CN202107793U - Adjustable pressure synthesis container - Google Patents
Adjustable pressure synthesis container Download PDFInfo
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- CN202107793U CN202107793U CN201120210437XU CN201120210437U CN202107793U CN 202107793 U CN202107793 U CN 202107793U CN 201120210437X U CN201120210437X U CN 201120210437XU CN 201120210437 U CN201120210437 U CN 201120210437U CN 202107793 U CN202107793 U CN 202107793U
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- crucible
- layer crucible
- inner crucible
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Abstract
The utility model relates to an adjustable pressure synthesis container, which is formed by combining an inner layer crucible and an outer layer crucible, wherein the inner layer crucible is a silica tube with one open end and one sealed end in the original state, the end part of the sealed end of the inner layer crucible is provided with a support rod, the outer layer crucible is a silica tube with one open end and one end sealed by a support sleeve in the original state, the inner diameter of the outer layer crucible is greater than the outer diameter of the inner layer crucible, the length of the outer layer crucible is greater than the length of the inner layer crucible, and the inner diameter and the length of the support sleeve of the outer layer crucible are matched with the support rod arranged on the inner layer crucible. The inner layer crucible is a silica tube with two sealed ends in the work state, the end parts of the two sealed ends of the inner layer crucible are respectively provided with support rods, the outer layer crucible is a silica tube with two ends respectively sealed by support sleeves in the work state, the inner layer crucible is positioned in the outer layer crucible, the support rods arranged at the end parts of the two sealed ends of the inner layer crucible are respectively inserted into the support sleeves arranged at both ends of the outer layer crucible, and the outer wall of the inner layer crucible and the inner wall of the outer layer crucible form an annular air chamber.
Description
Technical field
The utility model belongs to the ternary semiconductor field of material preparation, particularly a kind of polycrystal synthetic container that is used for.
Background technology
The multicrystal synthetic direct synthesis technique that is mostly of ternary semiconductor, but when synthesizing some compound, because high (for example, the synthetic CdSiP of the vp of raw material
2Polycrystal, the about 20atm of phosphorus vp in the time of 550 ℃), at high (for example, the CdSiP of dissociation pressure of melting temperature
2The about 22atm of polycrystalline), thereby very easily causes the quartz crucible blast, make synthetic very difficulty.Patent ZL200710049050.9 discloses a kind of two regional vapor transportation synthesising containers, is made up of body and feed-pipe, and body is the quartz glass tube of closed at both ends; The one of which end is A; The other end is B, is that the x place is provided with groove in the length apart from body B end end, and the degree of depth h of this groove is 1/2～2/3 of a body inner diameter d; It is being in portion's section of x apart from body B end tip lengths that feed-pipe passes through mutually; Its opening for feed and groove notch are in the opposite direction, and the angle β of its axis and body axis is 45～70 °, and material is a silica glass.Though this kind synthesising container can effectively stop the slippage of phosphorus raw material; Combine with the real-time temperature control of two warm areas that the synthetic initial stage adopts; Guaranteed that phosphorus reacts with other raw material from the A end that the B end of crucible all is transported to crucible with the form of gas phase safely; Solved the explosive technical barrier of crucible when synthetic, but manufacture difficulty is bigger, the encapsulation difficulty of charging and crucible is bigger.
Summary of the invention
The purpose of the utility model provides a kind of adjustable container that is pressed into, and when improving the synthesising container voltage endurance capability, reduces manufacture difficulty and the charging and the encapsulation difficulty of synthesising container.
The said adjustable container that is pressed into of the utility model; Combined by inner crucible and outer crucible, the original state of inner crucible is the silica tube of an end opening, end sealing, and its closedend end is provided with support bar; The original state of outer crucible is the silica tube that an end opening, an end are sealed by support set; Its internal diameter is greater than the external diameter of inner crucible, and its length is greater than the length of inner crucible, and the support bar of the internal diameter of its support set and length and inner crucible setting is complementary; The working order of inner crucible is the silica tube of closed at both ends; Its two closedends end is provided with support bar; The working order of outer crucible is the silica tubes of two ends by the support set sealing; Inner crucible is positioned at outer crucible, and the support bar that its two closedends end is provided with inserts the support set at outer crucible two ends respectively, and the outer wall of inner crucible surrounds ring-shaped air chamber with the inwall of outer crucible.
The said adjustable container that is pressed into of the utility model, preferred 3 mm of the thickness～6mm of the outer wall of inner crucible and the ring-shaped air chamber that inwall surrounded of outer crucible.
The utlity model has following beneficial effect:
1, the said adjustable container that is pressed into of the utility model adopts double-deck quartz crucible structure; And the inner crucible outer wall with outside fill with nitrogen in the ring-shaped air chamber that surrounds of crucible inwall; Can be with the synthetic middle high-vapor-pressure that produces of ternary semiconductor polycrystal high temperature; Mode through inner crucible wall, inflated with nitrogen chamber, outer sidewall of crucible successively reduce pressure successively is delivered to space outerpace, thereby effectively reduces the pressure difference of internal layer (individual layer) sidewall of crucible both sides; Improve the voltage endurance capability of quartz crucible, had good explosion-proof function.
2, because the said adjustable container that is pressed into of the utility model is double-deck quartz crucible structure, thereby can be according to the synthesis technique needs, the nitrogen amount of filling of the ring-shaped air chamber that adjustment inner crucible outer wall and outer crucible inwall surround, thereby the voltage endurance capability of adjustment synthesising container;
3, compare with ZL200710049050.9 patent disclosed two regional vapor transportation synthesising containers; The said adjustable manufacture difficulty that container not only greatly reduces crucible that is pressed into of the utility model; With the synthesis material crucible same position of packing into, also simplified the difficulty of charging and crucible encapsulation greatly.
Description of drawings
Fig. 1 is the said adjustable structural representation that is pressed into the inner crucible of container in original state of the utility model;
Fig. 2 is the said adjustable structural representation that is pressed into the outer crucible of container in original state of the utility model;
Fig. 3 is the said adjustable inner crucible and the combination synoptic diagram of outer crucible in the charging process that is pressed into container of the utility model;
Fig. 4 is the said adjustable container structural representation in working order that is pressed into of the utility model;
Fig. 5 is the said adjustable a kind of placement synoptic diagram in two zone heating tube furnaces behind the container loading that are pressed into of the utility model.
Among the figure, 1-inner crucible, 2-feed-pipe, 3-support bar, the outer crucible of 4-, 5-support set, 6-extraction pipe, 7-cadmium, silicon, phosphorus raw material, 8-nitrogen, 9-phosphorous vapor, 10-cadmium vapor, 11-phosphorus cadmic compound, 12-body of heater, 13-heating unit, 14-high-temperature zone I temperature-control heat couple, 15-high-temperature zone II temperature-control heat couple, 16-cold zone III temperature monitoring thermopair.
Embodiment
Adjustablely be pressed into container and be used for multicrystal synthetic being described further of phosphorus silicon cadmium the utility model is said through embodiment below in conjunction with accompanying drawing.
In the present embodiment, adjustable shape and the structure that is pressed into container is as shown in Figure 4, is combined by inner crucible 1 and outer crucible 4.The original state of inner crucible is the silica tube of an end opening, end sealing, and its closedend end is provided with support bar 3, and its opening end is connected with feed-pipe 2, and is as shown in Figure 1.The original state of outer crucible 4 is the silica tube that an end opening, an end are sealed by support set 5; Its internal diameter is greater than the external diameter of inner crucible; Its length is greater than the length of inner crucible, and the support bar of the internal diameter of its support set and length and inner crucible setting is complementary, and is as shown in Figure 2.
The working order of inner crucible is the silica tube of closed at both ends; Its two closedends end is provided with support bar 3; The working order of outer crucible 4 is the silica tubes of two ends by support set 5 sealings, and their assembling mode is: inner crucible is positioned at outer crucible, and the support bar 3 that its two closedends end is provided with inserts the support set 5 at outer crucible two ends respectively; The outer wall of inner crucible surrounds ring-shaped air chamber with the inwall of outer crucible, and is as shown in Figure 4.
In the present embodiment, the outer wall of inner crucible 1 is 4mm with the thickness H of the ring-shaped air chamber that inwall surrounded of outer crucible 4.
Inner crucible and outer crucible are as shown in Figure 3 from the assemble method of original state to working order: with pack into the closedend of inner crucible of load weighted raw material, vacuumizing degasification then, is 10 at pressure
-3Sealed knot inner crucible during Pa, and support bar 3 is set at the sealed knot end of inner crucible, then that sealed knot is the good inner crucible outer crucible of packing into makes the support bar 3 of one of which end insert the support set 5 of outer crucible; The opening end of crucible is fired and is connected an extraction pipe 6 outside, vacuumizes degasification then, and the pressure in the crucible is 10 outside
-3In it, charge into high pure nitrogen during Pa to pressure 2.0atm, continue after sealed knot extraction pipe 6, extraction pipe behind the sealed knot forms support set.
Present embodiment uses the embodiment 1 said adjustable synthetic CdSiP of container that is pressed into
2Polycrystal.Raw material cadmium (Cd), silicon (Si), phosphorus (P) are the 6N level, and during batching, the mol ratio of each raw material is Si: Cd: P=1: 1: 2; The add-on of phosphorus increases by 0.5% on the weight basis of calculating by above-mentioned mol ratio, according to aforementioned proportion, and cadmium 11.76145 grams; Silicon 2.93980 grams, phosphorus 6.51391 grams.
The structure of synthetic used two zone heating tube furnaces is seen Fig. 5; Comprise body of heater 12, be installed in the heating unit 13 at body of heater two ends; The two ends of said two zone heating tube furnaces are respectively high-temperature zone I and high-temperature zone II; The center is cold zone III, and high-temperature zone I is equipped with that temperature-control heat couple 14, high-temperature zone II are equipped with temperature-control heat couple 15, cold zone III is equipped with temperature monitoring thermopair 16.
Process step is following:
(1) cleaning of synthesising container is with dry
After soaking flushing inner crucible and outer crucible inwall with tap water; Injected hydrofluoric acid dips more respectively 3～5 minutes; Then with tap water flushing to neutral, place the ultrasonic cleaning tank vibration to clean 8～10 minutes, rinse well repeatedly with the high resistant deionized water again and get final product.With inner crucible after cleaning and the outer crucible mark that drains the water, place on the rough vacuum mechanical pump, externally (heating and temperature control is at 130 ℃) aspirate under the condition of heating, remove the water vapour of crucible inside after, take off subsequent use;
(2) charging
With pack into the successively closedend B of inner crucible of load weighted silicon, cadmium, phosphorus, vacuumize degasification then, be 10 at pressure
-3Sealed knot inner crucible during Pa; And support bar 3 is set at the sealed knot end A of inner crucible; The inner crucible that sealed knot is the good outer crucible of packing into makes the support bar of its closedend B insert the support set 5 of outer crucible, and the opening end of crucible is fired extraction pipe 6 of connection outside; Vacuumize degasification then, the pressure in the crucible is 10 outside
-3In it, charge into high pure nitrogen during Pa to pressure 2.0atm, continue after sealed knot extraction pipe 6, extraction pipe behind the sealed knot forms support set, is used for the support bar 3 that plug-in mounting inner crucible sealed knot end A is provided with.
(3) synthetic
The synthesising container that 1. raw material and sealed knot at first will be housed is put into two zone heating tube furnaces of horizontal positioned; The B end that raw material is housed is positioned at high-temperature zone II; The A end that is unkitted raw material is positioned at high-temperature zone I, and the middle part C of synthesising container is positioned at cold zone III, and the place, two ends of synthesising container is temperature controlling point; The middle part of synthesising container is the temperature monitoring point, and is as shown in Figure 5;
2. high-temperature zone I, the high-temperature zone II with two zone heating tube furnaces all was heated to 550 ℃ with the speed of 60 ℃/h simultaneously, and this moment, the temperature of cold zone III was 520～530 ℃, this temperature insulation 24 hours; Speed with 2.5 ℃/h is heated to 600 ℃ simultaneously with said high-temperature zone I, high-temperature zone II then; This moment, the temperature of cold zone III was 570～580 ℃; This temperature insulation 24 hours; In this stage, phosphorus and C zone, cadmium vapor transportation to inner crucible middle part fully reaction generate the phosphorus cadmic compound and condense upon this, and silicon is still stayed inner crucible B end; Continue after with the speed of 10 ℃/h said high-temperature zone I, high-temperature zone II are continued heating simultaneously; When the temperature at place, synthesising container two ends rises to 850 ℃; 90 ° of rotating furnace bodies make the axial perpendicular to the ground and inner crucible B end of synthesising container downward, and fused phosphorus cadmic compound is mixed with silicon; When rotating furnace body and body of heater rotation still said high-temperature zone I and high-temperature zone II are heated after putting in place with the speed of 10 ℃/h, reach 1180 ℃ until the temperature of said high-temperature zone I, high-temperature zone II;
3. after the temperature of said high-temperature zone I, high-temperature zone II reaches 1180; Be incubated 30 hours; The discontinuity rotating furnace carries out mechanical oscillation in the time of insulation; And between 1180 ℃ and 1110 ℃, carry out temperature oscillation 5 times, make reaction of material thorough mixing and the molten intravital phosphorous vapor more than needed of elimination in the synthesising container;
4., after building-up reactions accomplishes, high-temperature zone I (inner crucible A end) is maintained 1180 ℃, high-temperature zone II (inner crucible B end) is cooled to 900 ℃ with the speed of 80 ℃/h, then, high-temperature zone I, the speed of high-temperature zone II while with 60 ℃/h is cooled to room temperature.
Claims (2)
1. the adjustable container that is pressed into is characterized in that said synthesising container is combined by inner crucible (1) and outer crucible (4),
The original state of inner crucible is the silica tube of an end opening, end sealing; Its closedend end is provided with support bar (3); The original state of outer crucible (4) is the silica tube that an end opening, an end are sealed by support set (5), and its internal diameter is greater than the external diameter of inner crucible, and its length is greater than the length of inner crucible; The support bar of the internal diameter of its support set and length and inner crucible setting is complementary
The working order of inner crucible is the silica tube of closed at both ends; Its two closedends end is provided with support bar (3); The working order of outer crucible (4) is the silica tubes of two ends by support set (5) sealing; Inner crucible is positioned at outer crucible, and the support bar (3) that its two closedends end is provided with inserts the support set (5) at outer crucible two ends respectively, and the outer wall of inner crucible surrounds ring-shaped air chamber with the inwall of outer crucible.
2. the adjustable container that is pressed into according to claim 1, the outer wall that it is characterized in that inner crucible (1) is 3mm～6mm with the thickness of the ring-shaped air chamber that inwall surrounded of outer crucible (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120210437XU CN202107793U (en) | 2011-06-21 | 2011-06-21 | Adjustable pressure synthesis container |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120210437XU CN202107793U (en) | 2011-06-21 | 2011-06-21 | Adjustable pressure synthesis container |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202107793U true CN202107793U (en) | 2012-01-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201120210437XU Expired - Lifetime CN202107793U (en) | 2011-06-21 | 2011-06-21 | Adjustable pressure synthesis container |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202107793U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344126A (en) * | 2011-06-21 | 2012-02-08 | 四川大学 | Synthesis method and synthesis container of phosphorus-silicon-cadmium polycrystal |
| CN104051628A (en) * | 2014-06-26 | 2014-09-17 | 中国科学院电工研究所 | Method for preparing organic/inorganic hybrid perovskite membrane and purposes of membrane |
| CN105908254A (en) * | 2016-06-12 | 2016-08-31 | 中国科学院上海技术物理研究所 | Casing pipe type cavity structure for preparing semiconductor material |
-
2011
- 2011-06-21 CN CN201120210437XU patent/CN202107793U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344126A (en) * | 2011-06-21 | 2012-02-08 | 四川大学 | Synthesis method and synthesis container of phosphorus-silicon-cadmium polycrystal |
| CN102344126B (en) * | 2011-06-21 | 2013-01-23 | 四川大学 | Synthesis method and synthesis container of phosphorus-silicon-cadmium polycrystal |
| CN104051628A (en) * | 2014-06-26 | 2014-09-17 | 中国科学院电工研究所 | Method for preparing organic/inorganic hybrid perovskite membrane and purposes of membrane |
| CN104051628B (en) * | 2014-06-26 | 2017-02-15 | 中国科学院电工研究所 | Method for preparing organic/inorganic hybrid perovskite membrane and purposes of membrane |
| CN105908254A (en) * | 2016-06-12 | 2016-08-31 | 中国科学院上海技术物理研究所 | Casing pipe type cavity structure for preparing semiconductor material |
| CN105908254B (en) * | 2016-06-12 | 2018-07-06 | 中国科学院上海技术物理研究所 | A kind of bushing type cavity body structure for being used to prepare semi-conducting material |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20120111 Effective date of abandoning: 20130710 |
|
| RGAV | Abandon patent right to avoid regrant |