CN100564615C - The preparation method of multi-element compounds semiconductor single-crystal and growing apparatus - Google Patents
The preparation method of multi-element compounds semiconductor single-crystal and growing apparatus Download PDFInfo
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- CN100564615C CN100564615C CNB2007100490496A CN200710049049A CN100564615C CN 100564615 C CN100564615 C CN 100564615C CN B2007100490496 A CNB2007100490496 A CN B2007100490496A CN 200710049049 A CN200710049049 A CN 200710049049A CN 100564615 C CN100564615 C CN 100564615C
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Abstract
A kind of preparation method of multi-element compounds semiconductor single-crystal, processing step is: 1. clean crucible, 2. feed and the degasification sealed knot, 3. crystal growth, 4. annealing and cooling.Contain removable stove well heater down with the supporting single-crystal growing apparatus of this method and contain the monocrystal growing furnace of middle part auxiliary heater, it can be flexibly according to the crystal habit of multi-element compounds, realization is to the warm field control in crystallization temperature gradient district, obtain the crystallization temperature field distribution of the required narrow warm area of compound monocrystal growth, big temperature ladder, keep the stable of solid-liquid interface, realize the plane interface growth of single crystal.Use this growing apparatus, adopt falling crucible method can successfully grow the multiple multi-element compounds semiconductor single-crystal body that outward appearance is complete, crystal property is good.
Description
Technical field
The invention belongs to inorganic monocrystal material preparation field, particularly a kind of method of melt method for growing multi-element compounds semiconductor single-crystal and corresponding growing apparatus.
Background technology
Multi-element compounds semiconductor single-crystal, for example ZnGeP
2, CdGeAs
2, AgGaS
2, AgGaSe
2, AgGa
1-xIn
xSe
2, Cd
1-xZn
xTe etc., owing to have excellent infrared non-linear optical property or indoor temperature nucleus radiation detection performance, can be in the frequency inverted and the widespread use of indoor temperature nucleus radiation field of detecting of mid and far infrared wave band.Above-claimed cpd semiconductor single-crystal growth difficulty, general available Brigdman-Stockarger (being called for short the B-S method) method growing single-crystal, but these compound component are many, the fusing point difference is big, the saturated vapor pressure difference is big, high temperature easily decomposes down, and the melt viscosity factor is big in addition, also can produce the precipitation branch under the low temperature and parse second phase; Especially in the crystallisation process, owing to form the segregation coefficient difference of each constituent element material of compound, the heat conductivility difference of solid and melt is big in addition, along with the variation of solid-liquid amount in the crystal growing process, the temperature field of crystallizing field is changed, cause solid-liquid interface to drift about, be difficult to keep required flat (or dimpling) interface growth of crystal growth, so common B-S method is difficult to obtain the good compound semiconductor single crystal of integrity, has restricted the widespread use of its device.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of multi-element compounds semiconductor single-crystal the preparation method and with the matching used single-crystal growing apparatus of this method, the multiple multi-element compounds semiconductor single-crystal body that outward appearance is complete to prepare, crystal property is good.
The present invention is directed to the technological difficulties of multi-element compounds semiconductor single-crystal growth, design a kind of single-crystal growing apparatus with removable stove well heater down and middle part auxiliary heater, it can be flexibly according to the crystal habit of multi-element compounds, realization is to the warm field control in crystallization temperature gradient district, obtain the crystallization temperature field distribution of the required narrow warm area of compound monocrystal growth, big temperature ladder, keep the stable of solid-liquid interface, realize the plane interface growth of single crystal.Use this growing apparatus, it is complete to adopt falling crucible method can successfully grow outward appearance, the multiple multi-element compounds semiconductor single-crystal body that crystal property is good.
The preparation method of multi-element compounds semiconductor single-crystal of the present invention is a raw material with the multi-element compounds nulti-crystal powder, is growth container with the quartz crucible, comprises following processing step successively:
1. clean crucible
The cleaning crucible is the processing of the crucible inwall being removed impurity;
2. feed and the degasification sealed knot
With the multi-element compounds nulti-crystal powder pack into the cleaning after crucible in, the degasification of under 200 ℃～350 ℃, finding time then, the air pressure in crucible reduces to 10
-3～10
-4Sealed knot during Pa;
3. crystal growth
A, the crucible behind the sealed knot is put into monocrystal growing furnace, allow the crucible tip be positioned at 3～5cm place on the temperature-controlling thermal couple of stove well heater, to go up stove and be warming up to above 50 ℃～100 ℃ of multi-element compounds fusing point with the speed of 2～3 ℃/min, following stove is warming up to below the multi-element compounds fusing point, takes off more than the molten decomposition temperature with same speed, the controlled temperature of auxiliary heater is the melting temperature of multi-element compounds, be incubated 24 hours～36 hours
After B, above-mentioned insulation finish, with temperature-controlling thermal couple place, the speed decline crucible tip of 10mm/h～15mm/h to auxiliary heater, be incubated that the speed decline crucible with 0.2mm/h～0.5mm/h begins crystal growth after 4 hours～6 hours, through 2～4 time-of-weeks, allow melt all move through solid-liquid interface;
4. annealing and cooling
Finish behind the single crystal growth crucible is dropped to stove isothermal region annealing 2～4 days, outage is then taken out after allowing crystal ingot cool to room temperature with the furnace.
Multi-element compounds semiconductor single-crystal growing apparatus of the present invention, comprise body of heater, last stove well heater, auxiliary heater and the following stove well heater of independent heating temperature control separately, the heating element of last stove well heater and auxiliary heater axially is installed on the body of heater from top to bottom along body of heater successively, the heating assembly of following stove well heater is installed on the hoisting appliance of bottom, and its main body stretches into body of heater and is positioned under the heating element of auxiliary heater; At the heating element range of distribution of auxiliary heater l
2The overlapping from bottom to top composite thermal insulation layer of forming by lower floor's heat conduction ring, middle level heat conduction ring and upper strata heat insulating ring of having installed, the internal diameter of lower floor's heat conduction ring, middle level heat conduction ring and upper strata heat insulating ring and the physical dimension of multi-element compounds semiconductor single-crystal growth crucible are complementary; The temperature-controlling thermal couple of auxiliary heater is installed between upper strata heat insulating ring and the middle level heat conduction ring, the temperature-controlling thermal couple of last stove well heater is installed in the lower end of stove well heater heating element, the temperature-controlling thermal couple of following stove well heater is installed in down the upper end of stove well heater heating element, and last furnace temperature monitoring thermocouple is installed in stove well heater heating element range of distribution l
1The middle part.Zone between the temperature-controlling thermal couple of the temperature-controlling thermal couple of last stove well heater and following stove well heater is the crystallization temperature gradient district, operation bottom hoisting appliance, the heating assembly that makes down the stove well heater axially moves up and down along body of heater, can change the width in crystallization temperature gradient district.
The effect of upper strata heat insulating ring is to stop radiation, convection current and the conduction of the heat of stove high-temperature zone to gradient zones, to reduce the temperature difference of high-temperature zone, keeps the stable of temperature field; The effect of middle level heat conduction ring and lower floor's heat conduction ring is to form passage of heat, forms the required big temperature ladder of growth compound crystal by leading away the part heat.Therefore, the external diameter of lower floor's heat conduction ring is greater than the external diameter of middle level heat conduction ring and upper strata heat insulating ring, and the heat insulating layer of lower floor's heat conduction ring and body of heater joins.
Setting up of auxiliary heater helps to stablize solid-liquid interface.Experiment shows, the heating element range of distribution l of auxiliary heater
2Length be advisable with 8cm～12cm.
The present invention has following beneficial effect:
1, passes through the lift adjustment of stove well heater heating assembly down, can regulate the width in crystallization temperature gradient district neatly; Simultaneously the temperature controlling point of upper and lower stove is moved to the upper and lower edge in crystallization temperature gradient district by common well heater heating element middle part, avoided changing (because K because of the heat transfer property that change solid in the crystallisation process, the melt amount causes
s, K
lDifference is bigger).
2, adopt three layers of composite thermal insulation layer, help to produce the bigger temperature difference in the crystallization temperature gradient district, thereby the process of growth of solid-liquid interface is compressed in one than in the narrow region in the less Δ T on keeping stove high-temperature zone.
3, in the crystallization temperature gradient district, set up the short interval auxiliary heater heating element that distributes, its temperature controlling point is arranged on the solid-liquid interface place between upper strata heat insulating ring and the middle level heat conduction ring, help to stablize solid-liquid interface, it is not drifted about, also can further regulate simultaneously the warm field distribution in crystallization temperature gradient district, form the temperature field of narrow warm area, big gradient, this temperature field can reduce the crystalline component segregation in crystallisation process.
4, by temperature-controlling thermal couple being set, can understand and monitor the moving process of solid-liquid interface in real time, be equivalent to indirectly observe the moving process of solid-liquid interface, help to control the growth of complete monocrystalline at solid-liquid interface.
5, form on the basis in the terraced crystallization temperature gradient district of the big temperature of narrow warm area at crystal growing furnace, in crystal growing process, to go up furnace temperature and be arranged on 50～100 ℃ of scopes on the multi-element compounds fusing point, following furnace temperature is arranged on below the melting point compound, takes off on the molten decomposition temperature, help to solve that multi-element compounds semiconductor crystalline material high temperature easily decomposes, the problem of the easy precipitation of low temperature, also help to reduce the to grow stress of crystal ingot is for the good single crystal growing of integrity provides favourable condition guarantee.
Description of drawings
Fig. 1 is the structure diagram of crystal growing apparatus of the present invention and the synoptic diagram of crystal growth phase solid-liquid interface present position;
Fig. 2 is the warm field pattern of crystal growing furnace of the present invention;
Fig. 3 is the AgGaS of the method for the invention preparation
2The crystal ingot photo;
The AgGaS of Fig. 4 the method for the invention preparation
2The X-ray diffraction spectrum of crystal ingot cleavage surface;
Fig. 5 is the CdGeAs of device preparation of the present invention
2The multistage diffraction spectra of X ray of single crystal (101) face.
Among the figure, heating assembly, 12-bottom hoisting appliance, 13-top hoisting appliance, 14-crucible, 15-solid-liquid interface, the l of stove well heater under the temperature-controlling thermal couple of stove well heater, the 11-under the temperature-controlling thermal couple of the temperature-controlling thermal couple of the last furnace temperature of heating element, the 3-of 1-body of heater, the last stove well heater of 2-monitoring thermocouple, the last stove well heater of 4-, the heating element of 5-auxiliary heater, 6-upper strata heat insulating ring, 7-auxiliary heater, 8-middle level heat conduction ring, 9-lower floor heat conduction ring, the 10-
1Heating element range of distribution, the l of-last stove well heater
2The heating element range of distribution of-auxiliary heater, l
3The heating element range of distribution of-following stove well heater.
Embodiment
Embodiment 1: the multi-element compounds semiconductor single-crystal growing apparatus
In the present embodiment, the structure of multi-element compounds semiconductor single-crystal growing apparatus as shown in Figure 1, comprise body of heater 1, separately independent heating temperature control last stove well heater, auxiliary heater, down the stove well heater, go up furnace temperature monitor, lower floor's heat conduction ring 9, middle level heat conduction ring 8, upper strata heat insulating ring 6, bottom hoisting appliance 12, top hoisting appliance 13.
The heating element 2 of last stove well heater and the heating element 5 of auxiliary heater axially are installed on the body of heater from top to bottom along body of heater successively, the heating assembly 11 of following stove well heater is installed on the bottom hoisting appliance 12, and its main body stretches into body of heater and is positioned under the heating element of auxiliary heater;
Upper strata heat insulating ring 6 is made by heat insulating is cotton, and middle level heat conduction ring 8 is made by corundum, and lower floor's heat conduction ring 9 is made by uralite; The internal diameter of lower floor's heat conduction ring 9, middle level heat conduction ring 8 and upper strata heat insulating ring 6 and the physical dimension of multi-element compounds semiconductor single-crystal growth crucible are complementary, and the thickness sum of lower floor's heat conduction ring 9, middle level heat conduction ring 8 and upper strata heat insulating ring 6 is less than auxiliary heater heating element range of distribution l
2The composite thermal insulation layer that lower floor's heat conduction ring 9, middle level heat conduction ring 8 and upper strata heat insulating ring 6 are formed is with auxiliary heater heating element range of distribution l
2The lower end be benchmark, overlapping from bottom to top installation; The external diameter of lower floor's heat conduction ring 9 is greater than the external diameter of middle level heat conduction ring 8 and upper strata heat insulating ring 6, and the heat insulating layer of lower floor's heat conduction ring 9 and body of heater joins.
The temperature-controlling thermal couple 7 of auxiliary heater is installed between upper strata heat insulating ring 6 and the middle level heat conduction ring 8, and temperature-controlling thermal couple 7 places of auxiliary heater are crystal growth phase solid-liquid interface present position; The temperature-controlling thermal couple 4 of last stove well heater is installed in the lower end of stove well heater heating element, the temperature-controlling thermal couple 10 of following stove well heater is installed the upper end of stove well heater heating element down, and the zone between the temperature-controlling thermal couple of the temperature-controlling thermal couple of last stove well heater and following stove well heater is the crystallization temperature gradient district; Last furnace temperature monitoring thermocouple 3 is installed in stove well heater heating element range of distribution l
1The middle part.
Embodiment 2:AgGaS
2The preparation of single crystal
In the present embodiment, with AgGaS
2Nulti-crystal powder is a raw material, is growth container with the quartz crucible, uses embodiment 1 described crystal growing apparatus, in this device, and auxiliary heater heating element range of distribution l
2Length be 12cm.The preparation method comprises following processing step successively:
1. clean crucible
The cleaning crucible adopts comprehensive the cleaning and the vacuum bakeout process combined, at first soak flushing crucible inwall with tap water, injecting the hydrofluoric acid washing lotion then soaked 3 minutes, extremely neutral with the tap water flushing again, place the ultrasonic cleaner vibration to clean 8 minutes and washed repeatedly at last with the high resistant deionized water, cleaned crucible is placed vacuum drying oven, and temperature is controlled at 130 ℃, and storing time is 3.5 hours;
2. feed and the degasification sealed knot
With 100g left and right sides AgGaS
2Polycrystal powder pack into the cleaning after crucible in, the degasification of under 300 ℃, finding time then, the air pressure in crucible reduces to 10
-3Pa uses the oxyhydrogen flame sealed knot down,
3. crystal growth
The crucible of A after with sealed knot put into monocrystal growing furnace, allow the crucible tip be positioned at 4cm place on the temperature-controlling thermal couple of stove well heater, to go up stove and be warming up to 1080 ℃ with the speed of 3 ℃/min, following stove is warming up to 880 ℃ with same speed, and the controlled temperature of auxiliary heater is AgGaS
2996 ℃ of fusing points, be incubated 24 hours,
After B, above-mentioned insulation finish, with temperature-controlling thermal couple 7 places, the speed decline crucible tip of 12mm/h to auxiliary heater, be incubated that the speed decline crucible with 0.3mm/h begins crystal growth after 5 hours,, allow melt all move through the solid-liquid interface crystallization through 3 all left and right sides times;
4. annealing and cooling
Finish behind the single crystal growth crucible is dropped to stove isothermal region annealing 3 days, outage is then taken out after allowing crystal ingot cool to room temperature with the furnace.
The AgGaS that present embodiment is prepared
2Single crystal is seen Fig. 3, AgGaS
2The X-ray diffraction spectrum of crystal ingot cleavage surface is seen Fig. 4, and from figure as can be seen, crystalline structure is complete, crystal property good.
Embodiment 3:CdGeAs
2The preparation of single crystal
In the present embodiment, with CdGeAs
2Nulti-crystal powder is a raw material, is growth container with the quartz crucible, uses embodiment 1 described crystal growing apparatus, in this device, and auxiliary heater heating element range of distribution l
2Length be 8cm.The preparation method comprises following processing step successively:
1. clean crucible
The cleaning crucible adopts comprehensive the cleaning and the vacuum bakeout process combined, at first soak flushing crucible inwall with tap water, injecting the hydrofluoric acid washing lotion then soaked 3 minutes, extremely neutral with the tap water flushing again, place the ultrasonic cleaner vibration to clean 8 minutes and washed repeatedly at last with the high resistant deionized water, cleaned ampoule is placed vacuum drying oven, and temperature is controlled at 130 ℃, and storing time is 3.5 hours;
2. feed and the degasification sealed knot
With 30g left and right sides CdGeAs
2Polycrystal powder is packed in the crucible after the cleaning, and in the room temperature degasification of finding time, the air pressure in crucible reduces to 10 then
-3Pa uses the oxyhydrogen flame sealed knot down;
3. crystal growth
The crucible of A after with sealed knot put into monocrystal growing furnace, allow the crucible tip be positioned at 3cm place on the temperature-controlling thermal couple of stove well heater, to go up stove and be warming up to 730 ℃ with the speed of 2 ℃/min, following stove is warming up to 500 ℃ with same speed, and the controlled temperature of auxiliary heater is CdGeAs
2654 ℃ of fusing points, be incubated 36 hours,
After B, above-mentioned insulation finish, with temperature-controlling thermal couple 7 places, the speed decline crucible tip of 10mm/h to auxiliary heater, be incubated that the speed decline crucible with 0.2mm/h begins crystal growth after 4 hours,, allow melt all move through solid-liquid interface through 2 all left and right sides times;
4. annealing and cooling
Finish behind the single crystal growth crucible is dropped to stove isothermal region annealing 72 hours, outage is then taken out after allowing crystal ingot cool to room temperature with the furnace.
The CdGeAs that present embodiment is prepared
2The multistage diffraction spectra of X ray of single crystal (101) face is seen Fig. 5.
Claims (6)
1, a kind of preparation method of multi-element compounds semiconductor single-crystal is a raw material with the multi-element compounds nulti-crystal powder, is growth container with quartz crucible (14), it is characterized in that comprising successively following processing step:
1. clean crucible
The cleaning crucible is the processing of the crucible inwall being removed impurity;
2. feed and the degasification sealed knot
With the multi-element compounds nulti-crystal powder pack into the cleaning after crucible in, the degasification of under 200 ℃～350 ℃, finding time then, the air pressure in crucible reduces to 10
-3～10
-4Sealed knot during Pa;
3. crystal growth
A, the crucible behind the sealed knot (14) is put into monocrystal growing furnace, allow the crucible tip be positioned at 3～5cm place on the temperature-controlling thermal couple (4) of stove well heater, to go up stove and be warming up to above 50 ℃～100 ℃ of multi-element compounds fusing point with the speed of 2～3 ℃/min, following stove is warming up to below the multi-element compounds fusing point, takes off more than the molten decomposition temperature with same speed, the controlled temperature of auxiliary heater is the melting temperature of multi-element compounds, be incubated 24 hours～36 hours
After B, above-mentioned insulation finish, speed decline crucible tip to the temperature-controlling thermal couple (7) of auxiliary heater with 10mm/h～15mm/h is located, be incubated that the speed decline crucible with 0.2mm/h～0.5mm/h begins crystal growth after 4 hours～6 hours, through 2 week～4 time-of-weeks, allow melt all move through solid-liquid interface (15);
4. annealing and cooling
Finish behind the single crystal growth crucible is dropped to stove isothermal region annealing 2 days～4 days, outage is then taken out after allowing crystal ingot cool to room temperature with the furnace;
Described multi-element compounds nulti-crystal powder is ZnGeP
2Nulti-crystal powder, CdGeAs
2Nulti-crystal powder, AgGaS
2Nulti-crystal powder, AgGaSe
2Nulti-crystal powder, AgGa
1-xIn
xSe
2Nulti-crystal powder, Cd
1-xZn
xA kind of in the Te nulti-crystal powder.
2, a kind of multi-element compounds semiconductor single-crystal growing apparatus, comprise body of heater (1), it is characterized in that also comprising last stove well heater, auxiliary heater and the following stove well heater of independent separately heating temperature control, the heating element (2) (5) of last stove well heater and auxiliary heater axially is installed on the body of heater from top to bottom along body of heater successively, the heating assembly (11) of following stove well heater is installed on the bottom hoisting appliance (12), its main body stretches into body of heater and is positioned under the heating element of auxiliary heater
At the heating element range of distribution of auxiliary heater l
2The overlapping from bottom to top composite thermal insulation layer of forming by lower floor's heat conduction ring (9), middle level heat conduction ring (8) and upper strata heat insulating ring (6) of having installed, the internal diameter of lower floor's heat conduction ring (9), middle level heat conduction ring (8) and upper strata heat insulating ring (6) and the physical dimension of multi-element compounds semiconductor single-crystal growth crucible are complementary
The temperature-controlling thermal couple of auxiliary heater (7) is installed between upper strata heat insulating ring (6) and the middle level heat conduction ring (8), the temperature-controlling thermal couple of last stove well heater (4) is installed in the lower end of stove well heater heating element, the temperature-controlling thermal couple of following stove well heater (10) is installed the upper end of stove well heater heating element down, and last furnace temperature monitoring thermocouple (3) is installed in stove well heater heating element range of distribution l
1The middle part.
3, multi-element compounds semiconductor single-crystal growing apparatus according to claim 2, it is characterized in that the external diameter of the external diameter of lower floor's heat conduction ring (9), and the heat insulating layer of lower floor's heat conduction ring (9) and body of heater joins greater than middle level heat conduction ring (8) and upper strata heat insulating ring (6).
4, according to claim 2 or 3 described multi-element compounds semiconductor single-crystal growing apparatuss, it is characterized in that upper strata heat insulating ring (6) by the cotton making of heat insulating, middle level heat conduction ring (8) is made by corundum, and lower floor's heat conduction ring (9) is made by uralite.
5,, it is characterized in that the heating element range of distribution l of auxiliary heater according to claim 2 or 3 described multi-element compounds semiconductor single-crystal growing apparatuss
2Length be 8cm～12cm.
6, multi-element compounds semiconductor single-crystal growing apparatus according to claim 4 is characterized in that the heating element range of distribution l of auxiliary heater
2Length be 8cm～12cm.
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|---|---|---|---|
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| CN102534758A (en) * | 2012-01-20 | 2012-07-04 | 上海中电振华晶体技术有限公司 | Growth method and growth device for bar-shaped sapphire crystals |
| CN102560631A (en) * | 2012-01-20 | 2012-07-11 | 上海中电振华晶体技术有限公司 | Growth method and equipment of sapphire crystal |
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