Manufacturing method of solid < 68 > Zn target for accelerator production of < 68 > Ga

Abstract

The invention discloses a manufacturing method of a solid < 68 > Zn target for accelerator production of < 68 > Ga, and relates to the technical field of nuclear medicine diagnos.The key points of the technical scheme are that a copper target is subjected to pretreatment operation; electroplating a nickel layer on the pretreated copper target; electroplating a gold layer on the nickel-plated copper target; the 68Zn is plated on a customized inert platinum metal plate, and then the 68Zn is used as an anode for electroplating, so that the concentration of zinc ions in a solution in the electroplating process is maintained, and the adhesive force and the uniformity of a zinc plating layer are guaranteed. According to the electroplating method, the copper target is sequentially plated with the nickel layer and the gold layer, the 68Zn is firstly plated on the customized platinum metal plate, and then the platinum metal plate plated with the 68Zn is used as an anode for electroplating, so that the quality of the electroplating target material can be effectively improved; the introduction of impurities when the target material is dissolved after the target shooting is completed is reduced, so that the separation and purification efficiency after the target shooting is completed is improved, and a more reliable technical scheme is provided for the production of the unstable isotope 68Ga by an accelerator.

Description

Technical Field

[0001] The present invention relates to the field of nuclear medicine diagnosis technology, and more specifically, to a method for producing an accelerator 68 Solid Ga 68 Method for preparing Zn target. Background Art

[0002] isotope 68 Ga is widely used in nuclear medicine diagnosis such as positron emission tomography. 68 Zn target is produced by accelerator 68 Ga target. In order to ensure 68 Ga production efficiency and quality, solid 68 Zn targets need to have uniform thickness, excellent adhesion, and high purity. 68 The commonly used methods for making Zn targets mainly include electroplating, vacuum evaporation and sputtering deposition. The vacuum evaporation method heats zinc metal to a high temperature, evaporates it in a vacuum environment, and condenses the zinc vapor on the surface of the cooled substrate to form a thin film layer. This method can generate thinner zinc targets, but the equipment cost is relatively high. The sputtering deposition method bombards the zinc target with high-energy ions, sputtering zinc atoms onto the target substrate to form a thin film. This method can achieve high-precision film deposition, but compared with the electroplating method, the process complexity and cost are higher. The electroplating method is widely used because of its simple equipment and low cost. This method deposits zinc ions on the surface of the metal substrate through an electrolytic process to form a zinc layer.

[0003] Existing solid 68 The electroplating method of Zn target has several defects in practical application: for cost considerations, copper is generally used as the substrate of the target. Since copper is easily oxidized, when the target material is dissolved with acid after accelerator target shooting, the oxidized copper substrate will be dissolved, introducing more impurities, making subsequent separation and purification more difficult; 68 Zn is generally 68 ZnO or compound form, electroplating method to make solid 68 The Zn target currently used contains 68 The solution of Zn salt deposits zinc ions in the solution through the electrolysis process. During the electroplating process, as the zinc ion concentration decreases, the amount of hydrogen reduced at the cathode increases, which easily forms pinholes or pits on the zinc coating, affecting the adhesion and uniformity of the zinc coating; when the required zinc coating thickness is large, the zinc ion concentration in the solution must be increased, and too high a concentration may cause the coating to deposit too quickly, resulting in roughness, dendrites or sintering, and insufficient adhesion of the coating.

[0004] Therefore, the present invention aims to provide a method for producing an accelerator 68 Solid Ga68 A method for preparing a Zn target is provided to solve the above problems. Summary of the invention

[0005] The purpose of the present invention is to provide a method for producing an accelerator 68 Solid Ga 68 The method for preparing a Zn target comprises the following steps: plating a nickel layer and a gold layer on a copper target in sequence, and first 68 Zn was plated onto a custom inert platinum metal plate and then plated 68 The electroplating method using a platinum metal plate with Zn as the anode can effectively improve the quality of the electroplating target and reduce the introduction of impurities when the target is dissolved after the target is shot, thereby improving the separation and purification efficiency and producing unstable isotopes for the accelerator. 68 Ga provides a more reliable technical solution.

[0006] The above technical objectives of the present invention are achieved through the following technical solutions: a method for producing an accelerator 68 Solid Ga 68 The method for preparing a Zn target comprises the following steps:

[0007] S1, pre-treating the copper target;

[0008] S2, electroplating a nickel layer on the pretreated copper target to prevent diffusion between gold and copper;

[0009] S3, electroplating a gold layer on the nickel-plated copper target to prevent more impurities from being introduced when dissolving the target;

[0010] S4. 68 Zn was plated onto a custom inert platinum metal plate and then plated 68 The platinum metal plate with Zn is used as the anode, the copper target plated with gold is used as the cathode, and the 68 The Zn salt solution is used as the electroplating solution for electroplating to maintain the zinc ion concentration in the solution during the electroplating process to ensure the adhesion and uniformity of the zinc coating.

[0011] The present invention is further configured as follows: the pretreatment operation of the copper target in step S1 includes the following process:

[0012] S11. Use sodium carbonate solution and ultrasonic cleaning equipment to clean the surface of the copper target to remove oil, dust and impurities;

[0013] S12, pickling with dilute sulfuric acid or dilute hydrochloric acid solution to remove oxides on the surface of the copper target, and thoroughly rinsing the cleaned copper target with deionized water;

[0014] S13. Use sandpaper to polish the surface of the copper target to ensure that its surface is smooth. After polishing, rinse it with dilute sulfuric acid or dilute hydrochloric acid solution, and then rinse it thoroughly with deionized water.

[0015] The present invention is further configured as follows: the process of electroplating the nickel layer on the pretreated copper target in step S2 is:

[0016] S21, prepare electroplating solution: nickel sulfate 200g / L, sulfuric acid 10-20g / L;

[0017] S22, using the copper target as a cathode and the nickel metal plate as an anode, and connecting them to a DC power supply respectively;

[0018] S23, set the current density at 10mA / cm in constant current mode 2 ;

[0019] S24, electroplating each side of the copper target for 10 minutes;

[0020] S25. After nickel plating, rinse with deionized water, then lightly polish the surface with sandpaper, and finally rinse with deionized water.

[0021] The present invention is further configured as follows: the process of electroplating the gold layer on the nickel-plated copper target in step S3 is as follows:

[0022] S31, prepare electroplating solution: 3g / L sodium chloroaurate, 20g / L potassium sulfate, 0.1g / L polyvinyl pyrrolidone, pH value is 2.5-3.5;

[0023] S32, using a nickel-plated copper target as a cathode and a platinum metal plate as an anode and connecting them to a DC power supply respectively;

[0024] S33, set the current density at 10mA / cm in constant current mode 2 ;

[0025] S34, electroplating each side of the nickel-plated copper target for 40 minutes;

[0026] S35. After the electroplating is completed, the target is taken out, rinsed with deionized water, and then dried. After drying, the zinc electroplating area is polished with sandpaper to ensure a smooth surface, and finally rinsed with deionized water.

[0027] The present invention is further configured as follows: in step S4, 68 Zn is plated onto an inert platinum metal plate customized according to the target and plating tank, and then plated 68 The platinum metal plate with Zn is used as the anode, the copper target plated with gold is used as the cathode, and the 68 The process of electroplating using a Zn salt solution as an electroplating solution is as follows:

[0028] S41, enrichment 68ZnO was dissolved in an appropriate amount of CMOS grade sulfuric acid, the pH was adjusted to 3.0-3.5 with NaOH solution, and diluted with CMOS grade sulfuric acid solution with a pH of 3.0 to a zinc ion concentration of 1 mol / L;

[0029] S42, using two platinum metal plates customized according to the target and the electroplating tank as cathode and anode respectively connected to a DC power supply;

[0030] S43, set the current density at 30mA / cm in constant current mode 2 , depositing zinc from the solution onto a platinum metal plate at the cathode;

[0031] S44, Configuration 68 Zn plating solution: 68 ZnSO4 65 g / L, potassium sulfate 20 g / L, boric acid 25 g / L, EDTA 10 g / L, sodium dodecyl sulfate 0.1 g / L, pH controlled at 3.0-3.5;

[0032] S45, with plating 68 The platinum metal plate of Zn as anode and the gold-plated target as cathode were connected to a DC power supply respectively;

[0033] S46. After connecting the circuit in constant current mode, observe the voltage change trend and adjust the current until the voltage is basically stable. 68 The Zn coating thickness is determined by the corresponding electroplating time.

[0034] In summary, the present invention has the following beneficial effects:

[0035] 1. The present invention optimizes solid 68 The method for making a Zn target, in which nickel and gold layers are plated on a copper target in sequence, can avoid the introduction of impurity elements from the source when the substrate is dissolved when the target is dissolved, thereby reducing the difficulty of subsequent separation and purification, which is beneficial to improving the separation and purification efficiency and improving the production of unstable isotopes in accelerators. 68 The yield and purity of Ga are of great significance;

[0036] 2. The present invention also comprises 68 Zn is plated onto a custom platinum metal plate and then plated 68 Platinum metal plate containing Zn as anode, 68 The solution of Zn salt is used as the electroplating solution. During the electroplating process, the anode platinum metal plate 68 Zn will lose electrons and become 68 Zn 2+The zinc ion concentration in the solution is maintained when entering the electroplating solution, and more hydrogen is prevented from being precipitated at the cathode, which can effectively solve the problems of uneven coating and poor adhesion faced in the prior art. Moreover, when the thickness of the zinc coating required for isotope production increases, the present invention only needs to extend the electroplating time without increasing the zinc ion concentration in the electroplating solution, which can avoid the excessively high zinc ion concentration from causing the coating to deposit too quickly, resulting in roughness, dendrites or sintering, etc., which affects the coating quality, and provides a more reliable technical solution for accelerator isotope production. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 It is a method for producing an accelerator in an embodiment of the present invention. 68 Solid Ga 68 Schematic diagram of the process for preparing a Zn target. DETAILED DESCRIPTION

[0038] The following is combined with Figure 1 The present invention is described in further detail.

[0039] Embodiment: A method for accelerator production 68 Solid Ga 68 The method for preparing a Zn target comprises the following steps:

[0040] 1) Pre-treatment of the copper target, including surface cleaning, pickling and polishing operations:

[0041] Clean the surface: Use sodium carbonate solution and ultrasonic cleaning equipment to clean the surface of the copper target to remove impurities such as oil, dust, etc.

[0042] Pickling: Use dilute sulfuric acid or dilute hydrochloric acid solution for pickling to remove surface oxides. The cleaned copper target is thoroughly rinsed with deionized water.

[0043] Grinding: Grind the surface of the copper target with sandpaper to ensure that its surface is smooth. After grinding, rinse it with dilute sulfuric acid or dilute hydrochloric acid solution, and then rinse it thoroughly with deionized water.

[0044] 2) Electroplating a nickel layer on the pretreated copper target to prevent diffusion between gold and copper, the process is as follows:

[0045] Prepare the plating solution: 200g / L nickel sulfate, 10-20g / L sulfuric acid. Connect the copper target (as cathode) and the nickel metal plate (as anode) to a DC power supply, and set the current density at 10mA / cm in constant current mode. 2 About 10 minutes were spent on each side of the copper target. After nickel plating, it was rinsed with deionized water, and then the surface was lightly polished with sandpaper and finally rinsed with deionized water.

[0046] 3) Electroplating a gold layer on the nickel-plated copper target, the process is as follows:

[0047] Prepare the plating solution: 3g / L sodium chloroaurate, 20g / L potassium sulfate, 0.1g / L polyvinyl pyrrolidone, pH value 2.5-3.5. Use the nickel-plated copper target as the cathode and the platinum metal plate as the anode, connected to the DC power supply, and set the current density at 10mA / cm in constant current mode. 2 Each side of the nickel-plated copper target is electroplated for about 40 minutes. After the electroplating is completed, the target is taken out, rinsed with deionized water, and then dried. The zinc plating area is polished with sandpaper to ensure a smooth surface, and finally rinsed with deionized water.

[0048] 4) 68 Zn was plated onto a custom inert platinum metal plate and then plated 68 The platinum metal plate with Zn is used as the anode, the copper target plated with gold is used as the cathode, and the 68 The solution of Zn salt is used as the electroplating solution for electroplating to maintain the zinc ion concentration in the solution during the electroplating process to ensure the adhesion and uniformity of the zinc coating. The process is as follows:

[0049] Enrich enough 68 ZnO was dissolved in an appropriate amount of CMOS grade sulfuric acid, the pH was adjusted to 3.0-3.5 with NaOH solution, and diluted with CMOS grade sulfuric acid solution with a pH of 3.0 to a zinc ion concentration of 1 mol / L.

[0050] Two platinum metal plates customized according to the target and the electroplating tank are used as cathode and anode respectively and connected to a DC power supply.

[0051] The current density was set at 30 mA / cm in constant current mode. 2 The zinc in the solution is deposited onto the platinum metal plate at the cathode.

[0052] Configuration 68 Zn plating solution: main salt 68 ZnSO4 65 g / L, conductive salt potassium sulfate 20 g / L, boric acid (to refine the coating crystals) 25 g / L, EDTA (as a complexing agent) 10 g / L, sodium dodecyl sulfate (surfactant) 0.1 g / L, pH controlled at 3.0-3.5.

[0053] Plating 68 The Zn-platinum metal plate was used as the anode and the gold-plated target was used as the cathode and connected to a DC power supply.

[0054] After connecting the circuit in constant current mode, observe the voltage change trend and adjust the current until the voltage is basically stable. 68 The Zn coating thickness is determined by the corresponding electroplating time.

[0055] This embodiment preferably includes the obtained solid 68 The Zn target was inspected for appearance, firmness, heat resistance and composition. The inspection results are as follows:

[0056] Appearance inspection: The coating is silver-gray, the surface is flat and smooth, without bubbles, pits, or pitting, etc. The edge of the coating is not burnt, and no air flow marks, scratches, or other undesirable marks are observed. When the coating is rubbed by hand, no obvious shedding is observed.

[0057] Firmness inspection: The plated parts were placed at a height of 0.5m, 1m, and 1.5m and freely dropped to the ground. No peeling or shedding of the target layer was observed before and after the impact. The relative mass difference of the target before and after the impact was less than 3×10 -5 .

[0058] Heat resistance evaluation: The target was placed in an oven at 80°C for 1 hour. No coating shedding was observed after the target was taken out.

[0059] Composition inspection: Use hydrochloric acid to 68 The Zn coating was completely dissolved, and the zinc and possible impurity metal elements were analyzed by ICP-MS after sampling. The results showed that the purity of zinc was greater than 99.34%.

[0060] This specific embodiment is merely an explanation of the present invention and is not a limitation of the present invention. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed. However, as long as they are within the scope of the claims of the present invention, they are protected by the patent law.

Claims

1. A method for accelerator production 68 Solid Ga 68 The method for preparing a Zn target is characterized by: The following steps are involved: S1, pre-treating the copper target; S2, electroplating a nickel layer on the pretreated copper target to prevent diffusion between gold and copper; S3, electroplating a gold layer on the nickel-plated copper target to prevent more impurities from being introduced when dissolving the target; S4. 68 Zn was plated onto a custom inert platinum metal plate and then plated 68 The platinum metal plate with Zn is used as the anode, the copper target plated with gold is used as the cathode, and the 68 The Zn salt solution is used as the electroplating solution for electroplating to maintain the zinc ion concentration in the solution during the electroplating process to ensure the adhesion and uniformity of the zinc coating.

2. A method for producing an accelerator according to claim 1 68 Solid Ga 68 The method for preparing a Zn target is characterized by: The pretreatment operation of the copper target in step S1 includes the following process: S11. Use sodium carbonate solution and ultrasonic cleaning equipment to clean the surface of the copper target to remove oil, dust and impurities; S12, pickling with dilute sulfuric acid or dilute hydrochloric acid solution to remove oxides on the surface of the copper target, and thoroughly rinsing the cleaned copper target with deionized water; S13. Grind the surface of the copper target with sandpaper to ensure that the surface is smooth. After grinding, rinse it with dilute sulfuric acid or dilute hydrochloric acid solution, and then rinse it thoroughly with deionized water.

3. A method for accelerator production according to claim 1. 68 Solid Ga 68 The method for preparing a Zn target is characterized by: The process of electroplating a nickel layer on the pretreated copper target in step S2 is as follows: S21, prepare electroplating solution: nickel sulfate 200g / L, sulfuric acid 10-20g / L; S22, using the copper target as a cathode and the nickel metal plate as an anode, and connecting them to a DC power supply respectively; S23, set the current density at 10mA / cm in constant current mode 2 ; S24, electroplating each side of the copper target for 10 minutes; S25. After nickel plating, rinse with deionized water, then lightly polish the surface with sandpaper, and finally rinse with deionized water.

4. A method for accelerator production according to claim 1. 68 Solid Ga 68 The method for preparing a Zn target is characterized by: The process of electroplating a gold layer on the nickel-plated copper target in step S3 is as follows: S31, prepare electroplating solution: 3g / L sodium chloroaurate, 20g / L potassium sulfate, 0.1g / L polyvinyl pyrrolidone, pH value is 2.5-3.5; S32, using a nickel-plated copper target as a cathode and a platinum metal plate as an anode and connecting them to a DC power supply respectively; S33, set the current density at 10mA / cm in constant current mode 2 ; S34, electroplating each side of the nickel-plated copper target for 40 minutes; S35. After the electroplating is completed, the target is taken out, rinsed with deionized water, and then dried. After drying, the zinc electroplating area is polished with sandpaper to ensure a smooth surface, and finally rinsed with deionized water.

5. The method for producing an accelerator according to claim 1 68 Solid Ga 68 The method for preparing a Zn target is characterized by: In step S4, 68 Zn is plated onto an inert platinum metal plate customized according to the target and plating tank, and then plated 68 The platinum metal plate with Zn is used as the anode, the copper target plated with gold is used as the cathode, and the 68 The process of electroplating using a Zn salt solution as an electroplating solution is as follows: S41, enrichment 68 ZnO was dissolved in an appropriate amount of CMOS grade sulfuric acid, the pH was adjusted to 3.0-3.5 with NaOH solution, and diluted with CMOS grade sulfuric acid solution with a pH of 3.0 to a zinc ion concentration of 1 mol / L; S42, using two platinum metal plates customized according to the target and the electroplating tank as cathode and anode respectively connected to a DC power supply; S43, set the current density at 30mA / cm in constant current mode 2 , depositing zinc from the solution onto a platinum metal plate at the cathode; S44, Configuration 68 Zn plating solution: 68 ZnSO4 65 g / L, potassium sulfate 20 g / L, boric acid 25 g / L, EDTA 10 g / L, sodium dodecyl sulfate 0.1 g / L, pH controlled at 3.0-3.5; S45, with plating 68 The platinum metal plate of Zn as anode and the gold-plated target as cathode were connected to a DC power supply respectively; S46. After connecting the circuit in constant current mode, observe the voltage change trend and adjust the current until the voltage is basically stable. 68 The Zn coating thickness is determined by the corresponding electroplating time.

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