CN215800037U - Solid phase doping device and heavily arsenic-doped silicon single crystal production system - Google Patents
Solid phase doping device and heavily arsenic-doped silicon single crystal production system Download PDFInfo
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- CN215800037U CN215800037U CN202121781425.2U CN202121781425U CN215800037U CN 215800037 U CN215800037 U CN 215800037U CN 202121781425 U CN202121781425 U CN 202121781425U CN 215800037 U CN215800037 U CN 215800037U
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Abstract
The utility model provides a solid phase doping device and a heavily arsenic-doped silicon single crystal production system, and belongs to the technical field of heavily arsenic-doped silicon single crystals. The solid phase doping device comprises a quartz cup and a quartz floating rod, wherein the upper end of the quartz cup is provided with an opening and is provided with a hook used for being hung on a single crystal furnace, the lower end of the quartz cup is provided with a conical material guide part, and the lower end of the material guide part is connected with a discharging pipe. The quartz floating rod penetrates through the blanking pipe along the axial direction of the blanking pipe, a floating valve is arranged at the upper end of the quartz floating rod and can cover the upper end of the blanking pipe, and a floater is arranged at the lower end of the quartz floating rod. Practice shows that the solid phase doping device provided by the utility model can improve the ratio of low-resistivity products and reduce the probability of crystal transformation, the dosage of arsenic dopants is reduced by about 28.4% compared with that in a gas phase doping process, the structure is simple, and the operation is convenient.
Description
Technical Field
The utility model belongs to the technical field of heavily doped silicon single crystals, and particularly relates to a solid phase doping device and a heavily arsenic-doped silicon single crystal production system.
Background
At present, the semiconductor power device has increasingly vigorous demand along with the rising of the industry in the fields of photovoltaic power generation and new energy electric automobiles, so that the resistivity characteristic of power devices such as IGBT (insulated gate bipolar translator) and the like on N-type wafers is more and more high in requirement. At present, the resistivity specification requirement of N-type heavily arsenic-doped is generally below 0.003 omega-cm, and the extremely individual requirement is already below 0.002 omega-cm. However, the resistivity of the current large-size (more than 8 inches) arsenic-doped silicon single crystal is generally 0.0035-0.0045 omega-cm, and the requirement of low resistivity cannot be met.
At present, large-size heavily arsenic-doped silicon single crystals are doped in a gas phase doping mode, a doping agent is placed in a doping container, the doping agent is gasified at high temperature and then brought into the silicon liquid level by argon gas for doping, the doping efficiency is low, and in order to achieve the aim of low resistivity, the total amount of arsenic impurities during doping is increased. Meanwhile, arsenic is also a harmful substance to the environment and human health, and a large amount of arsenic causes serious environmental pollution.
SUMMERY OF THE UTILITY MODEL
In view of this, the present invention provides a solid phase doping apparatus to solve the technical problems of low doping efficiency and easy crystal transformation in the prior art.
The utility model also provides a production system of the heavily arsenic-doped single crystal.
The technical scheme adopted by the utility model for solving the technical problems is as follows:
a solid phase doping apparatus comprising:
the upper end of the quartz cup is provided with an opening and is provided with a hook used for being hung on the single crystal furnace; the lower end of the quartz cup is provided with a conical material guide part, and the lower end of the material guide part is connected with a discharging pipe; and
the quartz floating rod penetrates through the blanking pipe along the axial direction of the blanking pipe, and a floating valve is arranged at the upper end of the quartz floating rod and can cover the upper end of the blanking pipe; the lower end of the quartz floating rod is provided with a floater; the upper end of the float valve forms a conical discharge part, and the lower end forms an inverted cone-shaped covering part.
Preferably, the bottom surface of the float is planar.
Preferably, the float is of a frustum shape.
A heavily arsenic-doped silicon single crystal production system comprises a seed crystal chuck arranged on a single crystal furnace, a crucible arranged in the single crystal furnace and the solid phase doping device; the hook can be hung on the seed crystal chuck, and the lower end of the floater can extend into the crucible.
According to the above technical solution, the present invention provides a solid phase doping apparatus for implementing the solid phase doping method. The solid phase doping device comprises a quartz cup made of quartz materials, the upper end of the quartz cup can be hung on a seed crystal chuck of the single crystal furnace, and the lower end of the quartz cup is provided with a discharging pipe. A quartz floating rod is arranged in the blanking pipe, a floating valve is arranged at the upper end of the quartz floating rod, and a floater is arranged at the lower end of the quartz floating rod. After the silicon material is melted, the quartz cup filled with the arsenic-containing dopant is hung on a seed crystal chuck of a single crystal furnace, and at the moment, the floating valve covers the upper end of the feeding tube under the action of the gravity of the quartz floating rod, so that the arsenic-containing dopant is prevented from falling into the silicon melt. And along with the descending of the seed chuck, the floater at the lower end of the quartz floating rod is contacted with the liquid level of the silicon melt, the quartz floating rod is jacked up under the buoyancy action of the silicon melt, so that the floating valve is separated from the upper end of the feeding tube, and the dopant in the quartz cup falls into the silicon melt through the feeding tube under the action of gravity to finish solid phase doping. The solid phase doping device is simple in structure and convenient to operate.
Practice shows that the solid phase doping device provided by the utility model is adopted to produce the heavily arsenic-doped silicon single crystal, the ratio of low-resistivity products can be obviously improved, and the solid phase doping device is particularly suitable for producing the arsenic-doped silicon single crystal with the resistivity of 0.003 omega-cm or less. Moreover, the residue of the dopant in the gas phase is reduced, so that the probability of crystal change in the crystal pulling process is effectively reduced, and the single crystal is easier to form. More importantly, under the same production conditions and process requirements, the solid phase doping device provided by the utility model is adopted to produce the heavily arsenic-doped silicon single crystal, the dosage of the arsenic dopant is reduced by about 28.4 percent compared with the dosage of the arsenic dopant in a gas phase doping process, the dosage of the arsenic dopant is effectively reduced, and the production cost is reduced.
Drawings
FIG. 1 is a schematic structural diagram of a solid phase doping apparatus.
Fig. 2 is a cross-sectional view of a solid phase doping apparatus.
FIG. 3 is a schematic structural diagram of a heavily arsenic-doped silicon single crystal production system.
FIG. 4 is a line graph showing resistivity distributions of the crystal ingots obtained in comparative examples and examples.
In the figure: the solid phase doping device 10, the quartz cup 100, the hook 110, the material guiding part 120, the discharging pipe 130, the quartz float rod 200, the float valve 210, the discharging part 211, the covering part 212 and the float 220.
Detailed Description
The technical solutions and effects of the embodiments of the present invention will be further described in detail below with reference to the accompanying drawings of the present invention.
Referring to fig. 1 and 2, in another embodiment of the present invention, a solid phase doping apparatus 10 is provided, the solid phase doping apparatus 10 includes: the quartz glass comprises a quartz cup 100 and a quartz floating rod 200, wherein the upper end of the quartz cup 100 is opened and is provided with a hook 110 used for being hung on a single crystal furnace. The lower end of the quartz cup 100 is provided with a conical material guiding portion 120, and the lower end of the material guiding portion 120 is connected with a discharging pipe 130. The quartz floating rod 200 penetrates through the blanking pipe 130 along the axial direction of the blanking pipe 130, a floating valve 210 is arranged at the upper end of the quartz floating rod 200, and the floating valve 210 can cover the upper end of the blanking pipe 130; the lower end of the quartz float rod 200 is provided with a float 220.
After the silicon material is melted, the quartz cup 100 filled with the arsenic-containing dopant is hung on a seed crystal chuck of the single crystal furnace, and at this time, the floating valve 210 covers the upper end of the feeding tube 130 under the action of the gravity of the quartz floating rod 200, so as to prevent the arsenic-containing dopant from falling into the silicon melt. With the descending of the seed chuck, the float 220 at the lower end of the quartz float rod 200 contacts with the liquid level of the silicon melt, the quartz float rod 200 is jacked up under the buoyancy of the silicon melt, so that the float valve 210 is separated from the upper end of the feeding tube 130, and the dopant in the quartz cup falls into the silicon melt through the feeding tube 130 under the action of gravity, thereby completing the solid phase doping. The solid phase doping device 10 is simple in structure and convenient to operate.
Further, the bottom surface of the float 220 is a plane, so as to increase the contact area between the float 220 and the liquid level of the silicon melt, improve the buoyancy force applied to the quartz float rod 200, and ensure that the float valve 210 is normally opened.
Further, the float 220 is of a frustum shape. That is, the cross-sectional area of the float 220 becomes gradually larger from the top to the bottom, thereby forming a guide surface above the float 220. In the process that the solid dopant or the dopant containing the solid dopant falls from top to bottom, the solid dopant or the dopant containing the solid dopant firstly falls on the guide surface above the floater 220 and is immersed into the silicon melt after speed reduction and buffering, so that the solid dopant or the dopant containing the solid dopant is prevented from directly falling into the silicon melt to cause the silicon melt to be splashed, and the safety risk is reduced.
In another embodiment, the upper end of the float valve 210 forms a conical discharge portion 211, and during the process that the quartz float bar 200 is lifted upwards, the solid dopant or the dopant containing solid dopant on the float valve 210 is branched by the discharge portion 211 to two sides, so that the solid dopant or the dopant containing solid dopant falls into the silicon melt completely in a short time, and the vaporization of the solid dopant or the dopant containing solid dopant is reduced.
Further, the lower end of the float valve 210 forms an inverted cone-shaped covering part 212, when the float valve 210 covers the upper end of the feeding tube 130, the covering part 212 partially extends into the feeding tube 130, and contacts with the nozzle of the feeding tube 130 through the side wall, so as to realize full-sealing covering and prevent material leakage before the float 220 does not contact the silicon melt liquid surface.
Further, in some embodiments, when the evaporation of the dopant is not considered, the opening size of the feeding pipe 130 can be controlled by controlling the height of the solid phase doping apparatus 10, so as to realize slow doping or batch doping.
Referring to FIG. 3, in another embodiment, a heavily arsenic-doped silicon single crystal production system is provided, which comprises a seed chuck 20 disposed on a single crystal furnace, a crucible 30 disposed in the single crystal furnace, and the solid phase doping apparatus 10. The hook can be hung on the seed crystal chuck, and the lower end of the floater can extend into the crucible. The detailed definition and explanation of the heavily arsenic-doped silicon single crystal production system are the same as above, and are not repeated here.
In another embodiment, a method for producing heavily arsenic-doped silicon single crystal is provided, which comprises the following steps:
s10, melting materials, namely loading silicon materials into the crucible arranged in the single crystal furnace, and melting the silicon materials under the melting technological parameters to form silicon melt.
S20, high-temperature treatment is carried out, the temperature is increased to enable the liquid level temperature to be larger than or equal to 1520 ℃, and the liquid level temperature is maintained for a preset time under the conditions of low furnace pressure and low crucible rotating speed. For example, the liquid surface temperature is not less than 1520 ℃, and the temperature is maintained for 0.5 to 2 hours under the conditions that the furnace pressure is 1kPa to 3kPa and the crucible rotating speed is 1rp/min to 2 rp/min. The main purpose of the high temperature treatment is to reduce the oxygen content of the silicon melt.
S30, stabilizing the silicon melt for one time, stabilizing the silicon melt for 1-2 h, raising the position of the crucible to the position of a seeding crucible, and setting the furnace pressure as the seeding furnace pressure.
S40, carrying out primary seed crystal temperature test to ensure that the liquid level temperature reaches the seeding temperature.
S50, arsenic doping, wherein the arsenic doping is carried out by adopting the solid phase doping method.
S60, secondary stabilization of silicon melt: the silicon solution is stable for 1h-2 h.
S70, secondary seed crystal temperature testing is carried out, and the liquid level temperature is ensured to reach the seeding temperature.
S80, seeding, shouldering, equalizing diameter and ending to obtain the heavily arsenic-doped silicon single crystal.
In the above steps, the processes including melting, stabilizing, seeding, shouldering, equalizing diameter, ending and the like are not emphasized, and conventional design parameters can be adopted, which are not described herein again.
Practice shows that the solid phase doping device provided by the utility model is adopted to produce the heavily arsenic-doped silicon single crystal, the ratio of low-resistivity products can be obviously improved, and the solid phase doping device is particularly suitable for producing the arsenic-doped silicon single crystal with the resistivity of 0.003 omega-cm or less. Moreover, the residue of the dopant in the gas phase is reduced, so that the probability of crystal change in the crystal pulling process is effectively reduced, and the single crystal is easier to form. More importantly, under the same production conditions and process requirements, the solid phase doping method provided by the utility model is adopted to produce the heavily arsenic-doped silicon single crystal, the dosage of the arsenic dopant is reduced by about 28.4 percent compared with the dosage of the arsenic dopant in a gas phase doping process, the dosage of the arsenic dopant is effectively reduced, and the production cost is reduced.
Referring to fig. 4, the technical solution and the technical effect of the present invention are further described below by specific embodiments. It is worth to be noted that the following specific experimental examples all adopt a hanhong 2408SR single crystal furnace to produce 8 inches heavily arsenic-doped silicon single crystal with low resistivity (the resistivity target is 0.003 ohm. cm) by the solid phase doping method provided by the utility model. In the experimental examples of the present invention, the process parameters which are not particularly limited are generally parameters which can be obtained by those skilled in the art.
When the adjustment is not enhanced, in the same process of the following experimental examples, 2 batches (i.e. 20 crystal rods pulled in total) are produced by using 10 hanhong 2408SR single crystal furnaces arranged in parallel as the statistical background base.
Comparative example 1
The target heavily arsenic-doped silicon single crystal is produced by the following process flow: charging, melting, high-temperature treatment, primary stabilization, primary seed crystal temperature testing, gas phase doping, secondary seed crystal temperature testing, seeding, shouldering, isometric diameter ending.
Wherein, in the high-temperature treatment process, the temperature is increased to ensure that the liquid level temperature is more than or equal to 1520 ℃, and the temperature is maintained for 1h under the conditions that the furnace pressure is 2kPa and the crucible rotating speed is 1 rp/min. The dosage of silicon is 120kg, and the dosage of the arsenic doping agent is 950 g. Other process parameters (including furnace pressure, argon flow, temperature, crucible rotation speed, single crystal growth speed, etc.) are parameters of general significance that can be obtained by a person skilled in the art.
And (3) counting the crystal variation occurrence probability under the process, detecting the resistivity distribution of the obtained complete crystal bar, and referring to the table 1 for counting and detecting results.
Comparative example No. two
The dosage of the arsenic doping agent is increased to 1000g, and other technological processes and parameters are the same as those of the first comparative example. And (3) counting the crystal variation occurrence probability under the process, detecting the resistivity distribution of the obtained complete crystal bar, and referring to the table 1 for counting and detecting results.
Comparative example No. three
The dosage of the arsenic doping agent is reduced to 850g, and other technological processes and parameters are the same as those of the comparative example I. And (3) counting the crystal variation occurrence probability under the process, detecting the resistivity distribution of the obtained complete crystal bar, and referring to the table 1 for counting and detecting results.
Experimental example 1
The target heavily arsenic-doped silicon single crystal is produced by the following process flow: charging, melting, high-temperature treatment, primary stabilization, primary seed crystal temperature testing, solid phase doping, secondary seed crystal temperature testing, seeding, shouldering, isometric ending.
Wherein, in the high-temperature treatment process, the temperature is increased to ensure that the liquid level temperature is more than or equal to 1520 ℃, and the temperature is maintained for 1h under the conditions that the furnace pressure is 2kPa and the crucible rotating speed is 1 rp/min. The dosage of silicon is 120kg, and the dosage of the arsenic doping agent is 950 g. Other process parameters (including furnace pressure, argon flow, temperature, crucible rotation speed, single crystal growth speed, etc.) are parameters of general significance that can be obtained by a person skilled in the art.
And (3) counting the crystal variation occurrence probability under the process, detecting the resistivity distribution of the obtained complete crystal bar, and referring to the table 1 for counting and detecting results.
Second to eighth experimental examples
Gradually reducing the feeding amount of the arsenic dopant, respectively taking 900g, 850g, 800g, 750g, 700g, 680g and 650g, and counting the crystal change occurrence probability under the process by using the same other process procedures and parameters as those of the first experimental example, detecting the resistivity distribution of the obtained complete crystal bar, and referring to the table 1 for counting and detecting results.
TABLE 1 statistics and test results of comparative and experimental examples
Referring to table 1 and fig. 4 together, comparative examples one to one disclose that doping by a gas phase doping method increases the amount of dopant added, which is beneficial to improving the resistivity of heavily arsenic-doped silicon single crystal, but increases the crystallization rate (the probability of partially or completely converting the heavily arsenic-doped silicon single crystal into polycrystal) due to the presence of more dopant gas in the gas phase of the single crystal furnace, and decreases the amount of dopant added, which is beneficial to decreasing the crystallization rate, but the resistivity of the heavily arsenic-doped silicon single crystal cannot be effectively ensured due to the less dopant amount of the dopant. This conclusion is consistent with current theory for heavily doped silicon single crystals.
Compared with the first experimental example, the first comparative example shows that the resistivity of the heavily arsenic-doped silicon single crystal rod can be greatly reduced by changing the doping mode and changing the gas phase doping into the solid phase doping mode provided by the utility model, particularly, the resistivity of the head of the heavily arsenic-doped silicon single crystal rod reaches within 0.0027 omega-cm, the resistivity of the tail of the heavily arsenic-doped silicon single crystal rod even reaches within 0.002 omega-cm, and the qualification rate of the heavily arsenic-doped silicon single crystal rod is greatly improved. Meanwhile, compared with gas phase doping, solid phase doping can reduce the probability of crystal change of the heavily arsenic-doped silicon single crystal bar to a certain extent, improve the yield of finished products and reduce the production cost.
The first experimental example to the eighth comparative example show that the probability of crystal change of the obtained heavily-doped arsenic-silicon single crystal rod is gradually reduced along with the continuous reduction of the input amount of the arsenic dopant, and when the input amount of the arsenic dopant is 680 g-950 g, the resistivity of the obtained heavily-doped arsenic-silicon single crystal rod is good, and the overall resistivity can be kept within 0.003 omega. When the input amount of the arsenic dopant is less than or equal to 650, the resistivity of the obtained heavily-doped arsenic silicon single crystal bar partially exceeds 0.003 omega cm, and unqualified products are generated.
On the contrary, when the solid phase doping method provided by the utility model is adopted to produce the heavily arsenic-doped silicon single crystal, compared with a gas phase doping mode, the method can greatly reduce the dosage of the arsenic dopant and reduce the production cost when the low resistivity is not required deliberately.
While the utility model has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the utility model.
Claims (4)
1. A solid phase doping apparatus, comprising:
the upper end of the quartz cup is provided with an opening and is provided with a hook used for being hung on the single crystal furnace; the lower end of the quartz cup is provided with a conical material guide part, and the lower end of the material guide part is connected with a discharging pipe; and
the quartz floating rod penetrates through the blanking pipe along the axial direction of the blanking pipe, and a floating valve is arranged at the upper end of the quartz floating rod and can cover the upper end of the blanking pipe; the lower end of the quartz floating rod is provided with a floater; the upper end of the float valve forms a conical discharge part, and the lower end forms an inverted cone-shaped covering part.
2. The solid phase doping apparatus of claim 1, wherein the bottom surface of the float is planar.
3. The solid phase doping apparatus of claim 2, wherein the float is of a frustum shape.
4. A heavily arsenic-doped silicon single crystal production system, which comprises a seed chuck arranged on a single crystal furnace and a crucible arranged in the single crystal furnace, and is characterized by further comprising a solid phase doping device according to any one of claims 1 to 3; the hook can be hung on the seed crystal chuck, and the lower end of the floater can extend into the crucible.
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