A precursor sublimation device and method for semiconductor thin film deposition

Abstract

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

[0001] The present invention relates to the field of material separation devices, and in particular to a precursor sublimation device and method for semiconductor thin film deposition. Background Art

[0002] The sublimation process refers to the process in which solid substances directly form gases without passing through the liquid state. The sublimation process can separate mixtures of different volatilities, or separate substances that cannot sublime from substances that can sublime. Therefore, solid sublimation is a common means of purification in chemical processes. Sublimators use the principle of sublimation and are widely used to improve the purity of solid substances.

[0003] Precursors used for semiconductor thin film deposition usually have extremely high purity requirements. In the prior art, sublimation is usually used to purify them, but it is difficult to purify them to the ideal purity using ordinary sublimators.

[0004] Ordinary sublimators add solid substances directly into containers. During the addition process, the solid substances will come into contact with the air environment. For some solid substances that are easily reactive with water and oxygen in the air, there will be potential dangers of solid substance deterioration or safety issues. As the heating sublimation proceeds, substances with different volatilities gradually separate. During the sublimation process, when the mass of the solid substance is large, there will be uneven heat transfer. The difference in heat will cause impurities and products to sublimate at the same time, so it is difficult to improve the sublimation efficiency. At the same time, unsublimated solid substances and impurities are extremely easy to harden in the container, delaying the sublimation process. Easily separable impurities will first be deposited in the collection device. Therefore, in order to avoid contact with the product, it is necessary to use multiple collection tanks or remove the easily separable impurities before subsequent collection, which increases equipment investment and sublimation steps. Summary of the invention

[0005] The present invention is made to solve the above-mentioned problems, and its purpose is to provide a semiconductor thin film deposition precursor sublimation device with high sublimation efficiency and requiring only one collecting tank, and a semiconductor thin film deposition precursor sublimation method using the sublimation device.

[0006] The present invention provides a precursor sublimation device for semiconductor thin film deposition, which has the following characteristics: a fluidizing part, which has at least one fluidizing barrel for containing a material to be sublimated, and is used to put the material to be sublimated in a fluidized state, and the fluidizing barrel has an inlet and an outlet;

[0007] The air inlet is arranged at the inlet of the fluidizing part and is used to introduce gas into the fluidizing barrel.

[0008] a light component settling section, which is in communication with the fluidizing section; and

[0009] The collecting part includes a collecting barrel for collecting target materials, 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.

[0010] Wherein, the light component deposition part comprises:

[0011] Light component deposition tube;

[0012] a feed pipe, disposed at one end of the light component deposition pipe, connected to the light component deposition pipe, and used for introducing a cleaning liquid or a carrier gas into the light component deposition pipe; and

[0013] A discharge pipe is arranged on the light component deposition pipe and away from one end of the feed pipe, is communicated with the light component deposition pipe, and is used for discharging cleaning liquid or carrier gas.

[0014] In the semiconductor thin film deposition precursor sublimation device provided by the present invention, it can also have the following characteristics: wherein the air inlet portion includes:

[0015] A main air inlet pipe is arranged at the inlet of the fluidizing barrel, and is detachably connected to the fluidizing barrel and communicated with the inside thereof;

[0016] A first branch pipe, one end of which is connected to the main air intake pipe and the other end of which is used to be connected to the air source, wherein the first branch pipe is provided with a first air intake valve and a second air intake valve;

[0017] A second branch pipe, one end of which is connected to the main air intake pipe and the other end of which is used to be connected to a vacuum source, and the second branch pipe is provided with a third air intake valve;

[0018] A flow controller, installed on the first branch pipe and located between the first valve of the air intake part and the second valve of the air intake part, for controlling the air intake flow;

[0019] The air intake heating jacket is arranged outside the first branch pipe, the second branch pipe and the main air intake pipe, and is used to control the temperature inside the first branch pipe, the second branch pipe and the main air intake pipe.

[0020] In the semiconductor thin film deposition precursor sublimation device provided by the present invention, it can also have the following characteristics: the fluidization part includes:

[0021] Fluidizing barrel;

[0022] A first valve of the fluidizing part, arranged at the inlet of the fluidizing barrel;

[0023] A lower sieve plate, arranged inside the fluidizing barrel and located above the first valve of the fluidizing part;

[0024] An upper sieve plate, arranged inside the fluidizing barrel and above the lower sieve plate;

[0025] A second valve of the fluidizing part is arranged at the fluidizing barrel and located above the upper sieve plate;

[0026] An air outlet pipe is arranged at the outlet of the fluidizing barrel, one end of which is detachably connected to the fluidizing barrel and communicated with the inside, and the other end of which is communicated with the light component deposition pipe;

[0027] A third valve of the fluidizing part is arranged on the gas outlet pipe;

[0028] An outlet pipe heating sleeve, which is arranged outside the outlet pipe and is used to control the temperature inside the outlet pipe;

[0029] The fluidizing section temperature control unit is used to control the temperature inside the fluidizing barrel.

[0030] In the semiconductor thin film deposition precursor sublimation device provided by the present invention, it can also have the following characteristics: the collecting part also includes:

[0031] The collection part temperature control unit is used to control the temperature inside the collection bucket.

[0032] The light component deposition section further comprises:

[0033] The light component deposition section temperature control unit is used to control the temperature inside the light component deposition tube.

[0034] The precursor sublimation device for semiconductor thin film deposition provided by the present invention may also have the following features: the top of the collecting bucket has an opening for the connecting tube to pass through, and the vacuum tube has a vacuum tube valve.

[0035] The precursor sublimation device for semiconductor thin film deposition provided by the present invention may also have the following feature: the portion of the vacuum tube inside the collecting bucket extends upward and opens upward.

[0036] The precursor sublimation device for semiconductor thin film deposition provided by the present invention may also have the following feature: the light component deposition tube is a coil.

[0037] In the precursor sublimation device for semiconductor thin film deposition provided by the present invention, it can also have the following characteristics: 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, tetrakis(dimethylamino)zirconium, hafnium tetrachloride, zirconium tetrachloride, molybdenum dioxide dichloride, molybdenum pentachloride, tungsten pentachloride, ferrocene or magnesiumocene.

[0038] The present invention provides a precursor sublimation device for semiconductor thin film deposition, which has the following characteristics: using any of the above sublimation devices to perform sublimation, comprising the following steps:

[0039] a. Fill the material to be sublimated into the fluidized barrel;

[0040] b. introducing a carrier gas into the fluidizing barrel through the air inlet so that the material to be sublimated is in a fluidized state;

[0041] c. At least one valve of the connecting pipe is in a closed state, so that the light component impurities in the material to be sublimated are deposited in the light component deposition tube;

[0042] d. introducing a cleaning solvent into the light component deposition tube through the feed pipe and discharging it from the discharge pipe, thereby removing light component impurities deposited in the light component deposition tube;

[0043] e. Make sure that all valves on the connecting pipes are in an open state, make sure that the valve on the vacuum tube is in an open state, and make the inside of the collection barrel in a negative pressure state, so that the material to be sublimated can enter the inside of the collection barrel.

[0044] The semiconductor thin film deposition precursor sublimation method provided by the present invention may also have the following characteristics: when the material to be sublimated is a substance sensitive to water and / or air, the sublimation is performed using the above-mentioned sublimation device, and further comprises the following steps:

[0045] f. Introduce inert gas into the main air intake pipe through the first branch pipe and discharge it from the second branch pipe;

[0046] g. Introduce inert gas into the light component deposition tube through the feed pipe and discharge it from the discharge pipe.

[0047] According to the semiconductor thin film deposition precursor sublimation device and the corresponding semiconductor thin film deposition precursor sublimation method involved in the present invention, because it has a light component deposition part, the sublimation device provided by the present invention can first deposit the light component impurities in the material to be sublimated in the light component deposition tube for separation, and then collect the target material, thereby effectively improving the sublimation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0048] Figure 1 It is the precursor sublimation device for semiconductor thin film deposition in embodiment 1 of the present invention;

[0049] Figure 2 It is a pressure difference diagram of the fluidized barrel at different flow rates after adding aluminum chloride in Example 2 of the present invention. DETAILED DESCRIPTION

[0050] In order to make the technical means, creative features, objectives and effects achieved by the present invention easier to understand, the present invention is described in detail below in conjunction with embodiments and drawings.

[0051] Embodiment 1: A precursor sublimation device for semiconductor thin film deposition;

[0052] This embodiment provides a precursor sublimation device for semiconductor thin film deposition, such as Figure 1 As shown, the sublimation device provided in this embodiment includes: an air inlet part, a fluidizing part, a light component deposition part and a collection part.

[0053] The air intake section includes: a main air intake pipe 105, a first branch pipe 108, a second branch pipe 109, a flow controller 104, and an air intake heating jacket (not shown in the figure).

[0054] One end of the main air inlet pipe 105 is connected to the inlet end of the fluidizing barrel 205 of the fluidizing part through the first flange interface 106, and the other end is a closed end.

[0055] One end of the first branch pipe 108 is connected to the main air intake pipe 105, and the other end is used to communicate with the gas source, so as to introduce gas into the main air intake pipe 105. The first branch pipe 108 is provided with a first air intake valve 101 and a second air intake valve 102.

[0056] One end of the second branch pipe 109 is connected to the main air intake pipe 105, and the other end is connected to a vacuum source to provide negative pressure to the inside of the main air intake pipe 105. The second branch pipe 109 is provided with a third air intake valve 103.

[0057] The flow controller 104 is installed on the first branch pipe 108 and is located between the first intake valve 101 and the second intake valve 102. The flow controller 104 is used to control and detect the flow rate of the gas entering the first branch pipe 108 and the main intake pipe 104.

[0058] The air intake heating sleeve is disposed on the outer surfaces of the main air intake pipe 105 , the first branch pipe 108 and the second branch pipe 109 , and is used to heat the main air intake pipe 105 , the first branch pipe 108 and the second branch pipe 109 .

[0059] The fluidizing section includes: a fluidizing barrel 205, a first valve 201 of the fluidizing section, a lower sieve plate 203, an upper sieve plate 204, a lower pressure gauge 209, an upper pressure gauge 210, a second valve 202 of the fluidizing section, an air outlet pipe 208, an air outlet pipe heating jacket (not shown in the figure), an air outlet pipe valve 211 and a fluidizing section temperature control unit 206.

[0060] The fluidizing barrel 205 has an inlet and an outlet, wherein the inlet end is connected to the main air inlet pipe 105 through the first flange interface 106, and the outlet end is connected to the air outlet pipe 208 through the second flange interface 207. The fluidizing barrel 205 is arranged vertically when in use.

[0061] The first valve 201 of the fluidizing part is disposed at the inlet end of the fluidizing barrel 205. When the first valve 201 of the fluidizing part is in a closed state, the gas in the main air inlet pipe 105 cannot enter the fluidizing barrel 205, and vice versa.

[0062] The lower sieve plate 203 is arranged inside the fluidizing barrel 205 and above the first valve 201 of the fluidizing part. The lower sieve plate 203 preferably uses a sieve plate with a mesh number smaller than that of the material to be sublimated, so as to prevent the solid material to be sublimated from leaving the fluidizing barrel.

[0063] The lower pressure gauge 209 is used to detect the air pressure in the internal space of the fluidizing barrel 205 between the first valve 201 of the fluidizing section and the lower sieve plate 203 .

[0064] The upper sieve plate 204 is disposed inside the fluidizing barrel 205 and above the lower sieve plate 203. A space for accommodating the material to be sublimated is formed between the upper sieve plate 204 and the lower sieve plate 203. The upper sieve plate 204 preferably uses a sieve plate with a mesh number smaller than the mesh number of the material to be sublimated, so as to prevent the solid material to be sublimated from leaving the fluidizing barrel.

[0065] The second valve 202 of the fluidizing part is arranged at the outlet end of the fluidizing barrel 205 and is located above the upper sieve plate 204. When the second valve 202 of the fluidizing part is in a closed state, the gas in the fluidizing barrel 205 cannot enter the gas outlet pipe 208, and vice versa.

[0066] The upper pressure gauge 210 is used to detect the air pressure in the internal space of the fluidizing barrel 205 between the second valve 202 of the fluidizing section and the upper sieve plate 204 .

[0067] In this embodiment, the fluidizing section temperature control unit 206 is an air convection heating chamber, which is arranged outside the fluidizing barrel 205 and is used to heat the internal space of the fluidizing barrel 205 (especially the internal space between the upper sieve plate 204 and the lower sieve plate 203).

[0068] The air outlet pipe 208 is connected to the outlet end of the fluidizing barrel 205 through the second flange interface 207 .

[0069] The outlet pipe heating sleeve is disposed outside the outlet pipe 208 to heat the outlet pipe 208 .

[0070] The gas outlet pipe valve 211 is disposed on the gas outlet pipe 208 and is used to control the opening and closing between the gas outlet pipe 208 and the light component deposition pipe 303 .

[0071] The light component deposition section includes: a light component deposition pipe 303 , a feed pipe 308 , a feed pipe valve 301 , a discharge pipe 306 , a discharge pipe valve 302 , a connecting pipe 307 , a connecting pipe valve 305 and a light component deposition section temperature control unit 304 .

[0072] One end of the light component deposition tube 303 is connected to the gas outlet pipe 208, and the other end is connected to the connecting pipe 307. In this embodiment, the light component deposition tube 303 is a coil.

[0073] The feed pipe 308 is disposed on a side of the light component deposition pipe 303 close to the gas outlet pipe 208 , and is used to introduce solvent or carrier gas into the light component deposition pipe 303 .

[0074] The feed pipe valve 301 is installed on the feed pipe 308 and is used to control the opening and closing between the feed pipe 308 and the light component deposition pipe 303 .

[0075] The discharge pipe 306 is disposed on one side of the light component deposition tube 303 close to the connecting pipe 307 for discharging solvent or carrier gas. In some embodiments, it can be connected to a vacuum source to provide negative pressure in the light component deposition tube to further improve the efficiency of discharging solvent or carrier gas.

[0076] The discharge pipe valve 302 is installed on the discharge pipe 306 and is used to control the opening and closing between the discharge pipe 306 and the light component deposition pipe 303 .

[0077] One end of the connecting pipe 307 is connected to the discharge pipe 306 , and the other end extends into the interior of the collecting barrel 402 .

[0078] The connecting pipe valve 305 is installed on the connecting pipe 307 and is used to control the connection and closing between the connecting pipe 307 and the collecting bucket 402 .

[0079] The light component deposition section temperature control unit 304 is sleeved on the outside of the light component deposition tube 303 . In this embodiment, the light component deposition section temperature control unit is an air convection temperature control chamber, which is used to control the internal temperature of the light component deposition tube 303 .

[0080] The collecting part includes: a collecting bucket 402 , a vacuum tube 404 , a vacuum valve 401 and a collecting part temperature control unit 403 .

[0081] The top of the collecting bucket 402 has an opening for the connecting tube 307 to pass through, and the size of the opening is adapted to the size of the connecting tube 307. The bottom of the collecting bucket 402 has an opening for the vacuum tube 404 to pass through, and the size of the opening is adapted to the size of the vacuum tube 404.

[0082] One end of the vacuum tube 404 is located outside the collection barrel 402 and is used to connect to the vacuum source, and the other end is located inside the collection barrel 402. The portion of the vacuum tube 404 located inside the collection barrel 402 extends upward. The opening of the end of the vacuum tube 404 located inside the collection barrel 402 is upward.

[0083] The collection part temperature control unit 403 is used to control the temperature inside the collection barrel 402. In this embodiment, the collection part temperature control unit is an air convection temperature control chamber.

[0084] Example 2: A method for sublimating a precursor for semiconductor thin film deposition, used to purify aluminum trichloride; the sublimation method provided in this example is carried out using the semiconductor thin film deposition precursor sublimation device described in Example 1.

[0085] The sublimation method provided in this embodiment comprises the following steps:

[0086] Step 1, remove the fluidizing barrel 205 through the flange interface, and move the fluidizing barrel 205 into the glove box. In the glove box, confirm that the lower sieve plate 203 (mesh number 8000) has been cleaned and installed, open the second valve 202 of the fluidizing section, and confirm that the upper sieve plate 204 has been taken out. At this time, fill 1.2 kg of aluminum trichloride into the fluidizing barrel 205 and install the upper sieve plate 204 (mesh number 8000). Close the first valve 201 and the second valve 202 of the fluidizing section, then move the fluidizing barrel 205 out of the glove box, and Figure 1 Style installation.

[0087] Step 2, open the first valve 101 and the second valve 102 of the air inlet, introduce a small amount of carrier gas from the first branch pipe 108, then close the second valve 102 of the air inlet, open the third valve 103 of the air inlet, and repeat this operation six times. Open the outlet pipe valve 211 and the feed pipe valve 301, introduce a small amount of carrier gas from the feed pipe 308, then close the feed pipe valve 301, open the outlet pipe valve 302, and repeat this operation six times.

[0088] 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 fluidizing part, the second valve 202 of the fluidizing part, the valve 211 of the air outlet pipe and the valve 302 of the discharge pipe. Turn on the vacuum and introduce a stable amount of inert gas carrier gas through the flow controller 104. The flow rate of the inert gas carrier gas gradually increases from 1slm to 55slm. The readings of the upper pressure gauge 210 and the lower pressure gauge 209 are shown in Table 1 (pressure unit is Pa), where Δ2=P 210-B -P 209-B , Δ1=P 210-A -P 209-A , Δ=Δ2-Δ1, P 210-B is the reading of the upper pressure gauge 210 after adding aluminum chloride, P209-B is the reading of the pressure gauge 209 after adding aluminum chloride, P 210-A is the reading of the upper pressure gauge 210 in the empty fluidizing barrel, P 209-A It is the reading of the lower pressure gauge 209 in the empty fluidizing barrel (the pressure in the empty fluidizing barrel can be measured in advance).

[0089] Table 1

[0090]

[0091] As shown in Table 1 and Figure 2 As shown, when the flow rate exceeds 30slm, as the flow rate continues to increase, the value of Δ tends to remain unchanged. Therefore, it is determined that when the flow rate is 35slm, aluminum chloride has reached a fluidized state in the fluidizing barrel, so the flow rate remains unchanged at 35slm.

[0092] Step 4, maintain the flow rate of carrier gas introduced in step 3. Turn on the temperature control of the heating jacket of the air inlet part and set it at 50°C, turn on the temperature control of the temperature control unit 206 of the fluidizing part and set it at 80°C, turn on the temperature control of the heating jacket of the outlet pipe and set it at 40°C, turn on the temperature control of the temperature control unit 304 of the light component deposition part and set it at 30°C, and keep it for 1.5 hours.

[0093] Step 5, stop introducing carrier gas through the first branch pipe 108 and close the outlet pipe valve 211. Open the feed pipe valve 301 and the outlet pipe valve 302 (the rear end of the outlet pipe valve 302 is closed by vacuum), introduce tetrahydrofuran to dissolve the light component impurities in the coil and discharge them, then introduce carrier gas from the feed pipe valve 301 and open the rear end of the outlet pipe valve 302 to ensure that the residual ethanol is purged, and close the feed pipe valve 301 and the outlet pipe valve 302.

[0094] Step 6, open the outlet pipe valve 211, connect the pipe valve 305 and the vacuum valve 401, turn on the carrier gas and maintain the flow in step 3, and at the same time, open the vacuum at the rear end of the vacuum valve 401, turn on the temperature control unit 403 of the collection part to control the temperature to 20°C and maintain it for 8 hours, and collect 0.8 kg of high-purity aluminum chloride in the collection bucket 402. The test results of ICP-MS show that the purity of aluminum chloride is increased from 99.9% to greater than 99.9995%.

[0095] Example 3: A method for sublimating a precursor for semiconductor thin film deposition, used to purify hafnium tetrachloride; the sublimation method provided in this example is carried out using the semiconductor thin film deposition precursor sublimation apparatus described in Example 1.

[0096] The sublimation method provided in this embodiment comprises the following steps:

[0097] Step 1, remove the fluidizing barrel 205 through the flange interface and move the fluidizing barrel 205 into the glove box. In the glove box, confirm that the lower sieve plate 203 (mesh number 8000) has been cleaned and installed, open the second valve 202 of the fluidizing section, and confirm that the upper sieve plate 204 has been taken out. At this time, fill 1.4 kg of hafnium tetrachloride into the fluidizing barrel 205 and install the upper sieve plate 204 (mesh number 8000). Close the first valve 201 and the second valve 202 of the fluidizing section, then move the fluidizing barrel 205 out of the glove box, and Figure 1 Style installation.

[0098] Step 2, open the first valve 101 and the second valve 102 of the air inlet, introduce a small amount of carrier gas from the first branch pipe 108, then close the second valve 102 of the air inlet, open the third valve 103 of the air inlet, and repeat this operation ten times. Open the outlet pipe valve 211 and the feed pipe valve 301, introduce a small amount of carrier gas from the feed pipe 308, then close the feed pipe valve 301, open the outlet pipe valve 302, and repeat this operation ten times.

[0099] 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 fluidizing part, the second valve 202 of the fluidizing part, the valve 211 of the air outlet pipe and the valve 302 of the discharge pipe. Turn on the vacuum and introduce a stable amount of inert gas carrier gas through the flow controller 104. The flow rate of the inert gas carrier gas is gradually increased from 1slm to 55slm, and the readings of the upper pressure gauge 210 and the lower pressure gauge 209 are measured, and the fluidizing flow rate is determined to be 40slm according to the method in Example 2.

[0100] Step 4, maintain the flow rate of carrier gas introduced in step 3. Turn on the temperature control of the heating jacket of the air inlet part and set it at 120°C, turn on the temperature control of the temperature control unit 206 of the fluidizing part and set it at 195°C, turn on the temperature control of the heating jacket of the outlet pipe and set it at 30°C, turn on the temperature control of the temperature control unit 304 of the light component deposition part and set it at 10°C, and keep it for 2 hours.

[0101] Step 5, stop introducing carrier gas through the first branch pipe 108 and close the outlet pipe valve 211. Open the feed pipe valve 301 and the outlet pipe valve 302 (the rear end of the outlet pipe valve 302 is closed by vacuum), introduce acetone to dissolve the light component impurities in the coil and discharge them, then introduce carrier gas from the feed pipe valve 301 and open the rear end of the outlet pipe valve 302 to ensure that the residual ethanol is purged, and close the feed pipe valve 301 and the outlet pipe valve 302.

[0102] Step 6, open the outlet pipe valve 211, connect the pipe valve 305 and the vacuum valve 401, turn on the carrier gas and maintain the flow in step 3, and at the same time, open the vacuum at the rear end of the vacuum valve 401, turn on the temperature control unit 403 of the collection part to control the temperature to 10°C and maintain it for 10 hours, and collect 0.7 kg of high-purity hafnium tetrachloride in the collection bucket 402. The test results of ICP-MS show that the purity of hafnium tetrachloride is increased from 99.9% to greater than 99.999%.

[0103] Example 4: A method for sublimating a precursor for semiconductor thin film deposition, used to purify dicyclopentadienyl magnesium; the sublimation method provided in this example is carried out using the semiconductor thin film deposition precursor sublimation apparatus described in Example 1.

[0104] The sublimation method provided in this embodiment comprises the following steps:

[0105] Step 1, remove the fluidizing barrel 205 through the flange interface and move the fluidizing barrel 205 into the glove box. In the glove box, confirm that the lower sieve plate 203 (mesh size 8000) has been cleaned and installed, open the second valve 202 of the fluidizing section, and confirm that the upper sieve plate 204 has been taken out. At this time, fill 3.6 kg of bis(cyclopentadienyl)magnesium into the fluidizing barrel 205 and install the upper sieve plate 204 (mesh size 8000). Close the first valve 201 and the second valve 202 of the fluidizing section, then move the fluidizing barrel 205 out of the glove box and Figure 1 Style installation.

[0106] Step 2, open the first valve 101 and the second valve 102 of the air inlet, introduce a small amount of carrier gas from the first branch pipe 108, then close the second valve 102 of the air inlet, open the third valve 103 of the air inlet, and repeat this operation twelve times. Open the outlet pipe valve 211 and the feed pipe valve 301, introduce a small amount of carrier gas from the feed pipe 308, then close the feed pipe valve 301, open the outlet pipe valve 302, and repeat this operation twelve times.

[0107] 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 fluidizing part, the second valve 202 of the fluidizing part, the air outlet pipe valve 211 and the discharge pipe valve 302. Turn on the vacuum and introduce a stable amount of inert gas carrier gas through the flow controller 104. The inert gas carrier gas flow rate is gradually increased from 1slm to 80slm, and the readings of the upper pressure gauge 210 and the lower pressure gauge 209 are measured, and the fluidization flow rate is determined to be 65slm according to the method in Example 2.

[0108] Step 4, maintain the carrier gas flow rate introduced in step 3. Turn on the temperature control of the heating jacket of the air inlet part and set it at 50°C, turn on the temperature control of the fluidizing part temperature control unit 206 and set it at 70°C, turn on the temperature control of the outlet pipe heating jacket and set it at 30°C, turn on the temperature control of the light component deposition part temperature control unit 304 and set it at 20°C, and keep it for 4 hours.

[0109] Step 5, stop introducing carrier gas through the first branch pipe 108 and close the outlet pipe valve 211. Open the feed pipe valve 301 and the outlet pipe valve 302 (the rear end of the outlet pipe valve 302 is closed by vacuum), introduce acetone to dissolve the light component impurities in the coil and discharge them, then introduce carrier gas from the feed pipe valve 301 and open the rear end of the outlet pipe valve 302 to ensure that the residual ethanol is purged, and close the feed pipe valve 301 and the outlet pipe valve 302.

[0110] Step 6, open the outlet pipe valve 211, connect the pipe valve 305 and the vacuum valve 401, turn on the carrier gas and maintain the flow in step 3, and at the same time, open the vacuum at the rear end of the vacuum valve 401, turn on the temperature control unit 403 of the collection part to control the temperature to 20°C and maintain it for 12 hours, and collect 2.1g of high-purity bis(cyclopentadienyl)magnesium in the collection bucket 402. The test results of ICP-MS show that the purity of bis(cyclopentadienyl)magnesium is increased from 99.5% to greater than 99.99%.

[0111] According to the semiconductor thin film deposition precursor sublimation device and the corresponding semiconductor thin film deposition precursor sublimation method involved in the above-mentioned embodiments, because it has a light component deposition part, the sublimation device provided by the present invention can first deposit the light component impurities in the material to be sublimated in the light component deposition tube for separation, and then collect the target material, thereby effectively improving the sublimation efficiency and being able to increase the purity of the material to be sublimated to more than 99.99%.

[0112] Furthermore, since the sublimation device also has an air inlet portion, an inert gas can be introduced into the fluidized barrel, and thus the sublimation device can be used for sublimation of materials that are sensitive to air and / or water.

[0113] Furthermore, since the light component deposition tube is a coil, the light component can be deposited more fully, which is beneficial to further improve the purity of the target material.

[0114] Furthermore, since the portion of the vacuum tube inside the collecting barrel extends upward and opens upward, it is possible to avoid the target material entering the collecting barrel from being sucked away and causing loss.

[0115] The above-mentioned embodiments are preferred examples of the present invention and are not intended to limit the protection scope of the present invention.

Claims

1. A precursor sublimation device for semiconductor thin film deposition, characterized in that: include: A fluidizing part, which has at least one fluidizing barrel for containing the material to be sublimated and for making the material to be sublimated in a fluidized state, wherein the fluidizing barrel has an inlet and an outlet; The air inlet is arranged at the inlet of the fluidizing part and is used to introduce gas into the fluidizing barrel. a light component settling section, which is in communication with the fluidizing section; and The collecting part includes a collecting barrel for collecting target materials, 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. Wherein, the light component deposition part comprises: Light component deposition tube; a feed pipe, disposed at one end of the light component deposition pipe, connected to the light component deposition pipe, and used for introducing a cleaning liquid or a carrier gas into the light component deposition pipe; and A discharge pipe, which is arranged on the light component deposition pipe and is away from one end of the feed pipe, is communicated with the light component deposition pipe and is used to discharge the cleaning liquid or the carrier gas; The fluidizing section comprises: Fluidizing barrel; An air outlet pipe is arranged at the outlet of the fluidizing barrel, one end of which is detachably connected to the fluidizing barrel and communicated with the inside, and the other end of which is communicated with the light component deposition pipe; An outlet pipe heating sleeve, which is arranged outside the outlet pipe and is used to control the temperature inside the outlet pipe; The fluidizing section temperature control unit is used to control the temperature inside the fluidizing barrel.

2. The semiconductor thin film deposition precursor sublimation device according to claim 1, Features: in, The air intake portion comprises: A main air inlet pipe is arranged at the inlet of the fluidizing barrel, and is detachably connected to the fluidizing barrel and communicated with the inside thereof; A first branch pipe, one end of which is connected to the main air intake pipe and the other end of which is connected to the air source, wherein the first branch pipe is provided with a first air intake valve and a second air intake valve; A second branch pipe, one end of which is connected to the main air intake pipe and the other end of which is connected to a vacuum source, and the second branch pipe is provided with a third air intake valve; A flow controller, installed on the first branch pipe and located between the first valve of the air intake part and the second valve of the air intake part, for controlling the air intake flow; The air intake heating jacket is arranged outside the first branch pipe, the second branch pipe and the main air intake pipe, and is used to control the temperature inside the first branch pipe, the second branch pipe and the main air intake pipe.

3. The semiconductor thin film deposition precursor sublimation device according to claim 1, Features: in, The fluidizing section further comprises: A first valve of the fluidizing part, arranged at the inlet of the fluidizing barrel; A lower sieve plate, arranged inside the fluidizing barrel and located above the first valve of the fluidizing part; An upper sieve plate, arranged inside the fluidizing barrel and above the lower sieve plate; A second valve of the fluidizing part is arranged at the fluidizing barrel and located above the upper sieve plate; The third valve of the fluidizing part is arranged on the air outlet pipe.

4. The semiconductor thin film deposition precursor sublimation device according to claim 1, characterized in that: in, The collection department also includes: The collection part temperature control unit is used to control the temperature inside the collection bucket. The light component deposition section further comprises: The light component deposition section temperature control unit is used to control the temperature inside the light component deposition tube.

5. The semiconductor thin film deposition precursor sublimation device according to claim 1, characterized in that: in, The top of the collecting bucket is provided with an opening for the connecting pipe to pass through, and the vacuum pipe is provided with a vacuum pipe valve.

6. The semiconductor thin film deposition precursor sublimation device according to claim 5, characterized in that: in, The portion of the vacuum tube inside the collecting bucket extends upward and opens upward.

7. The semiconductor thin film deposition precursor sublimation device according to claim 1, characterized in that: in, The light component deposition tube is a coil.

8. The semiconductor thin film deposition precursor sublimation device according to claim 1, characterized in that: in, 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, tetrakis(dimethylamino)zirconium, hafnium tetrachloride, zirconium tetrachloride, molybdenum dioxide dichloride, molybdenum pentachloride, tungsten pentachloride, ferrocene or magnesiumocene.

9. A method for sublimating a precursor for semiconductor thin film deposition, using the semiconductor thin film deposition precursor sublimation device according to any one of claims 1 to 8 for sublimation, characterized in that: The steps include: a. Fill the material to be sublimated into the fluidized barrel; b. introducing a carrier gas into the fluidizing barrel through the air inlet so that the material to be sublimated is in a fluidized state; c. At least one valve of the connecting pipe is in a closed state, so that the light component impurities in the material to be sublimated are deposited in the light component deposition tube; d. introducing a cleaning solvent into the light component deposition tube through the feed pipe and discharging it from the discharge pipe, thereby removing light component impurities deposited in the light component deposition tube; e. Make sure that all valves on the connecting pipes are in an open state, make sure that the valve on the vacuum tube is in an open state, and make the inside of the collection barrel in a negative pressure state, so that the material to be sublimated can enter the inside of the collection barrel.

10. The method for sublimating a precursor for semiconductor thin film deposition according to claim 9, characterized in that: When the material to be sublimated is a substance that is sensitive to water and / or air, sublimation is performed using the sublimation device according to claim 2, further comprising the following steps: f. Introduce inert gas into the main air intake pipe through the first branch pipe and discharge it from the second branch pipe; g. Introduce inert gas into the light component deposition tube through the feed pipe and discharge it from the discharge pipe.

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