CN111912692A - Device and method for removing gallium from substrate - Google Patents
Device and method for removing gallium from substrate Download PDFInfo
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- CN111912692A CN111912692A CN202010686686.XA CN202010686686A CN111912692A CN 111912692 A CN111912692 A CN 111912692A CN 202010686686 A CN202010686686 A CN 202010686686A CN 111912692 A CN111912692 A CN 111912692A
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Abstract
The invention discloses a matrix gallium removing device and a method, wherein the device comprises a dry hydrogen chloride gas generating assembly, a gallium conversion gallium chloride generating assembly, a gallium chloride and excessive hydrogen chloride gas extracting assembly; the dry hydrogen chloride gas generating assembly comprises a constant-pressure dropping funnel, two bottles and a constant-temperature water bath; the gallium-to-gallium chloride generating component comprises a conical flask, a quartz reactor and a constant-temperature electric heating jacket; the gallium chloride and excessive hydrogen chloride gas pumping-out component comprises a three-way valve, a first gas washing bottle, a second gas washing bottle, a third gas washing bottle and a vacuum pump; the constant voltage dropping funnel is used for holding concentrated sulfuric acid, and two jars are used for holding sodium chloride, and quartz reactor is used for holding the assay, and the second gas washer is used for holding water, and the third gas washer is used for holding sodium hydroxide solution, and the tee bend valve is located on the pipeline between third gas washer and the vacuum pump. The invention can solve the problems of complex operation and long time consumption when the gallium of the matrix is removed in the prior art.
Description
Technical Field
The invention relates to the technical field of semiconductor material analysis, in particular to a matrix gallium removing device and method.
Background
The high-purity gallium mainly has four grades of 5N, 6N, 7N and 8N, and 6N and 7N are more on the market, and is a semiconductor raw material with wide application. Among them, 6N high purity gallium is mainly used in the field of optoelectronics, such as LED illumination and infrared detection; 7N high purity gallium is used primarily in the microelectronics field, such as integrated circuits and microwave devices. These products have different requirements on gallium purity, and therefore, the detection of gallium purity is particularly important.
The primary gallium often contains impurities such as Fe, Si, Pb, Zn, Sn, Mg, Cu, Mn, Cr, Ni, Na, Ca and the like, wherein the national standard requires that the total content (mass fraction) of the impurities in the 7N high-purity gallium is not more than 10 multiplied by 10-6Cu and Mn of not more than 0.2X 10, respectively-6And 0.3X 10-6All other impurities are not more than 0.6X 10-6。
At present, in a row standard method for detecting the purity of a high-purity gallium sample, a sample pretreatment process with complex operation and long time consumption is required, matrix gallium is removed to eliminate the interference of the matrix gallium, and then the impurity content is detected through inductively coupled plasma mass spectrometry (ICP-MS) or inductively coupled plasma spectroscopy (ICP-AES). For example, YS/T38.2-2009 and SJ 20713-1998, a sample is heated to be liquid at about 30 ℃, heated and dissolved by hydrochloric acid and nitric acid, and then extracted and separated from bulk gallium by isopropyl ether in a hydrochloric acid medium, wherein the method involves complicated operation processes such as acid expelling, extraction and the like; in YS/T474-. In the treatment process, the hydrogen chloride gas is slowly generated, and the reaction between the hydrogen chloride gas and the gallium is incomplete due to continuous negative pressure extraction, so that the separation time of the main gallium in the sample is long, and the treatment flow of a single sample (0.5g of high-purity gallium) needs hours.
Disclosure of Invention
The invention aims to provide a matrix gallium removing device and a matrix gallium removing method, which aim to solve the problems of complex operation and long time consumption in the prior art when removing matrix gallium.
A matrix gallium removing device comprises a dry hydrogen chloride gas generating assembly, a gallium conversion gallium chloride generating assembly, a gallium chloride and excessive hydrogen chloride gas extracting assembly;
the dry hydrogen chloride gas generating assembly comprises a constant-pressure dropping funnel, two bottles and a constant-temperature water bath;
the gallium-to-gallium chloride generating component comprises a conical flask, a quartz reactor and a constant-temperature electric heating jacket;
the gallium chloride and excessive hydrogen chloride gas pumping-out component comprises a three-way valve, a first gas washing bottle, a second gas washing bottle, a third gas washing bottle and a vacuum pump;
the constant-pressure dropping funnel is used for containing concentrated sulfuric acid, the two bottles are used for containing sodium chloride, and the two bottles are arranged in the constant-temperature water bath;
the quartz reactor is used for containing a test material, the quartz reactor is arranged in the conical flask, the conical flask is arranged in the constant-temperature electric heating sleeve, the second gas washing bottle is used for containing water, and the third gas washing bottle is used for containing a sodium hydroxide solution;
the first bottle mouth of the two-mouth bottle is connected with the constant-pressure dropping funnel;
the vacuum pump is characterized in that the second bottle openings of the two bottles, the conical bottle, the first gas washing bottle, the second gas washing bottle, the third gas washing bottle and the vacuum pump are sequentially connected through pipelines, the three-way valve is arranged on a pipeline between the third gas washing bottle and the vacuum pump, the first end of the three-way valve is connected with the vacuum pump through a pipeline, the second end of the three-way valve is connected with the third gas washing bottle through a pipeline, and the third end of the three-way valve is connected with the outside through a pipeline.
A matrix gallium removing method is applied to the matrix gallium removing device, and comprises the following steps:
weighing a test material and placing the test material in the quartz reactor, then placing the quartz reactor containing the test material in the conical flask, then placing the conical flask in the constant-temperature electric heating sleeve, starting the constant-temperature electric heating sleeve, and maintaining the temperature in the conical flask at a preset temperature;
rotating the three-way valve to enable a second end of the three-way valve to be communicated with a third end of the three-way valve, adding concentrated sulfuric acid into the constant-pressure dropping funnel, adding dry sodium chloride into the two-mouth bottle, and enabling a large amount of generated dry hydrogen chloride gas to enter the conical bottle through a pipeline, react with a test material in the quartz reactor to generate gallium trichloride and be discharged in a gas form;
discharging the generated gallium chloride and excessive hydrogen chloride gas out of the conical flask through a pipeline, and absorbing the gallium chloride and the excessive hydrogen chloride gas by water in the second gas washing bottle and a sodium hydroxide solution in the third gas washing bottle;
and rotating the three-way valves at intervals of a first preset time to seal the third ends of the three-way valves, communicating the first end of the three-way valve with the second end of the three-way valve, starting the vacuum pump, and pumping out the gallium chloride retained in the conical flask for a second preset time each time until the quartz reactor is dried.
According to the matrix gallium removing device and method provided by the invention, dry hydrogen chloride gas is prepared by a method of reacting concentrated sulfuric acid with sodium chloride, and then gallium chloride volatile gas generated by gallium treatment is extracted in times after the hydrogen chloride and the gallium are fully reacted for a period of time, so that the removal of the matrix gallium in a sample is realized, and the pretreatment process of the sample is simplified and speeded. The actual measurement shows that the method can finish the matrix gallium removal treatment of a single 0.5g sample in 20 minutes, the operation is simple, the treated sample is detected by ICP-MS, and the detection result is consistent with the GD-MS analysis result. The method is suitable for simultaneously measuring the contents of trace elements such as copper, lead, zinc, indium, iron, tin, nickel, magnesium, cobalt, chromium, manganese, iron, rubidium, molybdenum, bismuth and the like in high-purity gallium (99.999% < w (G a) < 99.99999%).
In addition, the method for removing the gallium from the matrix provided by the invention can also have the following additional technical characteristics:
further, to add concentrated sulfuric acid in the constant pressure dropping funnel, and to when adding dry sodium chloride solid in the two mouthfuls of bottles, the speed of controlling concentrated sulfuric acid to drip into sodium chloride is 3 ~ 4 seconds per drop.
Further, the preset temperature is 210-220 ℃.
Further, the first preset time is 5 minutes.
Further, the second preset time is 1 minute.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic structural diagram of a bulk gallium removal apparatus according to an embodiment of the invention.
Detailed Description
In order to make the objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. Several embodiments of the invention are presented in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," "up," "down," and the like are for illustrative purposes only and do not indicate or imply that the referenced device or element must be in a particular orientation, constructed or operated in a particular manner, and is not to be construed as limiting the present invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, a device for removing gallium from a substrate according to an embodiment of the present invention includes a dry hydrogen chloride gas generating assembly, a gallium-to-gallium chloride generating assembly, a gallium chloride-to-excess hydrogen chloride gas extracting assembly.
The dry hydrogen chloride gas generation assembly comprises a constant-pressure dropping funnel 11, a two-mouth bottle 12 and a constant-temperature water bath 13. Constant voltage dropping funnel 11 is used for holding concentrated sulfuric acid, two mouthfuls of bottles 12 are used for holding sodium chloride, two mouthfuls of bottles 12 are located in the constant temperature water bath 13, water bath temperature 40 ℃.
The gallium-to-gallium chloride generating assembly comprises a conical flask 21, a quartz reactor 22 and a constant-temperature electric heating jacket 23. The quartz reactor 22 is used for containing a sample, the quartz reactor 22 is arranged in the conical flask 21, and the conical flask 21 is arranged in the constant-temperature electric heating jacket 23.
The gallium chloride and excessive hydrogen chloride gas pumping-out component comprises a three-way valve 31, a first gas washing bottle 32, a second gas washing bottle 33, a third gas washing bottle 34 and a vacuum pump 35. The second gas washing bottle 33 is used for containing water, and the third gas washing bottle 34 is used for containing sodium hydroxide solution.
The first bottle mouth of the two-mouth bottle 12 is connected with the constant pressure dropping funnel 11.
The second bottle openings of the two-opening bottle 12, the conical bottle 21, the first gas washing bottle 32, the second gas washing bottle 33, the third gas washing bottle 34 and the vacuum pump 35 are sequentially connected through pipelines.
The three-way valve 31 is arranged on a pipeline between the third gas washing bottle 34 and the vacuum pump 35, the first end c of the three-way valve 31 is connected with the vacuum pump 35 through a pipeline, the second end a of the three-way valve 31 is connected with the third gas washing bottle 34 through a pipeline, and the third end b of the three-way valve 31 is connected with the outside through a pipeline. Specifically, the three-way valve 31 may be a glass three-way valve.
Based on the matrix gallium removing device, a matrix gallium removing method is provided, and comprises the following steps:
weighing a sample into the quartz reactor 22, specifically weighing 0.5000g of the sample into the quartz reactor 22 in this embodiment, then placing the quartz reactor 22 containing the sample into the conical flask 21, placing the conical flask 21 into the constant-temperature electric heating jacket 23, opening the constant-temperature electric heating jacket 23, and maintaining the temperature in the conical flask 21 at a preset temperature, specifically, the preset temperature is 210-;
rotating the three-way valve 31 to enable a second end a of the three-way valve 31 to be communicated with a third end b of the three-way valve 31, adding concentrated sulfuric acid into the constant-pressure dropping funnel 11, and adding dry sodium chloride into the two-mouth bottle 12, specifically, controlling the dropping speed of the concentrated sulfuric acid into the sodium chloride to be 3-4 seconds per drop, and enabling a large amount of generated dry hydrogen chloride gas to enter the conical flask 21 through a pipeline, react with a test material in the quartz reactor 22 to generate gallium trichloride, and volatilize the gallium trichloride gas into the hydrogen trichloride gas;
the generated gallium chloride and the excessive hydrogen chloride gas are discharged out of the conical flask 21 through a pipeline and are absorbed by the water in the second gas washing bottle 33 and the sodium hydroxide solution in the third gas washing bottle 34;
the three-way valves 31 are rotated every other first preset time, specifically, in this embodiment, the three-way valves 31 are rotated once every 5 minutes to close the third ends b of the three-way valves 31, and the first ends c of the three-way valves 31 are conducted with the second ends a of the three-way valves 31, the vacuum pump 35 is started to pump off the gallium chloride retained in the conical flask 21, and the duration of the second preset time is 1 minute each time in this embodiment until the quartz reactor 22 is dry, that is, all the samples volatilize, and the result shows that the substrate gallium removal treatment of a single 0.5g sample can be completed within 20 minutes.
And finally, dissolving the impurities remained in the quartz reactor 22 by using hydrochloric acid and nitric acid, and detecting the content of the impurities by adopting ICP-MS (inductively coupled plasma-mass spectrometry), wherein the detection result is consistent with the GD-MS (glow discharge mass spectrometry) analysis result, but the cost is lower than that of the GD-MS.
In summary, according to the device and the method for removing the gallium from the substrate, the dry hydrogen chloride gas is prepared by the reaction of the concentrated sulfuric acid and the sodium chloride, and then the gallium chloride volatile gas generated by the gallium treatment is extracted in times after the hydrogen chloride and the gallium are fully reacted for a period of time, so that the removal of the gallium from the substrate in the sample is realized, and the operation of the pretreatment process of the sample is simplified and speeded. The actual measurement shows that the method can finish the matrix gallium removal treatment of a single 0.5g sample in 20 minutes, the operation is simple, the treated sample is detected by ICP-MS, and the detection result is consistent with the GD-MS analysis result. The method is suitable for simultaneously measuring the contents of trace elements such as copper, lead, zinc, indium, iron, tin, nickel, magnesium, cobalt, chromium, manganese, iron, rubidium, molybdenum, bismuth and the like in high-purity gallium (99.999% < w (G a) < 99.99999%).
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. A matrix gallium removing device is characterized by comprising a dry hydrogen chloride gas generating assembly, a gallium conversion gallium chloride generating assembly, a gallium chloride and excessive hydrogen chloride gas extracting assembly;
the dry hydrogen chloride gas generating assembly comprises a constant-pressure dropping funnel, two bottles and a constant-temperature water bath;
the gallium-to-gallium chloride generating component comprises a conical flask, a quartz reactor and a constant-temperature electric heating jacket;
the gallium chloride and excessive hydrogen chloride gas pumping-out component comprises a three-way valve, a first gas washing bottle, a second gas washing bottle, a third gas washing bottle and a vacuum pump;
the constant-pressure dropping funnel is used for containing concentrated sulfuric acid, the two-mouth bottle is used for containing sodium chloride solid, and the two-mouth bottle is arranged in the constant-temperature water bath;
the quartz reactor is used for containing a test material, the quartz reactor is arranged in the conical flask, the conical flask is arranged in the constant-temperature electric heating sleeve, the second gas washing bottle is used for containing water, and the third gas washing bottle is used for containing a sodium hydroxide solution;
the first bottle mouth of the two-mouth bottle is connected with the constant-pressure dropping funnel;
the vacuum pump is characterized in that the second bottle openings of the two bottles, the conical bottle, the first gas washing bottle, the second gas washing bottle, the third gas washing bottle and the vacuum pump are sequentially connected through pipelines, the three-way valve is arranged on a pipeline between the third gas washing bottle and the vacuum pump, the first end of the three-way valve is connected with the vacuum pump through a pipeline, the second end of the three-way valve is connected with the third gas washing bottle through a pipeline, and the third end of the three-way valve is connected with the outside through a pipeline.
2. The matrix gallium removal device according to claim 1, wherein said three-way valve is a glass three-way valve.
3. A method for removing bulk gallium, applied to the bulk gallium removal apparatus of claim 1, the method comprising:
weighing a test material and placing the test material in the quartz reactor, then placing the quartz reactor containing the test material in the conical flask, then placing the conical flask in the constant-temperature electric heating sleeve, starting the constant-temperature electric heating sleeve, and maintaining the temperature in the conical flask at a preset temperature;
rotating the three-way valve to enable a second end of the three-way valve to be communicated with a third end of the three-way valve, adding concentrated sulfuric acid into the constant-pressure dropping funnel, adding dry sodium chloride into the two-mouth bottle, and enabling a large amount of generated dry hydrogen chloride gas to enter the conical bottle through a pipeline to react with a test material in the quartz reactor to generate gallium trichloride and to be discharged in a gas form;
discharging the generated gallium chloride and excessive hydrogen chloride gas out of the conical flask through a pipeline, and absorbing the gallium chloride and the excessive hydrogen chloride gas by water in the second gas washing bottle and a sodium hydroxide solution in the third gas washing bottle;
and rotating the three-way valves at intervals of a first preset time to seal the third ends of the three-way valves, communicating the first end of the three-way valve with the second end of the three-way valve, starting the vacuum pump, and pumping out the gallium chloride retained in the conical flask for a second preset time each time until the quartz reactor is dried.
4. The method for removing the gallium from the substrate according to claim 3, wherein the dropping speed of concentrated sulfuric acid into sodium chloride is controlled to be 3-4 seconds per drop when the concentrated sulfuric acid is added into the constant pressure dropping funnel and the dried sodium chloride is added into the two-mouth bottle.
5. The method as set forth in claim 3, wherein the predetermined temperature is 210-220 ℃.
6. The method according to claim 3, wherein the first predetermined time is 5 minutes.
7. The method according to claim 3, wherein the second predetermined time is 1 minute.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031762A (en) * | 1987-09-01 | 1989-03-15 | 北京有色金属研究总院 | The analytical approach of impurity element in the gallium |
| CN1042008A (en) * | 1988-10-20 | 1990-05-09 | 北京有色金属研究总院 | The new method of trace impurity in the enriched in metals |
| CN101993039A (en) * | 2010-10-15 | 2011-03-30 | 天津市泰源工业气体有限公司 | Technology for preparing hydrogen chloride by reacting concentrated sulphuric acid with hydrochloric acid or sodium chloride |
| CN203178122U (en) * | 2013-04-10 | 2013-09-04 | 株洲科能光电材料科技发展有限责任公司 | High-purity gallium separation device |
-
2020
- 2020-07-16 CN CN202010686686.XA patent/CN111912692A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031762A (en) * | 1987-09-01 | 1989-03-15 | 北京有色金属研究总院 | The analytical approach of impurity element in the gallium |
| CN1042008A (en) * | 1988-10-20 | 1990-05-09 | 北京有色金属研究总院 | The new method of trace impurity in the enriched in metals |
| CN101993039A (en) * | 2010-10-15 | 2011-03-30 | 天津市泰源工业气体有限公司 | Technology for preparing hydrogen chloride by reacting concentrated sulphuric acid with hydrochloric acid or sodium chloride |
| CN203178122U (en) * | 2013-04-10 | 2013-09-04 | 株洲科能光电材料科技发展有限责任公司 | High-purity gallium separation device |
Non-Patent Citations (4)
| Title |
|---|
| 中华人民共和国工业和信息化部: "《Y/ST 38.2-2009 高纯镓化学分析方法 第2部分：镁、钛、铬、锰、镍、钴、铜、锌、镉、锡、铅、铋量的测定 电感耦合等离子体质谱法》", 4 December 2009 * |
| 中华人民共和国电子工业部: "《SJ 20713-1998 砷化镓用高纯镓中铜、锰、镁、钒、钛等12种杂质的等离子体光谱分析法》", 18 March 1998 * |
| 国家发展和改革委员会: "《Y/ST 474-2005 高纯镓化学分析方法 痕量元素的测定 电感耦合等离子体质谱法》", 18 May 2005 * |
| 李来柱: "《药物化学实验指导》", 31 January 2014 * |
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