Canning method of semiconductor solid-state source precursor material, method for obtaining solid-state source precursor steam and application of solid-state source precursor steam

By sublimating and recrystallizing the semiconductor solid-state source precursor material and partitioning the particle size, it is filled into the precursor source bottle in a specific proportion, solving the problems of unstable evaporation and low utilization of solid-state source precursor material, achieving a more stable vapor concentration and higher material utilization.

CN119800324APending Publication Date: 2025-04-11DALIAN HENGKUN NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202411911090.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-24
Publication Date
2025-04-11

AI Technical Summary

Technical Problem

In the existing vapor deposition process of semiconductor precursor materials, the evaporation of solid-state source precursor materials is unstable and the utilization rate is low, resulting in severe fluctuations in the vapor concentration of solid-state source precursors, affecting the stability of the vapor deposition process.

Method used

The canning method of semiconductor solid-state source precursor material is adopted. After sublimation and recrystallization, it is divided into a variety of precursor materials with different particle sizes, and is filled into the tray of the precursor source bottle in a specific particle size ratio to improve the utilization rate of the material and evaporation stability.

Benefits of technology

By adjusting the particle size ratio, a more efficient stacking layer structure is formed, which reduces the low resistance channel of the carrier gas flow breaks through the stacking layer, improves the concentration stability of the solid-state source precursor vapor and the utilization rate of materials, and reduces the frequency of equipment shutdown.

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Abstract

The invention belongs to the technical field of semiconductor materials, and particularly relates to a canning method and application of a semiconductor solid-state source precursor material. The canning method comprises the following steps: performing sublimation recrystallization treatment on a solid source precursor material, then performing crushing and sieving treatment to obtain N precursor materials with different particle sizes, and then filling a tray of a precursor source bottle with the N precursor materials to complete canning, N being greater than or equal to 3; the maximum particle size of the N precursor materials is RN, the minimum particle size of the N precursor materials is RN, and RN is larger than or equal to RN; arranging RNgt according to the particle size from small to large; when RN < = 1, the maximum particle size RN of the Nth precursor material is less than or equal to the minimum particle size RN + 1 of the (N + 1) th precursor material, and RN: RN + 1 is (0.2-0.9): 1. According to the canning method of the semiconductor solid-state source precursor material, solid-state source precursor steam with stable concentration can be provided for a vapor deposition process, and the utilization rate of the solid-state source precursor material is increased.
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Description

Technical Field

[0001] The present invention belongs to the technical field of semiconductor materials, and in particular relates to a method for canning semiconductor solid-state source precursor materials and a method for obtaining solid-state source precursor vapor and applications thereof. Background Art

[0002] Semiconductor precursor materials are mainly used in the thin film deposition process in semiconductor manufacturing. They are the core materials of ALD and CVD thin film deposition processes, and are also the "precursors" of wafer manufacturing processes. In the ALD and CVD thin film deposition processes, solid source precursor materials need to be converted into gases to enter the reactor chamber of the system to obtain the deposition of target elements. Among them, good volatility and stability are the most core property requirements for solid source precursor materials in the ALD and CVD thin film deposition processes.

[0003] At present, in the solid-state source precursor vapor acquisition method currently implemented, it is generally to provide the solid-state source precursor vapor required for the vapor deposition process by adjusting the carrier gas flux and the external heat intensity. The solid-state source precursor vapor concentration provided by this method has a strong volatility that changes with time, because the solid-state source precursor is directly sublimated from the solid state to the gaseous state during use, and with the reduction of the amount during use, the sublimation amount of the material may be gradually reduced, making the utilization rate of the material low. At the same time, when the solid-state source precursor accumulation layer in the source bottle is penetrated by the carrier gas flow, a low-resistance airflow channel will appear, and a large amount of carrier gas will choose the low-resistance airflow channel to escape, which will cause the solid-state source precursor vapor concentration to decrease sharply, and with the increase of the carrier gas flux, this phenomenon will become more and more serious. The low-resistance channel and the solid-state source material caking will seriously affect the utilization rate of the solid-state precursor source in the source bottle, increase the frequency of equipment shutdown, and also affect the stability of the solid-state source precursor vapor concentration, which is very unfavorable for the vapor deposition process. Summary of the invention

[0004] One of the purposes of the present invention is to provide a method for canning semiconductor solid source precursor materials in view of the shortcomings of unstable evaporation and low utilization rate of solid source precursor materials in the existing semiconductor precursor material vapor deposition process.

[0005] Specifically, the canning method of the semiconductor solid-state source precursor material comprises the following steps: sublimating and recrystallizing the solid-state source precursor material, and then crushing and sieving to obtain N kinds of precursor materials with different particle sizes, and filling the N kinds of precursor materials with different particle sizes into the tray of the precursor source bottle to complete the canning, wherein N≧3; the maximum particle size of the N kinds of precursor materials is R N , the minimum particle size is R N ˋ, R N ≧RN ˋ; Arranged from small to large in particle size, the maximum particle size R of the Nth precursor material N ≦The minimum particle size R of the N+1th precursor material N+1 ˋ, and R N :R N+1 is (0.2~0.9):1.

[0006] In a preferred embodiment, R N >R N When R N+1 ˋ-R N =0~4mm; R N =R N When R N ˋ≠0, R N+1 -R N =1~4mm.

[0007] In a preferred embodiment, the R N -R N ˋ=0~4mm.

[0008] In a preferred embodiment, the precursor material includes first particles, second particles and third particles whose particle sizes increase in sequence.

[0009] In a preferred embodiment, the mass ratio of the first particles, the second particles and the third particles is (2-5):(2-4):1.

[0010] In a preferred embodiment, the particle size of the first particles is 0-2 mm, the particle size of the second particles is 2-4 mm, and the particle size of the third particles is 4-6 mm.

[0011] In a preferred embodiment, the particle size of the first particles is 0-2 mm, the particle size of the second particles is 2-4 mm, and the particle size of the third particles is 6-8 mm.

[0012] In a preferred embodiment, the solid source precursor material is selected from one of aluminum trichloride, hafnium tetrachloride, gallium trichloride and antimony trichloride.

[0013] In a preferred embodiment, the sublimation recrystallization treatment method includes: adding a solid source precursor material into a sublimation device, setting the sublimation temperature, vacuum degree and treatment time, and collecting the resulting product after the reaction is completed for crushing and sieving, thereby obtaining N kinds of precursor materials with different particle sizes.

[0014] In a preferred embodiment, the sublimation temperature and vacuum degree of the sublimation recrystallization treatment are determined according to the properties of the solid source precursor material.

[0015] The second object of the present invention is to provide a method for obtaining solid-state source precursor vapor, which method includes: using the above-mentioned canning method to obtain a precursor source bottle containing semiconductor solid-state source precursor material, connecting the precursor source bottle to a vapor deposition system, the carrier gas inlet of the precursor source bottle is connected to the carrier gas pipeline of the vapor deposition system, the mixed carrier gas outlet of the precursor source bottle is connected to the material conveying pipeline of the vapor deposition system, heating the precursor source bottle, and then introducing carrier gas, the carrier gas in the precursor source bottle is mixed with the evaporated solid-state precursor and then discharged from the mixed carrier gas outlet, so as to obtain solid-state source precursor vapor.

[0016] The third object of the present invention is to provide an application of the above-mentioned method for packaging semiconductor solid-state source precursor materials or the method for obtaining solid-state source precursor vapor in the field of semiconductor material technology.

[0017] The key of the present invention is to first sublimate and recrystallize the solid-state source precursor material to obtain N kinds of precursor materials with different particle sizes (N≧3) and regulate the specific particle size ratio between the N kinds of precursor materials, and then fill it into the tray of the precursor source bottle to complete the canning, so as to provide a solid-state source precursor vapor with stable concentration for the vapor deposition process, reduce the frequency of stopping to change bottles, and improve the utilization rate of semiconductor solid-state source precursor materials. This is mainly due to the accumulation layer formed by N kinds of precursor materials with different particle sizes with a specific particle size ratio can provide a more efficient utilization area. When the carrier gas passes through the precursor material accumulation layer, the channel left by the small-particle precursor material after evaporation with the carrier gas can be collapsed and blocked by the large-particle precursor material, which can effectively prevent the solid-state source precursor accumulation layer from being pierced by the carrier gas flow to form a low-resistance airflow channel, thereby improving the concentration stability of the solid-state source precursor vapor and the utilization rate of the solid-state source precursor material. DETAILED DESCRIPTION

[0018] The canning method of semiconductor solid-state source precursor materials provided by the present invention comprises the following steps: sublimating and recrystallizing the solid-state source precursor materials, and then crushing and screening to obtain N kinds of precursor materials with different particle sizes, and filling the N kinds of precursor materials with different particle sizes into the tray of the precursor source bottle to complete the canning, wherein N is an integer and N≧3, such as 3, 4, 5, 6, etc.

[0019] The maximum particle size of the N precursor materials is R N , the minimum particle size is R N ˋ, R N ≧R N That is, when R N >R N When R N =R NWhen ˋ, the particle size of the N precursor materials is a point value. The N precursor materials are obtained by crushing and sieving, and the particle size thereof can be a range value and / or a point value.

[0020] Arranged from small to large in particle size, the maximum particle size R of the Nth precursor material N ≦The minimum particle size R of the N+1th precursor material N+1 ˋ, and R N :R N+1 It is (0.2-0.9):1, such as 0.2:1, 0.25:1, 0.3:1, 0.33:1, 0.35:1, 0.4:1, 0.5:1, 0.6:1, 0.7:1, 0.8:1 or any value therebetween.

[0021] In the present invention, R N >R N When R N+1 ˋ-R N =0-4mm, such as 0, 0.5mm, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 4mm or any value therebetween; R N =R N When R N ˋ≠0, R N <R N+1 And R N :R N+1 For R N+1 -R N =1~4mm, such as 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 4mm or any value therebetween.

[0022] In the present invention, the R N -R N ˋ=0~4mm, such as 0, 0.5mm, 1mm, 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 4mm or any value therebetween.

[0023] In the present invention, the precursor material preferably includes first particles, second particles and third particles whose particle sizes increase successively. The mass ratio of the first particles, the second particles and the third particles is preferably (2-5):(2-4):1. Taking the mass of the third particle as 1 part by weight, the mass of the first particle is preferably 2-5 parts by weight, such as 2, 2.5, 3, 3.5, 4, 4.5, 5 parts by weight or any value therebetween; the mass of the second particle is preferably 2-4 parts by weight, such as 2, 2.5, 3, 3.5, 4 parts by weight or any value therebetween. At this time, it is more conducive to increasing the utilization area of ​​the semiconductor solid-state source precursor material and reducing the formation of low-resistance airflow channels, thereby improving the utilization rate and evaporation stability of the semiconductor solid-state source precursor material.

[0024] In addition, the terms "first", "second" and "third" are only used for descriptive purposes to facilitate distinction and should not be understood as special limitations on the type and quantity of technical features.

[0025] In a specific embodiment, the particle size of the first particles is preferably 0-2 mm, the particle size of the second particles is preferably 2-4 mm, and the particle size of the third particles is preferably 4-6 mm.

[0026] In a specific embodiment, the particle size of the first particles is preferably 0-2 mm, the particle size of the second particles is preferably 2-4 mm, and the particle size of the third particles is preferably 6-8 mm.

[0027] In a specific embodiment, the particle size of the first particles is preferably 0-2 mm, the particle size of the second particles is preferably 4-6 mm, and the particle size of the third particles is preferably 6-8 mm.

[0028] In a specific embodiment, the particle size of the first particles is preferably 0-3 mm, the particle size of the second particles is preferably 3-6 mm, and the particle size of the third particles is preferably 6-9 mm.

[0029] In a specific embodiment, the particle size of the first particles is preferably 2-4 mm, the particle size of the second particles is preferably 4-6 mm, and the particle size of the third particles is preferably 6-8 mm.

[0030] In the present invention, the specific type of the solid source precursor material is not limited and can be a conventional choice in the art. Specific examples thereof include but are not limited to: one of aluminum trichloride, hafnium tetrachloride, gallium trichloride, and antimony trichloride.

[0031] In the present invention, the sublimation recrystallization treatment method may include: adding a solid source precursor material into a sublimation device, setting the sublimation temperature, vacuum degree and treatment time, and collecting the resulting product after the reaction is completed, crushing and sieving, so as to obtain N kinds of precursor materials with different particle sizes.

[0032] Furthermore, the sublimation temperature and vacuum degree of the sublimation recrystallization treatment can be determined according to the properties of the solid source precursor material.

[0033] In a specific embodiment, when the solid source precursor material is aluminum chloride, the sublimation temperature is preferably 100-110°C, such as 100°C, 102°C, 105°C, 108°C, 110°C or any value therebetween; the vacuum degree is preferably 0.1-1.5 torr, such as 0.1 torr, 0.2 torr, 0.5 torr, 0.8 torr, 1 torr, 1.2 torr, 1.5 torr or any value therebetween; the processing time is preferably 36-60h, such as 36h, 38h, 40h, 44h, 48h, 50h, 52h, 55h, 58h, 60h or any value therebetween.

[0034] In a specific embodiment, when the solid source precursor material is hafnium tetrachloride, the sublimation temperature is preferably 190-230°C, such as 190°C, 200°C, 210°C, 220°C, 230°C or any value therebetween; the vacuum degree is preferably 0.1-1.5 torr, such as 0.1 torr, 0.2 torr, 0.5 torr, 0.8 torr, 1 torr, 1.2 torr, 1.5 torr or any value therebetween; the processing time is preferably 36-60h, such as 36h, 38h, 40h, 44h, 48h, 50h, 52h, 55h, 58h, 60h or any value therebetween.

[0035] The present invention provides a method for obtaining solid-state source precursor vapor, which comprises: obtaining a precursor source bottle filled with semiconductor solid-state source precursor material by the canning method provided by the present invention, connecting the precursor source bottle to a vapor deposition system, connecting a carrier gas inlet of the precursor source bottle to a carrier gas pipeline of the vapor deposition system, connecting a mixed carrier gas outlet of the precursor source bottle to a material conveying pipeline of the vapor deposition system, heating the precursor source bottle, introducing carrier gas, mixing the carrier gas with evaporated solid-state source precursor in the precursor source bottle and discharging the mixed carrier gas outlet, thereby obtaining solid-state source precursor vapor.

[0036] Furthermore, the carrier gas can be selected from argon (Ar) or nitrogen (N2), preferably argon.

[0037] Furthermore, the temperature of the heating treatment can be determined according to the properties of the solid source precursor material in the precursor source bottle.

[0038] The present invention will be described in detail below through specific embodiments.

[0039] Example 1

[0040] (1) 12 kg of aluminum chloride raw material was put into the heating zone of a sublimation equipment. The equipment parameters were: temperature 105° C., vacuum degree 1 torr, and time 48 h. After the sublimation was completed, the aluminum chloride material was collected, crushed, and sieved to obtain three different particle sizes of 0-2 mm, 2-4 mm, and 4-6 mm;

[0041] (2) three aluminum chloride materials with different particle sizes are uniformly filled into the tray grooves of six evaporation units in a mass ratio of 5:4:1, and then sequentially fed into the container, and the end cap and the container are sealed with bolts to form a complete precursor source bottle;

[0042] (3) Connect a precursor source bottle filled with 6 kg of precursor to the vapor deposition system, connect the carrier gas inlet to the system carrier gas pipeline, and connect the mixed vapor outlet to the system material delivery pipeline. Use a heating device to heat the source bottle to 120°C, introduce 2000 sccm of carrier gas Ar, mix the carrier gas with the evaporated solid, and then extract it from the source bottle in a vacuum environment to the reaction chamber for deposition.

[0043] [Results]: When the amount of material used in the source bottle was 0-5kg, the evaporation rate remained above 200g / h; when the amount of material used exceeded 5kg, the evaporation rate dropped below 200g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200g / h) reached 83%.

[0044] Example 2

[0045] (1) 12 kg of aluminum chloride raw material was put into the heating zone of a sublimation equipment. The equipment parameters were: temperature 105° C., vacuum degree 1 torr, and time 48 h. After the sublimation was completed, the aluminum chloride material was collected, crushed, and sieved to obtain three different particle sizes of 0-2 mm, 2-4 mm, and 4-6 mm;

[0046] (2) three aluminum chloride materials with different particle sizes are uniformly filled into the tray grooves of six evaporation units in a mass ratio of 4:4:2, and then sequentially fed into the container, and the end cap and the container are sealed with bolts to form a complete precursor source bottle;

[0047] (3) Connect a precursor source bottle filled with 6 kg of precursor to the vapor deposition system, connect the carrier gas inlet to the system carrier gas pipeline, and connect the mixed vapor outlet to the system material delivery pipeline. Use a heating device to heat the source bottle to 120°C, introduce 2000 sccm of carrier gas Ar, mix the carrier gas with the evaporated solid, and then extract it from the source bottle in a vacuum environment to the reaction chamber for deposition.

[0048] [Results]: When the amount of material used in the source bottle was 0-5.2 kg, the evaporation rate remained above 200 g / h; when the amount of material used exceeded 5.2 kg, the evaporation rate dropped below 200 g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200 g / h) reached 87%.

[0049] Example 3

[0050] (1) 12 kg of aluminum chloride raw material was put into the heating zone of a sublimation equipment. The equipment parameters were: temperature 105° C., vacuum degree 1 torr, and time 48 h. After the sublimation was completed, the aluminum chloride material was collected, crushed, and sieved to obtain three different particle sizes of 0-2 mm, 4-6 mm, and 6-8 mm;

[0051] (2) three aluminum chloride materials with different particle sizes are uniformly filled into the tray grooves of six evaporation units in a mass ratio of 5:4:1, and then sequentially fed into the container, and the end cap and the container are sealed with bolts to form a complete precursor source bottle;

[0052] (3) Connect a precursor source bottle filled with 6 kg of precursor to the vapor deposition system, connect the carrier gas inlet to the system carrier gas pipeline, and connect the mixed vapor outlet to the system material delivery pipeline. Use a heating device to heat the source bottle to 120°C, introduce 2000 sccm of carrier gas Ar, mix the carrier gas with the evaporated solid, and then extract it from the source bottle in a vacuum environment to the reaction chamber for deposition.

[0053] [Results]: When the amount of material used in the source bottle was 0-4kg, the evaporation rate remained above 200g / h; when the amount of material used exceeded 4kg, the evaporation rate dropped below 200g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200g / h) reached 67%.

[0054] Example 4

[0055] (1) 12 kg of hafnium tetrachloride raw material was put into the heating zone of a sublimation equipment. The equipment parameters were: temperature 190° C., vacuum degree 1 torr, and time 48 h. After the sublimation was completed, the hafnium tetrachloride material was collected, crushed, and sieved to obtain three different particle sizes of 0-2 mm, 2-4 mm, and 4-6 mm;

[0056] (2) three hafnium tetrachloride materials with different particle sizes are uniformly filled into the tray grooves of six evaporation units in a mass ratio of 4:3:1, and then sequentially fed into the container, and the end cap and the container are sealed with bolts to form a complete precursor source bottle;

[0057] (3) Connect a precursor source bottle filled with 6 kg of precursor to the vapor deposition system, connect the carrier gas inlet to the system carrier gas pipeline, and connect the mixed vapor outlet to the system material delivery pipeline. Use a heating device to heat the source bottle to 200°C, introduce 2000 sccm of carrier gas Ar, mix the carrier gas with the evaporated solid, and then extract it from the source bottle in a vacuum environment to the reaction chamber for deposition.

[0058] [Results]: When the amount of material used in the source bottle was 0-4.6 kg, the evaporation rate remained above 200 g / h; when the amount of material used exceeded 4.6 kg, the evaporation rate dropped below 200 g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200 g / h) reached 77%.

[0059] Example 5

[0060] The semiconductor solid-state source precursor material is canned in accordance with Example 1, except that the particle sizes of the aluminum chloride material are 0-2 mm, 2-4 mm, and 6-8 mm, respectively, and the other conditions are the same as in Example 1. The precursor source bottle thus obtained is connected to the vapor deposition system for testing. The precursor source bottle thus obtained is connected to the vapor deposition system for testing.

[0061] [Results]: When the amount of material used in the source bottle was 0-4.2 kg, the evaporation rate remained above 200 g / h; when the amount of material used exceeded 4.2 kg, the evaporation rate dropped below 200 g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200 g / h) reached 70%.

[0062] Example 6

[0063] The semiconductor solid-state source precursor material is canned in accordance with Example 1, except that the particle sizes of the aluminum chloride material are 0-3 mm, 3-6 mm, and 6-9 mm, respectively, and the other conditions are the same as in Example 1. The precursor source bottle thus obtained is connected to the vapor deposition system for testing. The precursor source bottle thus obtained is connected to the vapor deposition system for testing.

[0064] [Results]: When the amount of material used in the source bottle was 0-3.9 kg, the evaporation rate remained above 200 g / h; when the amount of material used exceeded 3.9 kg, the evaporation rate dropped below 200 g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200 g / h) reached 65%.

[0065] Example 7

[0066] The semiconductor solid-state source precursor material was canned according to the method of Example 1, except that aluminum chloride materials with three different particle sizes of 0-2 mm, 2-4 mm, and 4-6 mm were evenly filled into the tray grooves of six evaporation units in a mass ratio of 1:6:1, and the other conditions were the same as in Example 1. The precursor source bottle thus obtained was connected to the vapor deposition system for testing.

[0067] [Results]: When the amount of material used in the source bottle was 0-3.4 kg, the evaporation rate remained above 200 g / h; when the amount of material used exceeded 3.4 kg, the evaporation rate dropped below 200 g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200 g / h) reached 56%.

[0068] Comparative Example 1

[0069] (1) 12 kg of aluminum chloride raw material was put into the heating zone of the sublimation equipment. The equipment parameters were temperature: 105° C., vacuum degree: 1 torr, and time: 48 h. After the sublimation was completed, the aluminum chloride material was collected, crushed, and sieved to obtain a particle size of 0 to 2 mm;

[0070] (2) The aluminum chloride material is evenly filled into the tray grooves of the six evaporation units, and then sequentially fed into the container, and the end cap and the container are sealed with bolts to form a complete precursor source bottle;

[0071] (3) Connect a precursor source bottle filled with 6 kg of precursor to the vapor deposition system, connect the carrier gas inlet to the system carrier gas pipeline, and connect the mixed vapor outlet to the system material delivery pipeline. Use a heating device to heat the source bottle to 120°C, introduce 2000 sccm of carrier gas Ar, mix the carrier gas with the evaporated solid, and then extract it from the source bottle in a vacuum environment to the reaction chamber for deposition.

[0072] (4) [Results]: When the amount of material used in the source bottle was 0-0.8 kg, the evaporation rate remained above 200 g / h; when the amount of material used exceeded 0.8 kg, the evaporation rate dropped below 200 g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200 g / h) was 13%.

[0073] Comparative Example 2

[0074] (1) 12 kg of aluminum chloride raw material is put into the heating zone of a sublimation equipment. The equipment parameters are temperature: 105° C., vacuum degree: 1 torr, and time: 48 hours. After the sublimation is completed, the aluminum chloride material is collected, crushed, and sieved to obtain a particle size of 2 to 4 mm;

[0075] (2) The aluminum chloride material is evenly filled into the tray grooves of the six evaporation units, and then sequentially fed into the container, and the end cap and the container are sealed with bolts to form a complete precursor source bottle;

[0076] (3) Connect a precursor source bottle filled with 6 kg of precursor to the vapor deposition system, connect the carrier gas inlet to the system carrier gas pipeline, and connect the mixed vapor outlet to the system material delivery pipeline. Use a heating device to heat the source bottle to 120°C, introduce 2000 sccm of carrier gas Ar, mix the carrier gas with the evaporated solid, and then extract it from the source bottle in a vacuum environment to the reaction chamber for deposition.

[0077] [Results]: When the amount of material used in the source bottle was 0-3kg, the evaporation rate remained above 200g / h; when the amount of material used exceeded 3kg, the evaporation rate dropped below 200g / h, indicating that the effective utilization rate of the material (based on the evaporation rate of 200g / h) was 50%.

[0078] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations on the present invention. A person skilled in the art may change, modify, replace and modify the above embodiments within the scope of the present invention without departing from the principles and intent of the present invention.

Claims

1. A method for packaging semiconductor solid-state source precursor materials, characterized in that: The method comprises the following steps: performing sublimation recrystallization treatment on a solid source precursor material, and then performing crushing and sieving treatment to obtain N kinds of precursor materials with different particle sizes, and filling the N kinds of precursor materials with different particle sizes into a tray of a precursor source bottle to complete canning, wherein N≧3; the maximum particle size of the N kinds of precursor materials is R N , the minimum particle size is R N ˋ, R N ≧R N ˋ; Arranged from small to large in particle size, the maximum particle size R of the Nth precursor material N ≦The minimum particle size R of the N+1th precursor material N+1 ˋ, and R N :R N+1 is (0.2~0.9):

1.

2. The method for packaging semiconductor solid-state source precursor materials according to claim 1, characterized in that: R N >R N When R N+1 ˋ-R N =0~4mm; R N =R N When R N ˋ≠0, R N+1 -R N =1-4mm; preferably, the R N -R N ˋ=0~4mm.

3. The method for packaging semiconductor solid-state source precursor materials according to claim 1, characterized in that: The precursor material includes first particles, second particles and third particles whose particle sizes increase in sequence.

4. The method for packaging semiconductor solid-state source precursor materials according to claim 1, characterized in that: The mass ratio of the first particles, the second particles and the third particles is (2-5):(2-4):

1.

5. The method for packaging semiconductor solid-state source precursor materials according to claim 1, characterized in that: The particle size of the first particles is 0-2 mm, the particle size of the second particles is 2-4 mm, and the particle size of the third particles is 4-6 mm; Preferably, the particle size of the first particles is 0-2 mm, the particle size of the second particles is 2-4 mm, and the particle size of the third particles is 6-8 mm.

6. The method for packaging semiconductor solid-state source precursor materials according to claim 1, characterized in that: The solid source precursor material is selected from one of aluminum trichloride, hafnium tetrachloride, gallium trichloride and antimony trichloride.

7. The method for packaging semiconductor solid-state source precursor materials according to claim 1, characterized in that: The sublimation recrystallization treatment method comprises: adding a solid source precursor material into a sublimation device, setting a sublimation temperature, a vacuum degree and a treatment time, and collecting the obtained product after the reaction is completed, and performing crushing and sieving treatments to obtain N kinds of precursor materials with different particle sizes.

8. The method for packaging semiconductor solid-state source precursor materials according to claim 7, characterized in that: The sublimation temperature and vacuum degree of the sublimation recrystallization treatment are determined according to the properties of the solid source precursor material.

9. A method for obtaining solid source precursor vapor, characterized in that: The method comprises: obtaining a precursor source bottle filled with semiconductor solid source precursor material by the canning method described in any one of claims 1 to 8, connecting the precursor source bottle to a vapor deposition system, connecting a carrier gas inlet of the precursor source bottle to a carrier gas pipeline of the vapor deposition system, connecting a mixed carrier gas outlet of the precursor source bottle to a material conveying pipeline of the vapor deposition system, heating the precursor source bottle, introducing carrier gas, mixing the carrier gas with evaporated solid source precursor in the precursor source bottle and discharging the mixed carrier gas outlet, thereby obtaining solid source precursor vapor.

10. Use of the method for packaging semiconductor solid-state source precursor materials according to any one of claims 1 to 8 or the method for obtaining solid-state source precursor vapor according to claim 9 in the field of semiconductor material technology.