CN114086251A - Preparation method of high-electrical-uniformity low-resistance CdS polycrystalline material - Google Patents
Preparation method of high-electrical-uniformity low-resistance CdS polycrystalline material Download PDFInfo
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- CN114086251A CN114086251A CN202111457402.0A CN202111457402A CN114086251A CN 114086251 A CN114086251 A CN 114086251A CN 202111457402 A CN202111457402 A CN 202111457402A CN 114086251 A CN114086251 A CN 114086251A
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- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000010453 quartz Substances 0.000 claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 20
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 13
- 239000010980 sapphire Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 5
- 235000012431 wafers Nutrition 0.000 description 17
- 238000000034 method Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 10
- 229910052793 cadmium Inorganic materials 0.000 description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Classifications
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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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
-
- 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
- C30B29/50—Cadmium sulfide
Abstract
The invention relates to a preparation method of a CdS polycrystal material with high electrical uniformity and low resistance, wherein a cylindrical support structure is arranged on the left side in a quartz tube, a sapphire substrate is arranged close to the right side of the cylindrical support structure, a cadmium sulfide raw material quartz boat I is arranged in the middle, a quartz boat II for placing a Cd simple substance is arranged on the right side, a flange with an air outlet and a flange with an air inlet are respectively sealed at the left opening and the right opening of the quartz tube, the quartz tube (1) is horizontally placed in a three-temperature-zone resistance heating furnace, the CdS polycrystal material with good uniformity is obtained on the left side of the quartz tube through heating, constant temperature and cooling treatment in the environment, the resistivity results obtained through testing all meet the requirements of the range of 0.1-5 omega cm, and the resistivity deviation of different regions is less than 20%.
Description
Technical Field
The invention relates to a preparation method of a polycrystalline material for growing low-resistance CdS by a PVT method, in particular to a preparation method of a CdS polycrystalline material with high electrical uniformity and low resistance.
1. Background of the invention
CdS is a II-VI family wide band gap direct transition semiconductor material, has good photoelectric effect, and has been widely used in the fields of infrared/ultraviolet double-color detection and the like due to the characteristics of sensitivity to ultraviolet light and partial visible light and good infrared light transmission. At present, CdS mainly grows crystals by a physical vapor transport method (PVT), and because intrinsic CdS crystals which grow directly are usually in a high-resistance state, the use requirements of an infrared/ultraviolet double-color laminated detector cannot be met. In order to prepare the low-resistance CdS wafer, two common methods are adopted at present, firstly, the wafer is annealed in a sealing system under a Cd atmosphere to realize the preparation of the low-resistance CdS single wafer, but the problems of more complicated steps and longer time consumption exist due to low annealing diffusion speed, and the concentration of annealing atmosphere is changed due to the change of the quality of Cd in the annealing process, so that the uniformity and the consistency of the wafer are poor; secondly, a cadmium simple substance is directly mixed in cadmium sulfide powder to be used as growth source powder to carry out single crystal growth, because the volatilization temperature of the cadmium simple substance is far lower than the volatilization temperature of cadmium sulfide, the cadmium simple substance is volatilized into gas firstly in the temperature rising process, the cadmium sulfide powder is changed into gas to be mixed with cadmium vapor for crystallization after the temperature rising is continued to reach the volatilization temperature of the cadmium sulfide, the cadmium simple substance is gradually consumed along with the crystallization process of the crystal, the concentration of cadmium atmosphere in the crystal growth process is inconsistent, the axial resistivity of the crystal is changed, and the yield of the wafer is seriously influenced.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a preparation method of a CdS polycrystalline material with high electrical uniformity and low resistance.
The specific technical scheme is that the preparation method of the CdS polycrystalline material with high electrical uniformity and low resistance is characterized by comprising the following steps of: the preparation method comprises the following steps of (I) charging, placing a Cd simple substance (8) on a quartz boat II (9), placing a cadmium sulfide raw material (6) on a quartz boat I (7), in a quartz tube (1), a cylindrical support structure (5) is arranged on the left side, a sapphire substrate (4) is arranged close to the right side of the cylindrical support structure (5), a quartz boat I (7) is arranged in the middle, a quartz boat II (9) is arranged on the right side, a flange with an air outlet (11) and a flange with an air inlet (10) are respectively sealed at the left opening and the right opening of the quartz tube (1) to form a growth device, the quartz tube (1) is horizontally placed into a three-temperature-zone resistance heating furnace, so that a cadmium sulfide raw material (6) is placed in a second temperature zone of 1050-1100 ℃ in the middle of the three-temperature-zone resistance heating furnace, a simple substance Cd (8) is placed in a third temperature zone of 300-350 ℃, and the sapphire substrate (4) is placed in a first temperature zone of 1000-1050 ℃; vacuumizing, namely keeping the air inlet (11) of the right end flange of the quartz tube (1) closed, opening the air outlet (10) of the left end flange, vacuumizing for 20min, and removing air in the quartz tube; heating, namely opening an air inlet (10) of a flange at the right end of the quartz tube (1), continuously and slowly introducing argon into the quartz tube (1), slowly heating the first temperature zone and the second temperature zone at a heating speed of 2 ℃/min, slowly heating the third temperature zone at a heating speed of 0.5 ℃/min, raising the temperature of the first temperature zone of the resistance heating furnace of the three temperature zones to 980 ℃, raising the temperature of the second temperature zone to 1080 ℃, raising the temperature of the Cd elementary substance zone to 350 ℃, and raising the pressure of argon gas to 200 mbar; fourthly, keeping the temperature constant for 150 hours, keeping the pressure in the quartz tube (1) balanced at 200mbar, crystallizing the CdS polycrystal material and the Cd simple substance in the quartz tube (1) at the sapphire substrate (4), growing low-resistance CdS polycrystal, (fifthly), cooling, after the temperature is kept constant, filling argon into the quartz tube (1) to 1000mbar, keeping the pressure, and cooling the furnace body to room temperature after 8 hours, thus obtaining the low-resistance CdS polycrystal material with good uniformity at the left side of the quartz tube;
and (VI) detecting, namely selecting different regions of the same layer of wafer to carry out resistivity test, wherein the resistivity results obtained by the test all meet the requirement of the range of 0.1-5 omega-cm, and the resistivity deviation of the different regions is less than 20%.
The invention has the beneficial effects that the CdS polycrystal material with high electrical uniformity and low resistance is directly produced by adopting a PVT method, the polycrystal material is utilized for crystal growth, the resistivity of the wafer at the initial growth stage and the final growth stage of the crystal is tested, the resistivity range meets the requirement of 0.1-5 omega-cm, and the resistivity deviation of the wafers at different layers is less than 30%. And selecting different regions of the same layer of wafer to perform resistivity test, wherein the resistivity results obtained by the test all meet the requirement of the range of 0.1-5 omega cm, and the deviation of the resistivity of the different regions is less than 20%.
Drawings
FIG. 1 is a schematic diagram of the results of the crystal growing apparatus of the present invention;
FIG. 2 is a diagram of resistivity test positions of different regions of a wafer of the same layer of polycrystalline material grown according to the present invention.
Detailed Description
The invention is further explained by the figures and the examples.
Example one
A preparation method of CdS polycrystal material with high electrical uniformity and low resistance comprises the following steps,
charging furnace
10g of Cd elementary substance (8) is placed on a quartz boat II (9), about 150g of cadmium sulfide raw material (6) is placed on a quartz boat I (7), a cylindrical support structure (5) is placed on the left side in a quartz tube (1), a sapphire substrate (4) is placed close to the right side of the cylindrical support structure (5), the quartz boat I (7) is placed in the middle, the quartz boat II (9) is placed on the right side, the distance between the quartz boat 7 and the sapphire substrate (4) is 15cm, the distance between the quartz boat II (9) and the quartz boat 7 is 25cm, a flange with an air outlet (10) and a flange with an air inlet (11) are respectively sealed at the left opening and the right opening of the quartz tube (1), the quartz tube (1) is horizontally placed in a three-temperature-zone resistance heating furnace, the cadmium sulfide raw material (6) is placed in a second temperature zone of 1050 ℃ -1100 ℃ in the middle of the three-temperature-zone resistance heating furnace, the Cd elementary substance (8) is placed in a third temperature zone of 300 ℃ -350 ℃, the sapphire substrate (4) is placed in a first temperature zone of 1000-1050 ℃;
(II) vacuumizing
Keeping the air inlet (11) of the right end flange of the quartz tube (1) closed, opening the air outlet (10) of the left end flange, vacuumizing for 20min, and removing the air in the quartz tube;
(III) increasing the temperature
Opening an air inlet (11) with a flange at the right end of a quartz tube (1), continuously and slowly introducing argon into the quartz tube (1), simultaneously slowly heating a first temperature zone and a second temperature zone at a heating rate of 2 ℃/min, slowly heating a third temperature zone at a heating rate of 0.5 ℃/min, raising the temperature of the second temperature zone of a resistance heating furnace of the third temperature zone to 980 ℃, raising the temperature of the third temperature zone to 1080 ℃, raising the temperature of a Cd elementary substance zone to 350 ℃, and keeping the pressure of the argon at 200 mbar;
(IV) constant temperature
Keeping the temperature for 150 hours, keeping the pressure in the quartz tube (1) balanced at 200mbar, crystallizing the CdS polycrystal material and the Cd simple substance in the quartz tube (1) at the sapphire substrate (4) to grow low-resistance CdS polycrystal,
(V) temperature reduction
After the constant temperature is finished, filling argon into the quartz tube (1) to 1000mbar, keeping the pressure, and reducing the furnace body to room temperature after 8 hours, thus obtaining the low-resistance CdS polycrystal material with good uniformity on the left side of the quartz tube;
(VI) detection
Selecting different areas of the same layer of wafer to carry out resistivity test, wherein the resistivity results obtained by the test all meet the requirement of the range of 0.1-5 omega-cm, and the deviation of the resistivity of the different areas is 17.9%.
As shown in FIG. 2, the resistivity of the wafer in different regions is measured at selected positions, and the resistivity of the wafer in 1-5 regions is 1.30 Ω -cm, 1.33 Ω -cm, 1.47 Ω -cm, 1.36 Ω -cm and 1.24 Ω -cm, respectively.
Example two
A preparation method of a CdS polycrystalline material with high electrical uniformity and low resistance is the same as that in example 1, and is characterized in that during growth, the temperature of a second temperature zone is 1000 ℃, the temperature of a third temperature zone is 1100 ℃, the temperature of the third temperature zone is 300 ℃, and the pressure of argon is 300 mbar.
As shown in FIG. 2, after cooling down, the resistivity of the wafer in the same layer is measured at different selected positions, and the resistivity of the wafer in the 1-5 regions is 3.26, 3.29 Ω. cm, 3.44 Ω. cm, 3.77 Ω. cm, and 3.72 Ω. cm, respectively.
EXAMPLE III
A preparation method of a CdS polycrystalline material with high electrical uniformity and low resistance is the same as that in example 1, except that before growth, 20gCd simple substance and 200g of cadmium sulfide raw material are put in, and the growth time is 200 h. As shown in FIG. 2, after cooling down, the resistivity of the wafer in different regions is measured at selected positions, and the resistivity of the wafer in 1-5 regions is 0.83 Ω -cm, 0.77 Ω -cm, 0.88 Ω -cm, 0.93 Ω -cm and 0.86 Ω -cm, respectively.
And continuously introducing inert gas in the growth process, heating the Cd simple substance, the cadmium sulfide polycrystal raw material and the sapphire substrate in the growth process, carrying cadmium steam by using the inert gas by heating the Cd simple substance, mixing the cadmium steam with the volatilized cadmium sulfide gas in the transportation process, and finally crystallizing at the sapphire substrate to grow the low-resistance CdS polycrystal, wherein the electrical uniformity of the crystal is good.
Claims (1)
1. A preparation method of CdS polycrystal material with high electrical uniformity and low resistance is characterized in that: the preparation method comprises the following steps of,
charging furnace
Placing a Cd elementary substance (8) on a quartz boat II (9), placing a cadmium sulfide raw material (6) on a quartz boat I (7), placing a cylindrical support structure (5) on the left side in a quartz tube (1), placing a sapphire substrate (4) close to the right side of the cylindrical support structure (5), placing the quartz boat I (7) in the middle, placing the quartz boat II (9) on the right side, respectively sealing the left opening and the right opening of the quartz tube (1) by using a flange with an air outlet (10) and a flange with an air inlet (11), horizontally placing the quartz tube (1) into a three-temperature-zone resistance heating furnace, placing the cadmium sulfide raw material (6) in a second temperature zone of 1050-1100 ℃ in the middle of the three-temperature-zone resistance heating furnace, placing the Cd elementary substance (8) in a third temperature zone of 300-350 ℃, and placing the sapphire substrate (4) in a first temperature zone of 1000-1050 ℃;
(II) vacuumizing
Keeping an air inlet (11) with a flange at the right end of the quartz tube (1) closed, opening an air outlet (10) with a flange at the left end, vacuumizing for 20min, and removing air in the quartz tube;
(III) increasing the temperature
Opening an air inlet (11) with a flange at the right end of a quartz tube (1), continuously and slowly introducing argon into the quartz tube (1), simultaneously slowly heating a first temperature zone and a second temperature zone at a heating rate of 2 ℃/min, slowly heating a third temperature zone at a heating rate of 0.5 ℃/min, raising the temperature of the second temperature zone of a resistance heating furnace of the third temperature zone to 980 ℃, raising the temperature of the third temperature zone to 1080 ℃, raising the temperature of a Cd elementary substance zone to 350 ℃, and keeping the pressure of the argon at 200 mbar;
(IV) constant temperature
Keeping the temperature for 150 hours, keeping the pressure in the quartz tube (1) balanced at 200mbar, crystallizing the CdS polycrystal material and the Cd simple substance in the quartz tube (1) at the sapphire substrate (4) to grow low-resistance CdS polycrystal,
(V) temperature reduction
After the constant temperature is finished, filling argon into the quartz tube (1) to 1000mbar, keeping the pressure, and reducing the furnace body to room temperature after 8 hours, thus obtaining the low-resistance CdS polycrystal material with good uniformity on the left side of the quartz tube;
(VI) detection
Selecting different areas of the same layer of wafer to carry out resistivity test, wherein the resistivity results obtained by the test all meet the requirement of the range of 0.1-5 omega cm, and the deviation of the resistivity of the different areas is less than 20%.
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|---|---|---|---|---|
| FR1371137A (en) * | 1963-10-14 | 1964-08-28 | Bayer Ag | Process for the preparation of very pure chalcogenides of zinc and cadmium |
| US3362795A (en) * | 1962-10-13 | 1968-01-09 | Bayer Ag | Production of highly pure hexagonal crystals of cadmium and zinc chalkogenides by sublimation |
| US4190486A (en) * | 1973-10-04 | 1980-02-26 | Hughes Aircraft Company | Method for obtaining optically clear, high resistivity II-VI, III-V, and IV-VI compounds by heat treatment |
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