CN117623319A - Method for preparing diiodosilane - Google Patents
Method for preparing diiodosilane Download PDFInfo
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- CN117623319A CN117623319A CN202311593269.0A CN202311593269A CN117623319A CN 117623319 A CN117623319 A CN 117623319A CN 202311593269 A CN202311593269 A CN 202311593269A CN 117623319 A CN117623319 A CN 117623319A
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- diiodosilane
- temperature
- preparing
- dichlorosilane
- reaction
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- AIHCVGFMFDEUMO-UHFFFAOYSA-N diiodosilane Chemical compound I[SiH2]I AIHCVGFMFDEUMO-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 24
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- HSZCZNFXUDYRKD-UHFFFAOYSA-M lithium iodide Chemical compound [Li+].[I-] HSZCZNFXUDYRKD-UHFFFAOYSA-M 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000007789 sealing Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 239000004065 semiconductor Substances 0.000 abstract description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 239000006227 byproduct Substances 0.000 description 9
- 229910052581 Si3N4 Inorganic materials 0.000 description 8
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000012043 crude product Substances 0.000 description 6
- 238000001165 gas chromatography-thermal conductivity detection Methods 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- PARWUHTVGZSQPD-UHFFFAOYSA-N phenylsilane Chemical compound [SiH3]C1=CC=CC=C1 PARWUHTVGZSQPD-UHFFFAOYSA-N 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- OASAGXUWNYOMED-UHFFFAOYSA-N (4-methylphenyl)silane Chemical compound CC1=CC=C([SiH3])C=C1 OASAGXUWNYOMED-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000231 atomic layer deposition Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000001004 secondary ion mass spectrometry Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Abstract
The invention discloses a method for preparing diiodosilane, which belongs to the technical field of precursor materials for manufacturing semiconductor elements, and comprises the following steps: s1: under the inert gas atmosphere, anhydrous lithium iodide is added into a reaction kettle, and the temperature is reduced to minus 60 ℃ to 10 ℃ after the sealing; s2: after cooling, keeping the temperature unchanged, and introducing dichlorosilane, wherein the equivalent ratio of dichlorosilane to anhydrous lithium iodide is 1:1.5 to 10; s3: after the dichlorosilane is introduced, the temperature is raised to room temperature, the reaction is stirred in a closed way, the diiodosilane is distilled off under heating and reduced pressure after the reaction is finished, and the diiodosilane which is a high-purity electronic chemical is obtained through heating, reduced pressure rectification and purification. The method avoids the introduction of carbon element from the source, omits the operations of filtering and evaporating solvent, improves the way of separating products, realizes the recovery of LiCl, has no generation of three wastes in the preparation and production process, and avoids environmental pollution. LiCl can be recycled, so that the cost is reduced, and the waste of lithium resources is avoided.
Description
Technical Field
The invention belongs to the technical field of precursor materials for manufacturing semiconductor elements, and particularly relates to a method for preparing diiodosilane.
Background
Silicon nitride film is a widely used dielectric material. As an amorphous insulating material, a silicon nitride film has the advantages of compact structure, small pinhole density, enhanced blocking ability to mobile ions, good optical stability, high dielectric constant, and the like, and is widely used in the field of integrated circuit fabrication for surface packaging of barrier layers, insulating layers, semiconductor elements, and the like. With the development of chip process, higher requirements are put on the silicon nitride film, and the silicon nitride film needs to be deposited under more and more strict conditions. Diiodisilane (DIS) can generate more active silicon free radicals in plasma enhanced film deposition, and a reaction cavity has the characteristics of lower temperature and more controllable pressure operation on the premise of keeping a high deposition rate, so that the Diiodosilane (DIS) is attracting more attention.
Silicon nitride films deposited in PEALD mode deposited with diiodosilane as a precursor can form high quality silicon nitride films at lower temperatures (300 ℃) and exhibit excellent step coverage. Common atomic layer deposited silicon nitride films often contain a small amount of carbon residues, which cause the increase of film leakage and the generation of defects, thereby affecting the performance of the films. Therefore, in advanced semiconductor process, it is required that the PEALD deposited silicon nitride film is completely free of carbon (i.e., C remains below 1 ppm), so that the preparation of a completely carbon-free diiodosilane material is of great importance.
Diiodosilanes have a variety of synthetic routes, but are mostly unsuitable for commercial production: for example, the diiodosilane is prepared by the reaction of phenylsilane and iodine, so that the reaction is complex and cancerogenic benzene is generated; toluene is produced by replacing phenylsilane with p-methylphenyl silane, the toxicity of toluene is smaller than that of benzene, but the boiling point of toluene is similar to that of diiodosilane, the purification difficulty is increased, and the problem that the phenylsilane and the p-methylphenyl silane are difficult to obtain exists.
The diiodosilane is prepared by reacting anhydrous lithium iodide with dichlorosilane. The solvent used in the reaction is difficult to treat and recycle due to the acidic substances, a certain amount of diiodosilane is lost when the solvent is distilled off, and more or less solvent remains in the purified diiodosilane, so that the product contains carbon elements.
Patent CN112041324a reports that a method for producing a halosilane compound is invented, in which a halosilane compound is produced by using a reaction vessel containing a halide source provided inside, and the reactor is used for producing diiodosilane, which has not only the disadvantage that the equipment is complicated and is not suitable for further industrial enlargement, but also that an excess of dichlorosilane is required to be introduced when diiodosilane is produced by using the reactor, and that the excess dichlorosilane not only causes waste of resources, but also causes environmental pollution and safety accidents once disposed improperly.
Disclosure of Invention
The invention aims to provide a method for preparing diiodosilane, which aims to solve the problem that carbon element is contained in a product because of residual solvent in the process of preparing diiodosilane.
The aim of the invention can be achieved by the following technical scheme:
a method of preparing diiodosilane comprising the steps of:
s1: under the inert gas atmosphere, anhydrous lithium iodide is added into a reaction kettle, and the temperature is reduced to minus 60 ℃ to 10 ℃ after the sealing;
s2: after cooling, keeping the temperature unchanged, and introducing Dichlorosilane (DCS), wherein the equivalent ratio of the Dichlorosilane (DCS) to the anhydrous lithium iodide is 1:1.5 to 10;
s3: after the Dichlorosilane (DCS) is completely introduced, the temperature is raised to room temperature (20-30 ℃), the reaction is carried out under sealed stirring, the diiodosilane is distilled under heating and reduced pressure after the reaction is finished, and the Diiodosilane (DIS) which is a high-purity electronic chemical is obtained through heating, reduced pressure rectification and purification.
As a further scheme of the invention: the inert gas atmosphere is one of nitrogen and argon.
As a further scheme of the invention: in the step S1, the temperature is reduced to minus 30 ℃ to 10 ℃.
As a further scheme of the invention: and in the step S1, the temperature is reduced to-20 ℃ to 10 ℃.
As a further scheme of the invention: the equivalent ratio of dichlorosilane to anhydrous lithium iodide in step S2 is 1:2.3.
as a further scheme of the invention: the vacuum degree of heating and reduced pressure distillation in the step S3 is 3mbar-30mbar, and the heating temperature is 40 ℃ to 120 ℃. Preferably, the vacuum is 3mbar to 20mbar and the heating temperature is 80 ℃ to 100 ℃.
As a further scheme of the invention: in the step S3, the vacuum degree of heating and decompressing rectification is 3mbar-20mbar, and the heating temperature is 80 ℃ to 120 ℃. Preferably, the vacuum is 3mbar to 10mbar and the heating temperature is 80 ℃ to 90 ℃.
As a further scheme of the invention: after the diiodosilane was distilled off under reduced pressure by heating, the resulting residual solid LiCl was directly discharged from the bottom of the reaction vessel.
The invention has the beneficial effects that:
the invention provides a preparation method of diiodosilane for industrial production, which avoids the introduction of carbon element from the source, omits the operations of filtering and evaporating solvent, improves the way of separating products and realizes the recovery of LiCl. The method can realize industrialized production for preparing the diiodosilane as the silicon-based precursor material, improve the product quality, avoid the generation of three wastes in the preparation and production process and avoid environmental pollution. The LiCl byproduct generated by the reaction can be recycled, so that the cost is reduced, and the waste of lithium resources is avoided.
The invention provides a method for preparing diiodosilane, which reduces the waste of dichlorosilane, improves the reaction yield and reduces the risks of environmental pollution and safety accidents caused by the control of reaction conditions and the adjustment of the raw material consumption.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a gas chromatogram of a sample prepared in example 1 of the present invention;
FIG. 2 is a gas chromatogram of a sample prepared in example 3 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The present example provides a method of preparing diiodosilane comprising the steps of:
s1: under nitrogen atmosphere, 5004g (37.38 mol) of LiI was added to a stainless steel reaction vessel, the vessel was closed and the vessel temperature was lowered to below-28 ℃.
S2: the kettle temperature was controlled to be below-28℃and was controlled to pass through DCS1832g (18.84 mol; DCS: liI=1:1.98).
S3: and (5) recovering to room temperature. After stirring for 24h, the temperature was raised to 60℃and the DIS crude product was distilled off under reduced pressure (below 5 mbar). The crude product is rectified to obtain the non-carbon electronic grade product DIS 3787g with the purity of GC-TCD being more than 99.9 percent (the purity of diiodosilane measured by GC-TCD is 99.97 percent by area integration), the purity of metal being more than 99.99999 percent and the reaction yield being 72.6 percent. The byproduct LiCl is directly recovered by opening a kettle bottom valve to release (the byproduct lithium chloride can be directly recovered and utilized).
Example 2
The present example provides a method of preparing diiodosilane comprising the steps of:
s1: liI 5000g (37.35 mol) was added to a stainless steel reaction vessel under nitrogen atmosphere, the vessel was closed and the vessel temperature was lowered to below-20 ℃.
S2: the kettle temperature was controlled to be below-20 ℃ and was vented with DCS1886g (16.24 mol; DCS: lii=1:2.30) of gas.
S3: and (5) recovering to room temperature. After stirring for 24h, the temperature was raised to 70℃and the DIS crude product was distilled off under reduced pressure (below 10 mbar). The crude product is rectified to obtain a non-carbon electronic grade product DIS 4057g with the GC-TCD purity of more than 99.9 percent and the metal purity of more than 99.99999 percent, and the reaction yield is 88.06 percent. The byproduct LiCl is directly recovered by opening a kettle bottom valve to release (the byproduct lithium chloride can be directly recovered and utilized).
Example 3
The present example provides a method of preparing diiodosilane comprising the steps of:
s1: liI 5012g (37.44 mol) was added to a stainless steel reaction vessel under nitrogen atmosphere, the vessel was closed and the vessel temperature was lowered to below-10 ℃.
S2: the kettle temperature was controlled to be below-10 ℃ and 2522g (24.96 mol; DCS: lii=1:1.50) of gas was introduced.
S3: and (5) recovering to room temperature. After stirring for 24h, the temperature was raised to 50℃and the DIS crude product was distilled off under reduced pressure (below 10 mbar). The crude product was rectified to give a non-carbonaceous electronic grade product DIS2339g with a GC-TCD purity of greater than 99.9% (see FIG. 2, diiodosilane purity by GC-TCD, 99.94% by area integration), and a metal purity of greater than 99.99999%, with a reaction yield of 33.0%. The byproduct LiCl is directly recovered by opening a kettle bottom valve to release (the byproduct lithium chloride can be directly recovered and utilized).
Test case
A preparation method of a SiN film comprises the following steps:
(1) Placing a silicon wafer into a reaction cavity in atomic layer deposition equipment, wherein the heating temperature in the reaction cavity is 300 ℃, and the vacuum pressure in the cavity is 15Pa;
(2) The Diiodosilane (DIS) is arranged in a stainless steel source bottle with the heating temperature of 35 ℃, the stainless steel source bottle is connected with a reaction cavity through a pipeline, the heating temperature of the pipeline is 70 ℃, argon is used as carrier gas, the DIS is introduced into the reaction cavity through the pipeline in a pulse form, and the pulse duration is 0.3s; diiodosilane was derived from examples 1-3;
(3) Argon is introduced into the reaction cavity for purging, excessive DIS and reaction byproducts are purged, and the purging time is 15s;
(4) Will N 2 Introducing into the reaction chamber in pulse form, and igniting plasma with power of 300W and N 2 The pulse and plasma lighting time is 0.3s;
(5) Introducing argon into the reaction cavity to purge excessive N 2 And reaction byproducts, purging for 15s;
(6) Repeating the steps (2) - (5) for 500 times to obtain the SiN film.
The thickness of the SiN film was measured to be 13.5nm by ellipsometryThe deposition rate isCycle; the refractive index of the film was 2.05.
As is known from X-ray photoelectron spectroscopy (XPS), si in the film: the N content is 42.8:57.2% (N: si=1.336, close to Si) 3 N 4 1.333) of the formula (i).
As a result of Secondary Ion Mass Spectrometry (SIMS) test, the Si and N contents were 5.3X10, respectively 22 cm -3 And 7.4X10 22 cm -3 Of the order of magnitude, C content is less than 1x10 16 cm -3 On the order of magnitude. It can also be demonstrated that the content of C is less than 1ppm.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method of preparing diiodosilane comprising the steps of:
s1: under the inert gas atmosphere, anhydrous lithium iodide is added into a reaction kettle, and the temperature is reduced to minus 60 ℃ to 10 ℃ after the sealing;
s2: after cooling, keeping the temperature unchanged, and introducing dichlorosilane, wherein the equivalent ratio of dichlorosilane to anhydrous lithium iodide is 1:1.5 to 10;
s3: after the dichlorosilane is introduced, the temperature is raised to room temperature, the reaction is stirred in a closed way, the diiodosilane is distilled off under heating and reduced pressure after the reaction is finished, and the diiodosilane which is a high-purity electronic chemical is obtained through heating, reduced pressure rectification and purification.
2. A method for preparing diiodosilane according to claim 1, wherein the inert gas atmosphere is one of nitrogen and argon.
3. The method for preparing diiodosilane according to claim 1, wherein the temperature is reduced to-30 to 10 ℃ in step S1.
4. The method for preparing diiodosilane according to claim 1, wherein the temperature is reduced to-20 to 10 ℃ in step S1.
5. The method for preparing diiodosilane according to claim 1, wherein the equivalent ratio of dichlorosilane to anhydrous lithium iodide in step S2 is 1:2.3.
6. a process for the preparation of diiodosilane according to claim 1, characterized in that in step S3 the vacuum of the distillation under reduced pressure is 3mbar to 30mbar and the heating temperature is 40 ℃ to 120 ℃.
7. A process for the preparation of diiodosilane according to claim 1, characterized in that in step S3 the vacuum of the heating reduced pressure distillation is 3-20 mbar and the heating temperature is 80-120 ℃.
8. A method for preparing diiodosilane according to claim 1, wherein after heating and distilling off diiodosilane under reduced pressure, the resulting residual solid LiCl is directly discharged from the bottom of the reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202311593269.0A CN117623319A (en) | 2023-11-27 | 2023-11-27 | Method for preparing diiodosilane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311593269.0A CN117623319A (en) | 2023-11-27 | 2023-11-27 | Method for preparing diiodosilane |
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| CN117623319A true CN117623319A (en) | 2024-03-01 |
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| CN202311593269.0A Pending CN117623319A (en) | 2023-11-27 | 2023-11-27 | Method for preparing diiodosilane |
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| Country | Link |
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