CN112295717A - Device and method for preparing high-purity low-oxygen silicon powder through crushing - Google Patents
Device and method for preparing high-purity low-oxygen silicon powder through crushing Download PDFInfo
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- CN112295717A CN112295717A CN202011097999.8A CN202011097999A CN112295717A CN 112295717 A CN112295717 A CN 112295717A CN 202011097999 A CN202011097999 A CN 202011097999A CN 112295717 A CN112295717 A CN 112295717A
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- assembly
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
- B02C23/18—Adding fluid, other than for crushing or disintegrating by fluid energy
- B02C23/24—Passing gas through crushing or disintegrating zone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C23/00—Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
Abstract
The invention provides a device and a method for preparing high-purity low-oxygen silicon powder by crushing, wherein the device comprises a pressurizing assembly, a nitrogen-making assembly and a crushing assembly; the nitrogen making assembly is connected with the pressurizing assembly through a pipeline; the crushing assembly is connected with the pressurizing assembly through a circulating pipeline. The silicon powder prepared by the method has extremely low oxygen content, and can meet the use requirement of low-oxygen high-purity WSi.
Description
Technical Field
The invention belongs to the technical field of crushing, relates to a device and a method for crushing silicon powder, and particularly relates to a device and a method for preparing high-purity low-oxygen silicon powder through crushing.
Background
A plurality of high-purity WSi (silicon content of 29%) alloy targets are needed in semiconductor magnetron sputtering, the manufacturing method comprises the steps of mixing high-purity metal powder and high-purity silicon powder, and then carrying out hot pressing or hot isostatic pressing forming, wherein the needed silicon powder raw material generally requires more than 99.999%.
The semiconductor industry develops better and better, the technical requirements are more and more precise, and the quality of the tungsten silicon target material is more and more strict; the purity of the tungsten silicon target needs 99.999 percent, and the oxygen content of the gas is required to be less than 930ppm or even 500ppm, so that the oxygen content in W powder and Si powder is required to be low. The oxygen content in W powder is generally 300-400ppm, so that it is very important to control the oxygen content in Si powder. At present, most of Si powder is prepared by an open airflow crushing method, and the oxygen content of the Si powder prepared by the method reaches 2000-3000ppm, and the oxygen content is introduced in the process of mixing W powder and Si powder and hot pressing and die filling, so that the use of low-oxygen high-purity WSi of a semiconductor cannot be met.
CN109174390A provides a high-efficient broken and clean processingequipment of silica flour production line, including bucket elevator, jaw crusher, vertical disc mill, cyclone, collection feed bin and filter equipment, wherein, bucket elevator's output is connected with jaw crusher's feed inlet, be equipped with first water inlet and first delivery port on the jaw crusher, be connected with the inlet tube on the first water inlet, the one end of inlet tube is connected with water supply equipment, jaw crusher's discharge gate end is connected with the defeated material mechanism of spiral, the one end that the defeated material mechanism of spiral was kept away from jaw crusher runs through and extends to vertical disc mill's inner chamber middle part.
CN205308865U provides a silicon powder crushing processing device, wherein a horizontal mixer is installed on a chassis, a separation tank for receiving materials is arranged below and behind a discharge port of the horizontal mixer, the separation tank is supported on the top of a water tank by a positioning frame, a chassis is installed behind the water tank, a vertical crusher is installed on the chassis, a driven pulley is sleeved on the upper end of an input shaft of the vertical crusher, the driven pulley is connected with a driving pulley through a belt, the driving pulley is sleeved on an output shaft of a motor, and two air nozzles are installed on a shell of the vertical crusher; the material collecting box is arranged below the vertical crusher, the chute is arranged obliquely above the vertical crusher, the lower end of the chute extends into the vertical crusher, and the hopper is arranged at the upper end of the chute.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a device and a method for preparing high-purity low-oxygen silicon powder by crushing.
The invention aims to provide a device for preparing high-purity low-oxygen silicon powder by crushing, which comprises a pressurizing assembly, a nitrogen-making assembly and a crushing assembly;
the nitrogen making assembly is connected with the pressurizing assembly through a pipeline;
the crushing assembly is connected with the pressurizing assembly through a circulating pipeline.
As a preferred technical scheme of the invention, the nitrogen generating assembly comprises at least one nitrogen generator.
As a preferable technical scheme, the nitrogen production assembly is connected with the crushing assembly through a pipeline.
In the invention, the nitrogen making assembly is connected with the crushing assembly, and the atmospheric pressure nitrogen provided by the nitrogen making assembly and the compressed nitrogen provided by the pressurizing assembly simultaneously replace the air in the crushing assembly. The crushing assembly and the pressurizing assembly may be independently connected to a nitrogen generator.
As a preferred embodiment of the present invention, the circulation line between the crushing module and the pressurizing module is used to form a closed-loop flow of nitrogen gas.
In the invention, the closed-loop airflow for forming the nitrogen can ensure the oxygen-free environment in the equipment, and can save the use amount of the nitrogen, so that the nitrogen-making component does not need to work continuously.
As a preferable technical solution of the present invention, a pressurized nitrogen gas line is provided between the crushing module and the pressurizing module.
According to the invention, all inner walls in the crushing assembly are lined with polyurethane, so that silicon does not contact with metal, and the purity of silicon powder is ensured.
The invention also aims to provide a method for preparing high-purity low-oxygen silicon powder by crushing, which uses the device and comprises the following steps:
(1) nitrogen is provided by a nitrogen making assembly and enters the pressurizing assembly, and the pressurized nitrogen replaces the gas in the crushing assembly to form a nitrogen atmosphere;
(2) adding silicon particles into the crushing assembly, and starting the crushing assembly to prepare powder;
(3) in the powder making process, a closed cycle of nitrogen is formed between the crushing assembly and the pressurizing assembly through a circulating pipeline until the powder making is finished.
In a preferred embodiment of the present invention, the nitrogen-generating component in step (1) provides nitrogen with a purity of not less than 99.9%, such as 99.95%, 99.99%, 99.995%, or 99.999%, but not limited to the recited values, and other values not recited in the range of the recited values are also applicable.
Preferably, the pressurized nitrogen gas in step (1) has a pressure of 5 to 15kg, such as 6kg, 7kg, 8kg, 9kg, 10kg, 11kg, 12kg, 13kg or 14kg, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the nitrogen atmosphere in step (1) has an oxygen content of less than 1000ppm, such as 100ppm, 200ppm, 300ppm, 400ppm, 500ppm, 600ppm, 700ppm, 800ppm or 900ppm, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
As a preferable technical scheme of the invention, the particle size of the silicon particles in the step (2) is less than 1mm, and the purity is more than 99.999 percent; the particle size may be 0.1mm, 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.8mm, 0.9mm, etc., but is not limited to the values listed, and other values not listed in the numerical range are also applicable.
As a preferable technical scheme of the invention, in the closed circulation of the nitrogen in the step (3), the nitrogen in the crushing assembly enters the pressurizing assembly after being dedusted.
Preferably, the classifier power of the crushing assembly in the milling process is not lower than 50Hz, such as 60Hz, 70Hz, 80Hz, 90Hz, 100Hz, 150Hz, 200Hz or 250Hz, but not limited to the values listed, and other values not listed in the numerical range are also applicable.
In the invention, the grader can prepare high-purity oxygen-free fine silicon powder with the grain size less than 4 mu m when working at the power of 50 Hz.
As a preferred technical scheme of the invention, the method for preparing the high-purity low-oxygen silicon powder by crushing comprises the following steps:
(1) nitrogen with the purity not lower than 99.9% is provided by a nitrogen making assembly and enters the pressurizing assembly, the pressure of the pressurized nitrogen is 5-15 kg, and the pressurized nitrogen replaces the gas in the crushing assembly to form a nitrogen atmosphere with the oxygen content less than 1000 ppm;
(2) adding silicon particles into the crushing assembly, wherein the particle size of the silicon particles is less than 1mm, the purity of the silicon particles is more than 99.999%, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing assembly and the pressurizing assembly through a circulating pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing assembly enters the pressurizing assembly after dust removal, and the power of a classifier of the crushing assembly in the powder process is not lower than 50Hz until the powder process is finished.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a device and a method for preparing high-purity low-oxygen silicon powder by crushing, wherein the oxygen content of the silicon powder prepared by the method is extremely low within 1000ppm, and the use of low-oxygen high-purity WSi can be met.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing high-purity low-oxygen silicon powder by crushing according to example 1 of the present invention;
FIG. 2 is a block diagram of an apparatus for producing high-purity low-oxygen silicon powder by crushing according to example 2 of the present invention;
fig. 3 is a structural diagram of an apparatus for producing high-purity low-oxygen silicon powder by crushing according to example 3 of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a device for crushing and manufacturing high-purity low-oxygen silicon powder, the structure of which is shown in fig. 1, and the device comprises a pressurizing assembly 3, a nitrogen-making assembly 2 and a crushing assembly 1;
the nitrogen production component 2 is connected with the pressurizing component 3 through a pipeline;
the crushing assembly 1 is connected with the pressurizing assembly 3 through a circulating pipeline;
the circulation pipeline between the crushing assembly 1 and the pressurizing assembly 3 is used for forming a closed-loop airflow of nitrogen.
Example 2
The embodiment provides a device for crushing and manufacturing high-purity low-oxygen silicon powder, the structure of which is shown in fig. 2, and the device comprises a pressurizing assembly 3, a nitrogen-making assembly 2 and a crushing assembly 1;
the nitrogen production component 2 is connected with the pressurizing component 3 through a pipeline;
the crushing assembly 1 is connected with the pressurizing assembly 3 through a circulating pipeline;
the nitrogen making assembly 2 is connected with the crushing assembly 1 through a pipeline;
the circulation pipeline between the crushing assembly 1 and the pressurizing assembly 3 is used for forming a closed-loop airflow of nitrogen.
Example 3
The embodiment provides a device for crushing and manufacturing high-purity low-oxygen silicon powder, the structure of which is shown in fig. 3, and the device comprises a pressurizing assembly 3, a nitrogen-making assembly and a crushing assembly 1;
the nitrogen generation assembly comprises a first nitrogen generator 21 and a second nitrogen generator 22;
the first nitrogen generator 21 is connected with the pressurizing assembly 3 through a pipeline;
the crushing assembly 1 is connected with the pressurizing assembly 2 through a circulating pipeline;
the second nitrogen generator 22 is connected with the crushing assembly 1 through a pipeline;
the circulating pipeline between the crushing assembly 1 and the pressurizing assembly 2 is used for forming a closed-loop airflow of nitrogen;
an independent pipeline is arranged between the pressurizing assembly 3 and the crushing assembly 1 and used for providing pressurizing nitrogen for the crushing assembly 1 when the crushing assembly 1 forms a nitrogen atmosphere and closing the pipeline after the nitrogen atmosphere is formed.
Application example 1
The application example provides a method for preparing high-purity low-oxygen silicon powder by crushing, and the device provided by the embodiment 1 is used, and the method comprises the following steps:
(1) nitrogen with the purity of 99.99% is provided by the nitrogen making assembly 2 and enters the pressurizing assembly 3, the pressure of the pressurized nitrogen is 5kg, and the pressurized nitrogen replaces the gas in the crushing assembly 1 to form a nitrogen atmosphere with the oxygen content of less than 1000 ppm;
(2) adding silicon particles into the crushing assembly 1, wherein the particle size of the silicon particles is about 500 microns, the purity of the silicon particles is more than 99.999 percent, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing component 1 and the pressurizing component 3 through a circulation pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing component 1 enters the pressurizing component 3 after dust removal, and the power of a classifier of the crushing component in the powder process is 50Hz until the powder process is finished.
Application example 2
The application example provides a method for preparing high-purity low-oxygen silicon powder by crushing, and the device provided by the embodiment 1 is used, and the method comprises the following steps:
(1) nitrogen with the purity of 99.95% is provided by the nitrogen making assembly 2 to enter the pressurizing assembly 3, the pressure of the pressurized nitrogen is 15kg, and the pressurized nitrogen replaces the gas in the crushing assembly 1 to form a nitrogen atmosphere with the oxygen content of less than 500 ppm;
(2) adding silicon particles into the crushing assembly 1, wherein the particle size of the silicon particles is about 300 microns, the purity of the silicon particles is more than 99.999 percent, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing component 1 and the pressurizing component 3 through a circulation pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing component 1 enters the pressurizing component 3 after dust removal, and the power of a classifier of the crushing component in the powder process is 100Hz until the powder process is finished.
Application example 3
The application example provides a method for preparing high-purity low-oxygen silicon powder by crushing, and the device provided by the embodiment 1 is used, and the method comprises the following steps:
(1) nitrogen with the purity of 99.99% is provided by the nitrogen making assembly 2 and enters the pressurizing assembly 3, the pressure of the pressurized nitrogen is 10kg, and the pressurized nitrogen replaces the gas in the crushing assembly 1 to form a nitrogen atmosphere with the oxygen content of less than 800 ppm;
(2) adding silicon particles into the crushing assembly 1, wherein the particle size of the silicon particles is about 800 microns, the purity of the silicon particles is more than 99.999 percent, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing component 1 and the pressurizing component 3 through a circulation pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing component 1 enters the pressurizing component 3 after dust removal, and the power of a classifier of the crushing component in the powder process is 80Hz until the powder process is finished.
Application example 4
The application example provides a method for preparing high-purity low-oxygen silicon powder through crushing, and the device provided by the embodiment 2 is used, and the method comprises the following steps:
(1) nitrogen with the purity of 99.99% is provided by the nitrogen making assembly 2 and enters the pressurizing assembly 3, the pressure of the pressurized nitrogen is 10kg, the pressurized nitrogen replaces the gas in the crushing assembly 1, meanwhile, the nitrogen making assembly 2 provides normal-pressure nitrogen for the crushing assembly 1, and the pressurized nitrogen is matched to form a nitrogen atmosphere with the oxygen content of less than 800 ppm;
(2) adding silicon particles into the crushing assembly 1, wherein the particle size of the silicon particles is about 800 microns, the purity of the silicon particles is more than 99.999 percent, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing component 1 and the pressurizing component 3 through a circulation pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing component 1 enters the pressurizing component 3 after dust removal, and the power of a classifier of the crushing component in the powder process is 80Hz until the powder process is finished.
Application example 5
(1) Nitrogen with the purity of 99.99 percent is provided by the first nitrogen generator 21 to enter the pressurizing assembly 3, the pressure of the pressurized nitrogen is 10kg, the pressurized nitrogen replaces the gas in the crushing assembly 1, meanwhile, the second nitrogen generator 22 provides normal-pressure nitrogen for the crushing assembly 1, and the pressurized nitrogen is matched to form a nitrogen atmosphere with the oxygen content of less than 800 ppm;
(2) adding silicon particles into the crushing assembly 1, wherein the particle size of the silicon particles is about 800 microns, the purity of the silicon particles is more than 99.999 percent, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing component 1 and the pressurizing component 3 through a circulation pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing component 1 enters the pressurizing component 3 after dust removal, and the power of a classifier of the crushing component in the powder process is 80Hz until the powder process is finished.
The oxygen content of the silicon powder obtained in examples 1 to 5 was measured by ICP mapping, and the results are shown in Table 1.
TABLE 1
| Oxygen content/ppm | |
| Application example 1 | 695 |
| Application example 2 | 886 |
| Application example 3 | 796 |
| Application example 4 | 781 |
| Application example 5 | 753 |
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The device for preparing the high-purity low-oxygen silicon powder through crushing is characterized by comprising a pressurizing assembly, a nitrogen-making assembly and a crushing assembly;
the nitrogen making assembly is connected with the pressurizing assembly through a pipeline;
the crushing assembly is connected with the pressurizing assembly through a circulating pipeline.
2. The apparatus of claim 1, wherein the nitrogen-generating assembly comprises at least one nitrogen generator.
3. The apparatus of claim 1, wherein the nitrogen-generating assembly is connected to the crushing assembly by a conduit.
4. The apparatus of claim 1, wherein the circulation line between the breaking assembly and the pressurizing assembly is configured to form a closed flow of nitrogen.
5. The apparatus of claim 1, wherein a pressurized nitrogen line is disposed between the crushing assembly and the pressurizing assembly.
6. A method for preparing high-purity low-oxygen silicon powder through crushing, which is characterized by using the device of any one of claims 1-5, and comprises the following steps:
(1) nitrogen is provided by a nitrogen making assembly and enters the pressurizing assembly, and the pressurized nitrogen replaces the gas in the crushing assembly to form a nitrogen atmosphere;
(2) adding silicon particles into the crushing assembly, and starting the crushing assembly to prepare powder;
(3) in the powder making process, a closed cycle of nitrogen is formed between the crushing assembly and the pressurizing assembly through a circulating pipeline until the powder making is finished.
7. The method of claim 6, wherein the nitrogen-producing component of step (1) provides nitrogen gas having a purity of no less than 99.9%;
preferably, the pressure of the pressurized nitrogen in the step (1) is 5-15 kg;
preferably, the oxygen content in the nitrogen atmosphere of step (1) is less than 1000 ppm.
8. The method of claim 6, wherein the silicon particles of step (2) have a particle size of less than 1mm and a purity of greater than 99.999%.
9. The method of claim 6, wherein in the closed cycle of nitrogen gas in step (3), the nitrogen gas in the crushing assembly is dedusted and then enters the pressurizing assembly;
preferably, the classifier power of the crushing assembly in the milling process is not lower than 50 Hz.
10. Method according to any of claims 6-9, characterized in that the method comprises the steps of:
(1) nitrogen with the purity not lower than 99.9% is provided by a nitrogen making assembly and enters the pressurizing assembly, the pressure of the pressurized nitrogen is 5-15 kg, and the pressurized nitrogen replaces the gas in the crushing assembly to form a nitrogen atmosphere with the oxygen content less than 1000 ppm;
(2) adding silicon particles into the crushing assembly, wherein the particle size of the silicon particles is less than 1mm, the purity of the silicon particles is more than 99.999%, and starting the crushing assembly to prepare powder;
(3) in the powder process, a closed cycle of nitrogen is formed between the crushing assembly and the pressurizing assembly through a circulating pipeline, in the closed cycle of the nitrogen, the nitrogen in the crushing assembly enters the pressurizing assembly after dust removal, and the power of a classifier of the crushing assembly in the powder process is not lower than 50Hz until the powder process is finished.
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| JPH09301710A (en) * | 1996-05-13 | 1997-11-25 | Shin Etsu Chem Co Ltd | Low-oxygen silicon granule, its production and production of silicon nitride |
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