Pretreatment device for detecting metal impurities in iodo-silane and detection equipment thereof

Abstract

The utility model relates to a pretreatment device for detecting metal impurities in iodo-silane and detection equipment of the pretreatment device. The pretreatment device comprises a reaction tank, an empty bottle, an absorption bottle, a heating plate, a heating belt, a first connecting pipe and a second connecting pipe; the reaction tanks are located on the heating plate, the first connecting pipes correspond to the reaction tanks in a one-to-one mode, the reaction tanks are communicated with the empty bottles through the corresponding first connecting pipes, the empty bottles are communicated with the absorption bottles through the second connecting pipes, the absorption bottles are further provided with exhaust pipes used for exhausting, and first cover holes are formed in the reaction tanks. The first cover hole is used for being in butt joint with an external gas source and adding reactants, and the heating belt is wound around the first connecting pipes to heat the first connecting pipes; aiming at the technical problems existing in trace metal impurity detection of an iodo-silane sample, the pretreatment device disclosed by the utility model has the advantages that on one hand, the iodo-silane sample is effectively prevented from being in contact with the external environment in a test process, and the sample is prevented from being polluted and lost; and on the other hand, the problem of pipeline blockage is solved, the matrix elements in the iodo-silane sample are effectively separated, the interference of the matrix elements on trace metal impurity detection in the subsequent ICP-MS determination process is eliminated, the detection sensitivity and precision are improved, and the detection analysis of trace metal impurities under a complex matrix is realized.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of analysis and detection of semiconductor manufacturing materials, in particular to a pretreatment device for detecting metal impurities in iodosilane and a detection equipment thereof. BACKGROUND

[0002] High-purity iodosilane plays an increasingly important role in high-end semiconductor chips and is an important silicon source for chemical vapor deposition. However, the presence of metal impurities in iodosilane can cause the performance of semiconductor devices to decrease or even fail. Therefore, the content of metal impurities in iodosilane needs to be detected before use.

[0003] Before detecting the content of metal impurities in iodosilane, a sample liquid needs to be prepared from iodosilane to remove the matrix elements (such as silicon and iodine) in iodosilane, so as to avoid the high concentration of matrix elements (such as silicon and iodine) in iodosilane from causing mass spectrum interference and matrix effect on the detection of trace metal impurities when the content of metal impurities is detected by inductively coupled plasma mass spectrometry (ICP-MS), thereby affecting the sensitivity and accuracy of the detection.

[0004] However, iodosilane is prone to react with moisture in the air, and the sample loss and reaction products caused by the reaction make it difficult to ensure the accuracy of trace metal impurity analysis. In addition, the pipelines of the device are prone to blockage, which causes the sample liquid to be easily contaminated and the pressure in the reaction tank to be too high, thereby causing safety hazards. The sample liquid prepared by the device has mass spectrum interference and matrix effect when detected, which affects the sensitivity and accuracy of the detection.

[0005] In addition, since iodosilane is a corrosive flammable liquid, certain protective measures are needed before detection.

[0006] Therefore, it is necessary to develop a pretreatment device specifically for detecting metal impurities in iodosilane, which can effectively prevent iodosilane samples from contacting the external environment, avoid sample loss and the existence of byproduct, and ensure the accuracy of trace metal impurity analysis. CONTENT OF THE INVENTION

[0007] The application aims to at least solve one of the technical problems existing in the prior art. To this end, the utility model provides a kind of pretreatment device for detecting metal impurities in iodosilane on one hand, it includes reaction tank, empty bottle, absorption bottle, hot plate, heating band, first connecting pipe and second connecting pipe, reaction tank is at least provided with one, and it is located on hot plate, hot plate is used to provide the temperature required for reaction for each reaction tank, first connecting pipe is corresponding with reaction tank one by one, each reaction tank is communicated with empty bottle by corresponding first connecting pipe, empty bottle is communicated with absorption bottle by second connecting pipe, absorption bottle is also provided with exhaust pipe for exhausting, wherein, first cover hole is used to butt-joint external gas source and add reactant, heating band is wound on each first connecting pipe to heat each first connecting pipe.

[0008] Optionally, each reaction tank is provided with a first gas inlet pipe, and the first gas inlet pipe is plug-connected in the corresponding first cover hole, and the first gas inlet pipe is used to communicate the corresponding reaction tank with the external gas source.

[0009] Optionally, the pretreatment device for detecting metal impurities in iodosilane further comprises at least one control tank, the control tank is arranged on the hot plate, each control tank is communicated with the empty bottle through a third connecting pipe, and each control tank is provided with a first control cover hole, and the first control cover hole is used to butt-joint the external gas source and add the reactant.

[0010] Optionally, each control tank is provided with a second gas inlet pipe, and the second gas inlet pipe is used to communicate the corresponding control tank with the external gas source, and each second gas inlet pipe is plug-connected with the first control cover hole.

[0011] Optionally, the pretreatment device for detecting metal impurities in iodosilane further comprises a first pipe joint, the first pipe joint is provided with a gas inlet port corresponding to the external gas source and a gas outlet port corresponding to each reaction tank and each control tank, the external gas source is communicated with the gas inlet port of the first pipe joint, each reaction tank is communicated with the gas outlet port of the corresponding first pipe joint through the corresponding first gas inlet pipe, and each control tank is communicated with the gas outlet port of the corresponding first pipe joint through the corresponding second gas inlet pipe.

[0012] Optionally, the pretreatment device for detecting metal impurities in iodosilane further comprises a second pipe joint, the second pipe joint is provided with a gas inlet port corresponding to each reaction tank and each control tank and a gas outlet port corresponding to the empty bottle, each reaction tank is communicated with the gas inlet port of the corresponding second pipe joint through the corresponding first connecting pipe, each control tank is communicated with the gas inlet port of the corresponding second pipe joint through the corresponding third connecting pipe, and the empty bottle is communicated with the gas outlet port of the second pipe joint through a fourth connecting pipe.

[0013] The utility model provides another aspect of the detection equipment for detecting metal impurities in iodosilane by using the above pretreatment device.

[0014] Beneficial effects: the pretreatment device for detecting metal impurities in iodosilane provided by the utility model, which is used for making sample liquid (sample liquid required for detecting metal impurity content in iodosilane);The pretreatment device can effectively avoid the contact between iodosilane sample and external environment in the test process by taking the reaction tank as a reaction container and exhausting through the first connecting pipe, so as to avoid sample loss, avoid the occurrence of side reaction (reaction of iodosilane and water) and sample contamination;The waste gas generated in the reaction tank is heated when passing through the first connecting pipe by winding the heating belt on the first connecting pipe, so as to solve the problem of pipeline blockage, avoid the safety hazard caused by the excessive pressure in the reaction tank, effectively separate the matrix element in the iodosilane sample, eliminate the interference of the matrix element on the detection of trace metal impurities in the subsequent ICP-MS determination process, improve the sensitivity and precision of detection, and realize the detection and analysis of trace metal impurities under complex matrix. BRIEF DESCRIPTION OF DRAWINGS

[0015] The application will be further described below with reference to the drawings.

[0016] Figure 1 is a structure schematic view of the pretreatment device for detecting metal impurities in iodosilane with only one reaction tank in one embodiment of the application;

[0017] Figure 2 is a structure schematic view of the pretreatment device for detecting metal impurities in iodosilane with both a reaction tank and a control tank in one embodiment of the application.

[0018] Marked for explanation:

[0019] 1, reaction tank;2, empty bottle;3, absorption bottle;4, heating plate;5, heating belt;6, first connecting pipe;7, second connecting pipe;8, exhaust pipe;9, first air inlet pipe;10, control tank;11, third connecting pipe;12, second air inlet pipe;13, first pipe joint;14, second pipe joint;15, fourth connecting pipe. DETAILED DESCRIPTION

[0020] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the drawings in the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, not all the embodiments. Based on the embodiments in the application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the application.

[0021] Please refer to Figure 1As shown, in some embodiments, the present application provides a kind of metal impurity detection pretreatment device for iodosilane, for making the sample liquid required for detecting the metal impurity content in iodosilane.The metal impurity detection pretreatment device for iodosilane includes reaction tank 1, empty bottle 2, absorption bottle 3, heating plate 4, heating belt 5, first connecting pipe 6 and second connecting pipe 7.Reaction tank 1 is provided with at least one, and is located on the heating plate 4.The first connecting pipe 6 corresponds to the reaction tank 1, and each reaction tank 1 is communicated with the empty bottle 2 through the corresponding first connecting pipe 6, and the empty bottle 2 is communicated with the absorption bottle 3 through the second connecting pipe 7.The absorption bottle 3 is also provided with exhaust pipe 8 for exhausting gas.Each reaction tank 1 is provided with first cover hole, and the first cover hole is used for docking external gas source and adding reactant, and the heating belt 5 is wound on each first connecting pipe 6 to heat each first connecting pipe 6.

[0022] The specific steps of the metal impurity detection pretreatment device for iodosilane in the present application for making the sample liquid required for detecting the metal impurity content in iodosilane are as follows:

[0023] 1, the mass m of iodosilane sample is added into the reaction tank 1, and the filling cover of the reaction tank 1 is closed;

[0024] 2, use 1.0mL pipette, slowly add concentrated HF (hydrofluoric acid) acid into the reaction tank 1 from the first cover hole for 4 times;After the first slow addition of 1.0mL HF, the reaction is violent and there is a sound or splashing, and yellow smoke can be observed in the gas absorption bottle 3;When the reaction sound disappears, continue to add 1.0mL HF, generally add 3mL HF after adding, the reaction is slow and there is no sound, add the fourth 1.0mL HF to ensure the reaction is complete, the total amount of HF acid added in this process is about 4mL.(Note: in order to prevent pollution of concentrated HF acid, replace the new gun head from the original HF acid)

[0025] 3, use 0.1mL pipette, slowly add concentrated H2O2 (hydrogen peroxide) into the reaction tank 1 from the first cover hole for 2 times, about 0.2mL in total.After adding H2O2, black purple precipitate is rapidly generated in the solution, and there is a large amount of yellow brown color in the absorption bottle 3, and the reaction occurs in this process: 2I - +H2O2+2H + →I2+2H2O.

[0026] 4. The external gas source is used to transport inert gas (such as nitrogen or argon) into the reaction tank 1 through the first cover hole, and the input flow is about 0.3 mL / min. The heating plate 4 is heated to 150℃ to heat the reaction tank 1 for about 3 hours, and the generated silicon tetrafluoride and elemental iodine precipitate and excess HF are driven out of the reaction tank 1, so that the generated silicon tetrafluoride and elemental iodine and excess HF flow into the absorption bottle 3 through the first connecting pipe 6, the empty bottle 2 and the second connecting pipe 7 in sequence, and are absorbed by the 2% NaOH lye in the absorption bottle 3.

[0027] During the process of driving the HF and elemental iodine precipitate out of the reaction tank 1, the heating tape 5 is used to heat the first connecting pipe 6 at about 85℃, so that the subsequent elemental iodine flows into the absorption bottle 3 in the form of gas through the first connecting pipe 6, the empty bottle 2 and the second connecting pipe 7 in sequence and is absorbed by the NaOH lye, avoiding the blocking of the pipeline caused by the condensation of iodine vapor.

[0028] During the process, the heating tape 5 heats the first connecting pipe 6, so that the elemental iodine remains in the vapor state, effectively avoiding the blocking of the pipeline caused by the condensation of elemental iodine in the pipeline.

[0029] During the heating process of the heating plate 4 on the reaction tank 1, the original precipitate in the solution in the reaction tank 1 gradually decreases, and the color of the solution gradually changes from purple red to colorless. Continue to heat until there is no precipitate and the state is almost dry. After cooling, it is taken off from the heating plate 4, about 0.25 mL of concentrated HNO3 (nitric acid) is added, and then it is placed on the heating plate 4 at 80℃ for about 5 minutes to ensure that the various elements are completely redissolved. After cooling, it is diluted to 10.000 g with Mill-i-Q water to prepare a sample solution. The content of metal elements in the sample solution can be measured by the standard working curve method.

[0030] The pre-treatment device in the present application can ensure the efficient and high-quality preparation of the iodosilane sample solution, avoid the contact between the iodosilane sample and the external environment during the test process, thereby avoiding sample loss and the occurrence of side reactions (reaction of iodosilane with water) and contamination. It can also avoid pipeline blockage during the preparation of the sample solution, ensure safety and efficiency during the preparation process, effectively separate the matrix elements in the sample solution, and avoid the matrix interference and mass spectrum interference of the subsequent matrix elements on the detection of trace metal impurities.

[0031] Preferably, when the sample solution is prepared by the iodosilane metal impurity detection pre-treatment device, the iodosilane metal impurity detection pre-treatment device can be placed in a fume hood for operation, so that the fume hood can quickly blow away the gas overflowing during the operation to avoid harm to the body of the operator.

[0032] In some embodiments, each reaction tank 1 is provided with a first gas inlet pipe 9, and each first gas inlet pipe 9 is plug-connected in the corresponding first cover hole. When adding reactants into the reaction tank 1, the first gas inlet pipe 9 can be pulled out of the first cover hole, so that the reactants are added into the reaction tank 1 through the first cover hole. When the external gas source needs to ventilate into the reaction tank 1, the first gas inlet pipe 9 is installed in the first cover hole, so that the external gas source ventilates inert gas into the reaction tank 1 through the first gas inlet hole.

[0033] In some embodiments, the reaction tank 1 is also provided with a second cover hole. The heating plate 4 is used to provide the temperature required for the reaction of each reaction tank 1. The empty bottle 2 is used to prevent the solution in the absorption bottle 3 from being sucked into the reaction tank 1, and the empty bottle 2 is provided with a third cover hole and a fourth cover hole. The absorption bottle 3 contains a proper amount of 2% NaOH solution, which is used to absorb the waste generated by the reaction, and the absorption bottle 3 is provided with a fifth cover hole and a sixth cover hole.

[0034] In an embodiment, the heating belt 5 also extends to the empty bottle 2 to wrap the empty bottle 2, which increases the heating path length of the waste gas. Compared with wrapping the heating belt 5 only on the first connecting pipe 6, the heating temperature of the heating belt 5 can be appropriately reduced.

[0035] In some embodiments, only one reaction tank 1 is provided, and at this time, the first connecting pipe 6 is plug-connected with the second cover hole and the third cover hole at both ends, so as to communicate the digestion tank and the empty bottle 2; the second connecting pipe 7 is plug-connected with the fourth cover hole and the fifth cover hole at both ends, so as to communicate the empty bottle 2 and the absorption bottle 3; and the exhaust pipe 8 is plug-connected with the sixth cover hole, so as to exhaust the waste gas in the absorption bottle 3.

[0036] Please refer to Figure 2 In some embodiments, the iodosilane metal impurity detection pretreatment device also includes at least one control tank 10, and each control tank 10 is arranged on the heating plate 4. Each control tank 10 is communicated with the empty bottle 2 through the third connecting pipe 11.

[0037] The control tank 10 is used for blank control test. During the experiment, compared with the reaction bottle, only the iodosilane sample is not added in the control tank 10, and the other reactants and reaction conditions are the same as those in the reaction bottle, which will not be described in detail here.

[0038] Specifically, each control tank 10 is provided with a first control cover hole and a second control hole. The iodosilane metal impurity detection pretreatment device further comprises a second gas inlet pipe 12 corresponding to each control tank 10 and being plug-connected with the first control cover hole. When the reactant is added into the control tank 10, the second gas inlet pipe 12 is first pulled out of the first control cover hole, so that the reactant is directly added into the control tank 10 through the first control cover hole. When the external gas source is used to ventilate the control tank 10, the second gas inlet pipe 12 is plug-connected with the first control cover hole, so that the external gas source is used to ventilate the control tank 10 with inert gas through the second gas inlet hole.

[0039] The iodosilane metal impurity detection pretreatment device further comprises a first pipe joint 13 and a second pipe joint 14. The first pipe joint 13 is provided with an air inlet port corresponding to the external gas source and gas outlet ports corresponding to each reaction tank 1 and each control tank 10. The external gas source is communicated with the air inlet port of the first pipe joint 13, each reaction tank 1 is communicated with the gas outlet port of the corresponding first pipe joint 13 through the corresponding first gas inlet pipe 9, and each control tank 10 is communicated with the gas outlet port of the corresponding first pipe joint 13 through the corresponding second gas inlet pipe 12. The second pipe joint 14 is provided with gas inlet ports corresponding to each reaction tank 1 and each control tank 10 and a gas outlet port corresponding to the empty bottle 2. Each reaction tank 1 is communicated with the gas inlet port of the corresponding second pipe joint 14 through the corresponding first connecting pipe 6, and the corresponding first connecting pipe 6 of each reaction tank 1 is wound with a heating belt 5 to avoid the waste gas generated by the reaction tank 1 from blocking the subsequent pipeline. Each control tank 10 is communicated with the gas inlet port of the corresponding second pipe joint 14 through the corresponding third connecting pipe 11, and the empty bottle 2 is communicated with the gas outlet port of the second pipe joint 14 through the fourth connecting pipe 15. The external gas source is used to provide inert gas for each reaction tank 1 and each control tank 10 through the first pipe joint 13, and the waste gas generated in each reaction tank 1 and each control tank 10 is transported to the empty bottle 2 through the second pipe joint 14.

[0040] Specifically, the first gas inlet pipe 9 is connected to the gas outlet port of the corresponding first pipe joint 13 at one end and is connected to the first cover hole of the corresponding reaction tank 1 at the other end, thereby connecting the first pipe joint 13 to each reaction tank 1. The second gas inlet pipe 12 is connected to the gas outlet port of the corresponding first pipe joint 13 at one end and is connected to the first control cover hole of the corresponding control tank 10 at the other end, thereby connecting the first pipe joint 13 to each control tank 10. The first connecting pipe 6 is connected to the second cover hole of the corresponding reaction tank 1 at one end and is connected to the gas inlet port of the corresponding second pipe joint 14 at the other end, thereby connecting each reaction tank 1 to the second pipe joint 14. The third connecting pipe 11 is connected to the second control cover hole of the corresponding control tank 10 at one end and is connected to the gas inlet port of the corresponding second pipe joint 14 at the other end, thereby connecting each control tank 10 to the second pipe joint 14. The fourth connecting pipe 15 is connected to the gas outlet port of the second pipe joint 14 at one end and is connected to the third cover hole at the other end, thereby connecting the empty bottle 2 to the second pipe joint 14. The present application is connected between structures by plugging, facilitating the disassembly and assembly of the pretreatment device for detecting metal impurities in iodosilane.

[0041] In an optional embodiment, the reaction tank 1 is provided with a plurality of (for example, three) reaction tanks, and the control tank 10 is also provided with a plurality of (for example, three) control tanks, so that the pretreatment device for detecting metal impurities in iodosilane in the present application can simultaneously prepare multiple sample liquids and control liquids, thereby improving the preparation efficiency of the sample liquid and the control liquid, and further improving the accuracy of the subsequent experimental results.

[0042] The pretreatment device of the above-mentioned embodiment of the present application can be directly applied to or included in the metal impurity detection equipment for iodosilane.

[0043] The above describes one embodiment of the present application in detail, but the description is only a preferred embodiment of the present application and cannot be considered as limiting the scope of the present application. Any equivalent changes and improvements made within the scope of the present application should still be included in the patent coverage of the present application.

[0044] It should be noted that the terms "first", "second", and the like used in the present application do not represent any order, quantity or importance, but are only used to distinguish different components. The description of "left", "right", "left side", "right side", "upper", "lower", "top", "bottom" and the like in the present application are defined based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and therefore cannot be understood as limiting or implying that the structure must be constructed and operated in a particular orientation. Therefore, it cannot be understood as a limitation on the present application. In the description of the present application, "a plurality of" means two or more, unless otherwise specifically limited.

[0045] In the description of the application, unless specifically stated and limited otherwise, the terms "mounting", "connection", "connecting" should be understood broadly, for example, can be fixedly connected, can also be detachably connected, or integrally connected; can be directly connected, or indirectly connected through an intermediate medium, can be the communication inside two elements. For those skilled in the art, the specific meaning of the above terms in the application can be understood according to the specific circumstances.

Claims

1. A pretreatment device for detecting metal impurities in iodosilanes, characterized in that, The pre-treatment device comprises reaction tanks, empty bottles, absorption bottles, heating plates, heating belts, first connecting pipes and second connecting pipes. At least one reaction tank is arranged on the heating plate, and the heating plate is used to provide the required temperature for the reaction of each reaction tank. Each reaction tank is connected to the empty bottle through the corresponding first connecting pipe, and the empty bottle is connected to the absorption bottle through the second connecting pipe. An exhaust pipe is arranged on the absorption bottle for exhaust. Each reaction tank is provided with a first cover hole for connecting to an external gas source and adding reactants. The heating belt is arranged around each first connecting pipe to heat each first connecting pipe.

2. The pre-treatment device of claim 1, wherein, Each reaction tank is provided with a first gas inlet pipe which is plug-connected in the corresponding first cover hole. The first gas inlet pipe is used to connect the corresponding reaction tank to the external gas source.

3. The pre-treatment device of claim 2, wherein, The pre-treatment device further comprises at least one control tank which is arranged on the heating plate and connected to the empty bottle through the third connecting pipe. Each control tank is provided with a first control cover hole for connecting to the external gas source and adding reactants.

4. The pre-treatment device of claim 3, wherein Each control tank is provided with a second gas inlet pipe which is used to connect the corresponding control tank to the external gas source. The second gas inlet pipe is plug-connected with the first control cover hole.

5. The pre-treatment device according to claim 4, characterized in that The pre-treatment device further comprises a first pipe joint which is provided with a gas inlet port corresponding to the external gas source and a gas outlet port corresponding to each reaction tank and each control tank. The external gas source is connected to the gas inlet port of the first pipe joint. Each reaction tank is connected to the gas outlet port of the corresponding first pipe joint through the corresponding first gas inlet pipe. Each control tank is connected to the gas outlet port of the corresponding first pipe joint through the corresponding second gas inlet pipe.

6. The pre-treatment device of claim 3, wherein The pre-treatment device further comprises a second pipe joint which is provided with a gas inlet port corresponding to each reaction tank and each control tank and a gas outlet port corresponding to the empty bottle. Each reaction tank is connected to the gas inlet port of the corresponding second pipe joint through the corresponding first connecting pipe. Each control tank is connected to the gas inlet port of the corresponding second pipe joint through the corresponding third connecting pipe. The empty bottle is connected to the gas outlet port of the second pipe joint through the fourth connecting pipe.

7. An apparatus for detecting metal impurities in an iodosilane, characterized by: The detection equipment comprises the pre-treatment device according to any one of claims 1 to 6.

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