CN219496246U - Solid material's metal ion separates out content testing arrangement - Google Patents
Solid material's metal ion separates out content testing arrangement Download PDFInfo
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- CN219496246U CN219496246U CN202223591748.2U CN202223591748U CN219496246U CN 219496246 U CN219496246 U CN 219496246U CN 202223591748 U CN202223591748 U CN 202223591748U CN 219496246 U CN219496246 U CN 219496246U
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Abstract
The utility model discloses a device for testing the content of precipitated metal ions of a solid material, which is characterized in that: the device comprises a sample processing chamber, wherein a processing cavity is arranged in the sample processing chamber, and a sample placing position is arranged in the processing cavity; the top of the sample processing chamber is provided with a gaseous chemical fluid inlet and an exhaust port which are communicated with the processing cavity, and the gaseous chemical fluid inlet is opposite to the sample placing position. The utility model improves the testing efficiency, the testing sensitivity and the testing quality and reduces the testing cost.
Description
Technical Field
The utility model relates to the field of semiconductor production and processing, in particular to a device for testing the metal ion precipitation content of a solid material.
Background
Semiconductor processing is classified into dry and wet processes. Among them, in wet facilities, most require the use of acidic solutions or acidic gases, such as hydrofluoric acid. Acid-resistant materials used in the equipment, such as PFA and other materials, need to be cleaned, and the content precipitation condition of impurities (metal ions) is verified, so that the use quality of wet equipment is ensured.
In the prior art, a material to be tested is put into wet equipment and used in a chemical solution with known weight, then the concentration of impurities in the chemical solution is measured, and the precipitation content of a sample is calculated. For articles with larger volumes of material, more chemical solution is required. The concentration of the content of the precipitated impurities is reduced due to the increase of the amount of the chemical solution, namely, the concentration of the impurities is equivalent to that of the impurities which are diluted, so that the detection difficulty of metal ions in the impurities is higher, the amount of the chemical solution is also larger, and the cost is high.
Disclosure of Invention
The utility model aims to provide a device for testing the metal ion precipitation content of a solid material, which can improve the testing convenience, reduce the testing cost, improve the detection sensitivity and improve the testing precision.
In order to achieve the above purpose, the utility model adopts the following technical scheme: the device for testing the metal ion precipitation content of the solid material comprises a sample processing chamber, wherein a processing cavity is arranged in the sample processing chamber, and a sample placing position is arranged in the processing cavity;
the top of the sample processing chamber is provided with a gaseous chemical fluid inlet and an exhaust port which are communicated with the processing cavity, and the gaseous chemical fluid inlet is opposite to the sample placing position.
In the above technical solution, a first pipeline is installed on the gaseous chemical fluid inlet, an inner end of the first pipeline is inserted into the processing cavity, and an outer end of the pipeline is disposed outside the sample processing chamber and is connected with the gaseous chemical fluid providing device; the inner end of the first pipeline is detachably provided with a connecting disc, a plurality of groups of air outlet holes are formed in the connecting disc, and the air outlet holes are right opposite to the sample placing positions.
In the above technical solution, the gaseous chemical fluid supply device includes a vapor bottle, in which a chemical liquid is loaded, and a heating pad for heating the chemical liquid into a hot gaseous chemical fluid is provided outside the vapor bottle; the steam bottle is internally provided with an air inlet and an air outlet, the air inlet is connected with a first air inlet pipe, the inner end of the first air inlet pipe is inserted into the chemical liquid, and the outer end of the first air inlet pipe is arranged outside the steam bottle and is connected with a nitrogen source; the outer end of the first pipeline is connected with the air outlet, and the outer end of the first pipeline is arranged above the liquid level of the chemical liquid.
In the above technical solution, the top of the processing chamber is communicated with the top of the sample processing chamber, and a cover plate is arranged on the top of the sample processing chamber, and seals the top of the processing chamber; the gaseous chemical fluid inlet and the exhaust port are arranged on the cover plate.
In the above technical scheme, the exhaust port is connected with an exhaust pipe, the inner end of the exhaust pipe is inserted into the processing cavity, and the outer end of the exhaust pipe is arranged outside the sample processing cavity and is connected with an exhaust gas processing device; the inner end of the exhaust pipe is close to the bottom of the processing cavity, and the exhaust pipe is arranged beside the sample placing position.
In the above technical scheme, a hollow-out structure of the partition plate is arranged in the processing cavity, the partition plate divides the processing cavity into an upper cavity and a lower cavity which are mutually communicated, and the sample placing position is arranged in the upper cavity.
In the above technical scheme, a liquid outlet is arranged on the side wall of the bottom of the sample processing chamber, the liquid outlet is communicated with the bottom of the lower chamber, and a valve is arranged on the liquid outlet.
The utility model also provides a method for testing the metal ion precipitation content of the solid material, which comprises the following steps:
(1) placing a sample on a sample placement site of a process chamber;
(2) introducing gaseous chemical fluid into the treatment cavity through the gaseous chemical fluid inlet, contacting the gaseous chemical fluid with the surface of the sample, and simultaneously opening the waste gas treatment equipment to pump the waste gas reacted with the sample and the gaseous chemical fluid out through the exhaust port, wherein metal ions in the sample react with the gaseous chemical fluid and are separated out to the surface of the sample;
(3) after the duration of 5 minutes to 300 minutes in the step (2), stopping the feeding of the gaseous chemical fluid into the treatment cavity, and closing the waste gas treatment equipment;
(4) opening a cover plate at the top of the sample treatment chamber, flushing the sample with a small amount of cleaning liquid, wherein the cleaning liquid after flushing enters the bottom of the treatment cavity;
(5) and taking out all the solutions in the treatment cavity, weighing, and measuring the concentration of metal ions in the solutions to calculate the precipitation content of the metal ions.
In the above technical solution, after the gaseous chemical fluid contacts with the sample, a part of the gaseous chemical fluid is liquefied into a liquid chemical fluid, and flows into the bottom of the processing chamber.
In the above technical scheme, the cleaning solution adopts extracting solution, pure water or other liquid chemical fluid.
Due to the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
1. in the utility model, a product is directly placed in a processing cavity of a sample processing chamber, gaseous chemical fluid is fed through a gaseous chemical fluid inlet, the gaseous chemical fluid is contacted with the product, the gaseous chemical fluid is contacted with the sample surface, metal ions on the sample surface are precipitated and adhered to the sample surface, the condensed chemical fluid on the sample surface is taken away, and the sample surface is washed away by a subsequent washing liquid, the condensed chemical fluid and the washing liquid are collected, weighed, and then the metal ion content in the solution is detected, so that a large volume of sample can be detected by using the minimum chemical fluid, the consumption of the chemical fluid can be reduced, the cost is reduced, and meanwhile, the concentration of the metal ions in the solution can be improved, the detection sensitivity can be improved, and the detection limit is reduced;
2. according to the utility model, different chemical fluids can be adopted, and the corresponding chemical fluids can be selected according to the solution required by wet equipment, so that the application range is wide;
3. according to the utility model, the hollowed-out partition plate is arranged in the processing cavity, so that the sample can be supported, meanwhile, the condensed chemical fluid flows into the lower part of the partition plate, the cleaning fluid used for cleaning the surface of the sample also flows into the lower part of the partition plate, and then the cleaning fluid is discharged through the liquid outlet, so that the collection efficiency and convenience of the solution can be improved.
Drawings
FIG. 1 is a schematic view of a first embodiment of the present utility model;
FIG. 2 is a schematic diagram of the bottom structure of a connecting disc according to the first embodiment of the present utility model;
fig. 3 is a schematic end view of a separator according to an embodiment of the present utility model.
Wherein: 1. a sample processing chamber; 2. a processing chamber; 3. a sample placement site; 4. a gaseous chemical fluid inlet; 5. an exhaust port; 6. a sample; 7. a first pipeline; 8. a gaseous chemical fluid supply means; 9. a connecting disc; 10. an air outlet hole; 11. a steam bottle; 12. a chemical liquid; 13. a heating pad; 14. an air inlet; 15. an air outlet; 16. a first air inlet pipe; 17. a nitrogen source; 18. a cover plate; 19. an exhaust pipe; 20. an exhaust gas treatment device; 21. a partition plate; 22. an upper chamber; 23. a lower chamber; 24. a liquid outlet; 25. and (3) a valve.
Detailed Description
The utility model is further described below with reference to the accompanying drawings and examples:
embodiment one: referring to fig. 1 to 3, a device for testing the metal ion precipitation content of a solid material comprises a sample processing chamber 1, wherein a processing cavity 2 is arranged in the sample processing chamber, and a sample placing position 3 is arranged in the processing cavity;
the top of the sample processing chamber is provided with a gaseous chemical fluid inlet 4 and an exhaust port 5 which are communicated with the processing cavity, and the gaseous chemical fluid inlet is arranged opposite to the sample placing position.
In the utility model, in actual use, a large volume of sample 6 is directly placed on a sample placing position, then hot gaseous chemical fluid is fed through a gaseous chemical fluid inlet, the gaseous chemical fluid is directly contacted with the surface of the sample, metal ions possibly existing in the sample are separated out and can be separated out on the surface of the sample after the sample is contacted with the gaseous chemical fluid, a certain amount of cleaning liquid is poured into the sample to clean the surface of the sample, the metal ions on the surface of the sample are taken away, and then the content of the metal ions in the cleaning liquid is measured. Meanwhile, the utility model has wide application range and is suitable for large-volume samples.
The utility model also provides a method for testing the metal ion precipitation content of the solid material, which comprises the following steps:
(1) placing a sample on a sample placement site of a process chamber; in this embodiment, the sample is a sample made of PFA material;
(2) introducing gaseous chemical fluid into the treatment cavity through the gaseous chemical fluid inlet, contacting the gaseous chemical fluid with the surface of the sample, and simultaneously opening the waste gas treatment equipment to pump the waste gas reacted with the sample and the gaseous chemical fluid out through the exhaust port, wherein part of the gaseous chemical fluid is condensed into liquid chemical fluid and flows downwards to the bottom of the treatment cavity, metal ions in the sample react with the gaseous chemical fluid and are separated out to the surface of the sample, and part of the metal ions are mixed into the liquid chemical fluid and flow to the bottom of the treatment cavity together;
(3) after the duration of 5 minutes to 300 minutes in the step (2), stopping the feeding of the gaseous chemical fluid into the treatment cavity, and closing the waste gas treatment equipment;
(4) opening a cover plate at the top of the sample treatment chamber, flushing the sample with a small amount of cleaning liquid, wherein the cleaning liquid after flushing enters the bottom of the treatment cavity;
(5) taking out the mixed solution composed of the condensed liquid chemical fluid and the cleaning liquid in the sample processing chamber, weighing, and measuring the concentration of metal ions in the mixed solution by ICP-MS to calculate the content of precipitated metal ions. The concentration of metal ions is measured by measuring the weight of the mixed solution, and then dividing the mixed solution by the surface area of the sample, namely the content of metal ions precipitated from the sample in unit area. According to the metal ion content, data comparison is performed to see whether the metal ion content is within a specified range.
After the gaseous chemical fluid is contacted with the sample, the metal ions deposited on the sample may be on the surface of the sample, mixed in the condensed liquid chemical fluid, or mixed into a cleaning fluid.
Wherein the cleaning liquid can be an extracting solution, pure water or other liquid chemical fluid. The liquid and gaseous chemical fluids are preferably of uniform product, with one being gaseous and the other being liquid.
Referring to fig. 1, a first pipeline 7 is installed on the gaseous chemical fluid inlet, the inner end of the first pipeline is inserted into the processing cavity, and the outer end of the first pipeline is arranged outside the sample processing chamber and is connected with a gaseous chemical fluid supply device 8; the inner end of the first pipeline is detachably provided with a connecting disc 9, a plurality of groups of air outlet holes 10 are formed in the connecting disc, and the air outlet holes are opposite to the sample placing positions.
In this embodiment, through the setting of connection pad to set up multiunit venthole above the connection pad, gaseous state chemical fluid is sent into the processing chamber through first pipeline like this, can be sent out from multiunit venthole, directly spray on the surface of sample, multiunit venthole's setting for increase gaseous state chemical fluid and sample's area of contact, improve metal ion and separate out efficiency, reduce the quantity of chemical fluid like this as far as, reduce cost. And connection pad and first pipeline can dismantle the connection, can change the venthole of different width, different quantity according to the area of sample for be applicable to the sample of different volumes, improve application scope.
Referring to fig. 1, the gaseous chemical fluid supply apparatus includes a vapor bottle 11 in which a liquid chemical liquid 12 is contained, the vapor bottle having a heating pad 13 on the outside thereof for heating the liquid chemical liquid into a hot gaseous chemical fluid; the steam bottle is internally provided with an air inlet 14 and an air outlet 15, a first air inlet pipe 16 is connected to the air inlet, the inner end of the first air inlet pipe is inserted into the chemical liquid, and the outer end of the first air inlet pipe is arranged outside the steam bottle and is connected with a nitrogen source 17; the outer end of the first pipeline is connected with the air outlet, and the outer end of the first pipeline is arranged above the liquid level of the chemical liquid. In this embodiment, nitrogen enters the hot chemical liquid, and then carries out part of the hot chemical liquid to mix into the nitrogen, so as to form a hot gaseous chemical fluid.
In this embodiment, taking hydrofluoric acid as an example, a chemical fluid is added into a steam bottle, the chemical fluid is heated by a heating pad to become hot hydrofluoric acid steam, then a nitrogen source provides conveying pressure for the hydrofluoric acid steam, the hot hydrofluoric acid steam is driven to pass through an air outlet and then is sent into a processing cavity through a first pipeline, and the conveying flow and speed of the hydrofluoric acid steam are further regulated by regulating the nitrogen output flow and speed of the nitrogen source, so that the reaction is performed at a speed most suitable for separating out metal ions of a sample, the use amount of the chemical fluid is reduced, and the use cost is reduced. And the same is true. The heating temperature of the heating pad is matched with the nitrogen conveying amount of the nitrogen source, the conveying amount of hydrofluoric acid steam is also matched as much as possible each time, and the using amount of hydrofluoric acid is reduced.
Referring to FIG. 1, the top of the processing chamber is in communication with the top of the sample processing chamber, which is provided with a cover plate 18 that seals the top of the processing chamber; the gaseous chemical fluid inlet and the exhaust port are arranged on the cover plate.
When the cleaning liquid is required to be poured onto the surface of the sample and the sample is taken and placed, the cover plate is opened, the treatment cavity is completely opened, and when the metal ions on the surface of the sample are required to be separated out, the cover plate is closed, so that the inside of the treatment cavity is sealed, and the gaseous chemical fluid cannot be exposed and can be discharged only through the exhaust port.
Wherein, the exhaust port is connected with an exhaust pipe 19, the inner end of the exhaust pipe is inserted into the processing cavity, and the outer end of the exhaust pipe is arranged outside the sample processing cavity and is connected with an exhaust gas processing device 20; the inner end of the exhaust pipe is close to the bottom of the processing cavity, and the exhaust pipe is arranged beside the sample placing position.
Through the setting of blast pipe to blast pipe and exhaust-gas treatment equipment connect, can give the processing chamber like this and export, also can make gaseous chemical fluid can be smooth enter into the processing intracavity for the atmospheric pressure in the processing chamber balances, and exhaust-gas treatment equipment then can give the absorption with gaseous chemical fluid and the produced waste gas of sample reaction and handle, prevents the pollution of air, more environmental protection. Furthermore, a one-way valve can be arranged on the exhaust port, so that the exhaust pipe can only exhaust air and cannot enter air, and other mediums are prevented from interfering with the testing precision and quality.
Referring to fig. 1 and 3, a hollow-out partition 21 is disposed in the processing chamber, the partition divides the processing chamber into an upper chamber 22 and a lower chamber 23 that are mutually communicated, the sample placement position is disposed in the upper chamber, and the gaseous chemical fluid inlet and the gas outlet are both directly communicated with the upper chamber. The inner end of the exhaust pipe is close to the top surface of the partition board and is arranged beside the sample, and the contact reaction of the gaseous chemical fluid and the sample is not affected. And the gaseous chemical fluid is not directly sucked away.
In this embodiment, after the gaseous chemical fluid enters the processing cavity and contacts with the sample, most of the gaseous chemical fluid is extracted and discharged through the exhaust port, and part of the gaseous chemical fluid is directly condensed into liquid chemical fluid (for example, hydrofluoric acid vapor is adopted, which belongs to hot vapor and is condensed into liquid after contacting with the sample), so that part of metal ions separated out from the surface of the sample can be directly taken away by the condensed liquid chemical fluid, the heavy metal ions automatically drop down to the bottom of the processing cavity, the liquid solution is located in the lower cavity, and the solution mixed with the metal ions also directly falls into the lower cavity when the cleaning solution or the liquid chemical fluid is subsequently utilized to clean the surface of the sample, so that the solution in the lower cavity is taken out, the interference of the sample is avoided, the convenience of solution taking out is improved, and the detection sensitivity and quality are ensured.
Referring to fig. 1, a drain port 24 is provided on the bottom side wall of the sample processing chamber, and is in communication with the bottom of the lower chamber, and a valve 25 is provided on the drain port.
Through the setting of leakage fluid dram and valve, after the surface metal ion washs the sample is accomplished, directly open the valve, collect the solution discharge in the cavity down through the leakage fluid dram, can carry out subsequent detection, improve the convenience of detection, reduce operating personnel intensity of labour. Furthermore, the bottom of the lower chamber can be set to be an inclined plane, and the liquid outlet is positioned at the bottom of the inclined plane, so that the solution can be conveniently discharged.
Claims (7)
1. The utility model provides a solid material's metal ion separates out content testing arrangement which characterized in that: the device comprises a sample processing chamber, wherein a processing cavity is arranged in the sample processing chamber, and a sample placing position is arranged in the processing cavity;
the top of the sample processing chamber is provided with a gaseous chemical fluid inlet and an exhaust port which are communicated with the processing cavity, and the gaseous chemical fluid inlet is opposite to the sample placing position.
2. The apparatus for measuring the metal ion precipitation content of a solid material according to claim 1, wherein: the gaseous chemical fluid inlet is provided with a first pipeline, the inner end of the first pipeline is inserted into the processing cavity, and the outer end of the pipeline is arranged outside the sample processing chamber and is connected with the gaseous chemical fluid supply device; the inner end of the first pipeline is detachably provided with a connecting disc, a plurality of groups of air outlet holes are formed in the connecting disc, and the air outlet holes are right opposite to the sample placing positions.
3. The apparatus for measuring the metal ion precipitation content of a solid material according to claim 2, wherein: the gaseous chemical fluid supply device comprises a steam bottle, wherein chemical liquid is loaded in the steam bottle, and a heating pad for heating the chemical liquid into hot gaseous chemical fluid is arranged outside the steam bottle; the steam bottle is internally provided with an air inlet and an air outlet, the air inlet is connected with a first air inlet pipe, the inner end of the first air inlet pipe is inserted into the chemical liquid, and the outer end of the first air inlet pipe is arranged outside the steam bottle and is connected with a nitrogen source; the outer end of the first pipeline is connected with the air outlet, and the outer end of the first pipeline is arranged above the liquid level of the chemical liquid.
4. The apparatus for measuring the metal ion precipitation content of a solid material according to claim 1, wherein: the top of the processing cavity is communicated with the top of the sample processing chamber, the top of the sample processing chamber is provided with a cover plate, and the cover plate seals the top of the processing cavity; the gaseous chemical fluid inlet and the exhaust port are arranged on the cover plate.
5. The apparatus for measuring the metal ion precipitation content of a solid material according to claim 1 or 4, wherein: the exhaust port is connected with an exhaust pipe, the inner end of the exhaust pipe is inserted into the processing cavity, and the outer end of the exhaust pipe is arranged outside the sample processing cavity and is connected with an exhaust gas treatment device; the inner end of the exhaust pipe is close to the bottom of the processing cavity, and the exhaust pipe is arranged beside the sample placing position.
6. The apparatus for measuring the metal ion precipitation content of a solid material according to claim 1, wherein: the processing cavity is internally provided with a partition board with a hollow structure, the partition board divides the processing cavity into an upper cavity and a lower cavity which are mutually communicated, and the sample placing position is arranged in the upper cavity.
7. The apparatus for measuring the metal ion precipitation content of a solid material according to claim 6, wherein: the bottom side wall of the sample processing chamber is provided with a liquid outlet which is communicated with the bottom of the lower chamber, and the liquid outlet is provided with a valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223591748.2U CN219496246U (en) | 2022-12-30 | 2022-12-30 | Solid material's metal ion separates out content testing arrangement |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223591748.2U CN219496246U (en) | 2022-12-30 | 2022-12-30 | Solid material's metal ion separates out content testing arrangement |
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| CN219496246U true CN219496246U (en) | 2023-08-08 |
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| CN202223591748.2U Active CN219496246U (en) | 2022-12-30 | 2022-12-30 | Solid material's metal ion separates out content testing arrangement |
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