CN104047047B - A kind of horizontal growth device of phosphorus silicon Cd monocrystal and growing method - Google Patents
A kind of horizontal growth device of phosphorus silicon Cd monocrystal and growing method Download PDFInfo
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- CN104047047B CN104047047B CN201410253222.4A CN201410253222A CN104047047B CN 104047047 B CN104047047 B CN 104047047B CN 201410253222 A CN201410253222 A CN 201410253222A CN 104047047 B CN104047047 B CN 104047047B
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Abstract
The invention discloses a kind of horizontal growth device of phosphorus silicon Cd monocrystal and growing method, belong to phosphorus silicon Cd monocrystal preparing technical field.Described device includes outer layer quartz ampoule, the layered quartz tube being sleeved in outer layer quartz ampoule and the PBN navicular crucibles being sleeved in layered quartz tube.PBN navicular crucibles include：Nucleus growth section, changeover portion and the crystal growth section being sequentially connected with, by the first end of nucleus growth section is arranged to pinnacle shape, the homogeneity of crystal orientation when improving spontaneous nucleation.Designed by double-deck quartz ampoule, make between quartz ampoule, to be filled with inert gas, solve the problems, such as the booster easily occurred in crystal growing process, improve thermal field stability and grower durability.Methods described prepares phosphorus silicon Cd monocrystal by using horizontal gradient freezing method in the horizontal crystal growth stove for being placed with above-mentioned grower, makes crystallization process more stable, reduces the defect of parasitic nucleation, lattice complete CSP monocrystalline monocrystalline good beneficial to obtaining.The method is simple to operate, easy to control, low cost.
Description
Technical field
The present invention relates to phosphorus silicon Cd monocrystal preparing technical field, more particularly to a kind of horizontal growth device of phosphorus silicon Cd monocrystal
And growing method.
Background technology
Phosphorus silicon cadmium (CdSiP2, referred to as CSP) and crystal is a kind of II-IV-V races chalcopyrite based semiconductor compound, has
Very high transparency range (0.5-9.0 μm), crystal nonlinear factor (d36=4.5pm/V), thermal conductivity (3.6W/m K) and micro-
Hardness (30kg/mm2).Phosphorus silicon cadmium can serve as 1.064 μm of Nd:YAG laser, 1.55 μm of bait ion laser and 2.05
μm Ho:The laser pump (ing)s such as LYF laser instruments, in directional ir Laser interferometers, infrared track, laser radar, laser guidance, satellite
The military and civilian such as early warning, infrared remote sensing, environmental monitoring, infrared distance measurement, infrared imaging, infrared spectrum, Infrared Therapy field has
Have wide practical use.Therefore, it is the growing method with regard to phosphorus silicon Cd monocrystal to have a lot of researchs at present.
For example, Kevin T etc. are disclosed in a kind of transparent glass cover for being internally coated with layer gold, horizontal gradient grows
The method of phosphorus silicon Cd monocrystal, specifically may refer to Growth and characterization of large CdSiP2
single crystals,Journal of Crystal Growth,2010,312:1127-1132.In addition,
CN102168299A and CN102899714A also disclose a kind of in the growing container being disposed vertically using Bridgman method give birth to
Regular way is come the method that grows phosphorus silicon Cd monocrystal.
For the horizontal gradients such as Kevin T grow method of the phosphorus silicon every monocrystalline, during crystal growth is implemented, due to
The Gold plated Layer being plated on inside cloche is readily volatilized, so needing periodic replacement and increased cost.
Content of the invention
Embodiment of the present invention technical problem to be solved is, there is provided a kind of level of the phosphorus silicon Cd monocrystal of low cost
Grower.
In order to solve above-mentioned technical problem, the embodiment of the present invention provides following technical scheme：
In a first aspect, embodiments providing a kind of horizontal growth device pyrolytic boron nitride boat of phosphorus silicon Cd monocrystal
Shape crucible, including：Nucleus growth section, changeover portion and the crystal growth section being sequentially connected with,
The length and width of the nucleus growth section is respectively less than the length and width of the crystal growth section,
The first end of the nucleus growth section is in pinnacle shape,
The second end of the nucleus growth section is connected with the crystal growth section by the changeover portion.
Specifically, preferably, the first end of the nucleus growth section is wedge shaped.
Specifically, preferably, the key groove of the first end of the nucleus growth section is 10 ° -150 °.
Second aspect, embodiments provides a kind of horizontal growth device of phosphorus silicon Cd monocrystal, including：Outer layer quartz
Pipe, layered quartz tube and above-mentioned pyrolytic boron nitride navicular crucible provided in an embodiment of the present invention,
The pyrolytic boron nitride crucible pyrolytic boron nitride navicular crucible is sleeved in the layered quartz tube, the pyrolysis nitrogen
There is space between the outer wall and the inwall of the layered quartz tube of changing boron navicular crucible,
The layered quartz tube is sleeved in the outer layer quartz ampoule, the outer wall of the layered quartz tube and the outer layer stone
There is between the inwall of English pipe space.
Specifically, preferably, the horizontal growth device of the phosphorus silicon Cd monocrystal also includes multiple locating pieces, the positioning
Block is arranged on the outer wall of the layered quartz tube and the pyrolytic boron nitride navicular crucible.
The third aspect, embodiments provides the level using above-mentioned phosphorus silicon Cd monocrystal provided in an embodiment of the present invention
The method that grower grows phosphorus silicon Cd monocrystal, including：
Step a, phosphorus silicon cadmium polycrystalline is put in pyrolytic boron nitride navicular crucible, obtains the pyrolysis for being filled with phosphorus silicon cadmium polycrystalline
Boron nitride navicular crucible；
Step b, the pyrolytic boron nitride navicular crucible for being filled with phosphorus silicon cadmium polycrystalline is put into dry layered quartz tube
Interior, sealed after being vacuumized obtains the layered quartz tube for being filled with pyrolytic boron nitride navicular crucible；
Step c, the layered quartz tube for being filled with pyrolytic boron nitride navicular crucible is put into dry outer layer quartz ampoule
Interior, inert gas is imported after vacuumizing, then seal, obtain the double-deck quartz ampoule for being filled with pyrolytic boron nitride navicular crucible；
Step d, the double-deck quartz ampoule for being filled with pyrolytic boron nitride navicular crucible is put in horizontal crystal growth stove,
Make the horizontal crystal growth stove be warming up to 1133-1180 DEG C with the speed of 50-200 DEG C/h, make pyrolytic boron nitride navicular crucible
Interior phosphorus silicon cadmium polycrystalline is fused into melt；
Step e, the melt is made all to tie with the crystal growth rate of the thermograde of 5-20 DEG C/cm and 0.1-5mm/h
Crystalline substance, the thermograde gradually increase along the nucleus growth section of pyrolytic boron nitride navicular crucible to the direction of crystal growth section；
Step f, the horizontal crystal growth stove is made to be cooled to 1000 DEG C with the rate of temperature fall of 5～20 DEG C/h, then with 20～
The rate of temperature fall of 40 DEG C/h makes the horizontal crystal growth stove be cooled to 500 DEG C or less, is cooled to room temperature, obtains the phosphorus silicon
Cd monocrystal.
Specifically, preferably, in step a, the amount of being put into of the phosphorus silicon cadmium polycrystalline is so that the phosphorus silicon cadmium polycrystalline
Melt be distributed in the pyrolytic boron nitride navicular crucible, and make the melt of the phosphorus silicon cadmium polycrystalline positioned at nucleus growth section
Volume 1/5 being advisable more than or equal to the volume of nucleus growth section.
Specifically, preferably, in step b, by the pyrolytic boron nitride navicular earthenware for being filled with phosphorus silicon cadmium polycrystalline
Crucible is put in dry layered quartz tube, is sealed using quartzy plug, and then the layered quartz tube is evacuated to very
Reciprocal of duty cycle is less than 1.0 × 10-4During Pa, using butane or oxyhydrogen flame frit seal, obtain being filled with pyrolytic boron nitride navicular crucible
Layered quartz tube.
Specifically, preferably, in step c, the internal layer quartz that described will be filled with pyrolytic boron nitride navicular crucible
Pipe is put in dry outer layer quartz ampoule, is sealed using quartzy plug, and then the outer layer quartz ampoule is evacuated to very
Reciprocal of duty cycle is less than 1.0 × 10-2During Pa, importing inert gas into the outer layer quartz ampoule makes the throughput of the inert gas be
0.1-0.9atm, and using butane or oxyhydrogen flame frit seal, obtain the bilayer quartz for being filled with pyrolytic boron nitride navicular crucible
Pipe.
Specifically, preferably, in step d, the nucleus that monitors the pyrolytic boron nitride navicular crucible using thermocouple
Growth section and the temperature of the crystal growth section.
The beneficial effect that technical scheme provided in an embodiment of the present invention is brought includes：
Embodiments provide a kind of phosphorus silicon Cd monocrystal horizontal growth device pyrolytic boron nitride navicular crucible (with
Under equal abbreviation PBN naviculars crucibles), not there is Gold plated Layer internally, so low cost.In addition, the PBN boats of the embodiment of the present invention
Shape crucible includes：Nucleus growth section, changeover portion and the crystal growth section being sequentially connected with, by making length and the width of nucleus growth section
Degree is respectively less than the length and width of crystal growth section, beneficial to the spontaneous nucleation of phosphorus silicon cadmium crystal, by by the of nucleus growth section
One end is arranged to pinnacle shape, makes the spontaneous nucleation of melt crystallization previously occur in the first end, and the crystal orientation beneficial to nucleation is equal
One property.
The embodiment of the present invention additionally provides a kind of growing method of phosphorus silicon Cd monocrystal, above-mentioned by phosphorus silicon cadmium polycrystalline to be placed in
Grower in, temperature field is more stablized using the horizontal gradient freezing method under above-mentioned condition controllable, raising finishes
The stability of brilliant process；But also make melt less with the contact surface of PBN navicular crucibles, the defect of parasitic nucleation is reduced, profit
Monocrystalline good in preparing, the complete CSP monocrystalline of lattice.The method is simple to operate, easy to control, low cost.
Description of the drawings
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, below will be to making needed for embodiment description
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, can be obtaining other according to these accompanying drawings
Accompanying drawing.
Fig. 1 is the top view of the PBN navicular crucibles that one embodiment of the invention is provided；
Fig. 1 a are the top views of the nucleus growth section of the PBN navicular crucibles that the embodiment of the present invention 1 is provided；
Fig. 1 b are the top views of the nucleus growth section of the PBN navicular crucibles that the embodiment of the present invention 1 is provided；
Fig. 1 c are the top views of the nucleus growth section of the PBN navicular crucibles that the embodiment of the present invention 1 is provided；
Fig. 2 is the top view of the horizontal growth device of the phosphorus silicon Cd monocrystal that further embodiment of this invention is provided；
Fig. 3 is the growing method flow chart of the phosphorus silicon Cd monocrystal that one embodiment of the invention is provided；
Fig. 4 is the top view of the experimental rig for preparing phosphorus silicon Cd monocrystal that further embodiment of this invention is provided；
Fig. 5 is the growing method flow chart of the phosphorus silicon Cd monocrystal that further embodiment of this invention is provided；
Fig. 6 is the outward appearance photo of the phosphorus silicon Cd monocrystal that the embodiment of the present invention 7 is provided；
Fig. 7 is that phosphorus silicon Cd monocrystal (200) the crystal face X-ray monocrystalline that the embodiment of the present invention 8 is provided waves spectrogram.
Reference is represented respectively：
1 PBN navicular crucibles,
11 nucleus growth sections,
The first end of 111 nucleus growth sections,
12 changeover portions,
13 crystal growth sections,
2 layered quartz tubes,
21 first quartzy plugs,
3 outer layer quartz ampoules,
31 second quartzy plugs,
4 horizontal crystal growth stoves,
41 alundum tubes,
42 heater strips,
5 first thermocouples,
6 second thermocouples.
Specific embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing to the embodiment of the present invention
It is described in further detail.
In a first aspect, embodiments providing a kind of horizontal growth device PBN navicular crucibles of phosphorus silicon Cd monocrystal
1, as shown in Figure 1, the PBN naviculars crucible 1 includes：Nucleus growth section 11, changeover portion 12 and the crystal growth section being sequentially connected with
13,
The length and width of the nucleus growth section 11 is respectively less than the length and width of the crystal growth section 13,
The first end 111 of the nucleus growth section is in pinnacle shape,
The second end of the nucleus growth section 11 is connected with the crystal growth section 13 by the changeover portion 12.
Wherein, changeover portion 12 is used for being attached nucleus growth sections 11 different for width and crystal growth section 13, so
Changeover portion 12 is a kind of diameter-changing body, and along the length direction of nucleus growth section 11 to crystal growth section 13, its width (also is understood as
Radical length) increase, preferably gradually increase.
Wherein, the nucleus growth section 11 described in the embodiment of the present invention is referred to respectively with the length and width of crystal growth section 13
Be X-direction and Y direction length.
In the embodiment of the present invention, the pyrolytic boron nitride navicular crucible is the boat crucible of pyrolytic boron nitride material and (also may be used
Referred to as crucible boat).Herein, the agent structure of boat crucible can be interpreted as what those skilled in the art commonly used, or common
The agent structure of boat crucible, here do not make concrete restriction to which.
The horizontal growth device of phosphorus silicon Cd monocrystal provided in an embodiment of the present invention PBN naviculars crucible 1, including：Sequentially connect
Nucleus growth section 11, changeover portion 12 and the crystal growth section 13 for connecing, is distinguished with width by the length for making nucleus growth section 11 little
In length and the width of crystal growth section 13, beneficial to the spontaneous nucleation of phosphorus silicon cadmium polycrystalline, by by the first end of nucleus growth section
Portion 111 is arranged to pinnacle shape, improves the homogeneity of the crystal orientation of formed phosphorus silicon Cd monocrystal.
Further, the embodiment of the present invention additionally provides a kind of horizontal growth device PBN navicular earthenwares of phosphorus silicon Cd monocrystal
Crucible 1, wherein, the first end 111 of nucleus growth section is wedge shaped, key groove be preferably between 10 ° -150 ° (for example, 10 ° -
40 °, 30 ° -60 °, 50 ° -90 °, 80 ° -110 °, 100 ° -150 °, 35 °, 65 °, 77 °, 100 ° etc.).By to nucleus growth section
The structure of first end 111 carries out above-mentioned setting, makes melt start crystallization nucleation at the conical tip at first, is conducive to melt
The crystalline orientation of spontaneous nucleation, makes the arrangement of lattice in nucleus more orderly.
Second aspect, embodiments provides a kind of horizontal growth device of phosphorus silicon Cd monocrystal, as shown in Figure 2,
The horizontal growth device of phosphorus silicon Cd monocrystal includes：Outer layer quartz ampoule 3, layered quartz tube 2 and provided in an embodiment of the present invention above-mentioned
PBN naviculars crucible 1,
The PBN naviculars crucible 1 is sleeved in the layered quartz tube 2, the outer wall of the PBN naviculars crucible 1 with described
There is space between the inwall of layered quartz tube 2,
The layered quartz tube 2 is sleeved in the outer layer quartz ampoule 3, and the outer wall of the layered quartz tube 2 is outer with described
There is space between the inwall of layer quartz ampoule 3.
During the horizontal growth device of actually used phosphorus silicon Cd monocrystal, sealed by the first quartzy plug 21 respectively
Layered quartz tube 2, the second quartzy plug 31 seal outer layer quartz ampoule 3.By using stability and life that quartz ampoule improves thermal field
The durability of growth device.
As the horizontal growth device of phosphorus silicon Cd monocrystal provided in an embodiment of the present invention has three-decker, in high growth temperature
During phosphorus silicon Cd monocrystal, each interlayer can produce larger pressure differential, cause grower to explode.It is based on this, in order to
Balance the pressure differential of above-mentioned generation, the embodiment of the present invention by the inwall of the outer wall of PBN naviculars crucible 1 and layered quartz tube 2 and
Space is set between the inwall of the outer wall of layered quartz tube 2 and outer layer quartz ampoule 3 so that can be filled with argon gas or nitrogen in the space
The gases such as gas, to improve the explosion prevention function of grower.It can be seen that, the horizontal growth of phosphorus silicon Cd monocrystal provided in an embodiment of the present invention
Device is made to be filled with inert gas between quartz ampoule, is realized the partial pressure in crystal growing process by double-deck quartz ampoule design
Balance, solves the problems, such as the booster easily occurred in crystal growing process,
More specifically, in grower provided in an embodiment of the present invention, above-mentioned space is annular compartment.
Further, the horizontal growth device of the phosphorus silicon Cd monocrystal also includes that multiple locating pieces, the locating piece are arranged
On the outer wall of the layered quartz tube 2 and the PBN naviculars crucible 1.
By arranging locating piece on the outer wall of PBN naviculars crucible 1, it is easy to for PBN naviculars crucible 1 to be fixed on internal layer quartz
In pipe 2；By arranging locating piece on the outer wall of layered quartz tube 2, in order to layered quartz tube 2 is fixed on outer layer quartz ampoule
In 3.For example, a locating piece can be set in the centre position of PBN naviculars crucible 1 or the outer wall of layered quartz tube 2, or
Person is oppositely arranged two locating pieces on the outer wall.
The third aspect, embodiments provides a kind of horizontal growth device using above-mentioned phosphorus silicon Cd monocrystal and grows
The method of phosphorus silicon Cd monocrystal, flow chart of the accompanying drawing 3 for the method.As shown in Figure 3, the method includes：
Step 101, phosphorus silicon cadmium polycrystalline is put in PBN naviculars crucible 1, obtains the PBN naviculars for being filled with phosphorus silicon cadmium polycrystalline
Crucible 1.
Step 102, the PBN naviculars crucible 1 for being filled with phosphorus silicon cadmium polycrystalline is put in dry layered quartz tube 2,
Sealed after being vacuumized, obtains the layered quartz tube 2 for being filled with PBN naviculars crucible 1.
Step 103, the layered quartz tube 2 for being filled with PBN naviculars crucible 1 is put in dry outer layer quartz ampoule 3,
Inert gas is imported after vacuumizing, is then sealed, is obtained the double-deck quartz ampoule for being filled with PBN naviculars crucible 1.
Step 104, the double-deck quartz ampoule for being filled with PBN naviculars crucible 1 is put in horizontal crystal growth stove 4, with
The speed of 50-200 DEG C/h makes the horizontal crystal growth stove 4 be warming up to 1133-1180 DEG C, makes the phosphorus silicon in PBN naviculars crucible 1
Cadmium polycrystalline is fused into melt.
Step 105, make the melt whole with the crystal growth rate of the thermograde of 5-20 DEG C/cm and 0.1-5mm/h
Crystallization, the thermograde gradually increase along the nucleus growth section 11 of PBN naviculars crucible 1 to the direction of crystal growth section 13.
Step 106, the horizontal crystal growth stove 4 is made to be cooled to 1000 DEG C with the rate of temperature fall of 5～20 DEG C/h, then with 20
The rate of temperature fall of～40 DEG C/h makes the horizontal crystal growth stove 4 be cooled to 500 DEG C, is cooled to room temperature, obtains the phosphorus silicon cadmium
Monocrystalline.
A kind of growing method of phosphorus silicon Cd monocrystal is embodiments provided, by phosphorus silicon cadmium polycrystalline is placed in above-mentioned knot
In the grower of structure, thermal field is more stablized using the horizontal gradient freezing method under above-mentioned condition controllable, improve crystallization
The stability of process；Also so that melt is less with the contact surface of PBN naviculars crucible 1, the defect of parasitic nucleation is reduced, beneficial to system
Standby obtain monocrystalline good, the complete CSP monocrystalline of lattice.The method is simple to operate, easy to control, low cost.
The embodiment of the present invention additionally provides a kind of horizontal growth device growth phosphorus silicon cadmium using above-mentioned phosphorus silicon Cd monocrystal
The method of monocrystalline, during phosphorus silicon Cd monocrystal is prepared, the specifically used experimental provision of the embodiment is as shown in Figure 4.Attached
Fig. 5 is the flow chart of method provided in an embodiment of the present invention.As shown in Figure 5, the method includes：
Step 201, the phosphorus silicon cadmium polycrystalline by purity more than or equal to 99.9999% are put in PBN naviculars crucible 1, the phosphorus
The amount of being put into of silicon cadmium polycrystalline is so that the melt of the phosphorus silicon cadmium polycrystalline is distributed in the PBN naviculars crucible 1, and is made positioned at nucleus
The volume of the melt of the phosphorus silicon cadmium polycrystalline of growth section 11 is advisable more than or equal to the 1/5 of the volume of nucleus growth section 11.
In step 201, in order to improve the purity of prepared CSP monocrystalline, using phosphorus of the purity more than or equal to 99.9999%
Silicon cadmium polycrystalline, further, its purity preferably 99.99999%.
Before phosphorus silicon cadmium polycrystalline is put into PBN naviculars crucible 1, it is 1 using volume ratio:1 concentrated hydrochloric acid and red fuming nitric acid (RFNA)
Pickling is carried out, and deionized water is rinsed well, can be used after drying.
Monocrystalline is spontaneously formed and is caused in order to ensure nucleus, and is unlikely to make the monocrystalline for ultimately forming give PBN navicular earthenwares
Crucible 1 applies excessive pressure so that its explosion, in step 201, described in the amount of being put into of phosphorus silicon cadmium polycrystalline, phosphorus silicon cadmium polycrystalline is put into
Amount is so that the melt of the phosphorus silicon cadmium polycrystalline is distributed in the pyrolytic boron nitride navicular crucible, and is made positioned at nucleus growth section
The volume of the melt of the phosphorus silicon cadmium polycrystalline is advisable more than or equal to the 1/5 of the volume of nucleus growth section.It is understood that this
In bright embodiment, the melt of phosphorus silicon cadmium polycrystalline need to be distributed in the pyrolytic boron nitride navicular crucible, also be understood as at least spreading
The bottom of full the pyrolytic boron nitride navicular crucible nucleus growth section, changeover portion and crystal growing section.Above-mentioned make positioned at nucleus give birth to
The volume of the melt of the phosphorus silicon cadmium polycrystalline of long section is referred to not only in crystalline substance more than or equal to the 1/5 of the volume of nucleus growth section
Nucleus growth section has the melt of phosphorus silicon cadmium polycrystalline, while also having the melt of phosphorus silicon cadmium polycrystalline in changeover portion and crystal growing section.
Further, in the embodiment of the present invention, the upper limit of the amount of being put into of phosphorus silicon cadmium polycrystalline is the volume of the melt for making phosphorus silicon cadmium polycrystalline not
Exceed the volume of the pyrolytic boron nitride navicular crucible.
Step 202, the PBN naviculars crucible 1 for being filled with phosphorus silicon cadmium polycrystalline is put in dry layered quartz tube 2,
Sealed using quartzy plug, vacuum is then evacuated to the layered quartz tube 2 less than 1.0 × 10-4During Pa, use
Butane or oxyhydrogen flame frit seal, obtain the layered quartz tube 2 for being filled with PBN naviculars crucible 1.
In step 202, vacuum is evacuated to less than 1.0 × 10-4Pa can effectively prevent phosphorus silicon cadmium polycrystalline follow-up
Oxidized pollution in crystal growing process.
Step 203, the layered quartz tube 2 for being filled with PBN naviculars crucible 1 is put in dry outer layer quartz ampoule 3,
Sealed using quartzy plug, vacuum is then evacuated to the outer layer quartz ampoule 3 less than 1.0 × 10-2During Pa, to institute
When the throughput for stating importing inert gas to inert gas in outer layer quartz ampoule 3 is 0.1-0.9atm, using butane or oxyhydrogen flame
Frit seal, obtains the double-deck quartz ampoule for being filled with PBN naviculars crucible 1.
In step 203, by inert gas is imported into ectonexine quartz ampoule 3, improve the explosion-proof energy of layered quartz tube 2
Power.In order to realize the frit seal of outer layer quartz ampoule 3, the inert gas between layered quartz tube 2 and outer layer quartz ampoule 3
Throughput should be less than 1atm.In order to obtain preferable pressure compensation effect, the throughput of preferably inert gas is arrived for 0.5atm
Between 1atm.
Further, during vacuumizing to outer layer quartz ampoule 3, using inert gas argon gas drip washing quartz ampoule 3-10
Minute, preferably 10 minutes, with other gases in emptying outer layer quartz ampoule 3, and ensure fully being filled with for argon gas.
For example, in the embodiment of the present invention, the inert gas can be argon gas, helium, nitrogen etc., preferably argon gas.
Step 204, the double-deck quartz ampoule for being filled with PBN naviculars crucible 1 is put in horizontal crystal growth stove 4, with
The speed of 50-200 DEG C/h makes the horizontal crystal growth stove 4 be warming up to 1133-1180 DEG C, makes the phosphorus silicon in PBN naviculars crucible 1
Cadmium polycrystalline is fused into melt, the nucleus growth section 11 and the crystal growth section 13 for monitoring the PBN naviculars crucible 1 using thermocouple
Temperature.
In step 204, the temperature of nucleus growth section 11 of PBN naviculars crucible 1 is monitored and controls respectively by thermocouple (i.e.
Temperature at nucleus and melt posetionof weld) and crystal growth section 13 temperature (i.e. the temperature of melt).By to nucleus growth
The temperature control of section 11, realizes nucleus (alternatively referred to as seed crystal) and effective welding of melt of spontaneous nucleation formation, prevents seed crystal
All melted；By the temperature control to crystal growth section 13, prevent melt temperature to fluctuate, affect the crystallization of crystal growth.
In step 204, heating rate prevents temperature overshot and causes temperature fluctuation no more than 120 DEG C/h.It is preferred that heating up
Speed 80-100 DEG C/h, it is possible to achieve temperature is controlled accurately and stably.
In step 204, the temperature of the horizontal crystal growth stove 4 should be 1133-1180 DEG C, and the too low raw material that is easily caused melts
Change is insufficient, and the too high heat that is easily caused is conducted to seed crystal, melts seed crystal.It is preferred that 1150～1165 DEG C, can both make original
Expect abundant melting mixing, can ensure that seed crystal is not melted again.
Step 205, make the melt whole with the crystal growth rate of the thermograde of 5-20 DEG C/cm and 0.1-5mm/h
Crystallization, the thermograde gradually increase along the nucleus growth section 11 of PBN naviculars crucible 1 to the direction of crystal growth section 13.
In step 205, thermograde is unsuitable too high or too low.During less than 5 DEG C/cm, due to crystallization driving force deficiency, difficult
To grow the monocrystal of high-quality low-defect-density；Crystal is easily caused during higher than 20 DEG C/cm to answer thermal stress excessive and ftracture.
Thermograde preferably 10～15 DEG C/cm, can either provide enough crystallization driving forces, while thermal stress can be prevented excessive again.
In step 205, crystal growth rate is preferably controlled in the range of 0.1-5mm/h, too low is easily caused growth rate not
Surely, the disturbance of growth interface, the too high defect for being easily caused lattice arrangement is caused to increase and destroy crystal mass.Preferred growth speed
Rate is 0.3～0.8mm/h, both can ensure that stable mechanical movement, improves interface stability, while crystal growth rate and temperature
Degree gradient is mutually matched, and lattice arrangement in crystallization process in order, reduces defect.
Step 206, the horizontal crystal growth stove 4 is made to be cooled to 1000 DEG C with the rate of temperature fall of 5～20 DEG C/h, then with 20
The rate of temperature fall of～40 DEG C/h makes the horizontal crystal growth stove 4 be cooled to 500 DEG C or less, is cooled to room temperature, obtains described
Phosphorus silicon Cd monocrystal.
On the one hand step 206 prevents crystal cleavage, the opposing party by carrying out gradient cooling to horizontal crystal growth stove 4
Face reduces temperature fall time, improves rate of temperature fall.
Further, it is possible to use alternative steps of the following steps as step 206：After melt is fully crystallized, with not
Rate of temperature fall higher than 20 DEG C/h makes the horizontal crystal growth stove 4 be cooled to less than 500 DEG C, then naturally cools to room temperature,
Obtain the phosphorus silicon Cd monocrystal.
In the alternative steps, rate of temperature fall is easily caused crystal cleavage no more than 20 DEG C/h, too high rate of temperature fall.Drop
Warm speed preferably 8～12 DEG C/h, both can avoid crystal cleavage, while avoiding temperature fall time oversize and affecting efficiency.
Further, the embodiment of the present invention is additionally provided a kind of said method provided using the present invention and is being prepared
GaAs、CdSe、AgGaS2With the purposes in CdZnTe crystal.
Hereinafter the present invention will further be illustrated by specific embodiment.
Embodiment 1
As shown in Figure 1, a kind of horizontal growth device PBN navicular earthenwares of phosphorus silicon Cd monocrystal are embodiments provided
Crucible 1, including：Nucleus growth section 11, changeover portion 12 and crystal growth section 13,
The wedge shaped angle of the first end of the nucleus growth section 11 is 30 ° of wedge shape (referring to accompanying drawing 1a), the nucleus life
The second end of long section 11, the changeover portion 12 are sequentially connected with the crystal growth section 13,
The width of the nucleus growth section 11 is respectively 15mm and 60mm with length,
The width of the crystal growth section 13 is respectively 70mm and 200mm with length.
Embodiment 2
As shown in Figure 1, a kind of horizontal growth device PBN navicular earthenwares of phosphorus silicon Cd monocrystal are embodiments provided
Crucible 1, except the key groove of wedge shaped first end is 70 ° (referring to accompanying drawing 1b)；The width of the nucleus growth section 11 and length
Degree is respectively 2mm and 10mm；The width of the crystal growth section 13 is respectively 5mm and 20mm with the offer of embodiment 1 with length
Crucible is different outer, remaining the construction all same for the crucible that crucible provided in an embodiment of the present invention is provided with embodiment 1.
Embodiment 3
As shown in Figure 1, a kind of horizontal growth device PBN navicular earthenwares of phosphorus silicon Cd monocrystal are embodiments provided
Crucible 1, except the key groove of wedge shaped first end is 150 ° (referring to accompanying drawing 1c)；The width of the nucleus growth section 11 and length
Degree is respectively 20mm and 80mm；The width of the crystal growth section 13 is respectively 100mm and 300mm with length and is carried with embodiment 1
For crucible different outer, remaining the construction all same for the crucible that crucible provided in an embodiment of the present invention is provided with embodiment 1.
Embodiment 4
As shown in Figure 2, a kind of horizontal growth device of phosphorus silicon Cd monocrystal is embodiments provided, including：Outer layer
The PBN naviculars crucible 1 that quartz ampoule 3, layered quartz tube 2 and embodiment 1 are provided,
The PBN naviculars crucible 1 is sleeved in layered quartz tube 2, and the outer wall of PBN naviculars crucible 1 is interior with layered quartz tube 2
There is space between wall,
The layered quartz tube 2 is sleeved in outer layer quartz ampoule 3, the outer wall of layered quartz tube 2 and the outer layer quartz ampoule 3
There is between inwall space.
During the horizontal growth device of actually used phosphorus silicon Cd monocrystal, sealed by the first quartzy plug 21 respectively
Layered quartz tube 2, the second quartzy plug 31 seal outer layer quartz ampoule 3.
Embodiment 5
A kind of horizontal growth device of phosphorus silicon Cd monocrystal is embodiments provided, including：Outer layer quartz ampoule 3, internal layer
The PBN naviculars crucible 1 that quartz ampoule 2 and embodiment 2 are provided,
The PBN naviculars crucible 1 is sleeved in layered quartz tube 2, and the outer wall of PBN naviculars crucible 1 is interior with layered quartz tube 2
There is space between wall,
The layered quartz tube 2 is sleeved in outer layer quartz ampoule 3, the outer wall of layered quartz tube 2 and the outer layer quartz ampoule 3
There is between inwall space.
Embodiment 6
A kind of horizontal growth device of phosphorus silicon Cd monocrystal is embodiments provided, including：Outer layer quartz ampoule 3, internal layer
The PBN naviculars crucible 1 that quartz ampoule 2 and embodiment 3 are provided,
The PBN naviculars crucible 1 is sleeved in layered quartz tube 2, and the outer wall of PBN naviculars crucible 1 is interior with layered quartz tube 2
There is space between wall,
The layered quartz tube 2 is sleeved in outer layer quartz ampoule 3, the outer wall of layered quartz tube 2 and the outer layer quartz ampoule 3
There is between inwall space.
Embodiment 7
The horizontal growth device of the phosphorus silicon Cd monocrystal that the embodiment of the present invention is provided using embodiment 4 prepares phosphorus silicon Cd monocrystal.
Comprise the following steps that：
1) it is 1 CSP polycrystal materials successively to be used volume ratio:1 concentrated hydrochloric acid and red fuming nitric acid (RFNA) pickling and deionized water washing are done
After net, thermostatic drying chamber drying is put into.
2) weigh dry CSP polycrystal materials to be put in PBN naviculars crucible 1 so as to amount for PBN naviculars crucible 1 monocrystalline
(now the volume of the melt of phosphorus silicon cadmium polycrystalline is distributed in PBN crucibles 1, and is located at nucleus growth for the 2/3 of the volume of growth section 13
Section 11 at phosphorus silicon cadmium polycrystalline melt volume met the volume more than nucleus growth section 11 1/5).
3) the PBN naviculars crucible 1 that will be equipped with CSP polycrystal materials is transferred in the layered quartz tube 2 of cleaning, drying, is put into first
Quartzy plug 21, vacuumizing and exhausting, when vacuum is less than 1.0 × 10-4During Pa, using oxyhydrogen flame frit seal.
4) layered quartz tube 2 of good seal is transferred in outer layer quartz ampoule 3, is put into the second quartzy plug 31, vacuumizes
Exhaust, when vacuum is less than 1.0 × 10-2During Pa, argon gas (Ar) is imported, using argon gas (Ar) drip washing outer layer quartz ampoule 3-
10min, when the aeration quantity of argon gas in the outer layer quartz ampoule 3 is 0.6atm, using butane frit seal；
5) by sealing after 3 transfer level crystal growing furnace 4 of outer layer quartz ampoule in, the first thermocouple 5 is placed on level brilliant
At the nucleus growth section 11 of the fire door left end of bulk-growth stove 4 to PBN naviculars crucible 1, to monitor at seed crystal and melt posetionof weld
Temperature.Second thermocouple 6 is placed on the crystal growth section 13 of 4 fire door right-hand member of horizontal crystal growth stove to PBN naviculars crucible 1
At tail end, to monitor melt temperature state.Then the fire door of horizontal crystal growth stove 4 is sealed with insulation material.Wherein, level
Crystal growing furnace 4 is lined with alundum tube 41, provides temperature by the heating of heater strip 42, carries out temperature control by Continental Europe temperature control instrument.
6) heating schedule is adjusted, makes horizontal crystal growth stove 4 be warming up to 1160 DEG C with the speed of 100 DEG C/h, make PBN naviculars
Phosphorus silicon cadmium polycrystalline in crucible 1 is fused into melt；Melt is made with the crystal growth rate of the thermograde of 12 DEG C/cm and 3mm/h
All crystallize, thermograde gradually increases along the tapered end of PBN naviculars crucible 1 to the direction of crystal growth section 13；With 13 DEG C/
The rate of temperature fall of h makes horizontal crystal growth stove 4 be cooled to 1000 DEG C, then makes horizontal crystal growth stove with the rate of temperature fall of 30 DEG C/h
4 are cooled to 500 DEG C, close 4 power supply of horizontal crystal growth stove, are cooled to room temperature.Phosphorus silicon cadmium is taken out from horizontal crystal growth stove 4
The horizontal growth device of monocrystalline, obtains phosphorus silicon Cd monocrystal after carrying out crushing to which.
Outward appearance photo of the accompanying drawing 6 for prepared phosphorus silicon Cd monocrystal, it is seen then that phosphorus silicon Cd monocrystal prepared by the embodiment of the present invention
Completely, rule, with good profile.
Phosphorus silicon Cd monocrystal (200) the crystal face X-ray monocrystalline that embodiment of the present invention preparation is measured using X-ray diffractometer shakes
Put on airs figure, as shown in Figure 7, (200) crystallographic plane diffraction peak is sharp, and peak diffraction intensity is big, and diffraction peak symmetry is preferable.Can
See, phosphorus silicon Cd monocrystal provided in an embodiment of the present invention monocrystalline good, lattice is complete.
Embodiment 8
The horizontal growth device of the phosphorus silicon Cd monocrystal that the present embodiment is provided using embodiment 5 is walked preparing phosphorus silicon Cd monocrystal
Rapid as follows：
1) it is 1 CSP polycrystal materials successively to be used volume ratio:1 concentrated hydrochloric acid and red fuming nitric acid (RFNA) pickling and deionized water washing are done
After net, thermostatic drying chamber drying is put into.
2) weigh dry CSP polycrystal materials to be put in PBN naviculars crucible 1 so as to amount for PBN naviculars crucible 1 nucleus
(now the volume of the melt of phosphorus silicon cadmium polycrystalline is distributed in PBN crucibles 1, and is located at nucleus growth for the 1/3 of the volume of growth section 11
Section 11 at phosphorus silicon cadmium polycrystalline melt volume met the volume more than nucleus growth section 11 1/5).
3) the PBN naviculars crucible 1 that will be equipped with CSP polycrystal materials is transferred in the layered quartz tube 2 of cleaning, drying, is put into first
Quartzy plug 21, vacuumizing and exhausting, when vacuum is less than 1.0 × 10-4During Pa, using oxyhydrogen flame frit seal.
4) layered quartz tube 2 of good seal is transferred in outer layer quartz ampoule 3, is put into the second quartzy plug 31, vacuumizes
Exhaust, when vacuum is less than 1.0 × 10-2During Pa, argon gas (Ar) is imported, using argon gas (Ar) drip washing outer layer quartz ampoule 3-
10min, when the aeration quantity of argon gas in the outer layer quartz ampoule 3 is 0.1atm, using butane frit seal；
5) by sealing after 3 transfer level crystal growing furnace 4 of outer layer quartz ampoule in, the first thermocouple 5 is placed on level brilliant
At the nucleus growth section 11 of the fire door left end of bulk-growth stove 4 to PBN naviculars crucible 1, to monitor at seed crystal and melt posetionof weld
Temperature.Second thermocouple 6 is placed on the crystal growth section 13 of 4 fire door right-hand member of horizontal crystal growth stove to PBN naviculars crucible 1
At tail end, to monitor melt temperature state.Then the fire door of horizontal crystal growth stove 4 is sealed with insulation material.Wherein, level
Crystal growing furnace 4 is lined with alundum tube 41, provides temperature by the heating of heater strip 42, carries out temperature control by Continental Europe temperature control instrument.
6) heating schedule is adjusted, makes horizontal crystal growth stove 4 be warming up to 1133 DEG C with the speed of 50 DEG C/h, make PBN naviculars
Phosphorus silicon cadmium polycrystalline in crucible 1 is fused into melt；Melt is made with the crystal growth rate of the thermograde of 5 DEG C/cm and 0.1mm/h
All crystallize, thermograde gradually increases along the tapered end of PBN naviculars crucible 1 to the direction of crystal growth section 13；With 5 DEG C/h
Rate of temperature fall make horizontal crystal growth stove 4 be cooled to 1000 DEG C, then horizontal crystal growth stove 4 is made with the rate of temperature fall of 20 DEG C/h
500 DEG C are cooled to, 4 power supply of horizontal crystal growth stove are closed, is cooled to room temperature.Phosphorus silicon cadmium is taken out from horizontal crystal growth stove 4
The horizontal growth device of monocrystalline, obtains phosphorus silicon Cd monocrystal after carrying out crushing to which.
Embodiment 9
The horizontal growth device of the phosphorus silicon Cd monocrystal that the present embodiment is provided using embodiment 6 is walked preparing phosphorus silicon Cd monocrystal
Rapid as follows：
1) it is 1 CSP polycrystal materials successively to be used volume ratio:1 concentrated hydrochloric acid and red fuming nitric acid (RFNA) pickling and deionized water washing are done
After net, thermostatic drying chamber drying is put into.
2) weigh dry CSP polycrystal materials to be put in PBN naviculars crucible 1 so as to amount for PBN naviculars crucible 1 monocrystalline
(now the volume of the melt of phosphorus silicon cadmium polycrystalline is distributed in PBN crucibles 1, and is located at nucleus growth for the 4/5 of the volume of growth section 13
Section 11 at phosphorus silicon cadmium polycrystalline melt volume met the volume more than nucleus growth section 11 1/5).
3) the PBN naviculars crucible 1 that will be equipped with CSP polycrystal materials is transferred in the layered quartz tube 2 of cleaning, drying, is put into first
Quartzy plug 21, vacuumizing and exhausting, when vacuum is less than 1.0 × 10-4During Pa, using oxyhydrogen flame frit seal.
4) layered quartz tube 2 of good seal is transferred in outer layer quartz ampoule 3, is put into the second quartzy plug 31, vacuumizes
Exhaust, when vacuum is less than 1.0 × 10-2During Pa, argon gas (Ar) is imported, using argon gas (Ar) drip washing outer layer quartz ampoule 3-
10min, when the aeration quantity of argon gas in the outer layer quartz ampoule 3 is 0.9atm, using butane frit seal；
5) by sealing after 3 transfer level crystal growing furnace 4 of outer layer quartz ampoule in, the first thermocouple 5 is placed on level brilliant
At the nucleus growth section 11 of the fire door left end of bulk-growth stove 4 to PBN naviculars crucible 1, to monitor at seed crystal and melt posetionof weld
Temperature.Second thermocouple 6 is placed on the crystal growth section 13 of 4 fire door right-hand member of horizontal crystal growth stove to PBN naviculars crucible 1
At tail end, to monitor melt temperature state.Then the fire door of horizontal crystal growth stove 4 is sealed with insulation material.Wherein, level
Crystal growing furnace 4 is lined with alundum tube 41, provides temperature by the heating of heater strip 42, carries out temperature control by Continental Europe temperature control instrument.
6) heating schedule is adjusted, makes horizontal crystal growth stove 4 be warming up to 1180 DEG C with the speed of 200 DEG C/h, make PBN naviculars
Phosphorus silicon cadmium polycrystalline in crucible 1 is fused into melt；Melt is made with the crystal growth rate of the thermograde of 20 DEG C/cm and 5mm/h
All crystallize, thermograde gradually increases along the tapered end of PBN naviculars crucible 1 to the direction of crystal growth section 13；With 20 DEG C/
The rate of temperature fall of h makes horizontal crystal growth stove 4 be cooled to 1000 DEG C, then makes horizontal crystal growth stove with the rate of temperature fall of 40 DEG C/h
4 are cooled to 500 DEG C, close 4 power supply of horizontal crystal growth stove, are cooled to room temperature.Phosphorus silicon cadmium is taken out from horizontal crystal growth stove 4
The horizontal growth device of monocrystalline, obtains phosphorus silicon Cd monocrystal after carrying out crushing to which.
Presently preferred embodiments of the present invention is the foregoing is only, not in order to limit the scope of the invention, all at this
Within bright spirit and principle, any modification, equivalent substitution and improvements that is made etc. should be included in protection scope of the present invention
Within.
Claims (7)
1. a kind of horizontal growth device of phosphorus silicon Cd monocrystal, including：Outer layer quartz ampoule, layered quartz tube and pyrolytic boron nitride navicular
Crucible,
The pyrolytic boron nitride navicular crucible is sleeved in the layered quartz tube, the outer wall of the pyrolytic boron nitride navicular crucible
There is space and the inwall of the layered quartz tube between,
The layered quartz tube is sleeved in the outer layer quartz ampoule, the outer wall of the layered quartz tube and the outer layer quartz ampoule
Inwall between have space, for filling inert gas；
The pyrolytic boron nitride navicular crucible includes：Nucleus growth section, changeover portion and the crystal growth section being sequentially connected with,
The length and width of the nucleus growth section is respectively less than the length and width of the crystal growth section,
The second end of the nucleus growth section is connected with the crystal growth section by the changeover portion；
The first end of the nucleus growth section is wedge shaped, and the key groove of the first end of the nucleus growth section be 10 °-
150°.
2. the horizontal growth device of phosphorus silicon Cd monocrystal according to claim 1, it is characterised in that the phosphorus silicon Cd monocrystal
Horizontal growth device also includes that multiple locating pieces, the locating piece are arranged on the layered quartz tube and the pyrolytic boron nitride boat
On the outer wall of shape crucible.
3. the method for growing phosphorus silicon Cd monocrystal using the horizontal growth device of the phosphorus silicon Cd monocrystal described in claim 1 or 2, bag
Include：
Step a, phosphorus silicon cadmium polycrystalline is put in pyrolytic boron nitride navicular crucible, obtains the pyrolysis nitridation for being filled with phosphorus silicon cadmium polycrystalline
Boron navicular crucible；
Step b, the pyrolytic boron nitride navicular crucible for being filled with phosphorus silicon cadmium polycrystalline is put in dry layered quartz tube, is taken out
Seal after vacuum, obtain the layered quartz tube for being filled with pyrolytic boron nitride navicular crucible；
Step c, the layered quartz tube for being filled with pyrolytic boron nitride navicular crucible is put in dry outer layer quartz ampoule, is taken out
Inert gas is imported after vacuum, is then sealed, is obtained the double-deck quartz ampoule for being filled with pyrolytic boron nitride navicular crucible；
Step d, the double-deck quartz ampoule for being filled with pyrolytic boron nitride navicular crucible is put in horizontal crystal growth stove, with
The speed of 50-200 DEG C/h makes the horizontal crystal growth stove be warming up to 1133-1180 DEG C, makes the phosphorus silicon cadmium in PBN navicular crucibles
Polycrystalline is fused into melt；
Step e, the melt is made all to crystallize with the crystal growth rate of the thermograde of 5-20 DEG C/cm and 0.1-5mm/h, institute
Stating thermograde gradually increases along the nucleus growth section of pyrolytic boron nitride navicular crucible to the direction of crystal growth section；
Step f, make the horizontal crystal growth stove be cooled to 1000 DEG C with the rate of temperature fall of 5～20 DEG C/h, then with 20～40 DEG C/
The rate of temperature fall of h makes the horizontal crystal growth stove be cooled to 500 DEG C, is cooled to room temperature, obtains the phosphorus silicon Cd monocrystal.
4. method according to claim 3, it is characterised in that in step a, the amount of the being put into energy of the phosphorus silicon cadmium polycrystalline
The melt of the phosphorus silicon cadmium polycrystalline is distributed in the pyrolytic boron nitride navicular crucible, and make the institute positioned at nucleus growth section
The volume of melt of phosphorus silicon cadmium polycrystalline is stated more than or equal to the 1/5 of the volume of nucleus growth section.
5. method according to claim 3, it is characterised in that in step b, by the phosphorus silicon cadmium polycrystalline that is filled with
Pyrolytic boron nitride navicular crucible is put in dry layered quartz tube, is sealed using quartzy plug, then to the internal layer
Quartz ampoule is evacuated to vacuum less than 1.0 × 10-4During Pa, using butane or oxyhydrogen flame frit seal, obtain being filled with pyrolysis
The layered quartz tube of boron nitride navicular crucible.
6. method according to claim 3, it is characterised in that in step c, be filled with pyrolytic boron nitride boat by described
The layered quartz tube of shape crucible is put in dry outer layer quartz ampoule, is sealed using quartzy plug, then to the outer layer
Quartz ampoule is evacuated to vacuum less than 1.0 × 10-2During Pa, importing inert gas into the outer layer quartz ampoule makes the inertia
The throughput of gas is 0.1-0.9atm, and using butane or oxyhydrogen flame frit seal, obtains being filled with pyrolytic boron nitride navicular
The double-deck quartz ampoule of crucible.
7. method according to claim 3, it is characterised in that in step d, monitors the pyrolysis nitridation using thermocouple
The temperature of the nucleus growth section and crystal growth section of boron navicular crucible.
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| CN107268070A (en) * | 2017-06-10 | 2017-10-20 | 中国科学院合肥物质科学研究院 | A kind of method of low absorption phosphorus germanium zinc crystal growth |
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| CN111809241B (en) * | 2020-09-08 | 2020-12-15 | 宁波碲晶光电科技有限公司 | Method for preparing cadmium telluride or cadmium zinc telluride polycrystal material |
| CN111809236B (en) * | 2020-09-08 | 2020-12-22 | 宁波碲晶光电科技有限公司 | Method for preparing cadmium telluride or cadmium zinc telluride polycrystal material |
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