阅读说明：本技术 一种砷硅合金及其制备方法 (Arsenic-silicon alloy and preparation method thereof ) 是由 何建军 于 2021-07-23 设计创作，主要内容包括：本发明涉及一种砷硅合金及其制备方法,一种砷硅合金,其化学成分按照质量百分比为：As 70-90％,Si 10-30％,杂质含量小于0.1％；一种砷硅合金的制备方法,其创新点在于：包括以下步骤：S1、使用王水浸泡高纯的石英管组件并在通风柜中烘干；S2、将高纯砷、硅单质分别放置于石英舟内并置于石英管内；S3、使用真空封管系统,对石英管抽真空并封管处理；S4、将石英管放进高压水平炉内；S6、根据低温区的温度变化,对高压水平炉内充放氮气进行高压水平炉内压力控制,防止石英管爆裂；S7、控温程序结束,取出石英管,得到高纯的砷硅合金,解决砷掺杂硅单晶生长过程中,砷大量挥发导致的腔室污染以及砷单晶中砷掺杂浓度差压较大的问题,稳定性好。(The invention relates to an arsenic-silicon alloy and a preparation method thereof, wherein the arsenic-silicon alloy comprises the following chemical components in percentage by mass: 70-90% of As, 10-30% of Si and less than 0.1% of impurity content; the preparation method of the arsenic-silicon alloy has the innovation points that: the method comprises the following steps: s1, soaking the high-purity quartz tube assembly in aqua regia and drying in a ventilation cabinet; s2, respectively placing high-purity arsenic and silicon simple substances into a quartz boat and placing the quartz boat and the quartz tube; s3, using a vacuum tube sealing system to vacuumize and seal the quartz tube; s4, placing the quartz tube into a high-pressure horizontal furnace; s6, controlling the pressure in the high-pressure horizontal furnace by charging and discharging nitrogen in the high-pressure horizontal furnace according to the temperature change of the low-temperature region, and preventing the quartz tube from bursting; and S7, finishing the temperature control program, taking out the quartz tube to obtain the high-purity arsenic-silicon alloy, solving the problems of chamber pollution caused by a large amount of volatilization of arsenic and large differential pressure of arsenic doping concentration in the arsenic single crystal in the growth process of the arsenic-doped silicon single crystal, and having good stability.)

1. An arsenic silicon alloy, characterized by: the arsenic-silicon alloy comprises the following chemical components in percentage by mass: 70-90% of As, 10-30% of Si and less than 0.1% of impurity.

2. A method for producing the arsenic-silicon alloy as claimed in claim 1, wherein: the method comprises the following steps:

s1, soaking a high-purity quartz tube assembly comprising a quartz boat, a quartz sealing cap and a quartz tube in aqua regia, and drying in a fume hood;

s2, the quartz boat comprises a first quartz boat and a second quartz boat, high-purity arsenic is placed in the first quartz boat and is placed in the near-open end of the quartz tube through the clamping assembly, and the silicon simple substance is placed in the second quartz boat and is placed in the near-closed end of the quartz tube through the clamping assembly;

s3, using a vacuum tube sealing system to vacuumize and seal the quartz tube;

s4, placing the quartz tube into a high-pressure horizontal furnace, placing the first quartz boat containing the simple substance of arsenic in a low-temperature area in the high-pressure horizontal furnace, and placing the second quartz boat containing the simple substance of silicon in a high-temperature area in the high-pressure horizontal furnace;

s5, respectively and simultaneously controlling the temperature of the high-temperature area and the low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1120-1150 ℃, the highest temperature of the low-temperature area is 650-700 ℃, and the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature;

the temperature control program comprises a heating stage, a constant temperature stage and a low temperature stage, and the heating rate of the heating stage is 3-5 ℃/min for a high temperature zone; the constant temperature time of the constant temperature stage is 1-4 hours; the cooling rate of the cooling stage is 5-8 ℃/min;

s6, controlling the pressure in the high-pressure horizontal furnace by charging and discharging nitrogen in the high-pressure horizontal furnace according to the temperature change of the low-temperature region, and preventing the quartz tube from bursting;

and S7, finishing the temperature control program, and taking out the quartz tube to obtain the high-purity arsenic-silicon alloy.

3. The arsenic-silicon alloy and the preparation method thereof as claimed in claim 2, wherein: in step S2, the mass ratio of the high-purity arsenic to the simple substance silicon is (5-10): (1-5).

4. The arsenic-silicon alloy and the preparation method thereof as claimed in claim 2, wherein: in the step S6, when the temperature of the low-temperature region is lower than 610 ℃, the pressure in the furnace is 0-0.1 MPa; when the temperature of the low-temperature region is in the range of 610-650 ℃, the pressure in the furnace is adjusted to be 0.2-0.4MPa by charging and discharging nitrogen; when the temperature of the low-temperature region is in the range of 650-700 ℃, the pressure in the furnace is adjusted to be 0.3-0.6MPa by charging and discharging nitrogen.

5. The arsenic-silicon alloy and the preparation method thereof as claimed in claim 2, wherein: the quartz boat is of an integrated structure and comprises a quartz boat body and support legs fixed on the periphery of the bottom of the quartz boat body, the quartz tube comprises a tube body, the tube body is provided with an open end and a closed end which are opposite along the length direction, the quartz tube is provided with a preset tube body capacity, the open end of the quartz tube is provided with a quartz sealing cap through a connecting and sealing assembly and used for sealing the open end of the quartz tube, and a quartz boat mounting groove is formed in the quartz tube and used for placing the quartz boat;

the quartz sealing cap comprises a sealing cap body, wherein a circular connecting groove, a first annular connecting groove and a second annular connecting groove which are coaxially arranged are sequentially formed in the sealing cap body from one side far away from the quartz tube to one side close to the quartz tube, external threads are formed in the groove wall of the first annular connecting groove and the groove wall of the second annular connecting groove, and a sealing groove is formed in one side, close to the first annular connecting groove, of the circular connecting groove;

the connecting and sealing assembly comprises a fixing ring, a connecting seat and a sealing ring, the sealing ring is of a T-shaped structure consisting of a large ring body and a small ring body, the connecting seat is of a ring body structure, a ring body step is arranged at the end face of the outer side of the ring body structure, the ring body step comprises a large-diameter face and a small-diameter face which are coaxially arranged, and internal threads are arranged on the large-diameter face and the small-diameter face;

the fixing ring and the quartz tube are coaxial, the height of the fixing ring is smaller than that of the connecting seat, the fixing ring is fixed on the outer side of the opening end of the quartz tube, the connecting seat is sleeved on the outer side of the fixing ring and fixed, the bottom surfaces of the connecting seat and the fixing ring are positioned on the same straight line, the sealing cap body is matched with the internal thread through the external thread and is in threaded connection with the outer side of the connecting seat, the circular connecting groove is tightly connected with the opening end of the quartz tube, a T-shaped sealing groove is formed between the sealing groove and the connecting seat and the fixing ring, and the T-shaped sealing groove is sealed and fixed through the sealing ring;

the quartz boat mounting groove comprises a mounting groove body, wherein two parallel grooves are formed in the mounting groove body, and the inner diameter of each groove is gradually reduced from top to bottom.

6. The arsenic-silicon alloy and the preparation method thereof as claimed in claim 5, wherein: the mounting groove body is fixed at the near opening end and the near closing end on the inner wall of the quartz tube.

7. The arsenic-silicon alloy and the preparation method thereof as claimed in claim 5, wherein: the quartz sealing cap further comprises a handle, and a heat insulation layer is sleeved on the handle and fixed on the sealing cap body.

8. The arsenic-silicon alloy and the preparation method thereof as claimed in claim 5, wherein: the quartz boat is arranged in the quartz boat mounting groove through a clamping assembly;

the clamping assembly comprises an inner fixing assembly and an outer fixing assembly;

the inner side fixing assembly comprises a first inner side part, a second inner side part and an inner side limiting assembly, and the first inner side part and the second inner side part are hinged together through a middle shaft;

the first inner side part consists of a first opening plate and a first handle which are in an integral structure, and the second inner side part consists of a second opening plate and a second handle which are in an integral structure;

the inner side limiting assembly comprises a limiting groove, an arc limiting moving tooth, a limiting latch selectively clamped with the arc limiting moving tooth and an elastic steel sheet, the limiting groove is arranged on the second handle in a penetrating mode, a first meshing tooth is arranged on the outer arc edge of the arc limiting moving tooth, the end portion of the arc limiting moving tooth penetrates through the limiting groove and is fixed on the inner side of the first handle, a second meshing tooth matched with the first meshing tooth is arranged at the top end of the limiting latch, the bottom of the elastic steel sheet is fixed on the second handle and is located below the limiting groove, one end of the limiting latch in the extending direction penetrates through the limiting groove and is fixed at the top end of the elastic steel sheet, and an arc pressing plate is arranged at the other end of the limiting latch;

the outer side fixing assembly comprises a first limiting block, a second limiting plate and a connecting piece;

a first connecting plate is fixed on the first opening plate, a first limiting block is movably arranged on the first connecting plate and located on the outer side of the first opening plate, a first sliding groove is formed in the first connecting plate, a first sliding block is arranged in the first sliding groove, the first limiting block is arranged on the first connecting plate through the first sliding block, the first limiting block and the first opening plate are mutually parallel, one side, away from the first opening plate, of the first sliding block and one side, away from the first opening plate, of the first sliding groove are connected with a first reset spring, and the top of one side, in the width direction of the quartz boat body, is clamped through the cooperation of the first opening plate and the first limiting block;

a short block is fixed at the bottom of the second opening plate, a second limiting block is movably arranged on a second connecting plate and is positioned outside the second opening plate, a second sliding groove is formed in the second connecting plate, a second sliding block is arranged in the second sliding groove, the second limiting block is arranged on the second connecting plate through the second sliding block, one side, away from the second opening plate, of the second sliding block and one side, away from the second opening plate, of the second sliding groove are connected with a second reset spring, and the top of the other side, in the width direction of the quartz boat, is clamped through the short block and the second limiting block in a matching mode;

the connecting piece comprises a first connecting rope, a second connecting rope and a third connecting plate, one end of the first connecting rope penetrates through the first connecting plate and is fixed on the first limiting block, the other end of the first connecting rope is fixed on one end of the third connecting plate, one end of the second connecting rope penetrates through the second connecting plate and is fixed on the second limiting block, and the other end of the second connecting rope is fixed on the other end of the third connecting plate;

and a third handle is fixed on one side of the third connecting plate, which is close to the first handle.

Technical Field

The invention relates to the field of semiconductor materials, in particular to an arsenic-silicon alloy and a preparation method thereof.

Background

The semiconductor is a substance with conductivity between an insulator and a conductor, the conductivity of the semiconductor is easy to control, and the semiconductor can be used as an element material for information processing; semiconductors are very important from the viewpoint of technological or economic development.

Semiconductor devices typically use doped regions within a semiconductor structure as active semiconductor regions or as conductive regions. The doped regions are typically formed by ion implantation using either a p-conductivity type dopant (i.e., a dopant containing boron) or an n-conductivity type dopant (i.e., a dopant containing phosphorus or a dopant containing arsenic).

A particularly common use of doped regions within a semiconductor substrate is the source/drain regions within a field effect device. Field effect transistor devices are particularly popular. To optimize field effect device performance, the source/drain regions typically have a high level of active dopant (e.g., a concentration of about 1e20 to about 1e21 dopant atoms per cubic centimeter, or a dose of about 1e14 to about 1e16 dopant ions per square centimeter). High levels of active dopants result in low sheet resistance of the doped regions (e.g., about 150 to about 250 ohms/square).

Various factors affect dopant activation within doped regions, such as source/drain regions within a field effect device. Among these factors are dopant selection and type as well as the thermal annealing characteristics of the doped regions and related considerations.

As the growth of the arsenic-doped silicon single crystal generally adopts an element doping method, but because the vapor pressure of the arsenic is higher, a large amount of arsenic volatilizes in the growth process of the single crystal, and the arsenic is difficult to be effectively doped into the silicon single crystal, the environment of a growth chamber is polluted by a large amount of arsenic volatilized in the growth process, the doping amount of a dopant is difficult to control, the axial impurity concentration deviation of the single crystal silicon is larger, the longitudinal electrical parameter of an ingot is larger in change, the stability is poor, and the batch production cannot be carried out.

Disclosure of Invention

The invention aims to solve the technical problems of cavity pollution caused by a large amount of volatilization of arsenic in the growth process of an arsenic-doped silicon single crystal, large differential pressure of arsenic doping concentration in the silicon single crystal, poor stability and incapability of batch production.

In order to solve the technical problems, the technical scheme of the invention is as follows: the arsenic-silicon alloy is characterized in that: the arsenic-silicon alloy comprises the following chemical components in percentage by mass: 70-90% of As, 10-30% of Si and less than 0.1% of impurity.

The preparation method of the arsenic-silicon alloy has the innovation points that: the method comprises the following steps:

s1, soaking a high-purity quartz tube assembly comprising a quartz boat, a quartz sealing cap and a quartz tube in aqua regia, and drying in a fume hood;

s2, the quartz boat comprises a first quartz boat and a second quartz boat, high-purity arsenic is placed in the first quartz boat and is placed in the near-open end of the quartz tube through the clamping assembly, and the silicon simple substance is placed in the second quartz boat and is placed in the near-closed end of the quartz tube through the clamping assembly;

s3, using a vacuum tube sealing system to vacuumize and seal the quartz tube;

s4, placing the quartz tube into a high-pressure horizontal furnace, placing the first quartz boat containing the simple substance of arsenic in a low-temperature area in the high-pressure horizontal furnace, and placing the second quartz boat containing the simple substance of silicon in a high-temperature area in the high-pressure horizontal furnace;

s5, respectively and simultaneously controlling the temperature of the high-temperature area and the low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1120-1150 ℃, the highest temperature of the low-temperature area is 650-700 ℃, and the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature;

the temperature control program comprises a heating stage, a constant temperature stage and a low temperature stage, and the heating rate of the heating stage is 3-5 ℃/min for a high temperature zone; the constant temperature time of the constant temperature stage is 1-4 hours; the cooling rate of the cooling stage is 5-8 ℃/min;

s6, controlling the pressure in the high-pressure horizontal furnace by charging and discharging nitrogen in the high-pressure horizontal furnace according to the temperature change of the low-temperature region, and preventing the quartz tube from bursting;

and S7, finishing the temperature control program, and taking out the quartz tube to obtain the high-purity arsenic-silicon alloy.

Further, in step S2, the mass ratio of the high-purity arsenic to the simple substance silicon is (5-10): (1-5).

Further, in the step S6, when the temperature of the low temperature zone is lower than 610 ℃, the pressure in the furnace is 0-0.1 MPa; when the temperature of the low-temperature region is in the range of 610-650 ℃, the pressure in the furnace is adjusted to be 0.2-0.4MPa by charging and discharging nitrogen; when the temperature of the low-temperature region is in the range of 650-700 ℃, the pressure in the furnace is adjusted to be 0.3-0.6MPa by charging and discharging nitrogen.

Furthermore, the quartz boat is of an integrated structure and comprises a quartz boat body and support legs fixed on the periphery of the bottom of the quartz boat body, the quartz tube comprises a tube body, the tube body is provided with an open end and a closed end which are opposite along the length direction, the quartz tube is provided with a preset tube body capacity, the open end of the quartz tube is provided with a quartz sealing cap through a connecting and sealing assembly and used for sealing the open end of the quartz tube, and a quartz boat mounting groove is formed in the quartz tube and used for placing the quartz boat;

the quartz sealing cap comprises a sealing cap body, wherein a circular connecting groove, a first annular connecting groove and a second annular connecting groove which are coaxially arranged are sequentially formed in the sealing cap body from one side far away from the quartz tube to one side close to the quartz tube, external threads are formed in the groove wall of the first annular connecting groove and the groove wall of the second annular connecting groove, and a sealing groove is formed in one side, close to the first annular connecting groove, of the circular connecting groove;

the connecting and sealing assembly comprises a fixing ring, a connecting seat and a sealing ring, the sealing ring is of a T-shaped structure consisting of a large ring body and a small ring body, the connecting seat is of a ring body structure, a ring body step is arranged at the end face of the outer side of the ring body structure, the ring body step comprises a large-diameter face and a small-diameter face which are coaxially arranged, and internal threads are arranged on the large-diameter face and the small-diameter face;

the fixing ring and the quartz tube are coaxial, the height of the fixing ring is smaller than that of the connecting seat, the fixing ring is fixed on the outer side of the opening end of the quartz tube, the connecting seat is sleeved on the outer side of the fixing ring and fixed, the bottom surfaces of the connecting seat and the fixing ring are positioned on the same straight line, the sealing cap body is matched with the internal thread through the external thread and is in threaded connection with the outer side of the connecting seat, the circular connecting groove is tightly connected with the opening end of the quartz tube, a T-shaped sealing groove is formed between the sealing groove and the connecting seat and the fixing ring, and the T-shaped sealing groove is sealed and fixed through the sealing ring;

the quartz boat mounting groove comprises a mounting groove body, wherein two parallel grooves are formed in the mounting groove body, and the inner diameter of each groove is gradually reduced from top to bottom.

Further, the mounting groove body is fixed at the near opening end and the near closing end on the inner wall of the quartz tube.

Furthermore, the quartz sealing cap further comprises a handle, and a heat insulation layer is sleeved on the handle and fixed on the sealing cap body.

Furthermore, the quartz boat is arranged in the quartz boat mounting groove through a clamping assembly;

the clamping assembly comprises an inner fixing assembly and an outer fixing assembly;

the inner side fixing assembly comprises a first inner side part, a second inner side part and an inner side limiting assembly, and the first inner side part and the second inner side part are hinged together through a middle shaft;

the first inner side part consists of a first opening plate and a first handle which are in an integral structure, and the second inner side part consists of a second opening plate and a second handle which are in an integral structure;

the inner side limiting assembly comprises a limiting groove, an arc limiting moving tooth, a limiting latch selectively clamped with the arc limiting moving tooth and an elastic steel sheet, the limiting groove is arranged on the second handle in a penetrating mode, a first meshing tooth is arranged on the outer arc edge of the arc limiting moving tooth, the end portion of the arc limiting moving tooth penetrates through the limiting groove and is fixed on the inner side of the first handle, a second meshing tooth matched with the first meshing tooth is arranged at the top end of the limiting latch, the bottom of the elastic steel sheet is fixed on the second handle and is located below the limiting groove, one end of the limiting latch in the extending direction penetrates through the limiting groove and is fixed at the top end of the elastic steel sheet, and an arc pressing plate is arranged at the other end of the limiting latch;

the outer side fixing assembly comprises a first limiting block, a second limiting plate and a connecting piece;

a first connecting plate is fixed on the first opening plate, a first limiting block is movably arranged on the first connecting plate and located on the outer side of the first opening plate, a first sliding groove is formed in the first connecting plate, a first sliding block is arranged in the first sliding groove, the first limiting block is arranged on the first connecting plate through the first sliding block, the first limiting block and the first opening plate are mutually parallel, one side, away from the first opening plate, of the first sliding block and one side, away from the first opening plate, of the first sliding groove are connected with a first reset spring, and the top of one side, in the width direction of the quartz boat body, is clamped through the cooperation of the first opening plate and the first limiting block;

a short block is fixed at the bottom of the second opening plate, a second limiting block is movably arranged on a second connecting plate and is positioned outside the second opening plate, a second sliding groove is formed in the second connecting plate, a second sliding block is arranged in the second sliding groove, the second limiting block is arranged on the second connecting plate through the second sliding block, one side, away from the second opening plate, of the second sliding block and one side, away from the second opening plate, of the second sliding groove are connected with a second reset spring, and the top of the other side, in the width direction of the quartz boat, is clamped through the short block and the second limiting block in a matching mode;

the connecting piece comprises a first connecting rope, a second connecting rope and a third connecting plate, one end of the first connecting rope penetrates through the first connecting plate and is fixed on the first limiting block, the other end of the first connecting rope is fixed on one end of the third connecting plate, one end of the second connecting rope penetrates through the second connecting plate and is fixed on the second limiting block, and the other end of the second connecting rope is fixed on the other end of the third connecting plate;

and a third handle is fixed on one side of the third connecting plate, which is close to the first handle.

The invention has the advantages that:

1) according to the invention, the pressure in the high-pressure horizontal furnace is adjusted by charging and discharging nitrogen at different temperatures, so that mass production can be realized, the risk of tube explosion is effectively avoided, a high-purity quartz device and high-purity raw materials are used, the reaction temperature is controlled by controlling the feeding ratio of arsenic and silicon raw materials, alloy synthesis is carried out in a closed quartz tube, the vapor pressure of arsenic in the quartz tube is over higher than the equilibrium vapor pressure of the alloy, so that the high-purity arsenic silicon alloy material with 70-90% of arsenic content and 10-30% of silicon content can be obtained, the problems of chamber pollution caused by a large amount of volatilization of arsenic and large arsenic doping concentration differential pressure in an arsenic single crystal in the growth process of the arsenic-doped silicon single crystal are solved, and the stability is good.

2) The fixing ring is fixed on the outer side of the opening end of the quartz tube, the connecting seat sleeve is fixed on the outer side of the fixing ring, the sealing cap body is in threaded connection with the outer side of the connecting seat through matching of external threads and internal threads, so that the circular connecting groove is tightly connected with the opening end of the quartz tube, a T-shaped sealing groove is formed between the sealing groove and the connecting seat and the fixing ring, and the T-shaped sealing groove is sealed and fixed through the sealing ring, so that the sealing effect of the sealing cap is ensured while the connecting stability is ensured, the structure is simple, and the operation is convenient; nearly open end department and nearly closed end department on the quartz capsule inner wall all are fixed with the quartz boat mounting groove, and the recess internal diameter top-down of seting up on the mounting groove body steadilys decrease, are applicable to the quartz boat of different length, and the suitability is high, and stability is high, makes the inside thermally equivalent of quartz boat simultaneously, guarantees the effect of being heated.

3) The clamping assembly is matched with the limiting latch selectively clamped with the arc-shaped limiting latch through the arc-shaped limiting latch of the inner side limiting assembly and is used for propping the second opening plate to the inner wall of the top of the quartz boat in the length direction, the first opening plate and the short block are propped against the inner wall of the top of the quartz boat in the length direction, the first limiting block and the second limiting block are moved oppositely to the position where the first limiting block is matched with the first opening plate to clamp the top of one side of the quartz boat in the width direction, and the short block is matched with the second limiting block to clamp the top of the other side of the quartz boat in the width direction, so that the quartz boat is stably clamped.

Drawings

The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.

FIG. 1 is a front view of a cross-sectional view of a quartz tube assembly of an arsenic-silicon alloy and a method of making the same according to the present invention.

FIG. 2 is a partially enlarged view of a quartz tube assembly of an AsSiSi alloy and a method for making the same according to the present invention.

FIG. 3 is a front view of a clamping assembly of an AsSiSi alloy and method of making the same according to the present invention.

Detailed Description

As shown in fig. 1 to 3, the quartz boat 2 is an integrated structure, and includes a quartz boat body and support legs fixed around the bottom of the quartz boat body.

The quartz tube 1 comprises a tube body having an open end and a closed end opposite to each other along the length direction and having a predetermined tube body capacity, the open end of the quartz tube 1 is provided with a quartz sealing cap 3 through a connecting sealing component 4 for sealing the open end of the quartz tube 1, and the quartz tube 1 is internally provided with a quartz boat mounting groove 5 for placing a quartz boat 2.

The quartz sealing cap 3 comprises a sealing cap body, wherein the sealing cap body is provided with a circular connecting groove 31, a first annular connecting groove 32 and a second annular connecting groove 33 which are coaxially arranged in sequence from one side away from the quartz tube 1 to one side close to the quartz tube, an external thread is arranged on the groove wall of the first annular connecting groove 32 and the groove wall of the second annular connecting groove 33, and a sealing groove 34 is arranged on one side, close to the first annular connecting groove 32, of the circular connecting groove 31.

The quartz sealing cap 3 further comprises a handle 6, and a heat insulation layer is sleeved on the handle 6 and fixed on the sealing cap body.

Connect seal assembly 4 and include a solid fixed ring 41, connecting seat 42 and a sealing ring 43, sealing ring 43 is a T shape structure of compriseing a big annular body and a little annular body, and connecting seat 42 is an annular body structure, and has offered the annular body step in the outside terminal surface department of annular body structure, and the annular body step is including the big diameter face and the little diameter face of coaxial setting, and all offers the internal thread on big diameter face and the little diameter face.

Fixed ring 41 is coaxial and highly be less than the height of connecting seat with quartz capsule 1, fix in the 1 open end outside of quartz capsule, connecting seat 42 cover is established in the outside of fixed ring 41 and is fixed, and connecting seat 42 is in same straight line with the bottom surface of fixed ring 41, thereby the sealing cap body passes through external screw thread and interior screw-thread fit threaded connection in the connecting seat 42 outside, make circular connecting groove 31 and 1 open end zonulae occludens of quartz capsule, and sealing groove 34 and connecting seat 42 form a T shape seal groove with between the fixed ring 41, T shape seal groove passes through sealing ring 43 seal fixedly.

The quartz boat mounting groove 5 comprises a mounting groove body, two grooves which are parallel to each other are formed in the mounting groove body, and the inner diameter of each groove is gradually reduced from top to bottom.

The mounting groove body is fixed at the near opening end and the near closing end on the inner wall of the quartz tube 1.

Referring to fig. 3, which is a front view of a clamping assembly for a quartz tube assembly to facilitate sealing and fixing, a quartz boat 2 is placed in the quartz boat mounting groove 2 through a clamping assembly 7.

The clamping assembly 7 comprises an inner fixing assembly 71 and an outer fixing assembly 72.

The medial fixation assembly 71 includes a first medial member 711, a second medial member 712, and a medial stop assembly 13, the first medial member 711 and the second medial member 712 being hinged together by a central axis.

The first inner member 711 is composed of a first opening plate 7111 and a first handle 7112 which are integrally formed, and the second inner member 712 is composed of a second opening plate 7121 and a second handle 7122 which are integrally formed.

The inner limiting component 713 comprises a limiting groove, an arc-shaped limiting moving tooth 7131, a limiting clamping tooth 7132 selectively clamped with the arc-shaped limiting moving tooth and an elastic steel sheet 7133.

The second handle 7122 is provided with a limiting groove in a penetrating manner, the outer arc edge of the arc limiting moving tooth 7131 is provided with a first meshing tooth, the end part of the arc limiting moving tooth 7131 penetrates through the limiting groove to be fixed on the inner side of the first handle 7121, the top end of the limiting latch 7132 is provided with a second meshing tooth matched with the first meshing tooth, the bottom of the elastic steel sheet 7133 is fixed on the second handle 7122 and located below the limiting groove, one end of the extending direction of the limiting latch 7132 penetrates through the limiting groove to be fixed on the top end of the elastic steel sheet 7133, and the other end of the extending direction of the limiting latch 7132 is provided with an arc pressing plate.

The outside fixing assembly 72 comprises a first limiting block, a second limiting plate and a connecting piece 8.

Be fixed with first connecting plate 721 on the first board 7111 that struts, first stopper activity sets up and lies in the first board 7111 outside that struts on first connecting plate 721, first spout has been seted up on first connecting plate 721, be equipped with first slider in the first spout, first stopper sets up on first connecting plate 721 through first slider, first stopper is parallel to each other with first board 7111 that struts, one side that first board was kept away from to first slider is connected with first reset spring with one side that first board was kept away from to first spout, through the top of first board 7111 that struts and the cooperation of first stopper clamp quartz boat 2 width direction one side.

The bottom of second opening plate 7121 is fixed with the stub, the activity of second stopper sets up and is located the second opening plate outside on second connecting plate 722, the second spout has been seted up on second connecting plate 722, be equipped with the second slider in the second spout, the second stopper passes through the second slider setting on the second connecting plate, one side that the second opening plate was kept away from to the second slider is connected with second reset spring with one side that the second spout was kept away from to the second opening plate, press from both sides the top of tight 2 width direction opposite sides of quartz boat through stub and the cooperation of second stopper.

The short block, the first opening plate, the first limiting block and the second limiting block are all fixed with rubber cushions on one sides close to the quartz boat 2.

The connecting piece 8 comprises a first connecting rope 81, a second connecting rope 82 and a third connecting plate 83, one end of the first connecting rope 81 penetrates through the first connecting plate to be fixed on a first limiting block, the other end of the first connecting rope is fixed on one end of the third connecting plate 83, one end of the second connecting rope 82 penetrates through the second connecting plate to be fixed on the second limiting block, and the other end of the second connecting rope 82 is fixed on the other end of the third connecting plate 83.

A third handle 84 is fixed to the third connecting plate 83 on a side close to the first handle 7112.

The first embodiment is as follows:

an arsenic-silicon alloy comprises the following chemical components in percentage by mass: 70-90% of As, 78-30% of Si10 and less than 0.1% of impurity.

A preparation method of an arsenic-silicon alloy comprises the following steps:

s1, soaking a high-purity quartz tube assembly comprising a quartz boat 2, a quartz sealing cap 3 and a quartz tube 1 in aqua regia, and drying in a ventilation cabinet;

s2, the quartz boat 2 comprises a first quartz boat and a second quartz boat, and the mass ratio of the high-purity arsenic to the simple substance silicon is 5: 1, placing high-purity arsenic in a first quartz boat and a near-open end in a quartz tube 1 through a clamping assembly 7, and placing a silicon simple substance in a second quartz boat and a near-closed end in the quartz tube 1 through the clamping assembly 7;

s3, using a vacuum tube sealing system to vacuumize the quartz tube 1 and seal the tube;

s4, placing the quartz tube 1 into a high-pressure horizontal furnace, placing the first quartz boat containing the simple substance of arsenic in a low-temperature area in the high-pressure horizontal furnace, and placing the second quartz boat containing the simple substance of silicon in a high-temperature area in the high-pressure horizontal furnace;

s5, respectively and simultaneously controlling the temperature of a high-temperature area and a low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1150 ℃, the highest temperature of the low-temperature area is 700 ℃, and the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature;

the temperature control program comprises a temperature rise stage, a constant temperature stage and a low temperature stage, and the temperature rise rate of the temperature rise stage is 5 ℃/min for a high temperature zone; the constant temperature time of the constant temperature stage is 1 hour; the cooling rate of the cooling stage is 8 ℃/min;

s6, controlling the pressure in the high-pressure horizontal furnace by charging and discharging nitrogen in the high-pressure horizontal furnace according to the temperature change of the low-temperature region, and preventing the quartz tube from bursting;

when the temperature of the low-temperature region is lower than 610 ℃, the pressure in the furnace is 0.1 MPa; when the temperature of the low-temperature region is in the range of 610-650 ℃, the pressure in the furnace is adjusted to be 0.3MPa by charging and discharging nitrogen; when the temperature of the low-temperature zone is in the range of 650-700 ℃, the pressure in the furnace is adjusted to be 0.5MPa by charging and discharging nitrogen.

And S7, finishing the temperature control program, and taking out the quartz tube to obtain the high-purity arsenic-silicon alloy with the arsenic content of 89.94% and the silicon content of 9.95%.

Example two:

the rest is the same as the first embodiment, and only S5 is different as follows:

respectively and simultaneously controlling the temperature of a high-temperature area and a low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1150 ℃, the highest temperature of the low-temperature area is 700 ℃, the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature,

the temperature control program comprises a heating-up stage, a constant temperature stage and a low temperature stage, and the heating-up rate of the heating-up stage is 3 ℃/min for a high-temperature area; the constant temperature time of the constant temperature stage is 4 hours; the cooling rate of the cooling stage is 5 ℃/min;

finally, the high-purity arsenic-silicon alloy is obtained, wherein the arsenic content is 89.98%, and the silicon content is 9.99%.

Example three:

the rest is the same as the first embodiment, and only S5 is different as follows:

respectively and simultaneously controlling the temperature of a high-temperature area and a low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1150 ℃, the highest temperature of the low-temperature area is 700 ℃, the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature,

the temperature control program comprises a heating-up stage, a constant temperature stage and a low temperature stage, and the heating-up rate of the heating-up stage is 3 ℃/min for a high-temperature area; the constant temperature time of the constant temperature stage is 1 hour; the cooling rate of the cooling stage is 5 ℃/min;

finally, the high-purity arsenic-silicon alloy is obtained, wherein the arsenic content is 89.97%, and the silicon content is 9.99%.

Example four:

an arsenic-silicon alloy comprises the following chemical components in percentage by mass: 70-90% of As, 78-30% of Si10 and less than 0.1% of impurity.

A preparation method of an arsenic-silicon alloy comprises the following steps:

s1, soaking a high-purity quartz tube assembly comprising a quartz boat 2, a quartz sealing cap 3 and a quartz tube 1 in aqua regia, and drying in a ventilation cabinet;

s2, the quartz boat 2 comprises a first quartz boat and a second quartz boat, and the mass ratio of the high-purity arsenic to the simple substance silicon is 10: 5, placing high-purity arsenic into a first quartz boat and placing the high-purity arsenic into a near-opening end in the quartz tube 1 through a clamping assembly 7, and placing a silicon simple substance into a second quartz boat and placing the silicon simple substance into a near-closing end in the quartz tube 1 through the clamping assembly 7;

s3, using a vacuum tube sealing system to vacuumize the quartz tube 1 and seal the tube;

s4, placing the quartz tube 1 into a high-pressure horizontal furnace, placing the first quartz boat containing the simple substance of arsenic in a low-temperature area in the high-pressure horizontal furnace, and placing the second quartz boat containing the simple substance of silicon in a high-temperature area in the high-pressure horizontal furnace;

s5, respectively and simultaneously controlling the temperature of a high-temperature area and a low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1120 ℃, the highest temperature of the low-temperature area is 650 ℃, and the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature;

the temperature control program comprises a temperature rise stage, a constant temperature stage and a low temperature stage, and the temperature rise rate of the temperature rise stage is 5 ℃/min for a high temperature zone; the constant temperature time of the constant temperature stage is 1 hour; the cooling rate of the cooling stage is 8 ℃/min;

s6, controlling the pressure in the high-pressure horizontal furnace by charging and discharging nitrogen in the high-pressure horizontal furnace according to the temperature change of the low-temperature region, and preventing the quartz tube from bursting; when the temperature of the low-temperature region is lower than 610 ℃, the pressure in the furnace is 0.1 MPa; when the temperature of the low-temperature region is in the range of 610-650 ℃, the pressure in the furnace is adjusted to be 0.3MPa by charging and discharging nitrogen; when the temperature of the low-temperature zone is in the range of 650-700 ℃, the pressure in the furnace is adjusted to be 0.5MPa by charging and discharging nitrogen.

And S7, finishing the temperature control program, and taking out the quartz tube to obtain the high-purity arsenic-silicon alloy with the arsenic content of 89.92% and the silicon content of 9.93%.

Example five:

the rest is the same as the example, and only S5 is different as follows:

controlling the temperature of the high temperature zone and the low temperature zone respectively and simultaneously according to a set temperature control program, wherein the highest temperature of the high temperature zone is 1120 ℃, the highest temperature of the low temperature zone is 650 ℃, the lowest temperature of the high temperature zone and the low temperature zone is indoor temperature,

the temperature control program comprises a heating-up stage, a constant temperature stage and a low temperature stage, and the heating-up rate of the heating-up stage is 3 ℃/min for a high-temperature area; the constant temperature time of the constant temperature stage is 4 hours; the cooling rate of the cooling stage is 5 ℃/min;

example six:

the rest is the same as the example, and only S5 is different as follows:

respectively and simultaneously controlling the temperature of a high-temperature area and the temperature of a low-temperature area according to a set temperature control program, wherein the highest temperature of the high-temperature area is 1120 ℃, the highest temperature of the low-temperature area is 650 ℃, and the lowest temperature of the high-temperature area and the low-temperature area is indoor temperature;

the temperature control program comprises a heating-up stage, a constant temperature stage and a low temperature stage, and the heating-up rate of the heating-up stage is 3 ℃/min for a high-temperature area; the constant temperature time of the constant temperature stage is 1 hour; the cooling rate of the cooling stage is 5 ℃/min;

finally, the high-purity arsenic-silicon alloy is obtained, wherein the arsenic content is 89.96%, and the silicon content is 9.95%.

In conclusion, when the temperature, the constant temperature time and the pressure are the same, the lower the temperature rising or reducing rate is, the higher the purity of the obtained high-purity arsenic-silicon alloy is; under the condition that the temperature rising or reducing rate and the constant temperature time are the same as the pressure, the lower the temperature is, the higher the purity of the obtained high-purity arsenic-silicon alloy is; under the condition that the temperature rising or reducing rate and the constant temperature time are the same as the temperature, the longer the constant temperature time is, the higher the purity of the obtained high-purity arsenic-silicon alloy is.

It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.