CN101092748B - Method for preparing Te-Zn-Cd monocrystal in large volume - Google Patents
Method for preparing Te-Zn-Cd monocrystal in large volume Download PDFInfo
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- CN101092748B CN101092748B CN200710017996A CN200710017996A CN101092748B CN 101092748 B CN101092748 B CN 101092748B CN 200710017996 A CN200710017996 A CN 200710017996A CN 200710017996 A CN200710017996 A CN 200710017996A CN 101092748 B CN101092748 B CN 101092748B
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000013078 crystal Substances 0.000 claims abstract description 112
- 239000003708 ampul Substances 0.000 claims abstract description 30
- 239000010453 quartz Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010899 nucleation Methods 0.000 claims abstract description 18
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007789 sealing Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000007797 corrosion Effects 0.000 claims description 12
- 238000005260 corrosion Methods 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 6
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- MODGUXHMLLXODK-UHFFFAOYSA-N [Br].CO Chemical compound [Br].CO MODGUXHMLLXODK-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000007747 plating Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 238000003466 welding Methods 0.000 abstract description 4
- QWUZMTJBRUASOW-UHFFFAOYSA-N cadmium tellanylidenezinc Chemical compound [Zn].[Cd].[Te] QWUZMTJBRUASOW-UHFFFAOYSA-N 0.000 abstract 7
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000013021 overheating Methods 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 22
- 238000013461 design Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 230000002950 deficient Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000000407 epitaxy Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- NSRBDSZKIKAZHT-UHFFFAOYSA-N tellurium zinc Chemical compound [Zn].[Te] NSRBDSZKIKAZHT-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
This invention discloses a method for preparing large-volume cadmium zinc telluride (CZT) single crystal. The method comprises: (1) selecting high-melting-point CZT single crystal as the seed crystal;(2) coating a carbon film on the inner side of a quartz ampoule, placing CZT seed crystal in the seed crystal bag at the bottom of the ampoule so that the seeding growth surface of CZT seed crystal is upward, then adding low-melting-point CZT polycrystal, vacuumizing the quartz ampoule, and sealing by welding; (3) placing the quartz ampoule into an ACRT-B type crystal growth apparatus, heating the temperatures of the high-temperature zone and the low-temperature zone to 1135-1145 deg.C and 1030-1040 deg.C within 18-20 h, overheating for 12-16h, and descending the supporting bar at a speed of0.8 mm/h for 200-240 h; (4) cooling the high-temperature zone and the low-temperature zone to 870-890 deg. within 5-6 h, annealing the crystal ingot in situ for 144-168 h, then slowly cooling to 550-560 deg.C at a rate of 5 deg.C/h, shutting off the power source, and cooling to room temperature. The method can obtain large-volume CZT single crystal, and increase the single crystal ratio in the crystal ingot.
Description
Technical field
The present invention relates to a kind of preparation large volume tellurium zinc cadmium (Cd
1-xZn
xTe below is called for short CZT when not refering in particular to the x value) method of monocrystalline.
Background technology
Along with Hg
1-xCd
xThe progress of long alignment of Te and extensive focal plane array infrared eye is in order to satisfy epitaxy Hg
1-xCd
xThe needs of Te require to prepare uniform ingredients, and infrared transmittivity is higher, the large volume Cd that dislocation desity is less
0.96Zn
0.04The Te monocrystalline.On the other hand, in order to prepare the polylith large volume parallel C ZT detector of high detection efficiency, and the bin detector array that is used for imaging system, for resistivity height, less, the lower-cost large volume Cd of defect concentration
0.9Zn
0.1Te monocrystalline demand is also increasing.
In order to prepare large volume CZT monocrystalline, the way of solution is exactly to improve the monocrystalline rate of crystal ingot when increasing CZT crystal ingot size.Various forms of low-pressure growth technology, and realized that business-like high pressure growth technology all is applied in the CZT single crystal preparation, the subject matter that exists is the appearance of a large amount of twins and because the subgrain that heterogeneous forming core produces makes that CZT monocrystalline volume is less, the monocrystalline rate of crystal ingot is lower.
The method growth CZT monocrystalline that employing adds seed crystal is the comparatively ideal method of reporting at present.Document " IEEE NuclearScience Symposium Conference Record; 2003; Vol.9:3336-3337 " has reported that U.S. Yinnel scientific ﹠ technical corporation adopts improved Bridgman method and uses＜110〉± 10 ° of seed crystals, successfully grow the Cd of the many about 76mm of diameter
0.9Zn
0.1The Te crystal ingot, wherein 40% crystal ingot has and surpasses 3 * 10
5Mm
3The monocrystalline volume, 80% crystal ingot has and surpasses 1 * 10
5Mm
3The monocrystalline volume.But, can not be referred to as proper＜110 because seed crystal crystal orientation deviation is bigger〉growth of crystal orientation seeding.
Summary of the invention
In order to overcome the little deficiency of prior art growth CZT monocrystalline volume, the invention provides a kind of method for preparing Te-Zn-Cd monocrystal in large volume, employing adds the low-voltage vertical Bridgman method growth CZT crystal of seed crystal, solved of the influence of the polarity of seed crystal to the seeding growth, it is overheated by melt is carried out, obtain large volume CZT monocrystalline, can improve the monocrystalline rate of crystal ingot simultaneously.
The technical solution adopted for the present invention to solve the technical problems: a kind of method for preparing Te-Zn-Cd monocrystal in large volume is characterized in comprising the steps:
(a) select high-melting-point CZT monocrystalline, through orientation cutting, mechanical polishing, make polarity seed crystal＜111 or＜211, use HNO
3: HF=2: 1～3: the solution corrosion of 1 volume ratio preparation 3～4 seconds, the volume fraction of using bromine then is 2～4% bromine-methanol soln corrosion seed crystal 3～5 minutes, use washed with methanol after corrosion finishes, used the dehydrated alcohol ultrasonic cleaning again 5～10 minutes, use N after the taking-up
2Air-blowing is done;
(b) to the plating of the quartz ampoule inwall behind cleaning-drying carbon film, to put into the seed crystal bag of ampoule bottom through the seed crystal that step (a) is handled then, the seeding aufwuchsplate of seed crystal is put into the low melting point CZT polycrystal of 79 of purity up again, quartz ampoule is vacuumized, when vacuum tightness reaches 5 * 10
-5～6 * 10
-5During Pa, the sealing quartz ampoule;
(c) will put into ACRT-B N-type waferN growth apparatus through the quartz ampoule of step (b) sealing, begin heating, temperature with the high-temperature zone in 18～20 hours rises to 1135～1145 ℃, cold zone 9 temperature rise to 1030～1040 ℃, after reaching target temperature, after heat 12～16 hours, with the speed decent strut of 0.8mm per hour, be 200～240 hours fall time;
(d) stop to descend after, high-temperature zone and cold zone temperature reduced to 870～890 ℃ in 5～6 hours, after crystal ingot carries out 144～168 hours in-situ annealing, with per hour 5 ℃ slowly be cooled to 550～560 ℃ after the powered-down air cooling to room temperature; Prepared Te-Zn-Cd monocrystal in large volume is that volume surpasses 1 * 10
5Mm
3Monocrystalline.
The invention has the beneficial effects as follows: low-voltage vertical Bridgman method growth CZT crystal is improved because employing adds seed crystal, and melt is carried out overheated, when increasing CZT crystal ingot size, improved the monocrystalline rate of crystal ingot, obtained large volume CZT monocrystalline, reduced the cost of CZT single-chip, operation is simple simultaneously.System respectively goes out diameter 60mm and is about 140mm, and the monocrystalline volume surpasses 3 * 10
5Mm
3Cd
0.9Zn
0.1The Te crystal ingot, the monocrystalline rate of crystal ingot reaches 75%, and the resistivity of cutting back wafer reaches 1.8 * 10
9～2.6 * 10
10Ω cm satisfies the requirement of preparation large size high-performance CZT detector; Prepare diameter 60mm and be about 110mm, the monocrystalline volume surpasses 2 * 10
5Mm
3Cd
0.96Zn
0.04The Te crystal ingot, the monocrystalline rate of crystal ingot reaches 65%, and cutting back wafer is at wave number 500cm
-1～4000cm
-1Infrared transmittivity is more than 63% in the scope, and dislocation desity is lower, uniform ingredients, lattice misfit degree are very little, is suitable as excellent Hg
1-xCd
xThe Te epitaxial growth substrate.
Below in conjunction with drawings and Examples the present invention is elaborated.
Description of drawings
Fig. 1 is that the present invention prepares the used ampoule encapsulation of the method for Te-Zn-Cd monocrystal in large volume and is placed on synoptic diagram in the ACRT-B N-type waferN growth apparatus.
Fig. 2 is the method embodiment 1 prepared Cd that the present invention prepares Te-Zn-Cd monocrystal in large volume
0.9Zn
0.1The I-V curve of Te wafer.
Fig. 3 is the method embodiment 2 prepared Cd that the present invention prepares Te-Zn-Cd monocrystal in large volume
0.96Zn
0.04The infrared transmittivity collection of illustrative plates of Te wafer.
Among the figure, 1. quartz ampoule, 2. low melting point CZT polycrystal, 3. seeding aufwuchsplate, 4. high-melting-point CZT seed crystal, 5. support bar, 6. high-temperature zone, 7. gradient zones, 8. seed crystal bag, 9. cold zone.
Embodiment
Because the ionic and covalency of Cd-Te chemical bond is processed seed crystal according to the theoretical polarity monocrystalline of selecting of bonding, the consideration Atomic coordinate selects the B face as the seeding aufwuchsplate, realizes successful seeding in the CZT crystal.Owing to the increase along with Zn content of the fusing point of CZT increases, therefore can select the high low CZT crystal of CZT seeded growth Zn content of Zn content, thereby can realize melt overheat is overcome heterogeneous forming core, improve CZT monocrystalline volume.The newborn dislocation that produces when eliminating dislocation in the seed crystal and welding is introduced in the newborn crystal and is gone, and has designed suitable seed crystal bag 8.
Embodiment 1: the employing component is Cd
0.8Zn
0.2Te＜111〉crystal orientation seed crystals, the seeding aufwuchsplate is the B face, carries out the seeding growth.
At first, select Cd
0.8Zn
0.2The Te monocrystalline is through orientation cutting, mechanical polishing, process the long 35mm of diameter 10mm＜111〉crystal orientation seed crystals, crystal orientation deviation 40 '.Adopt HNO
3/ HF=3: the solution corrosion of 1 volume ratio preparation 3 seconds, determine A, the B face of seed crystal, and the B face carried out chamfering that to mark, the seeding aufwuchsplate is chosen as the B face.The volume fraction of using the 50ml bromine then is 2% a bromine-methanol soln corrosion seed crystal 5 minutes removing surperficial physical abuse and dirt, the corrosion back washed with methanol seed crystal that finishes.Adopt the dehydrated alcohol ultrasonic cleaning at last 10 minutes, and used N after the taking-up
2Air-blowing is done.
In second step, design quartz ampoule 1 and encapsulate low-melting Cd
0.9Zn
0.1Te polycrystal 2.Design suitable seed crystal bag 8 and make it to closely cooperate, thereby high-temperature fusant corrodes seed crystal when preventing to grow with seed crystal 4.The Design of length of seed crystal bag 8 is than the long 10mm of seed crystal, the newborn dislocation that produces when eliminating dislocation in the seed crystal 4 and welding.Inwall plating carbon film behind quartz ampoule 1 cleaning-drying.Then the seed crystal 4 that processes is put into the seed crystal bag 8 of ampoule bottom, seeding aufwuchsplate 3 is in the top, puts into the low melting point Cd of 79 of purity again
0.9Zn
0.1Te polycrystal 2 will be evacuated in the quartz ampoule 1, when vacuum tightness reaches 6 * 10
-5During Pa, sealing quartz ampoule 1.
In the 3rd step, the quartz ampoule that sealing-in is good is put into ACRT-B N-type waferN growth apparatus and is carried out crystal growth.The heating starting stage rose to 1145 ℃ with high-temperature zone 6 temperature in 20 hours, cold zone 9 temperature rise to 1040 ℃, after reaching target temperature, melt is 6 overheated 16 hours in the high-temperature zone, to eliminate heterogeneous forming core, improve the monocrystalline rate of crystal ingot, place the two ends end to end of seed crystal simultaneously respectively by 2 PtRh10/Rt thermopairs, the seed crystal two ends temperature of real-time monitoring, by rising and decent strut 5, make the upper end temperature of seed crystal be higher than 1125 ℃, and the lower end temperature is lower than 1125 ℃, thereby reach the seed crystal partial melting, realize the seeding growth.The thermograde of having measured the reality in the gradient zones 7 is 8 ℃/cm, thereby the fall off rate of the support bar when determining growth is 0.8mm per hour, and be 240 hours fall time.
The 4th step, in-situ annealing.The back ampoule that stops to descend places growth apparatus, high-temperature zone 6 reduced to 890 ℃ by 1145 ℃ in 6 hours, cold zone 9 temperature are reduced to 890 ℃ by 1040 ℃, and crystal ingot carries out 168 hours in-situ annealing, reducing or to eliminate thermal stresses in the crystal ingot, and reduce all kinds of defectives that produce therefrom.After in-situ annealing finishes, equipment with per hour 5 ℃ slowly be cooled to 550 ℃ after the powered-down air cooling to room temperature.
After measured, the Cd of growth
0.9Zn
0.1Te crystal ingot diameter 60mm is about 140mm, and the monocrystalline volume surpasses 3 * 10
5Mm
3, the monocrystalline rate surpasses 75%, adopts the Agilent4155C tester to test Cd
0.9Zn
0.1The I-V curve (referring to Fig. 2) of Te wafer goes out resistivity by The Fitting Calculation and reaches 1.8 * 10
9～2.6 * 10
10Ω cm, such high resistivity satisfy the requirement of preparation large size high-performance CZT detector fully.
Embodiment 2: the employing component is Cd
0.9Zn
0.1Te＜211〉crystal orientation seed crystals, the seeding aufwuchsplate is the B face, carries out the seeding growth.
At first, select Cd
0.9Zn
0.1The Te monocrystalline is through orientation cutting, mechanical polishing, process the long 30mm of diameter 10mm＜211〉crystal orientation seed crystal, crystal orientation deviation 30 '.Adopt HNO
3/ HF=2: the solution corrosion of 1 volume ratio preparation 4 seconds, determine A, the B face of seed crystal, and the B face carried out chamfering that to mark, the seeding aufwuchsplate is chosen as the B face.The volume fraction of using the 50ml bromine then is 4% a bromine-methanol soln corrosion seed crystal 3 minutes removing surperficial physical abuse and dirt, and the washed with methanol seed crystal is used in the corrosion back that finishes, and adopts the dehydrated alcohol ultrasonic cleaning at last 5 minutes, uses N after the taking-up
2Air-blowing is done.
In second step, design quartz ampoule 1 and encapsulate low-melting Cd
0.96Zn
0.04Te polycrystal 2.Design suitable seed crystal bag 8 and make it to closely cooperate, thereby high-temperature fusant corrodes seed crystal when preventing to grow with seed crystal 4.The Design of length of seed crystal bag 8 is than the long 15mm of seed crystal, the newborn dislocation that produces when eliminating dislocation in the seed crystal 4 and welding.Inwall plating carbon film behind quartz ampoule 1 cleaning-drying.Then the seed crystal 4 that processes is put into the seed crystal bag 8 of ampoule bottom, seeding aufwuchsplate 3 is in the top, puts into the low melting point Cd of 79 of purity again
0.96Zn
0.04Te polycrystal 2 will be evacuated in the quartz ampoule 1, when vacuum tightness reaches 5 * 10
-5During Pa, sealing quartz ampoule 1.
In the 3rd step, the quartz ampoule that sealing-in is good is put into ACRT-B N-type waferN growth apparatus and is carried out crystal growth.The heating starting stage rose to 1135 ℃ with high-temperature zone 6 temperature in 18 hours, cold zone 9 temperature rise to 1030 ℃, after reaching target temperature, melt is overheated 12 hours in the high-temperature zone, to eliminate heterogeneous forming core, improve the monocrystalline rate of crystal ingot, place the two ends end to end of seed crystal simultaneously respectively by 2 PtRh10/Rt thermopairs, the seed crystal two ends temperature of real-time monitoring, by rising and decent strut 5, make the upper end temperature of seed crystal be higher than 1113 ℃, and the lower end temperature is lower than 1113 ℃ of seed crystal partial meltings, realizes the seeding growth.The thermograde of having measured the reality in the gradient zones 7 is 8 ℃/cm, thereby the fall off rate of the support bar when determining growth is 0.8mm per hour, and be 200 hours fall time.
The 4th step, in-situ annealing.The back ampoule that stops to descend places growth apparatus, high-temperature zone 6 reduced to 870 ℃ by 1135 ℃ in 5 hours, cold zone 8 temperature are reduced to 870 ℃ by 1030 ℃, and crystal ingot carries out 144 hours in-situ annealing, reducing or to eliminate thermal stresses in the crystal ingot, and reduce all kinds of defectives that produce therefrom.After in-situ annealing finishes, equipment with per hour 5 ℃ slowly be cooled to 560 ℃ after the powered-down air cooling to room temperature.
After measured, the Cd of growth
0.96Zn
0.04Te crystal ingot diameter 60mm is about 110mm, and the monocrystalline volume surpasses 2 * 10
5Mm
3, the monocrystalline rate surpasses 65%, and the wafer that utilizes the Fourier transformation infrared spectrometer test is at wave number 500cm
-1～4000cm
-1Infrared transmittivity (referring to Fig. 3) is more than 63% in the scope, and the detail bit dislocation density is lower, uniform ingredients, lattice misfit degree are very little, is suitable as excellent Hg
1-xCd
xThe Te epitaxial growth substrate.
In addition to the implementation, also respectively different parameters combination is carried out verification experimental verification, all obtained good effect.
Claims (5)
1. method for preparing Te-Zn-Cd monocrystal in large volume, its feature comprises the steps:
(a) select high-melting-point CZT monocrystalline, through orientation cutting, mechanical polishing, make polarity seed crystal＜111 or＜211, use HNO
3: HF=2: 1～3: the solution corrosion of 1 volume ratio preparation 3～4 seconds, the volume fraction of using bromine then is 2～4% bromine-methanol soln corrosion seed crystal 3～5 minutes, use washed with methanol after corrosion finishes, used the dehydrated alcohol ultrasonic cleaning again 5～10 minutes, use N after the taking-up
2Air-blowing is done;
(b) to the plating of the quartz ampoule inwall behind cleaning-drying carbon film, to put into the seed crystal bag of ampoule bottom through the seed crystal that step (a) is handled then, the seeding aufwuchsplate of seed crystal is put into the low melting point CZT polycrystal of 79 of purity up again, quartz ampoule is vacuumized, when vacuum tightness reaches 5 * 10
-5～6 * 10
-5During Pa, the sealing quartz ampoule;
(c) will put into ACRT-B N-type waferN growth apparatus through the quartz ampoule of step (b) sealing, begin heating, temperature with the high-temperature zone in 18～20 hours rises to 1135～1145 ℃, the cold zone temperature rises to 1030～1040 ℃, after reaching target temperature, after heat 12～16 hours, with the speed decent strut of 0.8mm per hour, be 200～240 hours fall time;
(d) stop to descend after, high-temperature zone and cold zone temperature reduced to 870～890 ℃ in 5～6 hours, after crystal ingot carries out 144～168 hours in-situ annealing, with per hour 5 ℃ slowly be cooled to 550～560 ℃ after the powered-down air cooling to room temperature; Prepared Te-Zn-Cd monocrystal in large volume is that volume surpasses 1 * 10
5Mm
3Monocrystalline.
2. the method for preparing Te-Zn-Cd monocrystal in large volume according to claim 1 is characterized in that: described seed crystal diameter 10mm, long 30～35mm.
3. the method for preparing Te-Zn-Cd monocrystal in large volume according to claim 1 and 2 is characterized in that: described seed crystal crystal orientation deviation is 30～40 '.
4. the method for preparing Te-Zn-Cd monocrystal in large volume according to claim 1 is characterized in that: the length of described seed crystal bag is than the long 10～15mm of seed crystal.
5. the method for preparing Te-Zn-Cd monocrystal in large volume according to claim 1 is characterized in that: by be arranged on seed crystal end to end the thermopair at two ends monitor seed crystal two ends temperature in real time.
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| CN107192660B (en) * | 2017-05-27 | 2023-09-12 | 中国科学院上海技术物理研究所 | Device and method for dynamically observing tellurium-zinc-cadmium material chemical corrosion pits |
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| CN108624949B (en) * | 2018-04-26 | 2021-02-09 | 长安大学 | Preparation method of tellurium-magnesium-cadmium single crystal material, single crystal material and application thereof |
| CN111763984A (en) * | 2020-07-09 | 2020-10-13 | 刘欣 | Structural design of nine-temperature-zone crucible descending furnace |
| CN111893572A (en) * | 2020-08-14 | 2020-11-06 | 南京公诚节能新材料研究院有限公司 | Method for improving uniformity of doping elements of ZnTe crystal |
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