CN114113039A - Detection method and detection device for high purity carbon - Google Patents
Detection method and detection device for high purity carbon Download PDFInfo
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Abstract
The invention discloses a method and a device for detecting the purity of high-purity carbon, wherein the high-purity carbon is placed in a tube furnace, firstly, purging is carried out through high-purity argon, then, high-purity oxygen is introduced, heating reaction is carried out, the residual ash and impurities are dissolved by adopting acid after being collected, and the impurity content is measured through ICP-MS; and absorbing the tail gas by alkali liquor, and measuring the sulfur content by ICP-OES so as to obtain the purity of the high-purity carbon. The device is simple, the method is convenient to operate, matrix elements of the high-purity carbon can be removed, matrix interference is removed, impurity elements are enriched, the detection limit of the analysis method is improved, the detection result is reliable, and the production of the high-purity carbon can be effectively guided.
Description
Technical Field
The invention belongs to a high-purity carbon analysis and detection technology, and particularly relates to a high-purity carbon purity detection method and a high-purity carbon purity detection device.
Background
The high-purity carbon has the characteristics of high strength, high density, high purity, high chemical stability, compact and uniform structure, high temperature resistance, high conductivity, good wear resistance, self lubrication, easy processing and the like, and is widely applied to the industrial fields of metallurgy, chemical industry, aerospace, electronics, machinery, nuclear energy and the like. Especially large-size high-quality high-purity graphite, as a substitute material, has wide application space in the fields of high technology and new technology, and has wide application prospect.
Silicon carbide (SiC), also called carborundum, has a density of 3.2g/cm 3, and natural silicon carbide is very rare and is mainly synthesized artificially. Silicon carbide can be classified into two broad categories, according to the different crystal structures: α SiC and β SiC.
The silicon carbide material has excellent thermodynamic and electrochemical properties.
Thermodynamically, silicon carbide has a hardness of up to 9.2-9.3 mohs at 20 ℃, which is one of the hardest substances and can be used for cutting ruby; the thermal conductivity is higher than that of metal copper, is 3 times that of Si and 8-10 times that of GaAs, has high thermal stability, and cannot be melted under normal pressure;
in the aspect of electrochemistry, the silicon carbide has the characteristics of wide forbidden band and breakdown resistance, the forbidden band width is 3 times of that of Si, and the breakdown electric field is 10 times of that of Si; and the corrosion resistance is extremely strong, and all known corrosive agents can be immunized at normal temperature.
In the silicon carbide semiconductor industry chain, the quality and performance of high-purity carbon which is an upstream key raw material determine the quality, size and defect density of devices and products, and the quality, size and defect density are the first problems to be solved in the development of silicon carbide technology. How to develop and produce high-purity raw material high-purity carbon for manufacturing silicon carbide single crystal has very important scientific significance and social value for rapidly improving product performance and industry competitiveness.
The development and production of high-purity silicon are mature at present, the high-purity silicon can be purified to be more than 9N, but the development and production of high-purity carbon are in a high-speed development stage. Since carbon is difficult to dissolve in acid and alkali, the content of impurity elements in high-purity carbon cannot be detected by a conventional method. It is a very meaningful task how to detect the content of impurity elements in high-purity carbon, and thus determine and help improve the quality of the high-purity carbon.
Disclosure of Invention
The invention aims to provide a method and a device for detecting the purity of high-purity carbon, wherein the high-purity carbon is changed into carbon dioxide to be removed, the impurity sulfur is changed into sulfur dioxide gas to be absorbed by alkali solution and then is measured by adopting ICP-OES, and the residual ash impurities are measured by adopting ICP-MS, so that the purity of the high-purity carbon is obtained.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-purity carbon purity detection method comprises the steps of placing high-purity carbon in a tube furnace, firstly purging through high-purity argon, then introducing high-purity oxygen, carrying out heating reaction, collecting residual ash impurities, dissolving with acid, and measuring the content of the impurities through ICP-MS; and absorbing the tail gas by alkali liquor, and measuring the sulfur content by ICP-OES so as to obtain the purity of the high-purity carbon.
Preferably, the purity of the high-purity argon is not lower than 6N, and the purity of the high-purity oxygen is not lower than 5N.
Preferably, the flow rate of the high-purity oxygen is 0.5 to 5 ml/min.
Preferably, the temperature of the heating reaction is 500-1100 ℃, and the time is 1-8 h.
Preferably, the acid is ultrapure nitric acid.
Preferably, the alkali liquor is a high-purity sodium hydroxide solution.
The invention also provides a device for detecting the purity of the high-purity carbon, which comprises:
the high-purity argon source is used for purging the tube furnace;
a high purity oxygen source for providing high purity oxygen for the reaction;
a tube furnace serving as a reaction device and collecting remaining ash impurities;
and the tail gas collecting system is used for absorbing the sulfur-containing tail gas.
Preferably, a control valve and a precise flowmeter are arranged on a connecting pipeline between the high-purity argon gas source or the high-purity oxygen gas source and the tube furnace and are used for precisely adjusting and controlling the flow of the high-purity argon gas or the high-purity oxygen gas.
Preferably, the inlet and outlet ends of the tube furnace are both provided with quartz furnace plugs, the quartz furnace plugs are two high-purity quartz plates which are connected with the hollow quartz tube and have the diameter of 0.625-0.875 time that of the tube furnace quartz tube, and the diameter of the hollow quartz tube is 2-8 mm. According to the invention, the quartz furnace plug can isolate heat generated by the tube furnace from being transferred to two ends, so that a sealing member of the tube furnace is prevented from being damaged, and meanwhile, introduced high-purity argon and high-purity oxygen can enter the quartz tube in a turbulent flow manner, so that the phenomenon that the flow velocity of gas is too high, ash impurities are taken away, and the impurity collection is influenced is avoided.
Preferably, the tail gas collecting system is provided with a condensing device, the condensing device can cool the sulfur-containing tail gas, and excessive alkaline collecting liquid is prevented from volatilizing after the sulfur-containing tail gas enters the tail gas collecting system due to too high temperature.
The invention has the advantages that:
the method comprises the steps of carrying out oxidation reaction on high-purity carbon and oxygen under a high-temperature environment to generate carbon dioxide gas, removing the carbon dioxide gas, wherein sulfur dioxide gas is formed by non-metallic elements and the oxygen and is absorbed by alkali liquor, measuring the sulfur content through ICP-OES, simultaneously dissolving the residual ash impurities after reaction by adopting acid, and measuring the impurity content through ICP-MS, thereby obtaining the purity of the high-purity carbon.
The device is simple, the method is convenient to operate, matrix elements of the high-purity carbon can be removed, matrix interference is removed, impurity elements are enriched, the detection limit of the analysis method is improved, the detection result is reliable, and the production of the high-purity carbon can be effectively guided.
Drawings
FIG. 1 is a schematic view showing the construction of an apparatus for measuring the purity of high purity carbon according to the present invention;
wherein: 1. high-purity argon gas source, 2 high-purity oxygen gas source, 3, tube furnace, 4, tail gas collecting system, 5, control valve, 6, precision flowmeter, 7, quartz furnace stopper, 71, hollow quartz tube, 72, high-purity quartz piece.
Detailed Description
As shown in fig. 1, the schematic structural diagram of the apparatus for detecting high purity carbon according to the present invention includes:
the high-purity argon source is used for purging the tube furnace;
a high purity oxygen source for providing high purity oxygen for the reaction;
a tube furnace serving as a reaction device and collecting remaining ash impurities;
and the tail gas collecting system is used for absorbing the sulfur-containing tail gas.
A control valve and a precise flowmeter are arranged on a connecting pipeline between the high-purity argon gas source or the high-purity oxygen gas source and the tubular furnace and are used for precisely adjusting and controlling the flow of the high-purity argon gas or the high-purity oxygen gas;
the inlet end and the outlet end of the tube furnace are both provided with quartz furnace plugs, the quartz furnace plugs are two high-purity quartz plates which are connected with a hollow quartz tube and have the diameter of 0.625-0.875 time that of the quartz tube of the tube furnace, and the diameter of the hollow quartz tube is 2-8 mm. According to the invention, the quartz furnace plug can isolate heat generated by the tube furnace from being transferred to two ends, so that a sealing member of the tube furnace is prevented from being damaged, and meanwhile, introduced high-purity argon and high-purity oxygen can enter the quartz tube in a turbulent flow manner, so that the phenomenon that the flow velocity of gas is too high, ash impurities are taken away, and the impurity collection is influenced is avoided.
The tail gas collecting system still has condensing equipment, and condensing equipment can cool off the tail gas that contains sulphur, avoids containing sulphur tail gas temperature too high to volatilize too much alkaline collecting fluid behind getting into the tail gas collecting system.
Example 1
A batch of 10.5232 g of high purity carbon samples was weighed into a high purity quartz boat (soaked with aqua regia, washed with pure water, and air dried before use) in a clean environment while performing a blank test (i.e., a test under the same conditions except that no sample was placed in the high purity quartz boat).
And opening the stainless steel flange at the end part of the tube furnace, taking out the quartz furnace plug, pushing the high-purity quartz boat containing the high-purity carbon sample into the heating area of the tube furnace, then putting the quartz furnace plug, and installing the stainless steel flange to close the tube furnace.
Connecting high-purity argon and high-purity oxygen by using a clean polytetrafluoroethylene pipe, connecting a control valve and a precision flowmeter in the middle, connecting a stainless steel flange, connecting a condensing device, pouring 10mL of 2% high-purity sodium hydroxide solution into a tail gas collecting system, and checking the air tightness.
And introducing high-purity argon, adjusting a precision flowmeter, exhausting air in the tubular furnace by using the high-purity argon, and closing the high-purity argon. Then high-purity oxygen is introduced, a precision flowmeter is adjusted, the flow is set to be 0.5mL/min, and the high-purity oxygen slowly and uniformly passes through a quartz tube of the tube furnace and is filled.
The heating area of the tube furnace is set at 750 ℃, and the heating is stopped after the high-purity carbon sample in the high-purity quartz boat is completely volatilized (the time is 6.5 hours).
Adding 2mL of ultrapure nitric acid into a high-purity quartz boat to dissolve residues in the high-purity quartz boat, adding an internal standard, fixing the volume to 100mL, uniformly mixing, measuring the contents of impurity elements Mg, Al, Fe, Ni, Zn, Cu and Pb by ICP-MS, deducting a blank (excluding the influence of a blank experiment), measuring the contents of impurity elements Ca and P by ICP-OES, and deducting the blank; the acidification of the liquid in the collection tube was followed by determination of the sulfur content on ICP-OES and the blank was subtracted, the results of which are shown in tables 1 and 2.
TABLE 1
TABLE 2
Meanwhile, the batch of high-purity carbon samples are detected by a third-party detection mechanism GD-MS (see other evidence documents), and the detection result is consistent with that of the method and reaches more than 6N.
Claims (10)
1. A method for detecting the purity of high-purity carbon is characterized by comprising the following steps: placing high-purity carbon in a tube furnace, firstly purging by high-purity argon, then introducing high-purity oxygen, heating for reaction, collecting residual ash impurities, dissolving by adopting acid, and measuring the impurity content by ICP-MS; and absorbing the tail gas by alkali liquor, and measuring the sulfur content by ICP-OES so as to obtain the purity of the high-purity carbon.
2. The method for detecting the purity of high purity carbon according to claim 1, characterized in that: the purity of the high-purity argon is not lower than 6N, and the purity of the high-purity oxygen is not lower than 5N.
3. The method for detecting the purity of high purity carbon according to claim 1, characterized in that: the flow rate of the high-purity oxygen is 0.5-5 ml/min.
4. The method for detecting the purity of high purity carbon according to claim 1, characterized in that: the temperature of the heating reaction is 500-1100 ℃, and the time is 1-8 h.
5. The method for detecting the purity of high purity carbon according to claim 1, characterized in that: the acid is ultrapure nitric acid.
6. The method for detecting the purity of high purity carbon according to claim 1, characterized in that: the alkali liquor is high-purity sodium hydroxide solution.
7. The detecting apparatus for detecting the purity of high-purity carbon according to any one of claims 1 to 6, comprising:
the high-purity argon source is used for purging the tube furnace;
a high purity oxygen source for providing high purity oxygen for the reaction;
a tube furnace serving as a reaction device and collecting remaining ash impurities;
and the tail gas collecting system is used for absorbing the sulfur-containing tail gas.
8. The detection device according to claim 7, wherein: and a control valve and a precision flowmeter are arranged on a connecting pipeline between the high-purity argon gas source or the high-purity oxygen gas source and the tube furnace.
9. The detection device according to claim 7, wherein: the quartz furnace plug is formed by connecting two high-purity quartz plates with the diameter being 0.625-0.875 time of that of the quartz tube of the tubular furnace, and the diameter of the hollow quartz tube is 2-8 mm.
10. The detection device according to claim 7, wherein: the tail gas collecting system is provided with a condensing device.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114777497A (en) * | 2022-03-18 | 2022-07-22 | 浙江万里学院 | Furnace tube for three-tube cooperation high-temperature-resistant high-vacuum tube furnace |
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| JP2015118083A (en) * | 2013-11-15 | 2015-06-25 | 株式会社住化分析センター | Sample preparation method, analytic method, and quality management method |
| CN109721056A (en) * | 2019-02-28 | 2019-05-07 | 扬州中天利新材料股份有限公司 | The method that depth removes impurity element in high-purity silicon carbide powder |
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| CN114777497A (en) * | 2022-03-18 | 2022-07-22 | 浙江万里学院 | Furnace tube for three-tube cooperation high-temperature-resistant high-vacuum tube furnace |
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