CN209537670U - Crystal growth double crucible - Google Patents
Crystal growth double crucible Download PDFInfo
- Publication number
- CN209537670U CN209537670U CN201822255012.5U CN201822255012U CN209537670U CN 209537670 U CN209537670 U CN 209537670U CN 201822255012 U CN201822255012 U CN 201822255012U CN 209537670 U CN209537670 U CN 209537670U
- Authority
- CN
- China
- Prior art keywords
- crucible
- crystal growth
- double
- crystal
- raw material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The utility model discloses a kind of crystal growth double crucibles, are related to technical field of crystal growth, which includes the lower crucible for placing the upper crucible of raw material with being used for crystal growth；The top of the lower crucible is arranged in the upper crucible, and upper crucible bottom periphery and lower crucible opening periphery are tightly connected；The upper crucible bottom surface is provided with the material spilling hole for leading to the lower crucible；The upper crucible and lower crucible are pyrolytic boron nitride crucible.Application during VB method grows indium phosphide, using double crucible structure, and the crystal growth technique using the double crucible, it can make indium phosphide polycrystal raw material and dopant S full and uniform mixing, the carrier concentration range for growing S-InP monocrystalline is reduced, single crystal longitudinal direction carrier concentration deviation can control in (3-6) x1018/cm3, the crystal of high quality, high uniformity is obtained, and the piece rate of monocrystalline improves 5%.
Description
Technical field
The utility model relates to technical field of crystal growth, more particularly to a kind of crystal growth double crucible.
Background technique
Indium phosphide InP is one of great strategic important semiconductor material, optic communication, millimeter wave high frequency, low noise,
Broadband microelectronics is integrated to wait fields to have important application.
With the development of infrared detector technology in recent years, III-V centered on GaAs series, InP series is started
The designing technique of race's Effects of GaAs/AlGaAs Quantum Wells material is also wide to the research of the infrared detector of the superlattice structures such as Quantum Well
General development.Its principle is exactly a kind of light-detecting device made of the photoconductive effect using semiconductor material.So-called photoconduction effect
It answers, refers to a kind of physical phenomenon for causing illuminated material electric conductivity to change by radiation.Photoconductive detector is military and national
Economic every field has extensive use.It is mainly used for radionetric survey and detection, industry automatically in visible light or near infrared band
Control, Photometric Measurement etc.；Infrared band be mainly used for missile guidance, infrared thermal imaging, in terms of.Indium phosphide material
Material is all highly suitable as the core material of optical detector on electrology characteristic and material property.
Indium phosphide single crystal growing method is mainly VGF method (vertical gradient solidification) and VB method (vertical Bridgman at present
Method).Traditional VB method indium phosphide single crystal growth is to be mixed directly into indium phosphide raw material and dopant " sulphur " to be packed into together to nitrogenize
Then boron crucible carries out crystal growth technique, provide important raw material-for the preparation of indium phosphide single crystal substrate and mix sulphur indium phosphide list
Brilliant material S-InP.
In this case some problems be can bring about, since sulphur (S) is used as one VI race's elements, its dividing in indium phosphide crystal
Solidifying coefficient is smaller, indium phosphide single crystal preparation when directly with indium phosphide polycrystal raw material it is admixed together after, start crystal growth, this
Sample will cause a large amount of sulphur (S) and be deposited on crystal tail portion, cause doping concentration uneven, and head carrier concentration is low, and tail portion carries
The problems such as sub- concentration is then higher is flowed, uses traditional single crucible VB method crystal growth technique at present, whole the longitudinal of crystal carries
Flowing sub- concentration can be in (2-8) x1018/cm3, such a range, it can be seen that the range of entire concentration distribution is larger；And it is right
S-InP crystal growth rate can produce bigger effect, and the especially deviation of its doping concentration and full wafer uniformity all can be to device
Emission wavelength uniformity etc. has significant impact.
Utility model content
First purpose of the utility model is to carry out providing a kind of bilayer in S-InP crystal growing process using VB method
Crucible.First purpose of the utility model is realized by the following technical scheme:
A kind of crystal growth double crucible, which is characterized in that including the upper crucible for placing raw material and for crystalline substance
The lower crucible of body growth；The top of the lower crucible is arranged in the upper crucible, and upper crucible bottom periphery and lower crucible opening are outer
Week is tightly connected；The upper crucible bottom surface is provided with the material spilling hole for leading to the lower crucible；The upper crucible is with lower crucible
Pyrolytic boron nitride crucible.
As an improved technical scheme, the upper crucible bottom is flat or downward projection of arcuate bottom.
As an improved technical scheme, the quantity of the material spilling hole of the upper crucible bottom is one or more.
As an improved technical scheme, the lower crucible bottom is taper, and bottom is provided with seed crystal chamber.
The second purpose of the utility model is to be based on above-mentioned double crucible, provide a kind of crystal growth technique, keep indium phosphide more
Brilliant raw material are uniformly mixed with dopant sulphur, to grow the S-InP monocrystal of high quality, high uniformity.This is practical new
Second purpose of type is realized by the following technical scheme:
A kind of crystal growth technique uses above-mentioned crystal growth double crucible, which comprises the following steps:
S1: double crucible is put into a quartz ampoule, and polycrystal raw material and dopant are put into upper crucible；
S2: a quartzy sealing cap is covered at the top of quartz ampoule, then quartz ampoule is vacuumized, quartzy sealing cap is welded, completes stone
The sealing of English pipe；
S3: the temperature control of double crucible:
The temperature of upper crucible controls: being gradually heated to the melting point of polycrystal raw material, then maintains constant temperature；As the temperature rises
Lower crucible is slowly dropped by the material spilling hole of upper crucible bottom after polycrystal raw material and dopant thawing；When all raw material instills
After lower crucible, upper crucible continues to keep constant temperature, duration T；
The temperature of lower crucible controls: carrying out thermostatic control always to the temperature of lower crucible, temperature is controlled in polycrystal raw material
Melting point；After all raw material instills lower crucible, lower crucible continues to keep constant temperature, duration T.
S4: the cooling of double crucible completes crystal growth in lower crucible.
As an improved technical scheme, the polycrystal raw material is indium phosphide polycrystal raw material, and the dopant is sulphur.
As an improved technical scheme, in step S3, the temperature of described pair of upper crucible controls and the temperature control to lower crucible
System, temperatur-timel curve are preset in a program, carry out temperature control to upper crucible and lower crucible respectively by program.
As an improved technical scheme, in step S3, the temperature control of the upper crucible is control by stages, is specifically included
With the next stage:
First stage, heating start, and continue 2h, are warming up to 600 DEG C；
Second stage: continue 1.5h, be warming up to 850 DEG C；
Phase III: continue 2h, be warming up to 950 DEG C~1050 DEG C；
Fourth stage: continue 1h, be warming up to 1000 DEG C~1070 DEG C；
5th stage: duration 40h ± 1h, 1000 DEG C~1070 DEG C of constant temperature；5th stage included time T；
The temperature control of the lower crucible is 1000 DEG C~1070 DEG C of constant temperature, duration 46.5h ± 1h, includes time T.
As an improved technical scheme, after all raw material instills lower crucible, upper crucible and lower crucible continue to keep permanent
The duration T of temperature is 3~5h.
During beneficial having the technical effect that caused by the utility model grows S-InP single crystal material with VB method, adopt
With double crucible structure, and the crystal growth technique used using this double crucible, indium phosphide polycrystal raw material can be made and mixed
Miscellaneous dose of S is uniformly mixed, and reduces the carrier concentration deviation of S-InP monocrystal radial direction, crystal longitudinal direction carrier concentration deviation
It can control in (3-6) x1018/cm3, the crystal of high quality, high uniformity is obtained, and the piece rate of crystal improves
5%.
Detailed description of the invention
Fig. 1 is the longitudinal section structural drawing of double crucible provided by the embodiment of the utility model.
Fig. 2 is the temperatur-timel curve figure of upper crucible in the temperature controlled processes of the bright embodiment offer of this law.
Fig. 3 is the temperatur-timel curve figure of lower crucible in the temperature controlled processes of the bright embodiment offer of this law.
Specific embodiment
The utility model is described in further detail with specific embodiment with reference to the accompanying drawing.
As shown in Figure 1, crystal growth double crucible, which includes upper crucible 10 and lower crucible 20；Upper crucible
10 are arranged above lower crucible 20, and upper 10 bottom periphery of crucible and lower 20 opening periphery of crucible are tightly connected；Upper 10 bottom of crucible
For flat or downward projection of arcuate bottom, upper 10 bottom surface of crucible is provided with the material spilling hole 11 for leading to lower crucible 20, upper crucible 10
For placing raw material needed for crystal growth；Lower 20 lower part of crucible is taper, and bottom is provided with seed crystal chamber 21, and lower crucible 20 is used for
Crystal growth；Upper crucible 10 and lower crucible 20 are boron nitride crucible.
In use, double crucible is put into a quartz ampoule (conventional components, figure in do not show), by indium phosphide polycrystal block stock
It is put into upper crucible 10 with dopant sulphur, element sulphur at this time is added in upper crucible 10 with solid granular, the doping of sulphur
It is and to fully take into account its segregation coefficient in indium phosphide using the carrier concentration of required crystal as foundation, passes through
Science is calculated.Then a quartzy sealing cap (conventional components, figure in do not show) is covered at the top of quartz ampoule, then to quartz
Pipe is vacuumized, and after reaching suitable vacuum degree, is welded, is then heated to quartz ampoule, constant temperature to quartzy sealing cap
And the processes such as cooling, as the temperature rises, indium phosphide polycrystal block stock and dopant sulphur lead to after the thawing of upper crucible 10
The material spilling hole 11 for crossing 10 bottom surface of crucible slowly instills in lower crucible 20, completes crystal growth in lower crucible 20.
Based on above-mentioned double crucible, the present embodiment also discloses a kind of S-InP crystal growth technique, including following step
It is rapid:
S1: double crucible is put into a quartz ampoule, and indium phosphide polycrystal block stock and dopant sulphur are put into crucible 10；
S2: a quartzy sealing cap is covered at the top of quartz ampoule, then quartz ampoule is vacuumized, quartzy sealing cap is welded, completes stone
The sealing of English pipe；
S3: the heating and thermostatic control of double crucible
The heating and thermostatic control of upper crucible 10:
It is gradually heated to the melting point of indium phosphide polycrystal, then maintains constant temperature；Indium phosphide polycrystal raw material as the temperature rises
Lower crucible 20 is slowly dropped by the material spilling hole 11 of upper 10 bottom surface of crucible after melting with dopant sulphur；When under all raw material instillation
After crucible 20, upper crucible 10 continues to keep constant temperature, duration T；
As shown in Fig. 2, the heating and thermostatic control to upper crucible 10 are temperature control stage by stage, including with the next stage:
First stage, heating start, and continue 2h, are warming up to 600 DEG C；
Second stage: continue 1.5h, be warming up to 850 DEG C；
Phase III: continue 2h, be warming up to 950 DEG C~1050 DEG C；
Fourth stage: continue 1h, be warming up to 1000 DEG C~1070 DEG C；
5th stage: duration 40h ± 1h, 1000 DEG C~1070 DEG C of constant temperature；5th stage included time T；
The thermostatic control of lower crucible 20: as shown in figure 3, carrying out thermostatic control, temperature control always to the temperature of lower crucible 20
Make the melting point in indium phosphide polycrystal raw material；After all raw material instills lower crucible 20, lower crucible 20 continues to keep constant temperature, continues
Time is T.Wherein 1000 DEG C~1070 DEG C of thermostat temperature, duration 46.5h ± 1h include time T；
S4: double crucible is cooling, completes crystal growth in lower crucible 20.
The heating and thermostatic control of upper crucible 10 and the thermostatic control to lower crucible, temperatur-timel curve are set in advance in
In program, controlled by program.
Pass through the material spilling hole of upper 10 bottom of crucible after indium phosphide polycrystal raw material and dopant melt as the temperature rises
11 slowly instill lower crucible 20, can ensure that sulphur is full and uniform in upper crucible 10 to the temperature control of upper crucible 10 stage by stage
Be dissolved into indium phosphide raw material；The temperature of lower crucible 20 remains at 1070 DEG C, drips indium phosphide polycrystal and dopant sulphur
After entering lower crucible, be in melting state always, make element sulphur in indium phosphide material more sufficiently, uniform dissolution mixing；When upper
After all raw materials instill lower crucible 20 in crucible 10, continue constant temperature time T, time T is about 3~5h (liter of upper crucible 10
Warm and thermostatically controlled 5th stage and the thermostatic control time of lower crucible 20 include this time).
The raw material that the material spilling hole 11 of upper crucible 10 is set as needed one or more, but is to ensure that in crucible 10
The speed that lower crucible 20 is instilled after thawing is moderate, cannot be too fast, otherwise will cause S-InP mixing unevenly, influences final S-InP
The head piece of crystal and the carrier concentration deviation of cauda.The quantity that material spilling hole 11 is used in the present embodiment is one, is located at upper earthenware
10 bottom surface middle position of crucible.
After the completion of the heating and thermostatic control of double crucible, cooling treatment is carried out, S-InP monocrystalline is carried out in lower crucible 20
Growth.The crystal bar grown is sliced, the indices of a piece and cauda are measured, wherein being surveyed for carrier concentration
Obtain head piece 3.31x1018/cm3, cauda 5.13x1018/cm3, it can be seen that by double crucible disclosed in the utility model with
And crystal growth technique, the carrier concentration deviation of whole crystal head and tail portion is very small, can control in (3~6) x1018/
cm3Between, the crystal of high quality, high uniformity is not only obtained, the piece rate of crystal is further improved, piece rate can
Improve 5% or so.
The above is only the preferred embodiment of the present invention, is not intended to limit the utility model, for this field
Technical staff for, various modifications and changes may be made to the present invention.Within the spirit and principle of the utility model,
Without creative any modification, equivalent replacement, improvement and so on, should be included within the scope of protection of this utility model.
Claims (4)
1. a kind of crystal growth double crucible, which is characterized in that including the upper crucible for placing raw material and be used for crystal
The lower crucible of growth；The top of the lower crucible, upper crucible bottom periphery and lower crucible opening periphery is arranged in the upper crucible
It is tightly connected；The upper crucible bottom surface is provided with the material spilling hole for leading to the lower crucible；The upper crucible and lower crucible are heat
Solve boron nitride crucible.
2. double crucible according to claim 1, which is characterized in that the upper crucible bottom is flat or is downwardly projected
Arcuate bottom.
3. double crucible according to claim 1, which is characterized in that the quantity of the material spilling hole of the upper crucible bottom is one
It is a or multiple.
4. double crucible according to claim 1, which is characterized in that the lower crucible bottom is taper, and bottom is provided with
Seed crystal chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822255012.5U CN209537670U (en) | 2018-12-29 | 2018-12-29 | Crystal growth double crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201822255012.5U CN209537670U (en) | 2018-12-29 | 2018-12-29 | Crystal growth double crucible |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN209537670U true CN209537670U (en) | 2019-10-25 |
Family
ID=68267235
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201822255012.5U Active CN209537670U (en) | 2018-12-29 | 2018-12-29 | Crystal growth double crucible |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN209537670U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109576777A (en) * | 2018-12-29 | 2019-04-05 | 珠海鼎泰芯源晶体有限公司 | Crystal growth double crucible and crystal growth technique |
-
2018
- 2018-12-29 CN CN201822255012.5U patent/CN209537670U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109576777A (en) * | 2018-12-29 | 2019-04-05 | 珠海鼎泰芯源晶体有限公司 | Crystal growth double crucible and crystal growth technique |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101370970B (en) | Methods and apparatuses for manufacturing monocrystalline cast silicon and monocrystalline cast silicon bodies for photovoltaics | |
| US8231727B2 (en) | Crystal growth apparatus and method | |
| CN104911690B (en) | The growing method and grower of a kind of indium phosphide single crystal | |
| KR101030099B1 (en) | Indium phosphide substrate, indium phosphide single crystal and process for producing them | |
| CN109576777A (en) | Crystal growth double crucible and crystal growth technique | |
| CN104846437B (en) | What resistivity was evenly distributed mixes gallium crystalline silicon and preparation method thereof | |
| CN108166060A (en) | A kind of indium antimonide<211>The preparation method of direction monocrystalline | |
| CN109280978A (en) | A kind of preparation method of low dislocation indium antimonide<111>direction monocrystalline | |
| US7972439B2 (en) | Method of growing single crystals from melt | |
| CN109963967A (en) | The manufacturing method of compound semiconductor and compound semiconductor single crystal | |
| CN209537670U (en) | Crystal growth double crucible | |
| CN103255477B (en) | The growing method of a kind of shaped sapphire crystal and equipment | |
| CN206204472U (en) | It is capable of achieving quantity-produced crystal growing furnace | |
| CN106757331B (en) | A kind of polycrystal silicon ingot and preparation method thereof | |
| EP0751242A1 (en) | Process for bulk crystal growth | |
| CN107313110A (en) | A kind of p type inp single crystal preparation formula and preparation method | |
| CN106637383A (en) | Crystal growing furnace capable of realizing continuous production | |
| CN103774210A (en) | Equipment and method for producing crystal by vertical boat method | |
| JP3509556B2 (en) | Single crystal manufacturing method and manufacturing apparatus | |
| CN106591944B (en) | The forming method of monocrystal silicon and wafer | |
| Dutta | Bulk crystal growth of ternary III–V semiconductors | |
| CN100401602C (en) | Zinc oxide bluish violet light semiconductor growth using liquid phase epitaxial method | |
| US11866848B1 (en) | Method and system for liquid encapsulated growth of cadmium zinc telluride crystals | |
| US20190136404A1 (en) | Method for producing a semiconductor wafer of monocrystalline silicon, device for producing a semiconductor wafer of monocrystalline silicon and semiconductor wafer of monocrystalline silicon | |
| CN209194104U (en) | A kind of oval heater for sapphire crystallization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |