CN109576797A - Regulate and control the method for annealing of zinc telluridse crystal resistivity - Google Patents
Regulate and control the method for annealing of zinc telluridse crystal resistivity Download PDFInfo
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- CN109576797A CN109576797A CN201910046256.9A CN201910046256A CN109576797A CN 109576797 A CN109576797 A CN 109576797A CN 201910046256 A CN201910046256 A CN 201910046256A CN 109576797 A CN109576797 A CN 109576797A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
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Abstract
The invention discloses it is a kind of regulate and control zinc telluridse crystal resistivity method for annealing, the technical issues of the practicability is poor for solving existing method for annealing.Technical solution is the temperature parameter at this method adjustment two-part annealing furnace both ends, thermal field of the formation temperature section between 600~680 DEG C, temperature gradient is 7~8 DEG C/cm in thermal field, annealing frame is designed according to the thermal field of formation, annealing includes 600,620,640 every time, 660,680 DEG C of five annealing temperatures.By changing anneal duration, realize the resistivity of ZnTe crystal 102~108Regulate and control in the range of Ω cm.Since temperature gradient big in annealing process promotes diffusion process, the Zn atom filling V in atmosphere is acceleratedZn, regulate and control the carrier concentration of ZnTe crystal, change resistivity.The present invention only by adjusting anneal duration, realizes ZnTe crystal resistivity 102~108Regulation within the scope of Ω cm, practicability are good.
Description
Technical field
The present invention relates to a kind of method for annealing, in particular to a kind of method for annealing of regulation zinc telluridse crystal resistivity.
Background technique
Zinc telluridse (ZnTe) crystal has excellent photoelectric properties, has become most common generation and detection Terahertz at present
(THz) Electrooptic crystal material radiated.However, ZnTe body monocrystalline mainly uses Te flux method to be grown, and close material and crystalline substance
Due to the off-congruent evaporation on liquid-gas interface, V easy to form in body growth courseZnAnd TeiEtc. point defects.With natural lattice
It compares, it is weaker by lattice constraint at point defect, free carrier is readily become under DC Electric Field, to increase freedom
Carrier concentration reduces the resistivity of crystal.If point defect excessively causes resistivity too low in crystal, carrier concentration mistake
Height can generate THz wave and absorb and scatter, decline so as to cause the efficiency of terahertz emission.So using suitable annealing
Technique allows atmosphere atom to diffuse into crystal, fills VZn, carrier concentration is reduced, is to improve the resistivity of ZnTe crystal to mention
The effective ways of high its Terahertz response.
Document " Yoshino K, Yoneta M, Ohmori K, et al.Annealing effects of a high-
quality ZnTe substrate[J].Journal of electronic materials,2004,33(6):579-
582. " disclose a kind of Zn ambient anneal to ZnTe crystals point defect VZnInfluence.This method will grow state ZnTe crystal
It anneals with high purity zinc source Vacuum Package, the pressure in zinc source can anneal furnace temperature in 0.77Pa~34Pa range by the change
Interior adjusting.After annealing in the PL map of ZnTe crystal with VZnRelevant glow peak declines with the increase of the source Zn vapour pressure.Zn
Ambient anneal can effectively fill crystals VZn, reduce VZnConcentration.
In disclosed ZnTe crystal annealing method, annealing only obtains one group of V every timeZnQualitative data, and not to annealing after
The resistivity value of ZnTe crystal carries out quantitative test.
Summary of the invention
In order to overcome the shortcomings of existing method for annealing, the practicability is poor, and the present invention provides a kind of regulation zinc telluridse crystal resistivity
Method for annealing.This method adjusts the temperature parameter at two-part annealing furnace both ends, and formation temperature section is between 600~680 DEG C
Thermal field, temperature gradient is 7~8 DEG C/cm in thermal field, designs annealing frame according to the thermal field of formation, and annealing includes 600 every time,
620,640,660,680 DEG C of five annealing temperatures.By changing anneal duration, realize the resistivity of ZnTe crystal 102~108
Regulate and control in the range of Ω cm.Due to realizing 600,620 in primary annealing by thermal field adjustment and annealing frame design,
640,660,680 DEG C of five annealing temperatures, it is ensured that when annealing under different temperatures, the constancy of zinc vapor pressure, in annealing process
Big temperature gradient promotes diffusion process, accelerates the Zn atom filling V in atmosphereZn, regulate and control ZnTe crystal carrier it is dense
Degree changes resistivity.Only by adjusting 50~150h of anneal duration, the resistivity of ZnTe crystal can be realized 10 in the present invention2
~108Regulate and control in the range of Ω cm, practicability is good.
A kind of the technical solution adopted by the present invention to solve the technical problems: annealing side of regulation zinc telluridse crystal resistivity
Method, its main feature is that the following steps are included:
Step 1: the temperature parameter at adjustment two-part annealing furnace both ends, formation temperature section is between 600~680 DEG C
Thermal field, temperature gradient is 7~8 DEG C/cm in thermal field.
Step 2: selecting Zn, metal that purity is 69 is used as annealing source.Annealing pipe is impregnated 24 in acetone soln
~48h eliminates the organic impurities being attached on annealing pipe, then rinses out remaining acetone soln with deionized water, then use body
Product ratio is that 24~48h is impregnated in the concentrated hydrochloric acid and concentrated nitric acid mixed solution of 3:1, washes away the metal ion of annealing pipe surface attachment,
It is cleaned up repeatedly after taking-up using deionized water；It is finally placed in 100~120 DEG C of vacuum oven and dries 2~4h；
Step 3: ZnTe chip is inserted in the one end being fixed in quartz ampoule on quartz holder, Zn, source metal dresses of annealing
The other end for entering quartz ampoule will be evacuated in quartz ampoule, when vacuum degree reaches 3~8 × 10-5When Pa, sealing quartz ampoule；
Step 4: the good quartz ampoule of sealing and annealing pipe carrier are packed into two-part annealing furnace, it is horizontally arranged quartz ampoule,
The both ends of two-part annealing furnace are warming up to 550~600 DEG C, 700~750 DEG C respectively with the rate of 50~100 DEG C/h, so that stone
Annealing temperature on English bracket at wafer position is followed successively by 600,620,640,660,680 DEG C, and annealing source temperature is 725~
715 DEG C, 50~150h is kept the temperature, after annealing, taking-up chip is cooled to room temperature with the rate of 50~100 DEG C/h；
Step 5: the damaging layer of removal chip, plates Au electrode on ZnTe chip two sides, test I-V curve acquires resistivity.
The concentrated hydrochloric acid mass fraction concentration is 36.5%.
The concentrated nitric acid mass fraction concentration is 69.8%.
The beneficial effects of the present invention are: the temperature parameter at this method adjustment two-part annealing furnace both ends, formation temperature section
Thermal field between 600~680 DEG C, temperature gradient is 7~8 DEG C/cm in thermal field, designs annealing frame according to the thermal field of formation,
Annealing includes 600,620,640,660,680 DEG C of five annealing temperatures every time.By changing anneal duration, ZnTe crystal is realized
Resistivity is 102~108Regulate and control in the range of Ω cm.Due to being designed by thermal field adjustment and annealing frame, in primary annealing
Realize 600,620,640,660,680 DEG C of five annealing temperatures, it is ensured that when annealing under different temperatures, zinc vapor pressure it is constant
Property, big temperature gradient promotes diffusion process in annealing process, accelerates the Zn atom filling V in atmosphereZn, regulation ZnTe crystalline substance
The carrier concentration of body changes resistivity.The present invention only by adjusting 50~150h of anneal duration, realizes the electricity of ZnTe crystal
Resistance rate is 102~108Regulate and control in the range of Ω cm, practicability is good.
It elaborates with reference to the accompanying drawings and detailed description to the present invention.
Detailed description of the invention
Fig. 1 is the annealing thermal field and corresponding annealing frame that the method for annealing of present invention regulation zinc telluridse crystal resistivity uses
Schematic diagram.
Fig. 2 is the I-V song at 680 DEG C of positions before and after ZnTe crystal annealing after the annealing of embodiment of the present invention method 1 150h
Line.
Fig. 3 is resistivity before and after ZnTe crystal annealing at different annealing temperature after the annealing of embodiment of the present invention method 1 150h
Change curve.
Specific embodiment
Following embodiment referring to Fig.1-3.
Embodiment 1:
The first step, the temperature parameter for adjusting two-part annealing furnace both ends, formation temperature section is between 600~680 DEG C
Thermal field, temperature gradient is 7.5 DEG C/cm in thermal field.
Second step, Zn, metal that selection purity is 69 are used as annealing source.Annealing pipe is impregnated in acetone soln
For 24 hours, the organic impurities being attached on annealing pipe is eliminated, then rinses out remaining acetone soln with deionized water, then use volume
Than for 3:1 concentrated hydrochloric acid and concentrated nitric acid (concentrated hydrochloric acid mass fraction concentration is 36.5%, and concentrated nitric acid mass fraction concentration is
69.8%) 48h is impregnated in mixed solution, washes away the metal ion of annealing pipe surface attachment, after taking-up repeatedly using deionized water
It cleans up；It is finally placed in 120 DEG C of vacuum oven and dries 2h；
ZnTe chip is inserted in the one end being fixed in quartz ampoule on quartz holder by third step, and metal Zn is packed into quartz ampoule
The other end, and will be evacuated in quartz ampoule, when vacuum degree reaches 3 × 10-5When Pa, sealing quartz ampoule；
The good quartz ampoule of sealing and annealing pipe carrier are packed into two-part annealing furnace by the 4th step, are horizontally arranged quartz ampoule,
The both ends of annealing furnace are warming up to 550 DEG C, 750 DEG C respectively with the rate of 50 DEG C/h, so that moving back at 5 wafer positions on bracket
Fiery temperature is followed successively by 600,620,640,660,680 DEG C, and annealing source temperature is 720 DEG C, keeps the temperature 150h, after annealing, with
The rate of 50 DEG C/h cools down, and is down to room temperature and takes out chip；
5th step, the damaging layer for removing chip plate Au electrode on ZnTe chip two sides, and test I-V curve acquires resistivity.
Fig. 2 be the present embodiment annealing 150h after, annealing temperature be 680 DEG C at ZnTe change in resistance curve.From figure
As can be seen that the I-V curve of annealing front and back ZnTe crystal keeps good Ohmic contact with Au electrode.Crystal resistance before annealing
Rate is 13.24 Ω cm, and crystal resistivity has reached 1.966 × 10 after annealing8Ω cm improves 7 orders of magnitude.
Fig. 3 is the change in resistance of crystal at different annealing temperature after this example annealing 150h, as can be seen from the figure
Come, the resistivity of growth state ZnTe crystal is 102Ω cm magnitude, after annealing 150, the ZnTe in different annealing temperature is brilliant
Body resistivity is 106Ω cm to 108Regulate and control between Ω cm magnitude.
Embodiment 2:
The first step, the temperature parameter for adjusting two-part annealing furnace both ends, formation temperature section is between 600~680 DEG C
Thermal field, temperature gradient is 8 DEG C/cm in thermal field.
Second step, Zn, metal that selection purity is 69 are used as annealing source.Annealing pipe is impregnated in acetone soln
48h eliminates the organic impurities being attached on annealing pipe, then rinses out remaining acetone soln with deionized water, then use volume
Than for 3:1 concentrated hydrochloric acid and concentrated nitric acid (concentrated hydrochloric acid mass fraction concentration is 36.5%, and concentrated nitric acid mass fraction concentration is
69.8%) 36h is impregnated in mixed solution, washes away the metal ion of annealing pipe surface attachment, after taking-up repeatedly using deionized water
It cleans up；It is finally placed in 110 DEG C of vacuum oven and dries 3h；
ZnTe chip is inserted in the one end being fixed in quartz ampoule on quartz holder by third step, and metal Zn is packed into quartz ampoule
The other end, and will be evacuated in quartz ampoule, when vacuum degree reaches 6 × 10-5When Pa, sealing quartz ampoule；
The good quartz ampoule of sealing and annealing pipe carrier are packed into two-part annealing furnace by the 4th step, are horizontally arranged quartz ampoule,
The both ends of annealing furnace are warming up to 560 DEG C, 730 DEG C respectively with the rate of 60 DEG C/h, so that moving back at 5 wafer positions on bracket
Fiery temperature is followed successively by 600,620,640,660,680 DEG C, and annealing source temperature is 725 DEG C, keeps the temperature 100h, after annealing, with
The rate of 80 DEG C/h cools down, and is down to room temperature and takes out chip；
5th step, the damaging layer for removing chip plate Au electrode on ZnTe chip two sides, and test I-V curve acquires resistivity.
The ZnTe crystal resistivity that the present embodiment obtains is 104Ω cm to 107Regulate and control between Ω cm magnitude.
Embodiment 3:
The first step, the temperature parameter for adjusting two-part annealing furnace both ends, formation temperature section is between 600~680 DEG C
Thermal field, temperature gradient is 7 DEG C/cm in thermal field.
Second step, Zn, metal that selection purity is 69 are used as annealing source.Annealing pipe is impregnated in acetone soln
36h eliminates the organic impurities being attached on annealing pipe, then rinses out remaining acetone soln with deionized water, then use volume
Than for 3:1 concentrated hydrochloric acid and concentrated nitric acid (concentrated hydrochloric acid mass fraction concentration is 36.5%, and concentrated nitric acid mass fraction concentration is
69.8%) metal ion for washing away annealing pipe surface attachment for 24 hours is impregnated in mixed solution, after taking-up repeatedly using deionized water
It cleans up；It is finally placed in 100 DEG C of vacuum oven and dries 4h；
ZnTe chip is inserted in the one end being fixed in quartz ampoule on quartz holder by third step, and metal Zn is packed into quartz ampoule
The other end, and will be evacuated in quartz ampoule, when vacuum degree reaches 8 × 10-5When Pa, sealing quartz ampoule；
The good quartz ampoule of sealing and annealing pipe carrier are packed into two-part annealing furnace by the 4th step, are horizontally arranged quartz ampoule,
The both ends of annealing furnace are warming up to 600 DEG C, 700 DEG C respectively with the rate of 100 DEG C/h, so that moving back at 5 wafer positions on bracket
Fiery temperature is followed successively by 600,620,640,660,680 DEG C, and annealing source temperature is 715 DEG C, keeps the temperature 50h, after annealing, with
The rate of 100 DEG C/h cools down, and is down to room temperature and takes out chip；
5th step, the damaging layer for removing chip plate Au electrode on ZnTe chip two sides, and test I-V curve acquires resistivity.
The ZnTe crystal resistivity that the present embodiment obtains is 103Ω cm to 105Regulate and control between Ω cm magnitude.
Compared with the background art, experimental provision single anneal of the present invention can realize five different annealing temperature
Degree simplifies the process of experiment, and has done quantitative analysis to slice resistivity at different annealing temperature, realizes that slice resistivity exists
102Ω cm to 108Regulate and control between Ω cm.
Claims (3)
1. a kind of method for annealing of regulation zinc telluridse crystal resistivity, it is characterised in that the following steps are included:
Step 1: the temperature parameter at adjustment two-part annealing furnace both ends, thermal field of the formation temperature section between 600~680 DEG C,
Temperature gradient is 7~8 DEG C/cm in thermal field；
Step 2: selecting Zn, metal that purity is 69 is used as annealing source；Annealing pipe impregnates to 24 in acetone soln~
48h eliminates the organic impurities being attached on annealing pipe, then rinses out remaining acetone soln with deionized water, then use volume
Than impregnating 24~48h in the concentrated hydrochloric acid and concentrated nitric acid mixed solution for 3:1, the metal ion of annealing pipe surface attachment is washed away, is taken
It is cleaned up repeatedly after out using deionized water；It is finally placed in 100~120 DEG C of vacuum oven and dries 2~4h；
Step 3: ZnTe chip is inserted in the one end being fixed in quartz ampoule on quartz holder, Zn loading stones of source metal of annealing
The other end of English pipe will be evacuated in quartz ampoule, when vacuum degree reaches 3~8 × 10-5When Pa, sealing quartz ampoule；
Step 4: the good quartz ampoule of sealing and annealing pipe carrier are packed into two-part annealing furnace, it is horizontally arranged quartz ampoule, with 50
The both ends of two-part annealing furnace are warming up to 550~600 DEG C, 700~750 DEG C by the rate of~100 DEG C/h respectively, so that quartz branch
Annealing temperature on frame at wafer position is followed successively by 600,620,640,660,680 DEG C, and annealing source temperature is 725~715 DEG C,
50~150h is kept the temperature, after annealing, taking-up chip is cooled to room temperature with the rate of 50~100 DEG C/h；
Step 5: the damaging layer of removal chip, plates Au electrode on ZnTe chip two sides, test I-V curve acquires resistivity.
2. the method for annealing of regulation zinc telluridse crystal resistivity according to claim 1, it is characterised in that: the concentrated hydrochloric acid
Mass fraction concentration is 36.5%.
3. the method for annealing of regulation zinc telluridse crystal resistivity according to claim 1, it is characterised in that: the concentrated nitric acid
Mass fraction concentration is 69.8%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022032732A1 (en) * | 2020-08-14 | 2022-02-17 | 南京公诚节能新材料研究院有限公司 | Method for improving uniformity of doped elements of znte crystal |
| WO2022032733A1 (en) * | 2020-08-14 | 2022-02-17 | 南京公诚节能新材料研究院有限公司 | Method for maintaining stability of znte crystal |
| CN115161773A (en) * | 2022-07-15 | 2022-10-11 | 中南大学 | Nondestructive defect control technology for large-size CdZnTe single crystal |
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| CN102618935A (en) * | 2012-01-19 | 2012-08-01 | 中国科学院安徽光学精密机械研究所 | Annealing method for infrared nonlinear single crystal of multi-component compound containing easily volatile components |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022032732A1 (en) * | 2020-08-14 | 2022-02-17 | 南京公诚节能新材料研究院有限公司 | Method for improving uniformity of doped elements of znte crystal |
| WO2022032733A1 (en) * | 2020-08-14 | 2022-02-17 | 南京公诚节能新材料研究院有限公司 | Method for maintaining stability of znte crystal |
| CN115161773A (en) * | 2022-07-15 | 2022-10-11 | 中南大学 | Nondestructive defect control technology for large-size CdZnTe single crystal |
| CN115161773B (en) * | 2022-07-15 | 2024-07-02 | 中南大学 | Damage-free defect control technology for large-size CdZnTe single crystal |
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Application publication date: 20190405 |