Method for accurately calculating proton irradiation stored energy

Abstract

The invention discloses a method for accurately calculating proton irradiation stored energy, and belongs to the field of proton irradiation stored energy. The invention aims to solve the problem that no accurate method for calculating the stored energy of proton irradiation exists at present. The method comprises the following steps: preparing two samples, and performing complete annealing heat treatment; performing proton irradiation treatment on one of the surfaces; respectively carrying out DSC test on the non-irradiated sample and the irradiated sample to obtain a heat flow curve A1 of the non-irradiated sample and a heat flow curve B1 of the irradiated sample; data of the curve A1 and the curve B1 at the temperature of 200-800 DEG C are selected and recorded as A2 and B2 respectively, the difference value of the heat flow values of A2 and B2 at the temperature of 200 DEG C is an error value C, the error value C is subtracted from the heat flow value of the original B2 to obtain a curve B3, and the curve difference of B3 and A2 at the temperature of 600-800 DEG C is calculated to obtain a heat flow curve D; and performing baseline searching and peak searching on the curve D, searching the position of an exothermic peak, and calculating the area of the exothermic peak, namely the irradiation stored energy of the sample material under the irradiation condition. According to the method, few samples are required for calculation, and the result is accurate.

Description

Technical Field

[0001] The present invention belongs to the field of proton irradiation storage energy, and specifically relates to a method for accurately calculating proton irradiation storage energy. Background Art

[0002] Proton irradiation is an important method for surface modification of metals and alloys. After proton irradiation, irradiation energy is stored on the alloy surface. These stored energies can be used in subsequent processes and are pretreatment methods for processes such as diffusion bonding or interfacial reactions. Quantitative calculation of proton irradiation storage energy has important guiding significance for subsequent processes. For example, the interfacial diffusion coefficient can be quantitatively predicted through storage energy, and the connection temperature and pressure parameters can be optimized. However, there is currently no accurate method for calculating the storage energy of proton irradiation. Currently, methods such as computer software simulation are mainly used for estimation (such as calculating displacement damage dpa using the Monte Carlo method and then inferring storage energy), or theoretical model calculations are carried out based on irradiation dose (such as theoretical calculations using displacement damage models and thermodynamic models). However, due to reasons such as simplification of thermodynamic parameters and over-simplification of models, there are large deviations from the actual values. Summary of the Invention

[0003] The present invention aims to solve the technical problem that there is currently no accurate method for calculating the storage energy of proton irradiation, and provides a method for accurately calculating proton irradiation storage energy.

[0004] In order to achieve the above technical problem, the present invention adopts the following technical solutions:

[0005] The present invention aims to provide a method for accurately calculating proton irradiation storage energy, including the following steps:

[0006] Step 1: After making 2 specimens;

[0007] Step 2: Perform full annealing heat treatment on both specimens;

[0008] Step 3: Perform proton irradiation treatment on the surface of one of the annealed specimens;

[0009] Step 4: Perform DSC tests on the unirradiated and irradiated specimens respectively to obtain the heat flow curve A1 of the unirradiated specimen and the heat flow curve B1 of the irradiated specimen;

[0010] Step 5: Select the data of curve A1 from 200°C to 800°C as A2, and select the data of curve B1 from 200°C to 800°C as B2. The difference in heat flow values of B2 and A2 at 200°C (B2 - A2) is the error value C. Calibrate curve B2 through the error value C, that is, subtract the error value C from the original heat flow value of B2 to obtain curve B3. Calculate the curve difference between B3 and A2 from 600°C to 800°C, which is the heat flow difference, denoted as curve D. Perform baseline finding and peak finding on curve D, find the position of the exothermic peak, and calculate the area of the exothermic peak, which is the irradiation storage energy of the sample material under irradiation conditions.

[0011] Further defined, the present invention is applicable to the test of irradiation storage energy of titanium alloys, etc.; the titanium alloy can be TC4 titanium alloy, etc.

[0012] Further defined, in step 1, the material to be characterized is cut into a cuboid of 2mm×2mm×1mm to obtain the sample.

[0013] Further defined, in step 2, annealing heat treatment: the vacuum degree is not higher than 1×10 -3 Pa, heat up to 600°C at a heating rate of 7°C / min, heat up to 750°C at a heating rate of 5°C / min, hold for 120 min at 750°C, cool with the furnace to 480°C, and air-cool to room temperature.

[0014] Further defined, in step 3, proton irradiation treatment is performed on the surface of the 2mm×2mm sample.

[0015] Further defined, in step 5, the DSC test parameters are: use an inert gas (such as argon) as the protective gas, select an Al2O3 crucible, the flow rate of the protective gas is 25 mL / min, the heating rate is 10°C / min, and heat up to 1200°C.

[0016] Further defined, in step 5, the baseline finding adopts the asymmetric least squares smoothing method, and the peak finding adopts the maximum and minimum value method.

[0017] Further defined, in step 5, the peak area is calculated by the integration method.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] The present invention calculates the proton irradiation storage energy through an experimental method, has the advantages of high sensitivity, high calculation accuracy, avoiding the assumption errors of simulation and models, etc., and the results are closer to the true values. The samples required for calculation are extremely few, the measurement is simple, and the results are accurate.

[0020] To further understand the features and technical content of the present invention, please refer to the following detailed description of the present invention and the accompanying drawings. However, the attached drawings are only for reference and illustration purposes and are not used to limit the present invention. Description of the Drawings

[0021] Figure 1 is a flowchart of the method of the present invention;

[0022] Figure 2 is the heat flow curve A1 of the unirradiated specimen;

[0023] Figure 3 is the heat flow curve B1 of the irradiated specimen;

[0024] Figure 4 is the heat flow curve A2 of the unirradiated specimen at 200°C to 800°C;

[0025] Figure 5 is the heat flow curve B2 of the irradiated specimen at 200°C to 800°C;

[0026] Figure 6 is the heat flow curve B3 of the irradiated specimen after calibration and post-treatment;

[0027] Figure 7 is the heat flow difference curve D between the irradiated and unirradiated specimens. Detailed Embodiments

[0028] The present invention will be described in detail below in conjunction with specific embodiments. The following embodiments will help those skilled in the art to further understand the present invention, and at the same time do not limit the present invention in any form. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made. These all belong to the protection scope of the present invention.

[0029] Example 1:

[0030] Material to be characterized: TC4 titanium alloy.

[0031] Step 1. Fabricate DSC samples: Use wire electrical discharge machining to cut the base material into two cuboids with dimensions of 2 mm × 2 mm × 1 mm.

[0032] Step 2. Full annealing heat treatment: Perform full annealing heat treatment on the two specimens, evacuate to 1×10 -3 Pa, heat up at a heating rate of 7°C / min to 600°C, heat up at a heating rate of 5°C / min to 750°C, hold at 750°C for 120 min, cool with the furnace to 480°C, and air-cool to room temperature.

[0033] Step 3: Place one of the specimens in the irradiation chamber for irradiation test. Irradiate the surface of 2 mm × 2 mm with irradiation parameters of irradiation energy of 200 keV, irradiation flux of 5×10 11 p / cm 2 ·s, and irradiation fluence of 5×10 14 p / cm 2 .

[0034] Step 4: Conduct DSC tests on the unirradiated and irradiated specimens respectively. The equipment selected for the test is NETZSCH STA 449F3. Use Ar as the protective gas with a flow rate of 25 mL / min. Select an Al2O3 crucible. The heating rate is 10 °C / min and heat up to 1200 °C. Obtain the heat flow curve A1 ( Figure 2 ) of the unirradiated specimen and the heat flow curve B1 ( Figure 3 ) of the irradiated specimen:

[0035] 5. Calibrate the heat flow curve B1 of the irradiated specimen using the heat flow curve A1 of the unirradiated specimen; the method is:

[0036] Select the data of the A1 curve from 200 °C to 800 °C as A2 ( Figure 4 ), and select the data of the B1 curve from 200 °C to 800 °C as B2 ( Figure 5 ):

[0037] The heat flow value of A2 at 200 °C is 0.17572 mW / mg, and the heat flow value of B2 at 200 °C is 0.09567 mW / mg. The error value C = B2(200 °C) - A2(200 °C) = 0.09567 - 0.17572 = -0.08005 mW / mg.

[0038] Calibrate the curve B2 through the error value C to obtain the curve B3 ( Figure 6 ):

[0039] Calculate the curve difference between B3 and A2, which is the heat flow difference, and limit the temperature range of 600 °C to 800 °C, denoted as curve D.

[0040] Perform baseline finding and peak finding on the curve D ( Figure 7 ). For baseline finding, use the "asymmetric least squares smoothing method", and for peak finding, use the "maximum and minimum method" to find the position of the exothermic peak and calculate the area of the exothermic peak. The peak area is calculated by the integral method, which is the irradiation storage energy of the material under irradiation conditions.

[0041] According to the calculation, the irradiation energy is 200 keV, the irradiation flux is 5×10 11 p / cm 2 ·s, and the irradiation fluence is 5×10 14 p / cm2 The stored energy of proton irradiation of TC4 titanium alloy is 12.68 J / g at this time.

[0042] The specific embodiments of the present invention have been described above. It should be noted that the present invention is not limited to the above specific embodiments, and those skilled in the art can make various deformations or modifications within the scope of the claims, which does not affect the essence of the present invention.

Claims

1. A method for accurately calculating proton irradiation storage energy, characterized in that: The following steps are involved: Step 1: After making 2 samples; Step 2, performing complete annealing heat treatment on all samples; Step 3, performing proton irradiation treatment on the surface of one of the annealed samples; Step 4, performing DSC tests on the unirradiated and irradiated samples respectively to obtain a heat flow curve A1 of the unirradiated sample and a heat flow curve B1 of the irradiated sample; Step 5, select the 200℃~800℃ data of curve A1 as A2, select the 200℃~800℃ data of curve B1 as B2, the difference between the heat flow values ​​of A2 and B2 at 200℃ (B2-A2) is the error value C, calibrate curve B2 by the error value C, that is, subtract the error value C from the original heat flow value of B2 to obtain curve B3, calculate the curve difference between B3 and A2 at 600℃~800℃, that is, the heat flow difference, recorded as curve D; Perform baseline search and peak search on curve D, find the position of the exothermic peak, and calculate the exothermic peak area, which is the irradiation storage energy of the sample material under irradiation conditions.

2. The method according to claim 1, characterized in that: The material of the specimen is titanium alloy.

3. The method according to claim 1, characterized in that: The material of the sample is TC4 titanium alloy.

4. The method according to claim 1, characterized in that: The material to be characterized was cut into a cuboid of 2 mm × 2 mm × 1 mm to obtain the sample.

5. The method according to claim 4, characterized in that: The surface of the sample with an area of ​​2 mm × 2 mm was treated with proton irradiation.

6. The method according to claim 4, characterized in that: Annealing heat treatment: vacuum degree is not higher than 1×10 -3 Pa, heat up to 600 °C at a heating rate of 7 °C / min, heat up to 750 °C at a heating rate of 5 °C / min, keep at 750 °C for 120 min, cool to 480 °C with the furnace, and air cool to room temperature.

7. The method according to claim 1, characterized in that: The DSC test parameters are as follows: inert gas is used as the protective gas, Al2O3 crucible is selected as the crucible, the protective gas flow rate is 25 mL / min, the heating rate is 10°C / min, and the temperature is raised to 1200°C.

8. The method according to claim 7, characterized in that: The inert gas is argon.

9. The method according to claim 1, characterized in that: The baseline was found by asymmetric least squares smoothing method, and the peak was found by maximum and minimum method.

10. The method according to claim 1, characterized in that: The peak areas were calculated using the integration method.

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