellurium precipitated phase (now for liquid phase) that will quickly enter in Cdl-x_Znx_Te, and make its supersaturation occur
Extension, too high Cd pressure can make the top layer of cadmium-zinc-teiluride quickly proceed to rich cadmium state simultaneously so that it is Te atom
Equilibrium vapor pressure be greatly lowered, and then hinder in material Te atom to gas phase diffusion.As can be seen here,
In order to eliminate the Te atom of excess in rich tellurium precipitated phase defect, it is required to be rich tellurium material and one relatively low gas is provided
Phase Cd dividing potential drop, low Cd dividing potential drop is by the rich tellurium region at Cdl-x_Znx_Te dividing potential drop phasor that falls, the most so-called
Rich tellurium heat treatment.GREENBERG gives Cdl-x_Znx_Te and is in rich cadmium or the phasor of rich tellurium state[5],
It is in Cd dividing potential drop P corresponding to the Cdl-x_Znx_Te of positive stoichiometric proportioncdWith the relation of material temperature T it is,
log PCd(atm)=-12.255+0.01187T (DEG C) (1)
Cd dividing potential drop and Cd source temperature TCdRelation be then,
log PCd(atm)=-5317/TCd(K)+5.119, T > 594K (2)
The Cd temperature of rich tellurium heat treatment is typically chosen in the Cd source temperature being significantly less than corresponding to positive stoichiometric proportion,
Now balance Te corresponding to gas phase2Dividing potential drop is higher, and this to getting rid of the Te atom of excess in rich tellurium material is
Disadvantageous.But, in actual rich tellurium Technology for Heating Processing, system does not provide higher Te2Dividing potential drop, heat
It is practically at a kind of nonequilibrium condition that can not balance between the gaseous environment and the cadmium-zinc-teiluride solid phase that process.For
Slow down this nonequilibrium condition destruction to material surface crystal structure, heat treatment system can place certain
The powder of quantity, utilizes the Te atom being evaporated in powder to provide a relatively low Te for heat treatment system2
Dividing potential drop.With this understanding, the excessive Te atom in rich tellurium material will be effectively to external diffusion, meanwhile, and Cd
The entrance of atom is not enough to again cause supersaturation extension at defect area and form stress.Discharge from material
Te atomic quantity becomes positive correlation with heat treatment temperature, becomes negative correlation with Cd source temperature, is closed by selection
Suitable heat treatment condition, can control the Te atomic quantity in rich tellurium precipitated phase to slightly close to waiting quantity space tellurium
The quantity of Te atom in zincium-cadmium crystal.If the Te atomic quantity in rich tellurium precipitated phase is discharged by excess,
After next step rich cadmium Technology for Heating Processing, precipitated phase region will be left behind bigger cavity.
2. rich cadmium Technology for Heating Processing
After rich tellurium precipitated phase defect has the Te atom of excess no longer, rich cadmium heat treatment will be used to reduce
Or the precipitated phase defect in elimination material.Rich cadmium heat treatment is that material provides a higher Cd dividing potential drop,
The difference between relatively low Cd equilibrium vapor pressure corresponding to it and the material containing rich tellurium precipitated phase defect will be led
Cause gas phase Cd atom and enter Cdl-x_Znx_Te, make under high temperature the Cd content in the rich tellurium precipitated phase in liquid phase
Constantly it is gradually increased, until hypersaturated state, and then cause liquid precipitated phase at the plane of crystal outside defect
There is extension, make the space of defect in material diminish.Because of the rich tellurium heat treatment of the first step, rich tellurium sinks
Forming sediment and will freely be converted into tellurium-zincium-cadmium crystal in the space occupied by defect, this process will no longer produce
Internal stress, can cause increasing considerably of dislocation the most again in its periphery material.Equally, at rich cadmium heat
For the gaseous environment of reason is relative to Cdl-x_Znx_Te, also it is a nonequilibrium condition, this non-flat in order to slow down
The weighing apparatus state destruction to material surface crystal structure, also can place a number of powder in heat treatment system,
The Te atom being evaporated in powder is utilized to provide a relatively low Te for heat treatment system2Dividing potential drop.
3. the mode of Technology for Heating Processing
Heat treatment will be carried out in high-purity cavity individually controllable two sections of warm area temperature, and Fig. 2 is the present invention
The schematic diagram of used annealing device.Heat treatment system by heater 1, heat treatment cavity 2, specimen holder 3,
Sample 4, powder 5 and Cd source 6 form.Heat treatment cavity can be airtight quartz ampoule, it is also possible to
It is located in graphite cavity the most airtight in quartz ampoule cavity (Technology for Heating Processing of open pipe mode).Sample
Being placed on the high-temperature region of two-zone furnace, Cd source is placed on low-temperature space, and the amount that Cd source is placed should ensure that at Re Chu
Science and engineering skill will not all be evaporated to gas, to ensure that the Cd dividing potential drop of gas phase is controlled by Cd source temperature.
The amount of powder decides the degree of depth of material list surface layer damage zone, and after heat treatment, the removable thickness of material surface is big
Little is the reference frame selecting powder how many.
Two-step method Technology for Heating Processing (can be down in same one-time process by the temperature conditions of switching heat treatment
Room temperature, is not switched on cavity) in complete, it is possible to Technology for Heating Processing completes the most at twice.
4. the selection of heat treatment temperature
The selection of heat treatment temperature should make Cd and Te atom have higher migration rate in the material, experiment
Result shows, heat treatment temperature just need to can make in material Cd and Te atom at several time-of-weeks more than 550 DEG C
Interior migration amount be enough to change composition and the volume of precipitated phase in Cdl-x_Znx_Te.When heat treatment temperature exceedes
After 900 DEG C, the dislocation density of Cdl-x_Znx_Te increases starting, therefore, and the heat of two-step method Technology for Heating Processing
Treatment temperature should select between 550 DEG C to 900 DEG C.Using such heat treatment temperature, we use 550
DEG C, 800 DEG C and 900 DEG C of sample temperatures cadmium zinc telluride crystal wafer (thickness is 1mm) has been carried out rich tellurium heat treatment,
And using 700 DEG C of sample temperatures that material carries out second step richness Cadmium treated, the rich cadmium in result display material sinks
Shallow lake phase size is obviously reduced, and does not occurs dislocation to rise in value in the periphery material of precipitated phase defect simultaneously.
Two-step method eliminate the heat treatment technics of rich tellurium precipitated phase defect in Cdl-x_Znx_Te be special one for
The technology of rich tellurium precipitated phase defect being reduced or eliminated in Cdl-x_Znx_Te, compares with conventional art, this technology exists
The dislocation multiplication effect supervened around defect can be suppressed while reducing precipitated phase flaw size.
Accompanying drawing explanation
Fig. 1 change of System of Detecting Surface Defects For Material after rich cadmium heat treatment of the Cdl-x_Znx_Te containing rich tellurium precipitated phase defect
Changing, (a) is the surface topography of material before heat treatment, and (b) is the material surface pattern after heat treatment.At Re
The temperature conditions of science and engineering skill is 650 DEG C/600 DEG C (sample temperature/Cd source temperatures), and heat treatment time is 72 little
Time, material surface corrodes through Everson caustic[5]
Fig. 2 two-step method eliminates the heat treatment system schematic diagram of rich tellurium precipitated phase defect in Cdl-x_Znx_Te
Detailed description of the invention:
1. the preparation of heat treatment material
1) with transmission infrared microscopy, processed Cdl-x_Znx_Te is detected, precipitate as contained by material
The type (rich tellurium and rich cadmium precipitated phase defect) of phase defect and size are classified, each heat treatment work
Skill should select the sample that precipitated phase flaw size is roughly the same, and is carried out sample, and cleaning way is as follows;
A) sample is put in trichloro ethylene liquation be heated to boiling, sample is taken out from liquation, replacing three
It is again heated to boiling after vinyl chloride liquation, continuous 3 times or more than 3 times, puts in methanol liquation clear after taking-up
Wash 3 times or more than 3 times;
B) configuration Br methanol liquation (concentration is 0.5%~1%), puts into sample in Br methanol liquation and corrodes
10 seconds or more than 10 seconds, put into after quickly removing in methanol liquation and clean 3 times or more than 3 times, then exist
Deionized water cleans 3 times or more than 3 times, after taking-up, uses high-purity N2Air-blowing is dry rear stand-by.
2) a number of cadmium-zinc-teiluride polycrystal material is taken, with clean Achates device after cleaning by above-mentioned cleaning way
Tool carries out smashing process to bulk, obtains the powder particle size powder less than 1mm;
3) some purity Cd bar higher than 6N is taken standby.
4) processing and heat treatment technique quartz ampoule or make high purity graphite sample box, quartz ampoule or heat
Processing need to be higher than carrying out degasification (removal stone at a temperature of heat treated sample temperature 100 DEG C before sample box uses
English pipe and the adsorbed gas that may be present of graphite member material surface) process.
2. load
1) ampoule or heat treated sample box 2 are loaded after sample 4 and powder 5 are loaded specimen holder 3, powder
Measure depending on the control of surface damage layer depth being required by Technology for Heating Processing, (true in vacuum after putting into Cd source 6
Reciprocal of duty cycle is less than 10-4Pa) under, ampoule entrance is melted rear enclosed, or with lid, heat treated sample box is closed,
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 in two-zone furnace 1, position respectively, sample 4 and Cd source 6
High-temperature region and low-temperature space in two-zone furnace 1.As used the mode of heat treated sample box, need to be to hot processing chamber
Body 7 carries out evacuation (vacuum is less than 10Pa), and evacuation puts into the N of flowing after terminating2Gas, again
Evacuation also puts into the H of flowing2Gas.
3. heat treatment
1) sample temperature and Cd source temperature are set, in order to make in material by rich tellurium process of thermal treatment condition
Atom can occur effectively to migrate in Technology for Heating Processing, does not gives the perfection of lattice of material surface not
Causing serious destruction, the sample temperature of Technology for Heating Processing typically should be greater than 550 DEG C, but not can exceed that 900
℃.The Cd source temperature that rich tellurium heat treatment selects will be significantly lower than being calculated according to formula (1) and (2)
Cd source temperature (being typically less than more than 50 DEG C).According to selected heat treatment temperature to two sections of warm area stoves
Heater carry out temperature setting, heating rate is located between 3 DEG C/min~5 DEG C/min and (makes sample temperature
Reach setting value with Cd source temperature simultaneously), as used the open pipe Technology for Heating Processing of heat treated sample box, sample
The H that product temperature will flow after reaching setting value2Autogenous cutting is changed to the Ar gas of flowing;
2) after rich tellurium Technology for Heating Processing reaches rich tellurium heat treatment time, by rich cadmium process of thermal treatment condition
Adjust sample temperature and Cd source temperature.The range of choice of the sample temperature of rich cadmium Technology for Heating Processing is also 550
DEG C~900 DEG C between, Cd temperature will be apparently higher than according to formula (1) and 3) calculated Cd source temperature
Degree (the most also to exceed more than 50 DEG C);
1., after heat treatment time reaches the heat treatment time that rich cadmium Technology for Heating Processing sets, two sections of warm areas are cut off
The heating power supply of stove heater, makes heat treated sample 4 and Cd source 6 furnace cooling;
2., after the temperature in heat-treatment furnace is down to room temperature, quartz ampoule or heat treated sample box 2 are taken out, and
Take out processed Cdl-x_Znx_Te.
4. the detection of Cdl-x_Znx_Te performance and the judgement of thermal effectiveness
1) use Everson caustic that Cdl-x_Znx_Te surface is corroded[5].As observed at material surface
To the dislocation etch pit cluster as shown in Fig. 1 (a), then show that rich tellurium heat treatment is abundant not, should suitably increase
Heat treatment time or the sample temperature of increase heat treatment;
2) the precipitated phase defect in transmission infrared microscopy detection material is used.As in Cdl-x_Znx_Te still
It is observed that micron-sized volume defect, and the most there is not etch pit cluster in material, then show that rich tellurium is heat treated
The Te atom got rid of from rich tellurium precipitated phase defect in journey is the most excessive.Now the time of rich tellurium heat treatment should fit
When shortening (or the sample temperature of rich tellurium heat treatment should suitably reduce);Or need suitably to increase rich cadmium heat treatment
Time or the sample temperature of the rich cadmium heat treatment of increase.By adjusting heat treatment condition, by rich tellurium precipitated phase
Te atomic quantity controls to close to wait the quantity of Te atom in quantity space tellurium-zincium-cadmium crystal;
3) use X-ray diffractometer to measure the twin crystal half-peak breadth of material list surface layer, and observe twin crystal half-peak breadth
Remove the change of the degree of depth with surface layer, the depth of material of twin crystal half-peak breadth generation broadening is material surface damage
Layer thickness, makes the surface of material by the quantity adjusting the sample temperature of heat treatment, Cd source temperature and powder
Damage layer controls in the range of subsequent technique allows.
Claims (1)
1. a heat treatment method for rich tellurium precipitated phase defect during two-step method eliminates Cdl-x_Znx_Te, its feature exists
In comprising the following steps:
1) first Cdl-x_Znx_Te is carried out heat treatment under rich tellurium state, by excess in rich tellurium precipitated phase defect
Tellurium atom discharges sample;Heat treatment temperature 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, the size of the selection of heat treatment time rich tellurium precipitated phase defect with processed material and
Thickness of sample is relevant;
2) by rich cadmium Technology for Heating Processing, sample being carried out heat treatment again, the rich tellurium making Cd atom enter liquid sinks
Shallow lake phase, utilizes the process of the rich tellurium precipitated phase generation supersaturation extension of liquid to reduce the chi of rich tellurium precipitated phase defect
Very little, and accomplish heat treatment process does not produces stress and misfit dislocation to periphery material;Sample temperature controls
Between 550 DEG C to 900 DEG C, Cd source temperature is arranged on and makes sample be in rich cadmium state, the choosing of heat treatment time
Size and the thickness of sample of selecting tellurium precipitated phase defect rich with processed material are relevant;
3) heat treatment uses the heat treatment technics that a kind of Te dividing potential drop under-balanced state is controlled, to reduce heat treatment
During gas phase nonequilibrium condition to material surface layer crystal body structural damage;The sample of heat treatment is placed on double
The high-temperature region of warm area stove, Cd source is placed on low-temperature space, and the amount that Cd source is placed should ensure that in Technology for Heating Processing
Will not all be evaporated to gas, to ensure that the Cd dividing potential drop of gas phase is controlled by Cd source temperature, heat treatment
The Cd dividing potential drop that state is provided by Cd source controls, and places powder in sample area, by controlling Cd source temperature simultaneously
Degree and the quantity of powder, make the Te dividing potential drop that the gas phase maintenance of heat treatment is certain, to slow down in Technology for Heating Processing
In material, Te atom is in the degree of nonequilibrium condition.
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