CN113731299B - Particle size control process of trimethyl indium - Google Patents
Particle size control process of trimethyl indium Download PDFInfo
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- CN113731299B CN113731299B CN202111004097.XA CN202111004097A CN113731299B CN 113731299 B CN113731299 B CN 113731299B CN 202111004097 A CN202111004097 A CN 202111004097A CN 113731299 B CN113731299 B CN 113731299B
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- trimethyl indium
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- 239000002245 particle Substances 0.000 title claims abstract description 90
- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000000227 grinding Methods 0.000 claims abstract description 64
- 238000002156 mixing Methods 0.000 claims abstract description 62
- 239000000945 filler Substances 0.000 claims abstract description 32
- 238000009826 distribution Methods 0.000 claims abstract description 21
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 21
- 239000010935 stainless steel Substances 0.000 claims abstract description 21
- 238000012856 packing Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 238000005054 agglomeration Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 238000000859 sublimation Methods 0.000 abstract description 7
- 230000008022 sublimation Effects 0.000 abstract description 7
- 238000010586 diagram Methods 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000005465 channeling Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 235000000396 iron Nutrition 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 238000002488 metal-organic chemical vapour deposition Methods 0.000 description 1
- XZGYRWKRPFKPFA-UHFFFAOYSA-N methylindium Chemical compound [In]C XZGYRWKRPFKPFA-UHFFFAOYSA-N 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/10—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls with one or a few disintegrating members arranged in the container
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
Abstract
The invention provides a particle size control process of trimethyl indium, which is characterized in that one of a stainless steel triangular spring, stainless steel, a theta-ring, a ceramic ball, a ceramic rod, a stainless steel short pipe and a stainless steel perforated sheet is mixed with trimethyl indium particles in a mixing and grinding device, then the mixing and grinding device is used for mixing and grinding at the temperature of 30-60 ℃, the sublimation and sublimation of trimethyl indium are utilized to promote powdery trimethyl indium to grow into larger particles without agglomeration, a filler plays a dispersing effect in the mixing and grinding process to avoid trimethyl indium agglomeration, and in addition, the mixed filler can gradually grind down the oversize trimethyl indium particles to change the particle size distribution of the produced trimethyl indium.
Description
Technical Field
The invention relates to the field of trimethyl indium, in particular to a particle size control process of trimethyl indium.
Background
Trimethyl indium is an MO source organic metal compound, and is solid particles or powder at normal temperature, and the use mode of trimethyl indium is that inert carrier gas enters a source bottle, and trimethyl indium vapor in the steel bottle is carried to downstream MOCVD equipment for high-temperature deposition, so that the output concentration and the stability of trimethyl indium are extremely important, and particularly after the use amount reaches 70%, the phenomena of low output concentration and large fluctuation are particularly obvious, and the wavelength and the brightness of an epitaxial chip are seriously influenced. In general, the smaller the solid particle size, the higher the output concentration stability, but the too small particle size, the easy occurrence of particle hardening or local channeling "short circuit" in the source bottle; if the particles are too large, hardening can be avoided, but the amount of the trimethyl indium in the source bottle is reduced along with use, and the output steam concentration is easy to be insufficient.
To improve the above problems, there are three general improving methods in the industry: 1. optimally designing a steel cylinder structure, such as manufacturing a sleeve cylinder or a multi-cavity serial bottle to improve the concentration stability; 2. mixing a support in the trimethyl indium particles to avoid hardening and furrows; 3. the particle size of the trimethyl indium is changed. Wherein, the two improvements of No. 1 and No. 2 are mature in China, but No. 3 controls the particle size of the trimethyl indium, at present, no good process method exists in China, the particle size is determined in the production and receiving process of the trimethyl indium, and the particle size distribution cannot meet the problem of concentration stability in the later period of use. Particle size is a key quality parameter for solid sources, which is also an unsolved problem within the domestic industry today. The prior art patent CN105063570A discloses a method for improving the utilization rate of trimethyl indium, which can improve the utilization rate of trimethyl indium in use by mixing trimethyl indium with solid particles with the angle of repose of 25-45 degrees, which do not generate chemical reaction, and filling the mixture into a closed container. However, this patent only discloses that trimethylindium is mixed with solid particles, but there is no disclosure of how to mix to control the particle size of trimethylindium, and thus a process for controlling the particle size of trimethylindium particles is required.
Disclosure of Invention
In order to solve the problems, the invention provides a particle size control process of trimethyl indium, one of a stainless steel triangular spring, stainless steel, a theta-ring, a ceramic ball, a ceramic rod, a stainless steel short pipe and a stainless steel perforated sheet is mixed with trimethyl indium particles in a mixing and grinding device, then the mixing and grinding device is used for mixing and grinding at the temperature of 30-60 ℃, sublimation and sublimation of trimethyl indium are utilized to promote powdery trimethyl indium to grow into larger particles, a filler has a dispersing effect in the mixing and grinding process to avoid trimethyl indium agglomeration, in addition, the mixed filler can gradually grind down the oversize trimethyl indium particles, the particle size distribution of the produced trimethyl indium is changed, and the problems in the background technology are solved.
The invention aims to provide a particle size control process of trimethyl indium, which comprises the following steps:
the method comprises the following steps: selecting a finished product produced by trimethyl indium rectification, and determining the particle size distribution of the original state of the finished product by using a screen under the protection of inert atmosphere;
step two: mixing the trimethylindium particles and the filler in an inert gas atmosphere, adding the mixture into a mixing and grinding device, and testing the leakage rate of the mixing and grinding device to obtain the leakage rate<10 -9 M 3 •Pa/S；
Step three: and (3) installing the completely sealed mixed grinding device, starting mixing, carrying out integral heat tracing on the mixed grinding device, starting mixed grinding for 36-72h after the temperature reaches 30-60 ℃, stopping heat tracing, and stopping mixing after the temperature of the mixed grinding device is reduced to room temperature.
Step four: and (4) moving the mixing and grinding device to an inert atmosphere, opening the mixing and grinding device, pouring out trimethyl indium solid, screening, weighing and calculating the particle size distribution.
The further improvement lies in that: the filler is one of a stainless steel triangular spring, stainless steel for a west tower ring, a ceramic ball, a ceramic rod, a stainless steel short pipe and a stainless steel punching sheet.
The further improvement is that: the filler is a stainless steel triangular spring with the diameter of 1.5X 2mm to 5X 5mm.
The further improvement is that: the mixing and grinding speed is 5 to 60r/min; the packing density of the filler is 0.8 to 2.0g/cm < 3 >; the mixing volume ratio range of the trimethyl indium and the filler is as follows: 0.1 to 2; the volume of the mixture of the trimethyl indium and the filler is not more than 80 percent of the volume of the mixing and grinding device.
The further improvement lies in that: the mixing and grinding rotating speed is 10 to 30r/min; the packing density of the filler is 1 to 1.4 g/cm 3 (ii) a The mixing volume ratio range of the trimethyl indium and the filler is as follows: 0.2 to 0.8; the mixing volume of the trimethyl indium and the filler is not more than 30-60% of the volume of the mixing and grinding device.
The further improvement lies in that: the temperature of the mixing process in the third step is increased to 30-40 ℃ in a gradient way, then is increased to 40-60 ℃, is reduced to 30-40 ℃, is increased by 5 ℃ per hour, and is maintained at each temperature point for 1 hour.
The further improvement lies in that: the mixing and grinding device is one of a ball mill, a conical mixer, a V-shaped mixer and a horizontal mixer.
The further improvement lies in that: the maximum particle size of finished product particles produced by rectifying the trimethylindium in the step one is less than or equal to 10mm, wherein the weight ratio of the particles with the particle size of less than 0.6mm is less than or equal to 50%.
The invention has the beneficial effects that: according to the invention, one of a stainless steel triangular spring, a stainless steel Western-tower ring, a ceramic ball, a ceramic rod, a stainless steel short tube and a stainless steel perforated sheet is mixed with trimethyl indium particles in a mixing and grinding device, then the mixing and grinding device performs mixing and grinding at 30-60 ℃, sublimation and sublimation of trimethyl indium are utilized to promote powdery trimethyl indium to grow into larger particles without agglomeration, the filler has a dispersing effect in the mixing and grinding process, and trimethyl indium agglomeration is avoided, in addition, the mixed filler can gradually grind down the trimethyl indium with too large particles, so that the particle size distribution of the produced trimethyl indium is changed; IIIHeating and taking out the methyl indium under inert atmosphere to ensure the purity of the trimethyl indium; the temperature in the mixing process is changed in a gradient manner, and is increased and then decreased, so that the particle size control effect is better by matching with the mixing and grinding of the filler; the mixing volume ratio of the trimethyl indium to the filler is 0.2 to 0.8, so that the particle size control effect is further ensured; the mixed grinding device is used for carrying out leakage rate test and requiring leakage rate<10 -9 M 3 Pa/S, preventing the influence of micro-oxidation on the product quality in the mixed grinding process.
Drawings
FIG. 1 is a schematic diagram of trimethylindium before the first to fourth embodiments of mixed grinding.
FIG. 2 is a schematic diagram of the particles with a diameter of 5mm or more of trimethylindium after the first to fourth mixed grinding in examples.
FIG. 3 is a schematic diagram of trimethyl indium 2-5 mm granules obtained by mixing and grinding in the first to fourth steps.
FIG. 4 is a schematic diagram of 0.6-2mm trimethylindium granules after mixing and grinding in examples I to IV.
FIG. 5 is a schematic representation of trimethylindium <0.6mm particles after the first to fourth mixings of examples.
Detailed Description
In order to further understand the present invention, the following detailed description will be made with reference to the following examples, which are only used for explaining the present invention and are not to be construed as limiting the scope of the present invention.
The first embodiment is as follows:
firstly, determining the original state particle size distribution of trimethyl indium by using a screen, taking a ball mill as mixing equipment, taking a 5 x 5mm stainless steel theta ring as a filler, and taking the packing bulk density of the filler as 1.4 g/cm 3 Taking 200g of trimethyl indium, and mixing according to the volume ratio of filler/trimethyl indium = 1/3; the temperature is constant at 50 ℃; the rotating speed is 30r/min; and (5) carrying out mixed grinding for 48h. The particle size distribution before and after the mixed grinding is as follows, the schematic diagrams of trimethyl indium particles with different particle sizes are shown in figures 1-5,
 |
<0.6mm | 0.6~2mm | 2~5mm | ≥5mm |
| before mixed grinding | 24.8% | 29.6% | 30.6% | 15.0% |
| After mixed grinding | 19.8% | 35.5% | 34.4% | 10.3% |
According to the first embodiment: the particle size distribution before and after the mixed grinding is relatively balanced, and the embodiment is suitable for the condition of relatively balanced particle size distribution.
Example two
Firstly, determining the original state particle size distribution of trimethyl indium by using a screen, taking a ball mill as mixing equipment, taking a 5 x 5mm stainless steel triangular spring as a filler, and taking the packing bulk density as 1.1g/cm 3 Taking 200g of trimethyl indium, and mixing according to the volume ratio of filler/trimethyl indium = 1/3; the temperature gradient is: the temperature rises to 5 ℃ per hour at 30 ℃→ 50 ℃→ 30 ℃, and each temperature point is maintained for 1h; the rotating speed is 30r/min, and the mixed grinding is carried out for 48 hours. The particle size distribution before and after the mixed grinding is as follows, the trimethyl irons with different particle sizesSchematic diagrams of indium-based particles are shown in figures 1-5,
 |
<0.6mm | 0.6~2mm | 2~5mm | ≥5mm |
| before mixed grinding | 24.8% | 29.6% | 30.6% | 15.0% |
| After mixed grinding | 10.3% | 36% | 47.4% | 6.3% |
The second embodiment shows that: in the embodiment, the particle size of 0.6-2mm and 2-5mm trimethylindium particles are more distributed together, so that the condition that the particle size is more is adapted.
EXAMPLE III
Firstly, a sieve is used for determining the particle size distribution of trimethyl indium in the initial state, and a V-shaped mixer is usedAs mixing equipment, ceramic beads with the diameter of 5mm are used as filling materials, and the packing material bulk density is 1.6 g/cm 3 Taking 200g of trimethyl indium, mixing according to the volume ratio of filler/trimethyl indium =2/3, keeping the temperature at 40 ℃, rotating speed at 10r/min, and mixing and grinding for 48h. The particle size distribution before and after the mixing and grinding is as follows, the schematic diagrams of the trimethyl indium particles with different particle sizes are shown in figures 1-5,
 |
<0.6mm | 0.6~2mm | 2~5mm | ≥5mm |
| before mixed grinding | 24.8% | 29.6% | 30.6% | 15.0% |
| After mixed grinding | 24.5% | 48.4% | 20.8% | 6.3% |
According to the third embodiment: the mixing and grinding effect of the trimethylindium particles with the particle size of 2-5 mm or more is better, the control effect of the embodiment on the trimethylindium particles with large particle size is better, and the method is suitable for the condition that more trimethylindium particles with the required particle size of 0.6-2mm are needed.
In the first to third examples, the particle size distribution after the final mixing is the best when the particle size distribution before mixing is the same, the trimethylindium particles with the particle size of less than 0.6mm and not less than 5mm in the second example are obviously reduced, and the trimethylindium particles with the particle size of 0.6 to 2mm and 2 to 5mm are obviously increased, which is the best example.
Example four
Firstly, determining the particle size distribution of trimethyl indium in an initial state by using a screen, taking a V-shaped mixer as mixing equipment, taking a 3X 3mm stainless steel triangular spring as a filler, and setting the packing bulk density to be 1.2g/cm 3 Taking 200g of trimethyl indium, and mixing according to the volume ratio of filler/trimethyl indium = 2/3; the temperature gradient is: temperature rises to 5 degrees per hour in a range of 30 ℃→ 50 ℃→ 30 ℃, and each temperature point is maintained for 2 hours; and (5) carrying out mixed grinding for 72h. The particle size distribution before and after the mixed grinding is as follows, the schematic diagrams of trimethyl indium particles with different particle sizes are shown in figures 1-5,
 |
<0.6mm | 0.6~2mm | 2~5mm | ≥5mm |
| before mixed grinding | 27.3% | 60.4% | 12.3% | \ |
| After mixed grinding | 12.1% | 65.5% | 21.7% | 0.7% |
The fourth example shows that: in the case of a large number of small primary particle size distributions, the effect of controlling the small-particle size trimethylindium particles can be further enhanced by using this example.
In the embodiment, sublimation and desublimation of the trimethyl indium are utilized to promote the powdery trimethyl indium to grow into larger particles without agglomeration, the filler plays a role in dispersing in the mixing and grinding process, and trimethyl indium agglomeration is avoided.
Claims (2)
1. A particle size control process of trimethyl indium is characterized in that: the method comprises the following steps:
the method comprises the following steps: selecting a finished product produced by trimethyl indium rectification, and determining the particle size distribution of the original state of the finished product by using a screen under the protection of inert atmosphere; the maximum particle size of finished product particles produced by rectifying trimethyl indium is less than or equal to 10mm, wherein the weight ratio of particles with the particle size of less than 0.6mm is less than or equal to 50%;
step two: mixing the trimethylindium particles and the filler in an inert gas atmosphere, adding the mixture into a mixing and grinding device, and testing the leakage rate of the mixing and grinding device; the filler is a stainless steel triangular spring with the diameter of 1.5 x 2mm-5 x 5mm;
step three: installing the completely sealed mixed grinding device, starting mixing, carrying out integral heat tracing on the mixed grinding device, starting mixed grinding for 36-72h after the temperature reaches 30-60 ℃, stopping heat tracing, and stopping mixing after the temperature of the mixed grinding device is reduced to room temperature;
the mixed grinding speed is 5-60 r/min; the packing has a bulk density of 0.8 to 2.0g/cm 3 (ii) a The mixing volume ratio range of the trimethyl indium and the filler is as follows: 0.1 to 2; the mixing volume of the trimethyl indium and the filler is not more than 80 percent of the volume of the mixing and grinding device;
or the mixed grinding rotating speed is 10-30 r/min; the packing has a bulk density of 1 to 1.4 g/cm 3 (ii) a The mixing volume ratio range of the trimethyl indium and the filler is as follows: 0.2 to 0.8; the mixing volume of the trimethyl indium and the filler is not more than 30-60% of the volume of the mixing and grinding device;
the heat tracing temperature is changed in a gradient manner, firstly, the temperature is increased to 30-40 ℃, then, the temperature is increased to 40-60 ℃, then, the temperature is decreased to 30-40 ℃, the temperature is increased by 5 ℃ per hour, and each temperature point is maintained for 1 hour;
step four: and (3) moving the mixed grinding device to an inert atmosphere, opening the mixed grinding device, pouring out trimethyl indium solid, screening, weighing and calculating the particle size distribution.
2. The process for controlling the particle size of trimethylindium according to claim 1, wherein: the mixing and grinding device is one of a ball mill, a conical mixer, a V-shaped mixer and a horizontal mixer.
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| US5296189A (en) * | 1992-04-28 | 1994-03-22 | International Business Machines Corporation | Method for producing metal powder with a uniform distribution of dispersants, method of uses thereof and structures fabricated therewith |
| JP2002121077A (en) * | 2000-10-12 | 2002-04-23 | Ngk Insulators Ltd | Finely pulverized ceramic raw material and method of producing the same |
| FR2826299B1 (en) * | 2001-06-25 | 2003-09-26 | Wheelabrator Allevard | METHOD AND DEVICE FOR FINE GRINDING OF MINERAL PARTICLES |
| CN1868967A (en) * | 2006-02-06 | 2006-11-29 | 张润铎 | Technology of preparing nanometer composite oxide by mechanical grinding |
| JP2016145170A (en) * | 2015-02-09 | 2016-08-12 | 宇部興産株式会社 | Method for producing solid organic metallic compound and production device therefor |
| CN105063570A (en) * | 2015-08-31 | 2015-11-18 | 清远先导材料有限公司 | Method for improving trimethyl indium utilization rate |
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