Two, background technology
Existing growing tellurium zinc cadmium crystalline method adopts Bridgman melt growth technology, its roughly technical process (see figure 1): 1, tellurium zinc cadmium batching more, 2, Vacuum Package, 3, the synthetic furnace of packing into, and heating, 4, carry out combination reaction, 5, react the back cooling and generated the tellurium Zn-Cd alloy, 6, pack into crystal growing furnace and heating, 7, move the material pipe and grow into crystal, 8, the back that lowers the temperature takes out crystal, 9, carry out directed sliced crystal, 10, test.But because tellurium zinc cadmium inherent physics, chemistry and control golden characteristic, it is very difficult to allow the alloy crystal ingot be grown to serve as once whole single crystal, and form than the large single crystal body by several often, even on size, just there is not an available single crystal ingot, cause the monocrystalline crystal forming rate lower, have only about 40%, directly have influence on the height of yield rate, yield rate has only about 10%, and the cost that has increased research and production.This growth method causes the low major cause of monocrystalline crystal forming rate: (one) is the one-tenth nuclear volume that can't effectively control the crystal growth starting stage.(2) in numerous nucleus, the growth nucleus of a plurality of Pros and Cons is arranged probably, along with the continuation of growth, they are advanced side by side, and finally cause being made up of a plurality of big or small single crystal, and the large single crystal crystal forming rate is low.
Three, summary of the invention
Main task of the present invention is: according to the defective that the growing tellurium zinc cadmium crystal exists, on the basis of existing bridgeman growth method, improve.Seek a kind of new growth method and prepare tellurium-zincium-cadmium crystal, fundamentally improve the crystal forming rate and the crystal yield rate of large single crystal, effectively reduce production cost.
Main technical schemes of the present invention is; According to selected<110 〉,<211,<100 or<111〉advantage seeding crystal orientation, prepare the seed crystal piece or the rod of certain specification scope, seed crystal is packed at the bottom of the silica tube in the chamber, and the silica tube top tellurium Zn-Cd alloy crystal ingot of packing into carries out the growing tellurium zinc cadmium crystal.
The present invention is by using proof: adopt the seed crystal that presets advantage seeding crystal orientation to grow after the Technology of tellurium-zincium-cadmium crystal, make the monocrystalline crystal forming rate of tellurium Zn-Cd alloy crystal ingot bring up to present more than 65% by original 40%, yield rate improves more than 20% by original 10%, the reduction of first mate's degree production cost.
Five, embodiment
Describe the present invention below in conjunction with drawings and Examples.
Learn that according to analysis of experiments the monocrystalline crystal forming rate and the yield rate that will improve tellurium Zn-Cd alloy crystal ingot must solve two problems, 1, must control the crystal growth starting stage the one-tenth nuclear volume.2, must select to have the seeding crystallographic direction of growth vigor
With reference to Fig. 4, main technical schemes of the present invention be: according to selected<110 〉,<211,<100 or<111〉advantage seeding crystal orientation, prepare the seed crystal piece or the rod of certain specification scope, seed crystal is packed at the bottom of the silica tube in the chamber 1, the silica tube 3 tops tellurium Zn-Cd alloy crystal ingot 5 of packing into carries out the growing tellurium zinc cadmium crystal.
Crystal orientation described in the scheme, be to represent universally recognized in the world crystallographic direction, if a crystal has in individual direction, wherein<110 〉,<211,<100 or<111 represented be that the present invention is selected by test of many times, the most effective dominant growth crystal orientation in the crystal growing process.
Processing method with reference to preparation seed crystal among Fig. 2, the present invention is: A, on the Te-Zn-Cd monocrystal that a size meets the demands cuts a reference plane.B, grinding and polishing reference plane are to the minute surface light.C, decide the crystal orientation with X-ray diffractometer to the reference plane orientation, and find out required<110,<211,<100 or<111〉crystal orientation and reference plane between positions such as angle relations.D, according to the directed seed crystal piece that cuts out required size of position relation.E, according to the size and the tolerance in quartz material pipe seed crystal chamber, grind the seed crystal piece.F, the seed crystal piece is carried out comprehensive test by technical requirements.
Operation A, cut reference plane, generally adopt inside diameter slicer or wire drawing cutting machine.
Process B, E, grinding and polishing reference plane and grind the seed crystal piece generally adopts varigrained silicon carbide and diamond wheel.
With reference to Fig. 3,4, the concrete processing method that usefulness of the present invention presets the seeded growth tellurium-zincium-cadmium crystal in advantage seeding crystal orientation is: G, clean the seed crystal piece, wash metallics and other dirt of seed crystal face with the chemical burn into.H, seed crystal piece 2 is packed at the bottom of the silica tube in the chamber 1, seeded growth advantage crystal orientation 4 upwards, seed crystal 2 about half in chamber at the bottom of the silica tube 1, about second half in silica tube 3.I, in silica tube 3, pack into and prepare burden and synthetic good tellurium Zn-Cd alloy crystal ingot 5.J, silica tube is carried out Vacuum Package.K, with the silica tube crystal growing furnace of packing into, and be warmed to 1100-1150 ℃ of high temperature.L, mobile quartzy material pipe generate crystal, then are cooled to room temperature.M, taking-up crystal.N, carry out directed sliced crystal.O, test by technical requirements.
Operation G cleans the seed crystal piece, required auxiliary material: pure water, cleaning essence, toluene, acetone, ethanol, bromine etc.
Operation J, Vacuum Package, required equipment: vacuum unit.
With reference to Fig. 3,4, operation K, L, silica tube packed into generates crystal in the crystal growing furnace, before crystal growth begins, must guarantee the fusing of seed crystal 2 epimeres, and hypomere can not melt.
With reference to Fig. 3, to the description of two other embodiment of the present invention.
1, other operation and condition are constant, only in operation K, L, and when heating to 1100 ℃, growing crystal, the monocrystalline crystal forming rate reaches 65%, and yield rate reaches 20%.
2, other operation and condition are constant, only in operation K, L, and when heating to 1150 ℃, growing crystal, the monocrystalline crystal forming rate reaches 66%, and yield rate reaches 20%.
With reference to Fig. 4, groundwork principle of the present invention: utilize the seed crystal that presets with advantage seeding crystal orientation, making crystal growth is nucleus and along advantage crystal orientation 4 growth of seed crystal at the very start with the seed crystal, finally grows up to a main large single crystal body, thereby has improved the crystal forming rate and the yield rate of monocrystalline.
The present invention adopts the seed crystal the preset advantage seeding crystal orientation tellurium-zincium-cadmium crystal of growing. and every with this technology similar crystal that is used to grow, all at the row of protection.