CN102230213B - Method for growing tellurium-zinc-cadmium crystals by using tellurium solvent solution method - Google Patents
Method for growing tellurium-zinc-cadmium crystals by using tellurium solvent solution method Download PDFInfo
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- CN102230213B CN102230213B CN201110150914A CN201110150914A CN102230213B CN 102230213 B CN102230213 B CN 102230213B CN 201110150914 A CN201110150914 A CN 201110150914A CN 201110150914 A CN201110150914 A CN 201110150914A CN 102230213 B CN102230213 B CN 102230213B
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Abstract
The invention relates to a method and a device for growing tellurium-zinc-cadmium crystal by using a tellurium solvent solution method, which belong to the technical field of the growth of special crystals. The method is characterized by comprising the following steps: adding high purity raw materials with purification of 7N of Cd, Zn, Te of which the stoichiometric proportion satisfies Cd1-xZnxTe (x=0.04 to 0.5) into a quartz crucible, adding 30 to 80% mass percentage of excessive tellurium(Te), respectively vacuumizing and sealing and synthesizing materials in a rocking furnace; placing the quartz crucible after synthesizing into a crystal growth apparatus, wherein due to an addition of excessive Te, the growth temperature of the crystals decreases from 1092 DEG C - 1295 DEG C to 700 DEG C - 900 DEG C; putting quartz crucible in a high-temperature region before the crystal growth process is performed, maintaining the tellurium-zinc-cadmium polycrystalline and a solvent Te in the quartz crucible in a liquid phase, raising the furnace body at a speed of 0.04 to 2mm/h, wherein temperature gradient of a temperature gradient zone is from 15 to 25 DEG C/cm, decreasing the saturation of tellurium-zinc-cadmium in the solution with the decreasing temperature, continuously saturating and precipitating tellurium-zinc-cadmium crystals at the bottom of the crucible, using different donor dopings (In, C1-1,A1 and the like) for raising the resistivity of tellurium-zinc-cadmium crystals, thereby producing a detector grade tellurium-zinc-cadmium crystals. According to the invention, the crystals growth temperature, impurity concentration in crystals and defect density of crystals are substantially reduced.
Description
Technical field
The present invention relates to a kind of tellurium solvent solution method growing tellurium zinc cadmium crystalline method, belong to special crystal growth technique technical field.
Background technology
Tellurium zinc cadmium Cd
1-xZn
xTe (CZT) is a kind of semiconductor material with wide application prospect, and the preparation of its monocrystal material gets more and more people's extensive concerning always.Because its energy gap energy gap of CdZnTe (CZT) single crystal big (Eg=1.70eV), staple Cd, the Te ordination number is high, resistivity is high by (10
11Ω cm), electronics and void migration rate big (
μE=1100cm/Vs,
μH=100cm/Vs), wide (10keV～6MeV), energy resolution are high, anti-neutron and proton irradiation damage threshold are also higher for the energy investigative range; So the CZT detector has bigger uptake factor, higher CR; Especially do not need any cooling apparatus just can at room temperature work, thereby volume is less, it is convenient to use.But the growth difficulty of CdZnTe single crystal itself is big; And because the generation external environment of various environmental factorss restriction generation difficulty is bigger, crystal mass is difficult to reach the industrial standards that general commercial user formulates for detector usually in the process of growth of protocrystal.At present, the widespread use of CZT detector mainly receives the restriction of several respects such as crystal property, volume and cost, and the crystalline preparation method adopts high pressure Bridgman method or improved vertical bridgman method growth CZT crystal.
Nearest discovers; Impurity is enriched among the Te (being that Te is mingled with or inclusion) that exists with inclusion usually more easily in the CZT of rich Te crystal; The solution growth that for this reason adopts tellurium to make solvent can utilize the Te solvent that but the adsorption of impurity is stayed impurity in solvent, thereby improves crystalline purity.In addition, the crystalline growth temperature can drop to 700～900 ℃ from 1092 ℃～1295 ℃ original (difference according to the Zn component changes), and this will greatly reduce from the pollution to melt of the impurity of quartz crucible.In addition, low temperature is growth down, has reduced the thermodiffusion of crucible and has polluted, and reduced thermal stresses, and dislocation desity is lower.Tellurium solution growth method under the thermograde has the advantage of himself; Growth temperature is low, and the speed of growth is faster than travelling heating method (THM), and the synthetic of polycrystal is grown in the same quartz crucible with crystalline; Reduced the impurity that the secondary charging is introduced, and technology is simple etc.
Summary of the invention
The purpose of this invention is to provide a kind of tellurium solvent solution legal system and be equipped with Cd
1-xZn
xTe (x=0.04～0.5) crystalline method.The present invention can prepare tellurium-zincium-cadmium crystal under 700～900 ℃ temperature.Rich more Te in quartz crucible (rich Te30wt%～80wt%) as solvent; Because the adding of excessive Te makes tellurium-zincium-cadmium crystal separate out temperature and significantly reduces, along with moving of body of heater; When making quartz crucible through temperature gradient zone; Along with the saturation ratio decline of tellurium zinc cadmium in the reduction Te solvent of temperature, the saturated solution of low-temperature end is separated out tellurium-zincium-cadmium crystal, and promptly the crucible bottom grows tellurium-zincium-cadmium crystal.Adopt growing tellurium zinc cadmium crystal of the present invention significantly to reduce the defect concentration in the impurity concentration and crystal in crystalline growth temperature, the crystal; Adopt the method for donor doping to improve the resistivity of tellurium-zincium-cadmium crystal simultaneously, thereby grow the tellurium-zincium-cadmium crystal of detector grade.
The present invention adopts following technical scheme.
A kind of tellurium solvent solution of the present invention method growing tellurium zinc cadmium crystalline method is characterized in that having following technological process and step:
A. according to stoichiometric, will satisfy chemical formula Cd
1-xZn
xThe purity of x=0.04 among the Te～0.5 is that high-purity Cd, Zn, the Te raw material of 7N packed in the most advanced and sophisticated angled high-purity silica pot, and 30%～80% excessive Te of extra again adding raw materials quality summation is evacuated to 2.0 * 10
-4Sealing by fusing quartz crucible behind the Pa;
B. the above-mentioned quartz crucible that the polycrystal mixture of tellurium zinc cadmium is housed is put into and waved stove and carry out building-up reactions, obtain the mixture of tellurium zinc cadmium polycrystalline and solvent Te; Be warming up to 500 ℃ of insulation 3h slowly, and then be warming up to 1000 ℃ of insulation 24h slowly, wave stove in the process of insulation and slowly shake the raw material that makes in the quartz crucible and fully react, room temperature, end of synthesis are put in cooling slowly subsequently;
C. the quartz crucible of above-mentioned end of synthesis is put into crystal growing furnace; The high-temperature zone temperature of crystal growing furnace is set to 850～950 ℃; The cold zone temperature is set to 500～600 ℃; The temperature gradient zone temperature is set to 800～900 ℃, and the thermograde that makes its temperature gradient zone is at 15-25 ℃/cm; Before crystal growing process begins, quartz crucible is in high-temperature zone insulation 24h, makes its inner tellurium zinc cadmium polycrystalline and solvent Te all be in liquid phase; The adjustment body of heater subsequently with the speed rising body of heater of 0.04～2mm/h, guarantees that simultaneously support bar keeps transfixion; Be equivalent to quartz crucible and descend, during through temperature gradient zone, along with the reduction of temperature with identical speed; The saturation ratio of tellurium zinc cadmium descends in the Te solvent; When temperature drops to one regularly, the saturated tellurium zinc cadmium of separating out of the saturated solution of low-temperature end, promptly the crucible bottom grows tellurium-zincium-cadmium crystal; When the whole temperature gradient zone of quartz crucible process, growth ending, saturated the separating out of most of tellurium zinc cadmium in the solution forms tellurium zinc cadmium crystal ingot, and afterbody then is the CdZnTe-Te mixture;
D. the crystal ingot with growth ending takes out from quartz crucible, removes the CdZnTe-Te mixture of afterbody, and fore-end is the tellurium-zincium-cadmium crystal that freely selects crystalline substance that tellurium solvent solution method grows.Be prone in the crystal growing process produce receive major defects Cd room, a large amount of Cd rooms can significantly reduce crystalline resistivity in the tellurium-zincium-cadmium crystal, make crystal be p type conduction.Through introducing donor doping (In, Cl
-1, Al etc.), thereby compound Cd room reaches the purpose that improves resistivity.
The used isolated plant of this employing Te solvent solution method growing tellurium zinc cadmium crystalline method comprises body of heater, quartz crucible, support bar; It is characterized in that: body of heater is the three-temperature-zone process furnace, and high-temperature zone, gradient zones and cold zone, body of heater can realize that speed is from 0.02～2mm/h; 0.01 the vertical shifting that progress is adjustable; The thermograde in growth gradient district will be between 15-25 ℃/cm, and support bar adopts upper end hollow, band tapering alundum tube; The upper end tapering guarantees to be complementary with the quartz crucible head, guarantees the stable support quartz crucible.
The characteristics of the inventive method are:
The crystalline growth temperature can drop to 700～900 ℃ from original 1092 ℃～1295 ℃; This will greatly reduce from the pollution to melt of the impurity of quartz crucible; And synthetic and the crystalline of polycrystal are grown in the same quartz crucible; Reduced the impurity that the secondary charging is introduced, technology is simple, and what is more important can improve the quality and the performance of Te-Zn-Cd monocrystal.
Description of drawings
Fig. 1 is tellurium solvent solution method growing tellurium zinc cadmium crystalline growing apparatus and growing principle synoptic diagram.
Embodiment
Embodiment one
Tellurium-zincium-cadmium crystal growth of the present invention realizes through tellurium solvent solution method.
Referring to Fig. 1; Used tellurium-zincium-cadmium crystal growing apparatus comprises body of heater 1, quartz crucible 2, support bar 3 among the present invention: wherein body of heater 1 is divided into three sections heating; High-temperature zone 4, temperature gradient zone 5 and cold zone 6, the thermograde of temperature gradient zone 5 will be between 15-25 ℃/cm; Raw material is packed into and is vacuumized the back sealing by fusing in the quartz crucible 2; The quartz crucible 2 of charging placed wave stove and close material; Then quartz crucible 2 is placed on the support bar 3 crystal growing furnace and its coupling, to guarantee that quartz crucible 2 is in vertical steady state; The quartz crucible 2 initial high-temperature zone 4 insulation 24h that are in make its inner tellurium zinc cadmium polycrystalline and solvent Te all be in liquid phase; During the growth beginning; Body of heater 1 rises with certain speed; Quartz crucible is through temperature gradient zone 5, and the solubleness of solution lower region descends along with the reduction of temperature, when temperature drops to one regularly; Tellurium zinc cadmium saturated separating out from solution grows tellurium-zincium-cadmium crystal 8, top solution is to be the CZT saturated solution 7 of solvent with Te.
The concrete process step of instance of the present invention is described below:
(1) at first will satisfy the Cd of stoichiometric
0.9Zn
0.1The 7N high pure raw material of Te is packed in the high-purity silica pot, is evacuated to 2.0 * 10 behind 50% the excessive Te of extra again adding raw materials quality sum
-4Sealing by fusing behind the Pa puts into that to wave stove synthetic, obtains the mixture of tellurium zinc cadmium polycrystalline and solvent Te;
The quartz crucible 2 that (2) synthesis material will be housed places on the support bar 3 that matches, and guarantees that quartz crucible is 2 vertical, steadily;
(3) position of adjustment body of heater 1, it is good to make quartz crucible 2 be in the high-temperature zone 4 insulation 24, makes its inner material all be in liquid phase, and the lift velocity that body of heater 1 is set when beginning to grow is 0.4mm/h.Treat quartz crucible all through behind the temperature gradient zone, growth ending.Take out crystal, remove the remaining Te as solvent of afterbody, fore-end is the tellurium-zincium-cadmium crystal that freely selects crystalline substance that tellurium solvent solution method grows.
Embodiment two
Present embodiment adopts same growing apparatus in the foregoing description one.
Growth technique step and the foregoing description one in the present embodiment are identical, and different is to have changed some processing parameters.Its different parameter is: the rich Te amount in (1) raw mix is 70% of raw materials quality sum; Finally obtain tellurium-zincium-cadmium crystal.
Embodiment three
Present embodiment adopts same growing apparatus in the foregoing description one.
Growth technique step and the foregoing description one in the present embodiment are identical, and different is to have changed some processing parameters.Its different parameter is: the lift velocity of body of heater 1 is set to 0.8mm/h.Finally obtain tellurium-zincium-cadmium crystal.
Embodiment four
Present embodiment adopts same growing apparatus in the foregoing description one.
Growth technique step and the foregoing description one in the present embodiment are identical, and different is to have changed some processing parameters.Its different parameter is: press Cd
0.8Zn
0.2The weighing recently of the stoichiometry of Te, 50% excessive Te of extra again adding raw materials quality sum.Finally obtain tellurium-zincium-cadmium crystal.
Embodiment five
Present embodiment adopts same growing apparatus in the foregoing description one.
Growth technique step and the foregoing description one in the present embodiment are identical, and different is to have changed some processing parameters.Its different parameter is: the doping (In or the Cl that in the material of weighing, add 100ppm
-1, or Al), finally obtain tellurium-zincium-cadmium crystal.
Adopt tellurium solvent solution method growing tellurium zinc cadmium crystalline apparatus and method of the present invention; Simple to operate, reduced crystal growth temperature, reduced the pollution of impurity; The existence of the process of growth has simultaneously been played the effect of purifying to crystal; The highly purified tellurium-zincium-cadmium crystal of final acquisition adopts adulterated method to improve crystalline resistivity simultaneously, meets the requirement as material for detector fully.
Claims (1)
1. tellurium solvent solution method growing tellurium zinc cadmium crystalline method is characterized in that having following technological process and step:
A. according to stoichiometric, will satisfy chemical formula Cd
1-xZn
xThe purity of x=0.04 among the Te ~ 0.5 is that high-purity Cd, Zn, the Te raw material of 7N packed in the most advanced and sophisticated angled high-purity silica pot; 30%～80% excessive Te of extra again adding raw materials quality summation; Carry out donor doping simultaneously,, be evacuated to 2.0 * 10 then to improve crystalline resistivity
-4Sealing by fusing quartz crucible behind the Pa obtains the mixture of tellurium zinc cadmium polycrystalline and solvent Te;
B. the above-mentioned quartz crucible that the polycrystal mixture of tellurium zinc cadmium is housed is put into and waved stove and carry out building-up reactions; Slowly be warming up to 500 ℃ of insulation 3h; And then slowly be warming up to 1000 ℃ the insulation 24h; Wave stove in the process of insulation and slowly shake the raw material that makes in the quartz crucible and fully react, be cooled to room temperature, end of synthesis subsequently slowly;
C. the quartz crucible of above-mentioned end of synthesis is put into crystal growing furnace; The high-temperature zone temperature of crystal growing furnace is set to 850～950 ℃; The cold zone temperature is set to 500～600 ℃; The temperature gradient zone temperature is set to 800～900 ℃, and the thermograde that makes its temperature gradient zone is at 15-25 ℃/cm; Before crystal growing process begins, quartz crucible is in high-temperature zone insulation 24h, makes its inner tellurium zinc cadmium polycrystalline and solvent Te all be in liquid phase; The adjustment body of heater subsequently with the speed rising body of heater of 0.04～2mm/h, guarantees that simultaneously support bar keeps transfixion; Be equivalent to quartz crucible and descend, during through temperature gradient zone, along with the reduction of temperature with identical speed; The saturation ratio of tellurium zinc cadmium descends in the Te solvent; When temperature drops to one regularly, the saturated tellurium zinc cadmium of separating out of the saturated solution of low-temperature end, promptly crucible bottom grows tellurium-zincium-cadmium crystal; When the whole temperature gradient zone of quartz crucible process, growth ending, saturated the separating out of most of tellurium zinc cadmium in the solution forms tellurium zinc cadmium crystal ingot, and afterbody then is tellurium zinc cadmium-Te mixture;
D. the crystal ingot with growth ending takes out from quartz crucible, removes the tellurium zinc cadmium-Te mixture of afterbody, and fore-end is the tellurium-zincium-cadmium crystal that freely selects crystalline substance that tellurium solvent solution method grows.
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| CN201110150914A CN102230213B (en) | 2011-06-08 | 2011-06-08 | Method for growing tellurium-zinc-cadmium crystals by using tellurium solvent solution method |
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| CN201110150914A CN102230213B (en) | 2011-06-08 | 2011-06-08 | Method for growing tellurium-zinc-cadmium crystals by using tellurium solvent solution method |
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| CN102703983A (en) * | 2012-06-15 | 2012-10-03 | 上海大学 | Method and device for compressing free space in cadmium zinc telluride crystal growing crucible through double sealing sleeves |
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| CN114481329B (en) * | 2020-10-26 | 2023-11-14 | 昆明物理研究所 | Omnidirectional multi-section heating control tellurium-zinc-cadmium crystal growth furnace and crystal growth method |
| CN114481327B (en) * | 2020-10-26 | 2023-11-21 | 昆明物理研究所 | Method and device for synthesizing tellurium-zinc-cadmium crystal by adopting PBN crucible |
| CN114197041A (en) * | 2021-12-14 | 2022-03-18 | 苏州科睿浦光电科技有限公司 | Preparation method of trititanium pentoxide polycrystal material and trititanium pentoxide polycrystal material |
| CN114808134A (en) * | 2022-03-28 | 2022-07-29 | 安徽承禹半导体材料科技有限公司 | Preparation process of tellurium-zinc-cadmium single crystal wafer |
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