CN1884631A - Method and device for cleaning organic matter using electrochemical method - Google Patents
Method and device for cleaning organic matter using electrochemical method Download PDFInfo
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- CN1884631A CN1884631A CN 200610013851 CN200610013851A CN1884631A CN 1884631 A CN1884631 A CN 1884631A CN 200610013851 CN200610013851 CN 200610013851 CN 200610013851 A CN200610013851 A CN 200610013851A CN 1884631 A CN1884631 A CN 1884631A
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Abstract
This invention exposed a kind of cleaning method and device of cleaning organic substance by electrochemical method. It uses diamond film electrode as anode, within the current density range of 100-5000Am-2 to clean organic substance by electrochemical method. This invention makes full use of the advantage of diamond film electrode on the aspect of electrochemical oxidation technology to use it generate hydroxyl radical, oxygen free radical and other strong oxidation particle to clean organically. For example, it can be used to clean photoresist lift-off semiconductot device and avoid the heavy metal and alkali metals elements in traditional wet technology. Using it to regenerate active carbon can reduce cost significantly and it is also environment friendly.
Description
[ technical field]A method for producing a semiconductor device
The invention relates to the field of electrochemical oxidation, in particular to a method and a device for cleaning organic matters by an electrochemical method.
[ background of the invention]
Advanced oxidation treatment (AOP) technology is widely used to degrade or decompose organic matter, particularly refractory organic pollutants. At present, electrochemical oxidation treatment plays a very important role in the treatment of industrial wastewater, and the oxidation process is more and more concerned by people in the aspect of reducing toxic pollution. Meanwhile, photoresist stripping and activated carbon regeneration for the electrochemical oxidation process of semiconductor devices are also receiving more and more attention.
In the semiconductor device manufacturing process, plasma ashing and wet processes are generally used for photoresist stripping. In most cases, wet cleaning is performed after ashing to remove organic or polymer residues caused by the plasma process. The solution used for wet cleaning is typically a mixture of SPM-APM, where the SPM solution is sulfuric acid (H)2SO4) And hydrogen peroxide (H)2O2) The APM solution is a mixture of ammonium hydroxide, hydrogen peroxide and water. The traditional chemical cleaning agents SPM and APM both contain metal ion impurities, which have negative influence on the electrical performance of the novel gate structure; moreover, for cleaning reagents SPM and APM,if the cleaning efficiency and the electrical performance of the device are ensured, the cleaning reagents SPM and APM are required to be disposable, so that the cleaning cost is very high; in addition, the use of traditional chemical reagents and the consumption of water have a negative impact on the environment.
The activated carbon is a non-toxic and odorless excellent adsorbent with a developed pore structure and a large specific surface area. In the prior art, a large number of activated carbon adsorption methods are used for treating urban drinking water and industrial wastewater, treating carbon disulfide wastewater, treating oil refining wastewater, explosive wastewater, printing and dyeing wastewater, chemical wastewater, electroplating wastewater and the like. With the increasing application range of activated carbon, the recycling of activated carbon has been gaining attention. If the used activated carbon cannot be recycled, the treatment cost per ton of waste water will be increased, and secondary pollution to the environment will be caused. Therefore, the regeneration of activated carbon is of particular importance. The traditional activated carbon regeneration method comprises the traditional methods of activated carbon regeneration such as a thermal regeneration method and a biological regeneration method, and the currently emerging activated carbon regeneration technologies comprise a supercritical fluid method, a catalytic wet oxidation method and an ultrasonic wave method.
[ summary of the invention]
The invention aims to solve the problems in the prior art and provide a method and a device for cleaning organic matters by an electrochemical method.
The invention discloses a method for cleaning organic matters by an electrochemical method for realizing the aim of the invention. The method is characterized in that a cleaning object containing organic matters is placed in electrolyte; using diamond film electrode as anode, at current density of 100-5000Am-2In the range between electrochemical Oxidation of Hydroxyl (OH) groups in water-) Generating hydroxyl free radical (OH) and oxygen free radical (O), ozone (O)3) And hydrogen peroxide (H)2O2)。
The invention also discloses an electrochemical cleaning device special for the method for cleaning the organic matters by using the electrochemical method, which comprises an electrolytic cell, electrodes and an ionic membrane and is characterized in that the electrolytic cell is a single-compartment electrolytic cell or a double-compartment and multi-compartment electrolytic cell, and the middles of electrolytic cells of the double-compartment and multi-compartment electrolytic cells are separated by the ionic membrane; the electrodes are one or more groups, each group of electrode group consists of an anode-diamond membrane electrode and a cathode-common metal electrode, and the distance between two adjacent electrodes of the anode and the cathode is 0.5-50 mm; and meanwhile, the disturbance of the electrolyte is realized by a mechanical mode.
The invention fully utilizes the advantages of the diamond film electrode in the electrochemical oxidation technology and exerts the application potential of the diamond film electrode. The use of a diamond membrane electrode to generate oxidized particles such as hydroxyl radicals and oxygen radicals can be used for organic cleaning, for example: the cleaning agent is used for cleaning the photoresist to strip the semiconductor device, avoids heavy metal and alkali metal elements with certain content in the traditional wet process, and can meet the design requirement of the device; the method is used for regenerating the active carbon, can greatly reduce the cost and cannot cause environmental pollution. The device for organic cleaning by using the diamond membrane electrode is simple and convenient to operate, and does not produce secondary pollution. Low energy consumption, and can meet the requirements of low-cost manufacture and no harm to environment.
[ description of the drawings]
FIG. 1 is a schematic view of an electrochemical cleaning apparatus.
In the figure: 1. an anode; 2. a cathode; 3. a water pump; 4. a container; 5. a flow meter; 6. a power source.
[ detailed description]embodiments
The invention relates to a method for cleaning organic matters by an electrochemical method, which comprises the steps of placing a cleaning object in electrolyte, using a diamond film electrode as an anode, and performing cleaning at a current density of 100--2In the range between electrochemical Oxidation of Hydroxyl (OH) groups in water-) Generating hydroxyl free radical (OH. cndot.) oxygen free radical (O. cndot.),Ozone (O)3) And hydrogen peroxide (H)2O2)。
The electrochemical cleaning device of the invention comprises an electrolytic cell, electrodes, an ionic membrane, a flowmeter 5, a power supply 6 and the like. The electrolytic cell can be a single-chamber electrolytic cell or a double-chamber or multi-chamber electrolytic cell, and the electrolytic bath of the double-chamber and multi-chamber electrolytic cells is separated from the cathode bath and the anode bath by an ionic membrane. The electrodes can be one group or a plurality of groups, each group of electrode group consists of an anode-diamond membrane electrode and a cathode-common metal electrode, the distance between the two adjacent electrodes of the anode 1 and the cathode 2 is 0.5-50mm, and the electrodes are fixed in the treatment tank. The multiple groups of electrode sets can be connected in parallel or in series. In order to improve the cleaning efficiency, the disturbance or circulation of the electrolyte can be realized by arranging a water pump 3 or a stirrer.
In order to facilitate the cleaning of certain cleaning objects or the cleaning of a large number of cleaning objects, the electrolytic cell can also be connected with a cleaning object container 4 by a circulation pipeline and a circulation pump. The cleaning object is placed in a container, and the electrolyte is introduced into the cleaning container through a circulating pipeline and can be continuously circulated with the electrolyte in the electrolytic cell. For example, the container is used for containing organic pollutant activated carbon for activated carbon regeneration. When the electrolytic cell is a double-chamber or multi-chamber electrolytic cell, the circulating pipeline is communicated with the anode tank.
The present invention may be an organic cleaning of a photoresist-stripped semiconductor device as a cleaning object. The device to be cleaned is placed in a single-chamber electrolytic cell, or in the case of a double-chamber or multi-chamber electrolytic cell, in an anode tank. The electrode group is electrified with direct current electrolytic water, and the cleaning efficiency is controlled by controlling the current. The current density is larger, the efficiency is higher, and the current density range is 100-5000Am-2In the meantime.
The invention can also carry out activated carbon regeneration cleaning on the activated carbon polluted by organic matters as a cleaning object. The water is electrolyzed by a single-chamber or multi-chamber electrolytic cell processor, and the watercirculation between the processor and the activated carbon container is realized by a water pump. The larger the current density is, the higher the treatment efficiency is, and the current density ranges from 100-5000Am-2In the meantime.
The working principle of the invention for cleaning organic matters by an electrochemical method is as follows: when the diamond film electrode is used as an anode for electrolyzing water, because the oxygen evolution potential of the diamond film electrode is very high, the electrode potential of diamond (>+3V) can generate a large amount of hydroxyl radicals (OH.):
s is on the surface of the anode, and S (HO) is hydroxyl radical (OH) on the surface of the electrode. In general, the adsorbed HO · passivates the electrode on the electrode for reaction, but in a relatively stable electrode, for example a diamond membrane electrode, the adsorbed S (HO · S) is oxidized to oxygen:
the oxygen may be further oxidized by hydroxyl radicals at the electrode surface to O3,
except for O3In addition, S (HO.) generates H by binding202
Hydroxyl radicals and ozone particles have high oxidation properties, which are important for effective photoresist stripping and organic cleaning. Hydroxyl radicals are the key to organic cleaning. The regeneration of activated carbon is to remove organic waste adsorbed on the surface of activated carbon, oxygen free radical (O), ozone (O)3) Hydrogen peroxide (H)2O2) And high-strength oxidation reagents such as hydroxyl radical (OH), and the like can realize the oxidation removal of the organic matters, thereby realizing the regeneration of the activated carbon.
The first embodiment is as follows: uniformly coating high-temperature paraffin on polished silicon wafer with thickness of 1mm, placing into single-electrode group single-chamber electrolytic cell treatment device with distance of 1mm between adjacent positive and negative electrodes, voltage of 10V, current of 2.5A, and current density of 1000Am-2Left and right. After 1 hour of treatment, the paraffin is obviously dropped, and after 2 hours, the paraffin is completely dropped without residue.
Example two: uniformly coating high-temperature paraffin on polished silicon wafer with thickness of 1mm, placing into anode tank of single-electrode group double-chamber electrolytic cell treatment device, wherein the distance between adjacent positive and negative electrodes is 2mm, voltage is 13V, current is 2.5A, and current density is 1000Am-2Left and right. After 0.5 hour of treatment, the paraffin has obvious shedding phenomenon, and the paraffin completely sheds after 70 minutes without residue.
Example three: uniformly coating high-temperature paraffin on polished silicon wafer with thickness of 1mm, placing into a multi-electrode group single-chamber electrolytic cell processing device, wherein the distance between adjacent positive and negative electrodes is 1mm, voltage is 10V, current is 100A, and current density is 7000Am-2Left and right. After 2min of treatment, the paraffin has obvious shedding phenomenon, and after 10min, the paraffin is completely shed without residue.
Example four: placing saturated activated carbon into a container, connecting a single-chamber multi-electrode group electrochemical oxidation processor with the container, wherein the distance between adjacent positive and negative electrodes is 0.5mm, and pumping with a water pumpWater is circulated between the device and the container. Introducing direct current with voltage of 10V, current of 5A and current density of 1000Am-2Left and right. After 5 hours of washing, the activated carbon was taken out of the vessel, and the activity of the activated carbon was restored to the original state by the test.
Claims (8)
1. A method for cleaning organic matter by an electrochemical method is characterized in that a cleaning object containing the organic matter is placed in an electrolyte; using diamond film electrode as anode, at current density of 100-5000Am-2In the range between electrochemical Oxidation of Hydroxyl (OH) groups in water-) Generating hydroxyl free radical (OH) and oxygen free radical (O), ozone (O)3) And hydrogen peroxide (H)2O2)。
2. An electrochemical cleaning apparatus for use in a method of electrochemically cleaning organic matter according to claim 1, comprising an electrolytic cell, electrodes, and an ionic membrane, wherein said electrolytic cell is a single-compartment electrolytic cell or a two-compartment or multi-compartment electrolytic cell, and the electrolytic cells of the two-compartment and multi-compartment electrolytic cells are separated by the ionic membrane; the electrodes are one or more groups, each group of electrode group consists of an anode-diamond membrane electrode and a cathode-common metal electrode, and the distance between two adjacent electrodes of the anode and the cathode is 0.5-50 mm; and meanwhile, the disturbance of the electrolyte is realized by a mechanicalmode.
3. An electrochemical cleaning device according to claim 4, wherein the electrolyte in said electrolytic cell is connected to a container for objects to be cleaned through a circulation line and a circulation pump.
4. An electrochemical cleaning device according to claim 4 or 5, wherein said electrolytic cell is a two-compartment or multi-compartment electrolytic cell and the circulation line is in communication with the anode tank.
5. An electrochemical cleaning device according to claim 4 or 5, wherein said plurality of electrode sets are connected in parallel or in series.
6. An electrochemical cleaning device according to claim 6, wherein said plurality of electrode sets are connected in parallel or in series.
7. An electrochemical cleaning device according to claim 4 or 5 or 8, wherein said disturbance of the electrolyte is achieved mechanically by means of a pump or agitator.
8. An electrochemical cleaning device according to claim 7, wherein said disturbance of the electrolyte by mechanical means is a water pump or agitator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610013851 CN1884631A (en) | 2006-05-25 | 2006-05-25 | Method and device for cleaning organic matter using electrochemical method |
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| CN 200610013851 CN1884631A (en) | 2006-05-25 | 2006-05-25 | Method and device for cleaning organic matter using electrochemical method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102021639A (en) * | 2010-11-10 | 2011-04-20 | 安徽华东光电技术研究所 | Electrolytic degreasing process for traveling wave tube parts |
| CN102614537A (en) * | 2012-04-19 | 2012-08-01 | 牡丹江师范学院 | Air purification method and air purification device using same |
| CN101662961B (en) * | 2007-05-10 | 2013-09-11 | 仓敷纺织株式会社 | Method of washing and apparatus for use therein |
| CN103727599A (en) * | 2014-01-08 | 2014-04-16 | 波鹰(厦门)科技有限公司 | Air cleaning device and method for removing formaldehyde and PM2.5 |
| CN108404678A (en) * | 2018-03-23 | 2018-08-17 | 中海油天津化工研究设计院有限公司 | A kind of MBR films off-line cleaning device and cleaning method |
| CN113600549A (en) * | 2021-09-10 | 2021-11-05 | 何龙 | Method for electrochemically degrading organic pollutants outside cell and application |
-
2006
- 2006-05-25 CN CN 200610013851 patent/CN1884631A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101662961B (en) * | 2007-05-10 | 2013-09-11 | 仓敷纺织株式会社 | Method of washing and apparatus for use therein |
| CN102021639A (en) * | 2010-11-10 | 2011-04-20 | 安徽华东光电技术研究所 | Electrolytic degreasing process for traveling wave tube parts |
| CN102614537A (en) * | 2012-04-19 | 2012-08-01 | 牡丹江师范学院 | Air purification method and air purification device using same |
| CN102614537B (en) * | 2012-04-19 | 2014-07-23 | 牡丹江师范学院 | Air purification method and air purification device using same |
| CN103727599A (en) * | 2014-01-08 | 2014-04-16 | 波鹰(厦门)科技有限公司 | Air cleaning device and method for removing formaldehyde and PM2.5 |
| CN108404678A (en) * | 2018-03-23 | 2018-08-17 | 中海油天津化工研究设计院有限公司 | A kind of MBR films off-line cleaning device and cleaning method |
| CN113600549A (en) * | 2021-09-10 | 2021-11-05 | 何龙 | Method for electrochemically degrading organic pollutants outside cell and application |
| CN113600549B (en) * | 2021-09-10 | 2023-08-22 | 何龙 | Method for electrochemical degradation of organic pollutants outside tank and application |
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