CN201031265Y

CN201031265Y - Two regions gas-phase transport synthesizing container

Info

Publication number: CN201031265Y
Application number: CNU2007200794779U
Authority: CN
Inventors: 朱世富; 赵北君; 何知宇; 陈观雄
Original assignee: Sichuan University
Current assignee: Sichuan University
Priority date: 2007-05-09
Filing date: 2007-05-09
Publication date: 2008-03-05
Anticipated expiration: 2017-05-09

Abstract

The utility model relates to a two-zone vapor-phase transport synthetic vessel, comprising a main body and a feeding pipe. The main body is a quartz-glass tube with two closed ends (End A and End B). A groove is arranged at the location x (length) from End B of the main body, the groove is h deep (1/2-2/3 of the inside diameter (d) of the main body); the feeding pipe is intersected in the segment x (length) from End B of the main body, and the direction of the feeding hole is opposite to the rabbet of the groove, and the axial line of the feeding pipe and the axial line of the main body form an included angle of 45-70 degrees, and the material adopts quartz glass. The synthetic vessel can effectively prevent the material arranged at one end of the vessel from sliding to the other end; because the vessel combines 2-temperature-zone real-time control adopted at the early stage of synthesis, high-vapor-pressure raw material can be transported (in gas-phase form) from End B to End A of the vessel safely to react with other raw materials.

Description

Two regional vapor transportation synthesising containers

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 method of ternary compound mostly is direct synthesis technique, but when synthetic some compound (ZnGeP for example ₂), since the vapour pressure height of raw material (for example P is 12.1atm in the time of 530 ℃; Zn is 4atm in the time of 1030 ℃), very easily cause to synthesize and use container explosion, produce the material of inflammable severe toxicity.Therefore, restricted the acquisition of high-purity single-phase polycrystalline body.Though existing syntheticly have multiple structure with container, is difficult to adapt to the requirement of technology, the synthetic safely ternary compound polycrystal that is raw material with high vapour pressure material.

Summary of the invention

The purpose of this utility model is to overcome the deficiencies in the prior art, a kind of two regional vapor transportation synthesising containers of novel texture are provided, this kind synthesising container combines with rational technology, can be safely the ternary compound polycrystal synthesizes to being raw material with high vapour pressure material.

Described in the utility model two regional vapor transportation synthesising containers are made of body and feed-pipe, body is the quartz glass tube of closed at both ends, the one end is A, the other end is B, and the length in distance body B end end is that the x place is provided with groove, and the degree of depth h of this groove is 1/2～2/3 of a body inner diameter d, it is in portion's section of x that feed-pipe passes through in distance body B end tip lengths mutually, its opening for feed is opposite with groove notch direction, and the angle β of its axis and body axis is 45～70 °, and material is a silica glass.

Experiment shows that the length y of the groove that is provided with on the body is at least 15mm, preferred 20mm～30mm: apart from the length x of body B end end be body length l 1/10～1/7.

The beneficial effects of the utility model: use the container that is provided with groove structure to synthesize, can effectively stop the raw material that places container one end to the other end slippage, combine with the real-time temperature control of two warm areas that the synthetic initial stage adopts, guaranteed that high vapour pressure raw material reacts with other raw material from the A end that the B end of container all is transported to container safely with the form of gas phase, solved the explosive technical barrier of synthesising container when synthetic.

Description of drawings

Fig. 1 is a kind of structure iron of provided by the utility model two regional vapor transportation synthesising containers;

Fig. 2 is a kind of synoptic diagram behind synthesising container charging and the sealed knot;

Fig. 3 is synthetic assembling synoptic diagram with two warm area tube furnace bodies of heater and support;

Fig. 4 is the assembly drawing of synthetic fashion material container and two warm area tube furnaces and the warm field pattern in the stove;

Fig. 5 is synthetic product ZnGeP ₂Multicrystal X-ray diffraction spectrogram.

Among the figure, 1-body, 2-feed-pipe, 3-opening for feed, 4-germanium and zinc, 5-phosphorus, 6-body of heater, 7-support, 8-hinge, 9-heating unit, 10-explosion-proof monitoring thermocouple, 11-cold zone temperature-controlling thermal couple, 12-high-temperature zone temperature-controlling thermal couple, 13-monitoring are with temperature controller, 14-cold zone heating temperature controller, 15-high-temperature zone heating temperature controller, the I-synthetic initial stage temperature curve of field distribution, II-post-synthesis phase temperature curve of field distribution.

Embodiment

1: two regional vapor transportation synthesising container of embodiment

In the present embodiment, the shape of two regional vapor transportation synthesising containers and structure are as shown in Figure 1, constitute by body 1 and feed-pipe 2, body 1 is internal diameter 28mm, the quartz glass tube of the closed at both ends of length 400mm, the one end is A, the other end is B, length in distance body B end end is that the 45mm place is provided with groove, the length y of this groove is 25mm, degree of depth h is 1/2 of a body inner diameter d, it is in portion's section of 45mm that feed-pipe 2 passes through in distance body B end tip lengths mutually, its opening for feed 3 is opposite with groove notch direction, and the angle β of its axis and body axis is 60 °, and material is a silica glass.

Embodiment 2: synthetic with two warm area tube furnaces

In the present embodiment, synthetic structure with two warm area tube furnaces comprises body of heater 6, is installed in heating unit 9 on the body of heater, heats temperature controller 15 by the hinged support 7 of hinge 8 and body of heater, explosion-proof monitoring thermocouple 10, cold zone temperature-controlling thermal couple 11, high-temperature zone temperature-controlling thermal couple 12, monitoring with temperature controller 13, cold zone heating temperature controller 14 and high-temperature zone as shown in Figure 3, Figure 4.The assembling mode of above-mentioned member is as follows:

Heating unit 9 is along the axial distribution of body of heater and connect into two groups of independently heating systems, one group of cold zone heat supply that heating systems is a stove, and another group heating systems is the high-temperature zone heat supply of stove;

The temperature-sensitive end of explosion-proof monitoring thermocouple 10 is installed in the outer wall C place of the crucible body recess that contacts with phosphorus, and its other end is connected with temperature controller 13 with monitoring;

The temperature-sensitive end of cold zone temperature-controlling thermal couple 11 is installed in the cold zone that 5 sections of phosphorus are housed in the stove, and is positioned at the temperature-sensitive end corresponding section D with explosion-proof monitoring thermocouple 10, and its other end is connected with temperature control instrument in the cold zone heating temperature controller 14;

The high-temperature zone temperature-controlling thermal couple is installed in the furnace high-temperature district, and is positioned at the section corresponding section E of portion that the crucible body is equipped with germanium and zinc 4, and its other end is connected with the temperature control instrument that heat in the temperature controller 15 high-temperature zone;

Heating circuit in the cold zone heating temperature controller 14 is connected with the heating unit 9 that is installed in the body of heater cold zone, and the heating circuit in the high-temperature zone heating temperature controller 15 is connected with the heating unit 9 that is installed in the body of heater high-temperature zone.

Embodiment 3:ZnGeP ₂Multicrystal synthetic

In the present embodiment, the raw material zinc (Zn) of employing, germanium (Ge), phosphorus (P) are the 6N level, during batching, the mol ratio of each raw material is a zinc: germanium: phosphorus=1: 1: 2, prepare burden according to the suitable rich phosphorus of aforementioned proportion: zinc 8.87481 grams, germanium 9.8558l gram, phosphorus 8.41137 grams.Synthetic used container is embodiment 1 described two a regional vapor transportation synthesising container; Synthetic used tube furnace is embodiment 2 described two warm area tube furnaces.

The synthesis technique step is as follows:

1, the cleaning of synthesising container is with dry

After soaking flushing synthesising container inwall with tap water, inject the hydrofluoric acid washing lotion and soaked 3～5 minutes, then with the tap water flushing to neutral, place the ultrasonic cleaner vibration to clean 8～10 minutes, rinse well repeatedly with the high resistant deionized water again and get final product.With the mark that drains the water of the synthesising container after cleaning, place on the rough vacuum mechanical pump, externally (heating and temperature control is at 130 ℃) aspirate under Jia Re the condition, behind the water vapour of removal synthesising container inside, take off standby;

2, charging

At first load weighted germanium and zinc 4 are packed into the synthesising container body away from the A end of groove, the B end of the synthesising container body of then load weighted phosphorus 5 being packed into is located in the zone that body B end end wall and groove walls surrounded, and feeds to vacuumize degasification after finishing, in 10 ^-3Sealed knot under the Pa vacuum tightness, as shown in Figure 2.

3, synthetic

A, the synthesising container that at first raw material and sealed knot will be housed are put into the stove of horizontal positioned, modes of emplacement is to make the A end that germanium and zinc 4 are housed be positioned at the high-temperature zone, the B end that phosphorus 5 is housed is positioned at cold zone, and the outer wall place of the body recess that contacts with phosphorus is the temperature monitoring point, as shown in Figure 4:

B, the temperature of tube furnace high-temperature zone is risen to 1000 ℃, the temperature of cold zone with 3 ℃/min rise to 525 ℃ with 2 ℃/min, keep above-mentioned temperature field distribution by temperature monitoring and regulation and control, until phosphorus all is transported to the A end of synthesising container and germanium, zinc and reacts from the B end of synthesising container with the form of gas phase till;

C, the temperature of tube furnace high-temperature zone is elevated to 1060 ℃ with 2 ℃/min, temperature with the tube furnace cold zone rises to 1060 ℃ with 2 ℃/min again, be incubated 32 hours, rotating furnace 6 carries out mechanical oscillation in the time of insulation, make material thorough mixing reaction in the synthesising container, be incubated the rotating furnace body 6 that finishes the B of the former splendid attire phosphorus 5 of synthesising container is held vertically upward, finish the building-up reactions of phosphorus, germanium, zinc;

After D, building-up reactions are finished, between 1060 ℃ and 950 ℃, carry out temperature oscillation 8～10 times, eliminate phosphorus steam more than needed in the melt, then, be cooled to room temperature with 2 ℃/min.

The synthetic ZnGeP of present embodiment institute ₂Polycrystal is high-purity, single-phase, and its analytical results as shown in Figure 5.

Claims

1. regional vapor transportation synthesising container, it is characterized in that constituting by body (1) and feed-pipe (2), body (1) is the quartz glass tube of closed at both ends, the one end is A, the other end is B, length in distance body B end end is that the x place is provided with groove, the degree of depth h of this groove is 1/2～2/3 of a body inner diameter d, it is in portion's section of x that feed-pipe (2) passes through in distance body B end tip lengths mutually, its opening for feed (3) is opposite with groove notch direction, the angle β of its axis and body axis is 45～70 °, and material is a silica glass.

2. according to claim 1 two regional vapor transportation synthesising containers is characterized in that the length y of groove is at least 15mm.

3. according to claim 2 two regional vapor transportation synthesising containers, the length y that it is characterized in that groove is 20mm～30mm.

4. according to claim 1 or 2 or 3 described two regional vapor transportation synthesising containers, it is characterized in that apart from the length x of body B end end be body (1) length l 1/10～1/7.