Sample pretreatment auxiliary device for detecting metal impurity ions in trichlorosilane
By using auxiliary devices such as a reaction vessel and a shaking unit, the sample pretreatment process for metal impurity ions in trichlorosilane is simplified, solving the problems of impurity introduction and loss, and achieving more efficient sample pretreatment and detection accuracy.
Patent Information
- Application Number
- CN202423027357.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-09
- Publication Date
- 2025-11-18
- Estimated Expiration
- 2034-12-09
AI Technical Summary
Existing technologies for detecting metal impurity ions in trichlorosilanes are prone to introducing and losing impurities during sample pretreatment, are time-consuming and have poor accuracy, and suffer from matrix effects and elemental interference.
An auxiliary device consisting of a reaction vessel and a shaking unit is used. The shaking mechanism drives the vessel to move up and down, and combined with ice freezing, hydrolysis reaction and hydrofluoric acid dissolution, H2SiF6 is generated to volatilize metal impurities, simplifying the sample pretreatment procedure.
It improves the efficiency of sample pretreatment, reduces the possibility of impurity introduction, shortens processing time, and improves detection accuracy.
Smart Images
Figure CN223565371U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to polycrystal silicon production technical field especially relates to a kind of metal impurity ion detection sample pre-treatment auxiliary device in trichlorosilane. BACKGROUND
[0002] In the production process of polycrystalline silicon, SiHCl3 (trichlorosilane) impurity metal ion detection is important to ensure the quality of polycrystalline silicon products, and the traditional detection mainly includes two steps: sample pretreatment (silicon evaporation) and sample detection. First, trichlorosilane is added to a clean crucible, and then an appropriate amount of complexing agent and water are added to generate silicon dioxide. Then, hydrofluoric acid is added to dissolve the silicon dioxide, and the mixture is placed in a graphite furnace and dried using an electric heating plate. The residue is dissolved in nitric acid and diluted with ultrapure water. Finally, the impurity elements are quantitatively analyzed using inductively coupled plasma optical emission spectrometry (ICP-OES) (external standard method). However, trichlorosilane samples are prone to introduce impurities during the pretreatment process, and impurities are also prone to be lost during the silicon evaporation process. The entire process is time-consuming, and the sample analysis has many impurity elements with low content, obvious matrix effect, and mutual interference between impurity elements. The process is complex, time-consuming, and inaccurate. SUMMARY
[0003] Therefore, the utility model provides a kind of metal impurity ion detection sample pre-treatment auxiliary device in trichlorosilane, and the main purpose is to simplify the sample pretreatment procedure of metal ion detection analysis.
[0004] To achieve the above-mentioned purpose, the utility model mainly provides the following technical scheme:
[0005] The utility model provides a kind of metal impurity ion detection sample pre-treatment auxiliary device in trichlorosilane, and the device includes: reaction kettle and shake even department;
[0006] The reaction kettle includes kettle body and cover body, the cover body is detachably connected to the upper end of the kettle body, the cover body is provided with sample inlet and exhaust port, and the exhaust port is connected to gas collection bottle;
[0007] The shake even department includes two shake even mechanisms, and the two shake even mechanisms are symmetrically arranged on the opposite sides of the kettle body. Each shake even mechanism includes a disc, a horizontal slot body and a reciprocating rod. The center of the disc is rotatably connected to the bracket on the side of the kettle body. The edge of the disc is fixedly connected to a toggle lever. The toggle lever is slidably arranged in the horizontal slot body. The middle part of the horizontal slot body is fixedly connected to the upper end of the reciprocating rod. The reciprocating rod is slidably connected to the bracket. The central axis of the reciprocating rod and the central axis of the disc are perpendicular to each other. The shaft side of the reciprocating rod is connected to the kettle body.
[0008] The technical solutions of the utility model can further realize the purposes and solve the technical problems.
[0009] Optionally, the bracket is fixedly connected to the base.
[0010] Optionally, the constant-temperature water bath box is connected to the upper surface of the base through a lifting air cylinder.
[0011] Optionally, opposite side walls of the kettle body are fixedly connected to ear plates respectively, the shaft side of the reciprocating rod is fixedly connected to a bearing plate, the ear plates are provided with first limiting holes, the bearing plate is provided with second limiting holes, the first limiting holes and the second limiting holes correspond to each other and are used for penetrating and positioning bolts.
[0012] Optionally, the pressure gauge is connected to the cover body.
[0013] By means of the above technical solutions, the utility model has at least the following advantages:
[0014] The kettle body is placed in the constant-temperature water bath box, the trichlorosilane is hydrolyzed, the discs of the two shaking mechanisms are started, the discs rotate, the toggle levers slide in the transverse grooves, the transverse grooves and the reciprocating rods move up and down reciprocatingly, and the kettle body moves up and down, so that the trichlorosilane in the kettle body is hydrolyzed sufficiently to generate silicon dioxide.
[0015] Then, the sample inlet valve is opened, 15ml of hydrofluoric acid (excessive hydrofluoric acid) is added into the kettle body from the sample inlet by using a syringe, the sample inlet valve is closed, the discs of the two shaking mechanisms are started again, the discs rotate, the toggle levers slide in the transverse grooves, the transverse grooves and the reciprocating rods move up and down reciprocatingly, and the kettle body moves up and down, so that the HF is dissolved in SiO2 sufficiently, H2SiF6 is generated in the solution, under the acidic environment in the reaction kettle, metal impurities do not react, and H2SiF6 volatilizes, so that the purpose of silicon evaporation (silicon evaporation) is achieved.
[0016] After the above process is completed, the solution in the kettle body is poured into a 100ml volumetric flask, the inner wall of the kettle body is washed clean with pure water and poured into the 100ml volumetric flask, and then the 100ml volumetric flask is diluted to 100ml with pure water, so that subsequent inductively coupled plasma optical emission spectrometry (ICP-OES) can be used to quantitatively analyze impurity elements. BRIEF DESCRIPTION OF DRAWINGS
[0017] Figure 1The utility model discloses a kind of metal impurity ion detection sample pretreatment auxiliary device in trichlorosilane for the structure schematic diagram of the embodiment of the utility model provides.
[0018] Figure 2 It is the structure schematic diagram of the shaking mechanism.
[0019] The reference signs in the drawings of the specification include: kettle body 1, cover body 2, sample inlet 3, exhaust port 4, gas collecting bottle 5, disc 6, transverse groove body 7, reciprocating rod 8, support 9, toggle lever 10, base 11, constant temperature water bath 12, lifting cylinder 13, ear plate 14, bearing plate 15, bolt 16, pressure gauge 17. DETAILED DESCRIPTION
[0020] To further illustrate the technical means and effects adopted by the utility model to achieve the predetermined utility model purposes, the following will be combined with drawings and preferred embodiments to specifically describe the specific implementation, structure, features and effects according to the utility model application as follows. In the following description, different "an embodiment" or "embodiments" do not necessarily refer to the same embodiment. In addition, specific features, structures or characteristics in one or more embodiments can be combined in any suitable form.
[0021] The utility model will be further described in detail in combination with the drawings and embodiments.
[0022] As shown in Figure 1 and Figure 2 An embodiment of the utility model provides a kind of metal impurity ion detection sample pretreatment auxiliary device in trichlorosilane, it includes: reaction kettle and shake even department;
[0023] The reaction kettle includes kettle body 1 and cover body 2, the cover body 2 can be detachably connected to the upper end of the kettle body 1, the cover body 2 is equipped with sample inlet 3 and exhaust port 4, the exhaust port 4 is connected to gas collecting bottle 5;
[0024] The shake even department includes two shaking mechanisms, two the shaking mechanism is symmetrically set on the opposite side of the kettle body 1, and each shaking mechanism includes disc 6, transverse groove body 7 and reciprocating rod 8, the center of the disc 6 is rotatably connected to the support 9 on the side of the kettle body 1, the edge of the disc 6 is fixedly connected to toggle lever 10, the toggle lever 10 is slidably arranged in the transverse groove body 7, the middle part of the transverse groove body 7 is fixedly connected to the upper end of the reciprocating rod 8, the reciprocating rod 8 is slidably connected to the support 9, the central axis of the reciprocating rod 8 and the central axis of the disc 6 are perpendicular to intersect, and the shaft side of the reciprocating rod 8 is connected to the kettle body 1.
[0025] The working process of a kind of metal impurity ion detection sample pretreatment auxiliary device in trichlorosilane is as follows:
[0026] Add ice cubes in the kettle body 1, place in the refrigerator for 20 minutes, then take 5ml of trichlorosilane into the kettle body 1, then tightly cover the kettle body 1 with the cover body 2, place the kettle body 1 in the constant temperature water bath box 12, start the two disc-shaped discs 6 of the two uniform mechanisms, the disc-shaped discs 6 rotate, the driving rods 10 slide in the transverse groove bodies 7, the transverse groove bodies 7 and the reciprocating rods 8 reciprocate up and down, thereby driving the kettle body 1 to move up and down, so that the trichlorosilane in the kettle body 1 can be fully hydrolyzed to generate silicon dioxide.
[0027] Then open the valve of the sample inlet 3, use a syringe to add 15ml of hydrofluoric acid (excessive hydrofluoric acid) into the kettle body 1 from the sample inlet 3, close the valve of the sample inlet 3, start the two disc-shaped discs 6 of the two uniform mechanisms again, the disc-shaped discs 6 rotate, the driving rods 10 slide in the transverse groove bodies 7, the transverse groove bodies 7 and the reciprocating rods 8 reciprocate up and down, thereby driving the kettle body 1 to move up and down, so that the HF can be fully dissolved in the SiO2, H2SiF6 is generated in the solution, under the acidic environment in the reaction kettle, metal impurities will not react, and H2SiF6 will volatilize, so that the purpose of silicon volatilization (silicon volatilization) is achieved.
[0028] After the above process is completed, pour the solution in the kettle body 1 into a 100ml volumetric flask, wash the inner wall of the kettle body 1 with pure water, pour the pure water into the 100ml volumetric flask, and then dilute to 100ml with pure water, so as to facilitate subsequent inductively coupled plasma optical emission spectrometry (ICP-OES) for quantitative analysis of impurity elements.
[0029] In the technical scheme of the utility model, the device is used, in the reaction process, the reaction kettle moves up and down, the solution in the kettle body 1 is fully mixed and reacted, the sample pretreatment program of metal ion detection and analysis is simplified, the possibility of introducing impurities is reduced, and the sample pretreatment time is shortened.
[0030] Specifically, the cover body 2 is threadedly connected to the upper end of the kettle body 1.
[0031] In the specific embodiment, a base 11 is further included, and the support 9 is fixedly connected to the base 11.
[0032] In the embodiment, specifically, the lower end of the support 9 is fixedly connected to the base 11, the driving motor is fixedly installed on the upper end of the support 9 through foundation bolts, the output shaft of the driving motor is fixedly connected to the center of the disc-shaped disc 6, the reaction kettle is arranged between the two uniform mechanisms, and the base 11 provides stable support for the up-and-down movement of the reaction kettle.
[0033] Specifically, the two supports 9 on the two sides of the reaction kettle are a first support and a second support, one of the two driving motors is installed at the upper end of the first support, and the other driving motor is installed at the upper end of the second support; the remote controller is further provided, two frequency converters are arranged in the remote controller, one of the two frequency converters is electrically connected to one of the driving motors, and the other frequency converter is electrically connected to the other driving motor, the synchronous control mode of the two driving motors is that one is a master drive and the other is a slave drive, so as to control the synchronous rotation of the two disc-shaped bodies 6, and thus the synchronous up-down reciprocating movement of the two reciprocating rods 8 is controlled, so as to ensure the stable up-down movement of the reaction kettle.
[0034] In the specific embodiment, the thermostatic water bath 12 is connected to the upper surface of the base 11 through the lifting cylinder 13.
[0035] In the specific embodiment, when the device is used, the piston rod of the lifting cylinder 13 is retracted, so that the position of the thermostatic water bath 12 is lower than the lower end of the up-down movement track of the reaction kettle, and thus the positional relationship between the thermostatic water bath 12 and the reaction kettle is adjusted.
[0036] Specifically, the cylinder body of the lifting cylinder 13 is fixed to the base 11, and the thermostatic water bath 12 is placed on the upper end of the piston rod of the lifting cylinder 13.
[0037] In the specific embodiment, the opposite side walls of the kettle body 1 are fixedly connected to the ear plates 14, the shaft side of the reciprocating rod 8 is fixedly connected to the bearing plate 15, the ear plate 14 is provided with a first limiting hole, the bearing plate 15 is provided with a second limiting hole, the first limiting hole and the second limiting hole correspond to each other, and are used for penetrating and positioning the positioning bolt 16, and the bolt 16 is connected to the nut.
[0038] In the specific embodiment, the positioning bolt 16 penetrates the first limiting hole and the second limiting hole, so as to fix the relative positions of the ear plate 14 and the bearing plate 15, and facilitate the release of the positional relationship between the ear plate 14 and the bearing plate 15.
[0039] In the specific embodiment, the pressure gauge 17 is further provided, and the pressure gauge 17 is connected to the cover body 2.
[0040] In the specific embodiment, the operator can observe the indication of the pressure gauge 17 to determine the reaction degree in the reaction kettle.
[0041] The above merely describes the specific embodiments of the present application, but the protection scope of the present application is not limited to this. Any person skilled in the art can easily think of changes or replacements within the technical range disclosed by the present application, which should be covered in the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.
Claims
1. A sample pretreatment auxiliary device for detecting metal impurity ions in trichlorosilane, characterized in that, The utility model relates to a three-chlorosilane metal impurity ion detection sample pretreatment auxiliary device which comprises a reaction kettle, a shaking part and a base.
2. The three-chlorosilane metal impurity ion detection sample pretreatment auxiliary device according to claim 1, further comprising a base, wherein the bracket is fixedly connected to the base.
3. The three-chlorosilane metal impurity ion detection sample pretreatment auxiliary device according to claim 2, further comprising a constant-temperature water bath box, wherein the constant-temperature water bath box is connected to the upper surface of the base through a lifting cylinder.
4. The three-chlorosilane metal impurity ion detection sample pretreatment auxiliary device according to claim 1, wherein the opposite sidewalls of the kettle body are respectively fixedly connected to ear plates, the shaft side of the reciprocating rod is fixedly connected to a bearing plate, the ear plates are provided with first limiting holes, the bearing plate is provided with second limiting holes, and the first limiting holes and the second limiting holes correspond to each other and are used for inserting positioning bolts.
5. The three-chlorosilane metal impurity ion detection sample pretreatment auxiliary device according to any one of claims 1 to 4, further comprising a pressure gauge, wherein the pressure gauge is connected to the cover body.