CN107227482B - Electrodeposition sample preparation instrument suitable for alpha radioactive source preparation - Google Patents
Electrodeposition sample preparation instrument suitable for alpha radioactive source preparation Download PDFInfo
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- CN107227482B CN107227482B CN201710574762.6A CN201710574762A CN107227482B CN 107227482 B CN107227482 B CN 107227482B CN 201710574762 A CN201710574762 A CN 201710574762A CN 107227482 B CN107227482 B CN 107227482B
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- electrodeposition
- cistern
- sample preparation
- cooling device
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/02—Heating or cooling
Abstract
The invention relates to an electrodeposition sample preparation instrument, in particular to an electrodeposition sample preparation instrument suitable for preparing an alpha radioactive source. The invention provides an electrodeposition sample preparation instrument suitable for preparing an alpha radioactive source, which furthest reduces the self-absorption and scattering of the source by an electrodeposition method so as to adapt to the measurement of an alpha energy spectrum, and adopts a novel air cooling device to effectively reduce the cross contamination in the source preparation process.
Description
Technical Field
The invention relates to an electrodeposition sample preparation instrument, in particular to an electrodeposition sample preparation instrument suitable for preparing an alpha radioactive source.
Background
Because of the short range of alpha particles, the self-absorption of the source must be considered in preparing the alpha radiation source. The main method for preparing the alpha radioactive source is an electrodeposition method, the cooling mode adopted by the method is mainly water cooling, and the radioactive source prepared by the method is very high in leakage and cross contamination of radioactive solution.
Disclosure of Invention
The invention aims to solve the technical problems that: in order to solve the defect that the conventional source cooling method is easy to cause cross contamination, the invention provides an electrodeposition sample preparation instrument suitable for preparing an alpha radioactive source, and the leakage and cross contamination of radioactive solution in the preparation process of the radioactive source are reduced to the greatest extent by a cooling mode combining air cooling and semiconductor refrigeration.
The technical scheme adopted for solving the technical problems is as follows:
the utility model provides an electrodeposition sample preparation appearance suitable for alpha radiation source preparation, including cistern, bottle lid, bottom, positive pole, negative pole, facing, cooling device and DC voltage-stabilizing power supply, cistern one pot head is equipped with the bottle lid, and the other pot head of cistern is equipped with the bottom, and the positive pole is arranged in the cistern, and the bottle lid is passed to the one end of positive pole, is equipped with the facing between bottom and the cistern, is equipped with the negative pole on the terminal surface of bottom towards the cistern, and cistern fixed connection is in cooling device, and the end of positive pole links to each other with DC voltage-stabilizing power supply's positive pole, and the bottom end links to each other with DC voltage-stabilizing power supply's negative pole.
In particular, the liquid tank is fixedly connected in the cooling device through a bracket.
Specifically, a tray is arranged in the cooling device and is positioned below the liquid tank.
In particular, the cooling device is preferably a constant temperature refrigerator.
Specifically, the anode is made of platinum material.
Specifically, the lining is made of polytetrafluoroethylene.
Specifically, the bottom cover is made of stainless steel.
Specifically, the cathode is a stainless steel sheet.
Specifically, the liquid tank is made of organic glass.
The beneficial effects of the invention are as follows: the invention provides an electrodeposition sample preparation instrument suitable for preparing an alpha radioactive source, which furthest reduces the leakage and cross contamination of radioactive solution in the preparation process of the radioactive source by a cooling mode combining air cooling and semiconductor refrigeration.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic view of an electrodeposition cell of the present invention;
in the figure, a liquid tank 1, a bottle cap 2, a bottom cap 3, a positive electrode 4, a negative electrode 5, a lining 6, a cooling device 7, a direct-current stabilized power supply 8, a bracket 9 and a tray 10.
Detailed Description
The invention will now be described in further detail with reference to the accompanying drawings. The drawings are simplified schematic representations which merely illustrate the basic structure of the invention and therefore show only the structures which are relevant to the invention.
Fig. 1 is a schematic view of the structure of the present invention, and fig. 2 is a schematic view of the electrodeposition cell of the present invention.
The utility model provides an electrodeposition sample preparation appearance suitable for alpha radiation source preparation, including cistern 1, bottle lid 2, bottom 3, positive pole 4, negative pole 5, facing 6, cooling device 7 and direct current stabilized power supply 8, cistern 1 one end cover is equipped with bottle lid 2, cistern 1 other pot head is equipped with bottom 3, positive pole 4 is arranged in cistern 1, the one end of positive pole 4 passes bottle lid 2, be equipped with facing 6 between bottom 3 and the cistern 1, be equipped with negative pole 5 on the terminal surface of bottom 3 towards cistern 1, cistern 1 fixed connection is in cooling device 7, the end of positive pole 4 links to each other with direct current stabilized power supply 8's positive pole, bottom 3 end links to each other with direct current stabilized power supply 8's negative pole. The liquid tank 1 is fixedly connected in the cooling device 7 through a bracket 9. A tray 10 is arranged in the cooling device 7, and the tray 10 is positioned below the liquid tank 1. The cooling device 7 is preferably a thermostatic refrigerator. The anode 2 is made of platinum material. The lining 6 is made of polytetrafluoroethylene. The bottom cover 3 is made of stainless steel. The cathode 5 is a stainless steel sheet. The liquid tank 1 is made of organic glass.
The electrodeposition cell consists of a liquid tank 1, a bottle cap 2, a bottom cover 3, an anode 4, a cathode 5 and a lining 6 (shown in figure 2).
The preparation of alpha-radiation sources generally uses well polished stainless steel, aluminum, nickel, silver, platinum and gold as cathode 5, i.e., electroplated pieces, which proved to be a superior performance and moderate cost cathode 5 material and was widely used in most experiments. The mirror stainless steel sheet is used, and the material has a smooth and clean electroplating surface and is only subjected to simple cleaning treatment before electroplating. In order to avoid the introduction of excessive impurity ions, the anode 4 is generally made of insoluble anode materials, such as noble metal platinum with very high chemical inertia, a radioactive source with the effective area diameter smaller than phi=10mm is generally prepared, the anode 4 only needs one platinum wire, the anode material platinum is generally made into a sheet shape to ensure the uniformity of an electric field when the diameter is larger than the diameter, and the anode 4 platinum wire is made into a coil shape for stirring due to cost reasons. In the design of the scheme, the situation of the electroplating reaction needs to be observed in real time in the experiment, so that the material of the liquid tank 1 is selected to be colorless and transparent organic glass with acid-base corrosion. If the electrodeposition bath is an organic system, it is conceivable to change the electrodeposition bath to polytetrafluoroethylene.
The cathode and anode of the preparation instrument are connected with a direct current stabilized power supply 8 and are placed in a cooling device 7 to work, and main influencing factors and technical indexes of the electrodeposition effect of the equipment comprise control of deposition current, selection of electroplating solvent, optimal quality control of radionuclide and selection of electrodeposition time, and the conditions are not discussed herein. The electrolysis power supply satisfies the following conditions: the direct current stabilized voltage power supply 8 has the adjustable voltage range of 0-35V, is continuously adjustable within the range of 0.1A-3A (0.02A unit adjustment), has the current oscillation amplitude smaller than 0.2A (peak value), and can not be powered by direct current or countercurrent when the power supply is cut off or the equipment is not connected with a circuit.
The cooling device 7 is typically cooled in a water bath, but requires tightness of the device, and the entire electrodeposition device is placed in the water bath to cause corrosion of the electrodes. Air cooling is also adopted in experiments, but the refrigeration effect is not ideal, the electrodeposition effect is related to temperature, and overheating can affect the electroplating effect on the cathode surface. The device adopts a method of refrigerating by a constant temperature refrigerator (effectively combining air cooling and semiconductor refrigeration), and the electrodeposition tank is arranged in the cooling device 7, so that the rapid heat conduction is realized. Practice proves that the effect is much better than that of pure air cooling.
A bottom cover 3 provided with a cathode 2 is fixed at the lower end of the liquid tank 1, and an anode is fixed right above the liquid tank 1. During electroplating, electrolyte is added into the liquid tank 1, the temperature of the electrolyte is kept within the range of 20-50 ℃ by the cooling device 7, the distance between the anode and the cathode is adjusted, and the electrodeposition is started.
On the basis of the design, the preparation instrument adopts a method of combining machining and material purchase to complete the combined installation of the whole device, wherein the electro-deposition tank is completed in an external commission machining workshop according to the geometric dimension of the previous design, the cooling device 7 is formed by modifying a common refrigerator, and the direct-current regulated power supply 8 is a direct-current double-path tracking regulated power supply with the model DH 1718E-5.
The preparation instrument was subjected to a condition test using a 239Pu standard solution having an activity concentration of 1 Bq/ml. Plating fastness and surface uniformity were tested.
The steps are as follows:
1. setting the temperature of the refrigerator at 0 ℃, and refrigerating for 1h;
2. adding 10ml of electroplating solution (239 Pu is 1Bq in each electroplating tube) under a pre-configured ammonium nitrate system into four-way electroplating tubes respectively;
3. switching on a direct current stabilized power supply, setting the voltage to be 20V, the current to be constant, the current density to be 600mA/cm < 2 >, and the electrodeposition time to be 60min;
4. adding 1ml of ammonia water, continuing to electrodeposit for 1min, and switching off the power supply;
5. pouring out the electrolyte, and repeatedly washing the plating piece with water and ethanol;
6. baking under infrared lamp;
7. and (5) placing the sample in a semiconductor alpha spectrometer for measurement.
The activities of the four-way measurement were 0.941Bq, 0.905Bq, 0.950Bq, and 0.987Bq, respectively. Namely, the recovery rates of four-way electroplating are 94.1%, 90.5%, 95.0% and 98.7%, respectively. In conclusion, the recovery rate of electroplating reaches more than 90 percent.
The conditional experiments were run ten times in total to test the repeatability of the experiments. In the test, the long-term stability of the current was examined.
More than 90% of the deposition efficiency of the alpha radioactive sample; the structure is firm, the operation is easy, and the cleaning is easy; the electroplating has high repeatability; the cooling device is adopted, so that the electrolyte solution can be cooled rapidly, and the electrolyte solution is cleaner, so that cross contamination is avoided; two sets of electroplating tanks are designed according to the difference of the area of the electroplating source, and the replacement is convenient.
Device parameters:
1. an electrolysis electrode: platinum wire with screw head (purity 99.95%), specification phi 10mm x 150mm;
2. electrolytic current: DC regulated power supply 8, continuously adjustable, 0.1A-3A
Electrolytic current control:
the current regulation is continuous (0.02A unit regulation)
The amplitude of the current oscillation is less than 0.2A (peak value)
When the power is turned off or the device has no access to the circuit, no DC or reverse power supply can be applied
LCD is capable of displaying a two-bit decimal value of the current (stability: 0.01A)
3. LCD display screen: display current, voltage and electric polarity
4. The equipment mainly comprises the following materials: organic glass, engineering plastic, polyoxymethylene resin, nylon, stainless steel and copper
5. Cooling device 7: refrigerating in refrigerator at 0-5 deg.c
6. Electrodeposition cell, tray 10, plating bath bracket 9: a tray 10 is arranged below the electrodeposition tank to prevent the leakage of the electroplating solution from polluting the electrodeposition device, thus ensuring the safety of the whole system.
7. Size of the plating sheet: the diameters of the scale source are 10mm and 16mm respectively.
8. And (3) a power supply: 230V/50Hz
9. Operating temperature: the working external temperature is not higher than 45℃ from 0℃ to +45 DEG C
10. Storage temperature: -25 ℃ to +70 DEG C
With the above-described preferred embodiments according to the present invention as an illustration, the above-described descriptions can be used by persons skilled in the relevant art to make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the description, but must be determined according to the scope of claims.
Claims (6)
1. The utility model provides an electrodeposition sample preparation appearance suitable for alpha radiation source preparation, which is characterized by, including cistern (1), bottle lid (2), bottom (3), positive pole (4), negative pole (5), lining (6), cooling device (7) and direct current steady voltage power supply (8), cistern (1) one end cover is equipped with bottle lid (2), cistern (1) other end cover is equipped with bottom (3), positive pole (4) are arranged in cistern (1), the one end of positive pole (4) passes bottle lid (2), be equipped with lining (6) between bottom (3) and cistern (1), be equipped with negative pole (5) on the terminal surface of bottom (3) towards cistern (1), cistern (1) fixed connection is in cooling device (7), the end of positive pole (4) links to each other with the positive pole of direct current steady voltage power supply (8), the end of bottom (3) links to each other with the negative pole of direct current steady voltage power supply (8); the liquid tank (1) is fixedly connected in the cooling device (7) through the bracket (9);
a tray (10) is arranged in the cooling device (7), and the tray (10) is positioned below the liquid tank (1);
the cooling device (7) is a constant temperature refrigerator.
2. An electrodeposition sample preparation instrument suitable for use in alpha radiation source preparation according to claim 1, wherein: the anode (4) is made of platinum material.
3. An electrodeposition sample preparation instrument suitable for use in alpha radiation source preparation according to claim 1, wherein: the lining (6) is made of polytetrafluoroethylene.
4. An electrodeposition sample preparation instrument suitable for use in alpha radiation source preparation according to claim 1, wherein: the bottom cover (3) is made of stainless steel.
5. An electrodeposition sample preparation instrument suitable for use in alpha radiation source preparation according to claim 1, wherein: the cathode (5) is a stainless steel sheet.
6. An electrodeposition sample preparation instrument suitable for use in alpha radiation source preparation according to claim 1 or 2, characterized in that: the liquid tank (1) is made of organic glass.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710574762.6A CN107227482B (en) | 2017-07-14 | 2017-07-14 | Electrodeposition sample preparation instrument suitable for alpha radioactive source preparation |
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| CN201710574762.6A CN107227482B (en) | 2017-07-14 | 2017-07-14 | Electrodeposition sample preparation instrument suitable for alpha radioactive source preparation |
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| CN107227482B true CN107227482B (en) | 2023-07-25 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110438536A (en) * | 2019-07-30 | 2019-11-12 | 华东师范大学 | A kind of electro-deposition-auto-deposition prepares αsource experimental provision and its experimental method |
| CN114486414A (en) * | 2021-12-22 | 2022-05-13 | 中国原子能科学研究院 | Alpha nuclide sample source electrodeposition sample preparation device |
| CN114481267B (en) * | 2022-01-29 | 2023-04-18 | 西北核技术研究所 | Electrodeposition source making device for laser resonance ionization mass spectrometry and Sn source preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5974298A (en) * | 1982-10-20 | 1984-04-26 | Mayekawa Mfg Co Ltd | Electrodeposition painting device |
| JP2003193283A (en) * | 2001-12-28 | 2003-07-09 | Fujitsu Ltd | Electroplating solution and method of preparing the same, method of manufacturing semiconductor device and method of analyzing radioactive impurity |
| JP2004149848A (en) * | 2002-10-30 | 2004-05-27 | Japan Storage Battery Co Ltd | Catalyst for electrolysis type ozone-generating anode, and electrolysis type ozone-generating device |
| CN105821467A (en) * | 2016-03-31 | 2016-08-03 | 中国原子能科学研究院 | Electric deposition device for preparing high-resolution alpha source |
| CN206916248U (en) * | 2017-07-14 | 2018-01-23 | 中国环境科学研究院 | A kind of electro-deposition sample preparation instrument prepared suitable for αsource |
-
2017
- 2017-07-14 CN CN201710574762.6A patent/CN107227482B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5974298A (en) * | 1982-10-20 | 1984-04-26 | Mayekawa Mfg Co Ltd | Electrodeposition painting device |
| JP2003193283A (en) * | 2001-12-28 | 2003-07-09 | Fujitsu Ltd | Electroplating solution and method of preparing the same, method of manufacturing semiconductor device and method of analyzing radioactive impurity |
| JP2004149848A (en) * | 2002-10-30 | 2004-05-27 | Japan Storage Battery Co Ltd | Catalyst for electrolysis type ozone-generating anode, and electrolysis type ozone-generating device |
| CN105821467A (en) * | 2016-03-31 | 2016-08-03 | 中国原子能科学研究院 | Electric deposition device for preparing high-resolution alpha source |
| CN206916248U (en) * | 2017-07-14 | 2018-01-23 | 中国环境科学研究院 | A kind of electro-deposition sample preparation instrument prepared suitable for αsource |
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