CN118987668B - Precursor sublimation device and method for semiconductor film deposition - Google Patents
Precursor sublimation device and method for semiconductor film deposition Download PDFInfo
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Abstract
本发明提供了一种半导体薄膜沉积用前驱体升华装置及方法，属于物质分离装置领域。本发明提供的半导体薄膜沉积用前驱体升华装置，包括：流化部，其至少具有一个用于容纳待升华物料的流化桶，用于使待升华物料处于流化状态，流化桶具有一个入口和一个出口；进气部，设置在流化部的入口处，用于向流化桶通入气体，轻组分沉积部，其与流化部连通；收集部，包括用于收集目标物料的收集桶，收集桶通过带有至少一个阀门的连接管与流化部连通，收集桶内部设置有一个用于与外部真空源相连通的真空管。本发明提供的升华装置可以提升升华效率。
The present invention provides a precursor sublimation device and method for semiconductor thin film deposition, which belongs to the field of material separation devices. The precursor sublimation device for semiconductor thin film deposition provided by the present invention includes: a fluidizing part, which has at least one fluidizing barrel for accommodating the material to be sublimated, and is used to make the material to be sublimated in a fluidized state, and the fluidizing barrel has an inlet and an outlet; an air inlet part, which is arranged at the inlet of the fluidizing part, and is used to pass gas into the fluidizing barrel, and a light component deposition part, which is connected to the fluidizing part; a collecting part, including a collecting barrel for collecting target materials, and the collecting barrel is connected to the fluidizing part through a connecting pipe with at least one valve, and a vacuum tube for connecting to an external vacuum source is arranged inside the collecting barrel. The sublimation device provided by the present invention can improve the sublimation efficiency.
Description
Technical Field
The invention relates to the field of substance separation devices, in particular to a precursor sublimation device and method for depositing a semiconductor film.
Background
The sublimation process refers to a process in which a solid substance directly forms a gas without passing through a liquid state. Sublimation processes can separate mixtures of different volatilities, or non-sublimating substances from sublimable substances, and thus solid sublimation is a common means of purification in chemical processes. Sublimators are widely used for purity enhancement of solid materials by using the principle of sublimation.
The purity of the precursor for semiconductor thin film deposition is generally extremely high, and it is generally purified by sublimation in the prior art, but it is difficult to purify it to a desired purity by a general sublimator.
The common sublimator is to directly add the solid matter into the container, and the solid matter can contact with the air environment in the adding process, so that the solid matter is easy to react with water and oxygen in the air, and the hidden trouble of deterioration or safety of the solid matter can be caused. As the sublimation of heat proceeds, the substances of different volatilities gradually separate. In the sublimation process, when the solid matter is large in quantity, the phenomenon of uneven heat transfer exists, and impurities and products are sublimated simultaneously due to different heat, so that the sublimation efficiency is difficult to improve. At the same time, the non-sublimated solid matter and impurities are extremely easy to harden in the container, thus slowing down the sublimation process. The easily separated impurities will first be deposited in the collection device, so that to avoid contact with the product, multiple collection tanks are required or the easily separated impurities are removed before subsequent collection, increasing equipment investment and sublimation steps.
Disclosure of Invention
The present invention has been made to solve the above-described problems, and an object of the present invention is to provide a precursor sublimation apparatus for semiconductor thin film deposition having high sublimation efficiency and requiring only one collection tank, and a precursor sublimation method for semiconductor thin film deposition using the same.
The invention provides a precursor sublimating device for depositing a semiconductor film, which is characterized by comprising a fluidization part, a first liquid crystal display part and a second liquid crystal display part, wherein the fluidization part is provided with at least one fluidization barrel for containing materials to be sublimated and is used for enabling the materials to be sublimated to be in a fluidization state, and the fluidization barrel is provided with an inlet and an outlet;
an air inlet part arranged at the inlet of the fluidization part and used for introducing air into the fluidization barrel,
A light component deposition part communicated with the fluidization part, and
A collecting part comprising a collecting barrel for collecting target materials, wherein the collecting barrel is communicated with the fluidization part through a connecting pipe with at least one valve, a vacuum pipe for communicating with an external vacuum source is arranged inside the collecting barrel,
Wherein the light component deposition part comprises:
a light component deposition tube;
A feeding pipe arranged at one end of the light component deposition pipe and communicated with the light component deposition pipe for introducing cleaning liquid or carrier gas into the light component deposition pipe, and
The discharging pipe is arranged on the light component deposition pipe and is far away from one end of the feeding pipe, and is communicated with the light component deposition pipe and used for discharging cleaning liquid or carrier gas.
In the precursor sublimating device for depositing a semiconductor thin film provided by the invention, the gas inlet part may further comprise:
The main air inlet pipe is arranged at the inlet of the fluidization barrel, is detachably connected with the fluidization barrel and is internally communicated with the fluidization barrel;
one end of the first branch pipe is communicated with the main air inlet pipe, the other end of the first branch pipe is connected with an air source, and the first branch pipe is provided with an air inlet part first valve and an air inlet part second valve;
One end of the second branch pipe is communicated with the main air inlet pipe, the other end of the second branch pipe is connected with a vacuum source, and the second branch pipe is provided with a third valve of an air inlet part;
The flow controller is arranged on the first branch pipe and is positioned between the first valve of the air inlet part and the second valve of the air inlet part and used for controlling the air inlet flow;
And the air inlet part heating sleeve is sleeved outside the first branch pipe, the second branch pipe and the main air inlet pipe and is used for controlling the temperatures inside the first branch pipe, the second branch pipe and the main air inlet pipe.
In the precursor sublimating apparatus for depositing a semiconductor thin film provided by the present invention, the fluidization portion may further include:
a fluidization barrel;
The fluidization part first valve is arranged at the inlet of the fluidization barrel;
the lower sieve plate is arranged in the fluidization barrel and is positioned above the first valve of the fluidization part;
an upper sieve plate arranged inside the fluidization barrel and above the lower sieve plate;
The fluidization part second valve is arranged at the fluidization barrel and is positioned above the upper sieve plate;
The air outlet pipe is arranged at the outlet of the fluidization barrel, one end of the air outlet pipe is detachably connected with the fluidization barrel and is internally communicated with the fluidization barrel, and the other end of the air outlet pipe is communicated with the light component deposition pipe;
the third valve of the fluidization part is arranged on the air outlet pipe;
The air outlet pipe heating sleeve is sleeved on the outer side of the air outlet pipe and used for controlling the temperature inside the air outlet pipe;
and the fluidization part temperature control piece is used for controlling the temperature inside the fluidization barrel.
In the precursor sublimation apparatus for depositing a semiconductor thin film according to the present invention, the collecting section may further include:
A collecting part temperature control part for controlling the temperature inside the collecting barrel,
The light component deposition portion further includes:
And the temperature control part of the light component deposition part is used for controlling the temperature inside the light component deposition tube.
The precursor sublimating device for depositing the semiconductor film can be characterized in that the top of the collecting barrel is provided with an opening for the connecting pipe to pass through, and the vacuum pipe is provided with a vacuum pipe valve.
In the precursor sublimating apparatus for depositing a semiconductor thin film provided by the present invention, it may be further characterized in that the vacuum pipe extends upward at a portion inside the collecting vessel and opens upward.
The precursor sublimating device for depositing the semiconductor film can be characterized in that the light component depositing pipe is a coil pipe.
The precursor sublimating device for depositing the semiconductor thin film can be characterized in that the material to be sublimated is selected from any one of lithium tert-butoxide, sodium tert-butoxide, aluminum trichloride, antimony trichloride, gallium trichloride, carbon tetrabromide, molybdenum hexacarbonyl, tungsten hexacarbonyl, zirconium tetra (dimethylamino), hafnium tetrachloride, zirconium tetrachloride, molybdenum dichloride dioxide, molybdenum pentachloride, tungsten pentachloride, ferrocene or magnesium dicyclopentadiene.
The invention provides a precursor sublimating device for depositing a semiconductor film, which has the characteristics that the sublimating device is utilized to sublimate, and the device comprises the following steps:
a. Filling the material to be sublimated into a fluidization barrel;
b. introducing carrier gas into the fluidization barrel through the air inlet part so as to enable the material to be sublimated to be in a fluidization state;
c. At least one valve of the connecting pipe is in a closed state, so that light component impurities in the material to be sublimated are deposited in the light component deposition pipe;
d. Introducing a cleaning solvent into the light component deposition tube through the feed tube and discharging the cleaning solvent from the discharge tube, so as to remove light component impurities deposited in the light component deposition tube;
e. the valves on the connecting pipes are in an open state, the valves on the vacuum pipes are in an open state, and the inside of the collecting barrel is in a negative pressure state, so that the material to be sublimated enters the inside of the collecting barrel.
The precursor sublimation method for depositing the semiconductor thin film provided by the invention can be characterized in that when the material to be sublimated is a material sensitive to water and/or air, the sublimation is performed by using the sublimation device, and the method further comprises the following steps:
f. Inert gas is introduced into the main air inlet pipe through the first branch pipe and is discharged from the second branch pipe;
g. inert gas is introduced into the light component deposition tube through the feed tube and discharged from the discharge tube.
According to the precursor sublimation device for depositing the semiconductor thin film and the corresponding precursor sublimation method for depositing the semiconductor thin film, the sublimation device provided by the invention has the light component deposition part, so that the light component impurities in the material to be sublimated can be firstly deposited in the light component deposition tube to be separated, and then the target material is collected, thereby effectively improving the sublimation efficiency.
Drawings
FIG. 1 is a precursor sublimating apparatus for depositing a semiconductor thin film in example 1 of the present invention;
FIG. 2 is a graph showing the pressure difference of the fluidization bucket after adding aluminum trichloride in example 2 of the present invention at different flow rates.
Detailed Description
In order to make the technical means, the creation features, the achievement of the purpose and the effect of the present invention easy to understand, the present invention is specifically described below with reference to the embodiments and the drawings.
Example 1A precursor sublimating device for depositing a semiconductor thin film;
The embodiment provides a precursor sublimating device for depositing a semiconductor film, and as shown in fig. 1, the sublimating device provided by the embodiment comprises an air inlet part, a fluidization part, a light component depositing part and a collecting part.
The intake section includes a main intake pipe 105, a first branch pipe 108, a second branch pipe 109, a flow controller 104, and an intake section heating jacket (not shown).
One end of the main air inlet pipe 105 is connected with the inlet end of the fluidization barrel 205 of the fluidization part through a first flange interface 106, and the other end is a closed end.
One end of the first branch pipe 108 is communicated with the main air inlet pipe 105, and the other end is communicated with an air source, so that air is introduced into the main air inlet pipe 105. The first branch pipe 108 is provided with an intake first valve 101 and an intake second valve 102.
One end of the second branch pipe 109 is provided to communicate with the main intake pipe 105, and the other end is provided to be connected to a vacuum source, thereby providing negative pressure to the inside of the main intake pipe 105. The second branch pipe 109 is provided with an intake portion third valve 103.
The flow controller 104 is mounted on the first branch pipe 108 and is located between the intake first valve 101 and the intake second valve 102. The flow controller 104 is used to control and detect the flow rate of the gas entering the first manifold 108 and the main inlet pipe 104.
The air inlet portion heating jacket is sleeved on the outer surfaces of the main air inlet pipe 105, the first branch pipe 108 and the second branch pipe 109, and is used for heating the main air inlet pipe 105, the first branch pipe 108 and the second branch pipe 109.
The fluidization portion includes a fluidization bucket 205, a fluidization portion first valve 201, a lower screen 203, an upper screen 204, a lower pressure gauge 209, an upper pressure gauge 210, a fluidization portion second valve 202, an air outlet pipe 208, an air outlet pipe heating jacket (not shown), an air outlet pipe valve 211, and a fluidization portion temperature control member 206.
The fluidization barrel 205 has an inlet port connected to the main inlet pipe 105 via the first flange interface 106 and an outlet port connected to the outlet pipe 208 via the second flange interface 207. The fluidization bucket 205 is vertically disposed in use.
The fluidization portion first valve 201 is disposed at the inlet end of the fluidization barrel 205, and when the fluidization portion first valve 201 is in a closed state, the gas in the main gas inlet pipe 105 cannot enter the fluidization barrel 205, and vice versa.
The lower screen plate 203 is disposed inside the fluidization bucket 205 and above the fluidization portion first valve 201. The lower sieve plate 203 is preferably a sieve plate with a smaller mesh number than the mesh number of the material to be sublimated, so that the material to be sublimated in a solid state can be prevented from leaving the fluidization barrel.
The lower pressure gauge 209 is used to detect the air pressure of the inner space of the fluidization bucket 205 between the fluidization portion first valve 201 and the lower sieve plate 203.
An upper screen plate 204 is disposed inside the fluidization bucket 205 and above the lower screen plate 203. A space for accommodating the material to be sublimated is formed between the upper screen 204 and the lower screen 203. The upper screen 204 is preferably a screen with a smaller mesh than the material to be sublimated, so that the material to be sublimated in the solid state can be prevented from leaving the fluidization barrel.
The fluidization portion second valve 202 is disposed at the outlet end of the fluidization bucket 205 above the upper screen plate 204. When the second valve 202 of the fluidization portion is in the closed state, the gas in the fluidization bucket 205 cannot enter the gas outlet pipe 208, and vice versa.
The upper pressure gauge 210 is used to detect the air pressure of the inner space of the fluidization bucket 205 between the fluidization portion second valve 202 and the upper sieve plate 204.
The fluidization portion temperature control member 206, which is an air convection heating chamber in the present embodiment, is provided outside the fluidization barrel 205 for heating an inner space of the fluidization barrel 205 (particularly, an inner space between the upper screen plate 204 and the lower screen plate 203).
The air outlet pipe 208 is connected with the outlet end of the fluidization barrel 205 through a second flange interface 207.
The outlet pipe heating jacket is sleeved outside the outlet pipe 208 and is used for heating the outlet pipe 208.
An outlet valve 211 is provided on the outlet pipe 208 for controlling the opening and closing between the outlet pipe 208 and the light component deposition pipe 303.
The light fraction deposition section includes a light fraction deposition pipe 303, a feed pipe 308, a feed pipe valve 301, a discharge pipe 306, a discharge pipe valve 302, a connection pipe 307, a connection pipe valve 305, and a light fraction deposition section temperature control member 304.
One end of the light component deposition tube 303 is communicated with the gas outlet tube 208, and the other end is communicated with the connecting tube 307. In this embodiment, the light fraction deposition tube 303 is a coil.
A feed pipe 308 is provided at a side of the light component deposition pipe 303 close to the gas outlet pipe 208 for feeding a solvent or carrier gas into the light component deposition pipe 303.
A feed pipe valve 301 is mounted on the feed pipe 308 for controlling the opening and closing between the feed pipe 308 and the light fraction deposition pipe 303.
A discharge tube 306 is provided on the side of the light fraction deposition tube 303 adjacent to the connection tube 307 for discharging the solvent or carrier gas, and in some embodiments may be connected to a vacuum source to provide negative pressure into the light fraction deposition tube to further increase the efficiency of discharging the solvent or carrier gas.
A spout valve 302 is mounted on the spout 306 for controlling the opening and closing between the spout 306 and the light fraction deposition tube 303.
One end of the connecting pipe 307 is communicated with the discharging pipe 306, and the other end extends into the collecting bucket 402.
A connection pipe valve 305 is installed on the connection pipe 307 for controlling the opening and closing between the connection pipe 307 and the collection tub 402.
The light component deposition portion temperature control member 304 is sleeved outside the light component deposition tube 303, and in this embodiment, the light component deposition portion temperature control member is an air convection temperature control cavity and is used for controlling the internal temperature of the light component deposition tube 303.
The collection part comprises a collection barrel 402, a vacuum tube 404, a vacuum valve 401 and a collection part temperature control member 403.
The top of the collecting vessel 402 has an opening for the connection pipe 307 to pass through, the opening being sized to fit the size of the connection pipe 307. The bottom of the collection vessel 402 has an opening through which the vacuum tube 404 passes, the opening being sized to accommodate the vacuum tube 404.
Vacuum tube 404 is located at one end outside of collection tub 402 and is adapted to be connected to a vacuum source, and at the other end inside collection tub 402. The portion of vacuum tube 404 located inside collection tub 402 extends upward. The end of vacuum tube 404 that is located inside collection tub 402 is open upward.
The collector temperature control member 403 is used to control the temperature inside the collector 402, and in this embodiment, the collector temperature control member is an air convection temperature control chamber.
Example 2A sublimation method of a precursor for semiconductor thin film deposition for purifying aluminum trichloride, the sublimation method provided in this example was performed using the sublimation apparatus of a precursor for semiconductor thin film deposition described in example 1.
The sublimation method provided by the embodiment comprises the following steps:
Step 1, the fluidization bucket 205 is removed through a flange interface and the fluidization bucket 205 is moved into a glove box. In the glove box, the lower sieve plate 203 (mesh number 8000) was confirmed to be cleaned and mounted, and the fluidization portion second valve 202 was opened to confirm that the upper sieve plate 204 was taken out. At this time, 1.2kg of aluminum trichloride was charged into the fluidization bucket 205, and the upper screen plate 204 (mesh number 8000) was charged. The fluidization portion first valve 201 and the fluidization portion second valve 202 are closed, and the fluidization barrel 205 is removed from the glove box and installed as in the version of fig. 1.
Step2, opening the air inlet first valve 101 and the air inlet second valve 102, introducing a small amount of carrier gas from the first branch pipe 108, then closing the air inlet second valve 102, opening the air inlet third valve 103, and repeating the operation six times. The outlet valve 211 and the feed pipe valve 301 are opened, a small amount of carrier gas is fed through the feed pipe 308, then the feed pipe valve 301 is closed, the discharge pipe valve 302 is opened, and the operation is repeated six times.
Step 3, open the first valve 101 of the air inlet, the second valve 102 of the air inlet, the first valve 201 of the fluidization part, the second valve 202 of the fluidization part, the valve 211 of the air outlet pipe and the valve 302 of the discharging pipe. The vacuum is turned on and a steady amount of inert gas carrier gas is fed through the flow controller 104. The inert gas carrier gas flow gradually increased from 1slm to 55slm, and the readings of the upper pressure gauge 210 and the lower pressure gauge 209 obtained by measurement are shown in table 1 (the pressure unit is Pa), wherein Δ2=p 210-B-P209-B,Δ1=P210-A-P209-A,Δ=Δ2-Δ1,P210-B is the reading of the upper pressure gauge 210 after adding aluminum trichloride, P 209-B is the reading of the lower pressure gauge 209 after adding aluminum trichloride, P 210-A is the reading of the upper pressure gauge 210 in the empty fluidization bucket, and P 209-A is the reading of the lower pressure gauge 209 in the empty fluidization bucket (the pressure in the empty fluidization bucket can be measured in advance).
TABLE 1
As shown in table 1 and fig. 2, when the flow rate exceeds 30slm, the value of Δ tends to be constant as the flow rate continues to increase, and thus it is determined that at a flow rate of 35slm, aluminum trichloride reaches a fluidized state in the fluidization bucket, and thus the flow rate is maintained at 35 slm.
And 4, maintaining the flow rate of the carrier gas introduced in the step 3. The temperature control of the inlet heating mantle was turned on and set at 50 ℃, the temperature control of the fluidization portion temperature control member 206 was turned on and set at 80 ℃, the temperature control of the outlet heating mantle was turned on and set at 40 ℃, the temperature control of the light component deposition portion temperature control member 304 was turned on and set at 30 ℃, and the temperature was maintained for 1.5 hours.
Step 5, stopping the supply of carrier gas through the first branch pipe 108 and closing the outlet pipe valve 211. And opening a feed pipe valve 301 and a discharge pipe valve 302 (the rear end of the discharge pipe valve 302 is vacuum-closed), introducing light component impurities in the tetrahydrofuran dissolution coil pipe, discharging, introducing carrier gas from the feed pipe valve 301, opening the rear end of the discharge pipe valve 302, vacuum-opening the rear end of the discharge pipe valve 302, ensuring that residual ethanol is purged, and closing the feed pipe valve 301 and the discharge pipe valve 302.
And 6, opening the air outlet pipe valve 211, connecting the pipe valve 305 and the vacuum valve 401, opening the carrier gas, maintaining the flow in the step 3, simultaneously opening the vacuum at the rear end of the vacuum valve 401, opening the temperature control part 403 of the collecting part, controlling the temperature to 20 ℃ and maintaining the temperature for 8 hours, and collecting 0.8kg of high-purity aluminum trichloride in the collecting barrel 402. The purity of the aluminum trichloride was improved from 99.9% to greater than 99.9995% as determined by ICP-MS.
Example 3A sublimation method of a precursor for semiconductor thin film deposition for purifying hafnium tetrachloride, the sublimation method provided in this example was performed using the sublimation apparatus of a precursor for semiconductor thin film deposition described in example 1.
The sublimation method provided by the embodiment comprises the following steps:
step 1, the fluidization bucket 205 is removed through a flange interface and the fluidization bucket 205 is moved into a glove box. In the glove box, the lower sieve plate 203 (mesh number 8000) was confirmed to be cleaned and mounted, and the fluidization portion second valve 202 was opened to confirm that the upper sieve plate 204 was taken out. At this time, 1.4kg of hafnium tetrachloride was charged into the fluidization bucket 205, and the upper sieve plate 204 (mesh number 8000) was charged. The fluidization portion first valve 201 and the fluidization portion second valve 202 are closed, and the fluidization barrel 205 is removed from the glove box and installed as in the version of fig. 1.
Step2, opening the air inlet first valve 101 and the air inlet second valve 102, introducing a small amount of carrier gas from the first branch pipe 108, then closing the air inlet second valve 102, opening the air inlet third valve 103, and repeating the operation ten times. The outlet valve 211 and the feed pipe valve 301 were opened, a small amount of carrier gas was introduced through the feed pipe 308, then the feed pipe valve 301 was closed, and the discharge pipe valve 302 was opened, and the operation was repeated ten times.
Step 3, open the first valve 101 of the air inlet, the second valve 102 of the air inlet, the first valve 201 of the fluidization part, the second valve 202 of the fluidization part, the valve 211 of the air outlet pipe and the valve 302 of the discharging pipe. The vacuum is turned on and a steady amount of inert gas carrier gas is fed through the flow controller 104. The inert gas carrier gas flow was gradually increased from 1slm to 55slm, and the readings of the upper pressure gauge 210 and the lower pressure gauge 209 were measured to determine the fluidization flow rate to be 40slm by referring to the method in example 2.
And 4, maintaining the flow rate of the carrier gas introduced in the step 3. The temperature control of the inlet heating mantle was turned on and set at 120 ℃, the temperature control of the fluidization portion temperature control member 206 was turned on and set at 195 ℃, the temperature control of the outlet heating mantle was turned on and set at 30 ℃, the temperature control of the light component deposition portion temperature control member 304 was turned on and set at 10 ℃, and held for 2 hours.
Step 5, stopping the supply of carrier gas through the first branch pipe 108 and closing the outlet pipe valve 211. And opening a feed pipe valve 301 and a discharge pipe valve 302 (the rear end of the discharge pipe valve 302 is vacuum-closed), introducing light component impurities in the acetone dissolution coil pipe, discharging, introducing carrier gas from the feed pipe valve 301, opening the rear end of the discharge pipe valve 302, vacuum-opening the rear end of the discharge pipe valve 302, ensuring that residual ethanol is purged, and closing the feed pipe valve 301 and the discharge pipe valve 302.
And 6, opening the air outlet pipe valve 211, connecting the pipe valve 305 and the vacuum valve 401, opening the carrier gas, maintaining the flow in the step 3, simultaneously opening the vacuum at the rear end of the vacuum valve 401, opening the temperature control part 403 of the collecting part, controlling the temperature to 10 ℃ and maintaining the temperature for 10 hours, and collecting 0.7kg of high-purity hafnium tetrachloride in the collecting barrel 402. The purity of hafnium tetrachloride was improved from 99.9% to greater than 99.999% as determined by ICP-MS.
Example 4A sublimation method of a precursor for semiconductor thin film deposition for purifying magnesium dicyclopentadiene, the sublimation method provided in this example was performed using the sublimation apparatus of a precursor for semiconductor thin film deposition described in example 1.
The sublimation method provided by the embodiment comprises the following steps:
Step 1, the fluidization bucket 205 is removed through a flange interface and the fluidization bucket 205 is moved into a glove box. In the glove box, the lower sieve plate 203 (mesh number 8000) was confirmed to be cleaned and mounted, and the fluidization portion second valve 202 was opened to confirm that the upper sieve plate 204 was taken out. At this time, 3.6kg of magnesium dichloride was charged into the fluidization bucket 205 and charged into the upper screen plate 204 (mesh number 8000). The fluidization portion first valve 201 and the fluidization portion second valve 202 are closed, and the fluidization barrel 205 is removed from the glove box and installed as in the version of fig. 1.
Step 2, opening the air inlet first valve 101 and the air inlet second valve 102, introducing a small amount of carrier gas from the first branch pipe 108, then closing the air inlet second valve 102, opening the air inlet third valve 103, and repeating the operation twelve times. The outlet valve 211 and the feed pipe valve 301 are opened, a small amount of carrier gas is fed through the feed pipe 308, then the feed pipe valve 301 is closed, and the discharge pipe valve 302 is opened, and the operation is repeated twelve times.
Step 3, open the first valve 101 of the air inlet, the second valve 102 of the air inlet, the first valve 201 of the fluidization part, the second valve 202 of the fluidization part, the valve 211 of the air outlet pipe and the valve 302 of the discharging pipe. The vacuum is turned on and a steady amount of inert gas carrier gas is fed through the flow controller 104. The inert gas carrier gas flow was gradually increased from 1slm to 80slm, and the readings of the upper pressure gauge 210 and the lower pressure gauge 209 were measured to determine the fluidization flow rate to be 65slm by referring to the method in example 2.
And 4, maintaining the flow rate of the carrier gas introduced in the step 3. The temperature control of the inlet heating mantle was turned on and set at 50 ℃, the temperature control of the fluidization portion temperature control member 206 was turned on and set at 70 ℃, the temperature control of the outlet heating mantle was turned on and set at 30 ℃, the temperature control of the light component deposition portion temperature control member 304 was turned on and set at 20 ℃, and the temperature was maintained for 4 hours.
Step 5, stopping the supply of carrier gas through the first branch pipe 108 and closing the outlet pipe valve 211. And opening a feed pipe valve 301 and a discharge pipe valve 302 (the rear end of the discharge pipe valve 302 is vacuum-closed), introducing light component impurities in the acetone dissolution coil pipe, discharging, introducing carrier gas from the feed pipe valve 301, opening the rear end of the discharge pipe valve 302, vacuum-opening the rear end of the discharge pipe valve 302, ensuring that residual ethanol is purged, and closing the feed pipe valve 301 and the discharge pipe valve 302.
And 6, opening the air outlet pipe valve 211, connecting the pipe valve 305 and the vacuum valve 401, opening the carrier gas, maintaining the flow in the step 3, simultaneously opening the vacuum at the rear end of the vacuum valve 401, opening the temperature control part 403 of the collecting part, controlling the temperature to 20 ℃ and maintaining for 12 hours, and collecting 2.1g of high-purity magnesium dichloride in the collecting barrel 402. The purity of the magnesium dicyclopentadiene is improved from 99.5% to more than 99.99% as shown by the test result of ICP-MS.
According to the precursor sublimation device for depositing the semiconductor thin film and the corresponding precursor sublimation method for depositing the semiconductor thin film, which are related to the embodiments, the sublimation device provided by the invention has the light component deposition part, so that the light component impurities in the material to be sublimated can be firstly deposited in the light component deposition tube to be separated, and then the target material is collected, thereby effectively improving the sublimation efficiency, and improving the purity of the material to be sublimated to more than 99.99%.
Further, since the sublimation device is also provided with the air inlet part, inert gas can be introduced into the fluidization barrel, and the sublimation device can be suitable for sublimating materials sensitive to air and/or water.
Further, as the light component deposition tube is a coil, the light component can be more fully deposited, which is beneficial to further improving the purity of the target material.
Further, since the vacuum tube is upwardly extended and upwardly opened at a portion of the inside of the collecting vessel, it is possible to prevent the target material introduced into the inside of the collecting vessel from being sucked away to cause loss.
The above embodiments are preferred examples of the present invention, and are not intended to limit the scope of the present invention.
Claims (10)
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| CN102924207A (en) * | 2011-08-13 | 2013-02-13 | 广东阿格蕾雅光电材料有限公司 | Organic micromolecule sublimation purifying method |
| CN107452651A (en) * | 2016-05-20 | 2017-12-08 | 朗姆研究公司 | For solid and the steam carrying method and device of Liquid precursor |
| CN109289230A (en) * | 2018-08-08 | 2019-02-01 | 浙江工业大学 | A closed-circuit circulation-inert particle fluidized bed continuous sublimation sublimation separation and purification device and purification process |
| CN114712886A (en) * | 2022-03-29 | 2022-07-08 | 安徽贝意克设备技术有限公司 | A kind of organic metal compound purification equipment |
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| US10100406B2 (en) * | 2015-04-17 | 2018-10-16 | Versum Materials Us, Llc | High purity tungsten hexachloride and method for making same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102924207A (en) * | 2011-08-13 | 2013-02-13 | 广东阿格蕾雅光电材料有限公司 | Organic micromolecule sublimation purifying method |
| CN107452651A (en) * | 2016-05-20 | 2017-12-08 | 朗姆研究公司 | For solid and the steam carrying method and device of Liquid precursor |
| CN109289230A (en) * | 2018-08-08 | 2019-02-01 | 浙江工业大学 | A closed-circuit circulation-inert particle fluidized bed continuous sublimation sublimation separation and purification device and purification process |
| CN114712886A (en) * | 2022-03-29 | 2022-07-08 | 安徽贝意克设备技术有限公司 | A kind of organic metal compound purification equipment |
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