Patent Publication Number: US-2023160843-A1

Title: Method for manufacturing reference piece for x-ray measurement of residual stress and reference piece for x-ray measurement of residual stress

Description:
TECHNICAL FIELD 
     The present invention relates to a method for manufacturing a reference piece for X-ray measurement of residual stress and a reference piece for X-ray measurement of residual stress. 
     BACKGROUND 
     In order to confirm that a measuring instrument is operating normally in X-ray measurement of residual stress, the Society of Materials Science, Japan recommends measuring a reference piece using strain-free iron powder and confirming whether or not a result close to 0 MPa (free of stress) is measured (Non-Patent Document 1). Strain-free iron powder is a substance wherein iron powder that is nearly pure iron and has been sufficiently annealed has been solidified using an adhesive or the like. Using this, it can be understood that an instrument for X-ray measurement of residual stress is operating normally. 
     In recent years, the use of instruments for X-ray measurement of residual stress in industrial fields has become common. In industrial fields, there is the potential demand to make materials used in manufacturing the subject of measurement. That is, there is the potential demand to make substances other than strain-free iron powder the subject of reference pieces for X-ray measurement of residual stress. For example, in a spring manufacturing company there would be demand for using spring materials in reference pieces for X-ray measurement of residual stress and, in a gear manufacturing company there would be demand for using the steel materials used in gears in reference pieces for X-ray measurement of residual stress. 
     CITATION LIST 
     Non-Patent Literature 
     
         
         Non-Patent Document 1: The Society of Materials Science, Japan, Standard for X-Ray Stress Measurement (2002)=Iron and Steel=, p. 73 
       
    
     SUMMARY OF INVENTION 
     Technical Problem 
     The present invention addresses the problem of providing a metal material other than strain-free iron powder as a reference piece for X-ray measurement of residual stress. 
     Solution to Problem 
     The present inventors discovered that the abovementioned problem can be solved by, after at least a portion of a surface of a metal material has been nanocrystallized, removing inherent strain by means of annealing to eliminate stress and arrived at the present invention. 
     That is, the present invention relates to (1)-(14) below. 
     (1) A manufacturing method for a reference piece for X-ray measurement of residual stress, characterized by, after at least a portion of a surface of a metal material has been nanocrystallized, stress being eliminated by annealing the same. 
     (2) The manufacturing method for a reference piece for X-ray measurement of residual stress described in (1), wherein the nanocrystallization is performed by shot peening. 
     (3) The manufacturing method for a reference piece for X-ray measurement of residual stress described in (2), characterized by the orientation of the metal material being canceled by shot peening. 
     (4) The manufacturing method for a reference piece for X-ray measurement of residual stress described in (2) or (3), characterized by only crystal grains that can withstand X-ray measurement of residual stress being left in the metal material by shot peening. 
     (5) The manufacturing method for a reference piece for X-ray measurement of residual stress described in any one of (1) to (4), wherein nanocrystals are present on the metal material surface in the range of 0-50 μm. 
     (6) The reference piece for X-ray measurement of residual stress described in any one of (1) to (5), wherein the metal material is an alloy having iron as a main component. 
     (7) The manufacturing method for a reference piece for X-ray measurement of residual stress described in any one of (1) to (6), wherein the residual stress in the reference piece for X-ray measurement of residual stress is −55 MPa or greater and 55 MPa or less. 
     (8) A reference piece for X-ray measurement of residual stress, characterized by at least a portion of a surface of a metal material being nanocrystallized and stress being eliminated by annealing. 
     (9) The reference piece for X-ray measurement of residual stress described in (8), wherein the nanocrystallization is performed by shot peening. 
     (10) The reference piece for X-ray measurement of residual stress described in (9), characterized by the orientation of the metal material being canceled by shot peening. 
     (11) The reference piece for X-ray measurement of residual stress described in (9) or (10), characterized by only crystal grains that can withstand X-ray measurement of residual stress being left in the metal material by shot peening. 
     (12) The reference piece for X-ray measurement of residual stress described in any one of (8) to (11), wherein nanocrystals are present on the metal material surface in the range of 0-50 μm. 
     (13) The reference piece for X-ray measurement of residual stress described in any one of (8) to (12), wherein the metal material is an alloy having iron as a main component. 
     (14) The reference piece for X-ray measurement of residual stress described in any one of (8) to (13), wherein the residual stress is −55 MPa or greater and 55 MPa or less. 
     Effects of Invention 
     According to the present invention, a metal material other than strain-free iron powder can be provided as a reference piece for X-ray measurement of residual stress. 
    
    
     
       BRIEF DESCRIPTION OF DRAWINGS 
         FIG.  1    shows a Debye-Scherrer ring obtained when a raw spring material was annealed. The Debye-Scherrer ring is distorted, so it is understood that the effects when rolled remain even after annealing. 
         FIG.  2    shows a Debye-Scherrer ring obtained when, after annealing a metal material of which at least a portion of a surface thereof had been nanocrystallized by shot peening, the metal material was irradiated with X-rays. The orientation when rolled is eliminated by shot peening, so an orientation is not observed after annealing. 
     
    
    
     DESCRIPTION OF EMBODIMENTS 
     The present invention is not limited to the following embodiments and can be implemented by adding changes, as appropriate, so long as the changes do not hinder the effects of the present invention. In the present invention, “A-B” means “A or greater and B or less.” 
     Crystallinity is critical for stress-free reference pieces for X-ray measurement of residual stress. When measuring with X-rays, the conditions that (1) crystal grains should not coarsen, (2) there should be no orientation, that is, the direction of the crystals should not be aligned anywhere, and (3) the measurement results are obtained near 0 MPa (free of stress) are required. In (3), a stress measurement coefficient is multiplied by the slope obtained from a cos α graph or a sin 2Ψ graph, so in actuality, 0 MPa cannot be calculated. Accordingly, some degree of variation in the numerical values is permitted. 
     One embodiment of the present invention shall be explained in detail below. 
     [Nanocrystallization of the Surface of the Metal Material] 
     In the present invention, any method, so long as it is a means capable of nanocrystallization, can be used in the nanocrystallization of the surface of the metal material. For example, shot peening, ECAP (Equal-Channel Angular Pressing) methods, and HPT (High-Pressure Torsion) methods can be used. Among these, shot peening is preferred because it is capable of canceling the orientation of the metal material and, by setting conditions under which nanocrystals are generated on the surface of the metal material, even if crystallization conditions were to be met when annealing, it is capable of leaving only crystal grains that can withstand X-ray measurement of residual stress in the metal material. In the present invention, “canceling the orientation of the metal material” means scattering the orientation of metal crystal planes facing in the same direction generated by the manufacturing process by recrystallizing/micronizing the same largely by means of shot peening. Further, in the present invention, “only crystal grains that can withstand X-ray measurement of residual stress” means that a certain number of crystal grains for obtaining reliability in the results of the X-ray measurement of residual stress are present within the range of the X-ray measurement of residual stress. 
     As conditions for the shot peening, the hardness and particle diameter of the projected material and the projection speed must be selected according to the type of the metal material. For example, the hardness of the projected material is appropriately selected from the Vickers hardness (JIS Z 2244) range of HV 1200-3000 (preferably HV 1700-3000) and the grain size number (JIS R 6001) appropriately selected from the range of 20-220 (preferably 30-100). Further, for the projection speed, for example, when projecting (jetting) the projected material using an air acceleration device, the projection air pressure is selected, as appropriate, from the range of 0.05-1.0 MPa (preferably 0.1-0.5 MPa). 
     Nanocrystallization means crystallization on the nano scale. In the present invention, the grain diameter of the nanocrystals is preferably 1-50 nm, more preferably 1-10 nm, and yet more preferably 1-5 nm. 
     [Elimination of Stress by Annealing] 
     Annealing (tempering) means a process for heating a metal material to a suitable temperature and, after maintaining this temperature for a certain amount of time, slow-cooling. Annealing has effects such as the elimination of internal stress, the reduction of hardness, and the improvement of workability. In the present invention, “eliminating stress” means getting the residual stress of the reference piece as close to 0 MPa as can be by eliminating only the strain generated by working. 
     The number of times annealing is performed is preferably from 3 to 5. Further, by annealing at 720° or lower, coarsening of carbides is prevented and the micro state of carbides prior to quenching is maintained. Annealing is preferably performed by using a bright annealing furnace to heat to 180-500° C., more preferably to heat to 300-500° C., and yet more preferably to heat to 450-500° C. By using a bright annealing furnace, there is no generation of oxide scales on the surface of the metal material and a pickling process becomes unnecessary. 
     [Range in which the Nanocrystals are Present] 
     In the present invention, the nanocrystals are preferably present in a range of 0-50 μm on the metal material surface (in other words, a range of up to 50 μm in depth from the outermost surface), more preferably present in a range of 0-15 μm, and yet more preferably present in a range of 0-10 μm. 
     [Metal Material] 
     Various types of metal materials can be used in the present invention. Alloys having iron as a main component are preferred as the metal material in the present invention, in particular SCM (steel chromium molybdenum steel materials), SUP (spring steel steel materials), SPCC (normal steel), SPHC (general hot-rolled steel materials), and S10C (carbon steel for machine structures) are preferably used and SCM and SUP are more preferably used. 
     [Residual Stress of the Reference Piece for X-Ray Measurement of Residual Stress] 
     In the present invention, the residual stress of the reference piece for X-ray measurement of residual stress is preferably −55-55 MPa, more preferably −25-25 MPa, and yet more preferably −10-10 MPa. 
     Examples 
     The following examples are shown to more specifically explain the present invention, but the present invention is not limited by these examples. 
     [Shot Peening (SP)] 
     Shot peening (SP) was performed on SCM, SUP, SPCC, SPHC, and S10C under the conditions shown in Table 1 and nanocrystal layers formed on the surfaces of the metal materials. 
     [Annealing (Thermal Treatment)] 
     Next, annealing (thermal treatment) was performed under the conditions shown in Table 1 and stress eliminated. 
     Those cells in which “−” is written in Table 1 indicate that the relevant treatment was not performed. 
     Measurement of the residual stress for each piece was performed using the residual stress measurement instrument described in JP 2017-009356 A. The results are shown in Table 1. 
     
       
         
           
               
               
             
               
                 TABLE 1 
               
               
                   
               
             
            
               
                   
                 MATERIAL 
               
            
           
           
               
               
               
            
               
                   
                 SCM 
                 SUP 
               
            
           
           
               
               
            
               
                   
                 THERMAL TREATMENT 
               
            
           
           
               
               
               
               
               
               
               
               
            
               
                   
                   
                   
                   
                   
                   
                 ANNEALING 
                 ANNEALING 
               
               
                   
                   
                   
                   
                   
                   
                 QUENCHING 
                 QUENCHING 
               
               
                   
                   
                   
                 ANNEALING 
                   
                   
                 AND 
                 AND 
               
               
                   
                 ANNEALING 
                 ANNEALING 
                 VACUUM 
                 ANNEALING 
                 ANNEALING 
                 TEMPERING 
                 TEMPERING 
               
               
                   
                 — 
                 — 
                 CARBURIZATION 
                 — 
                 — 
                 HV 500 
                 HV 450 
               
               
                   
               
               
                 SHOT MATERIAL 
                 RCW03PS 
                 AM150B 
                 — 
                 — 
                 RCW03PS 
                 RCW03PS 
                 RCW03PS 
               
            
           
           
               
               
               
               
               
            
               
                 SHOT TECHNIQUE 
                 AIRYPE 
                   
                   
                 AIR PRESSURE 
               
            
           
           
               
               
               
               
               
               
               
               
            
               
                 PROJECTION 
                 0.1 
                 0.1 
                 — 
                 — 
                 0.1 
                 0.1 
                 0.1 
               
               
                 PRESSURE [MPa] 
                   
                   
                   
                   
                   
                   
                   
               
               
                 JETTING TIME [min] 
                 2 
                 1 
                 — 
                 — 
                 1 
                 1 
                 1 
               
               
                 RESIDUAL STRESS 
                 −34 
                 −31 
                 5 
                 −31 
                 −29 
                 −30 
                 −40 
               
               
                 [MPa] 
                   
                   
                   
                   
                   
                   
                   
               
               
                 HALF-WIDTH [deg] 
                 2.5 
                 2.5 
                 2.61 
                 2.55 
                 2.46 
                 2.52 
                 2.32 
               
               
                 COUNT RATE  
                 24.367 
                 24.033 
                 22.367 
                 25.187 
                 24.500 
                 24.167 
                 24.033 
               
               
                 [kcount/s] 
                   
                   
                   
                   
                   
                   
                   
               
               
                 DIFFRACTION RING 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
               
               
                   
               
            
           
           
               
               
            
               
                   
                 MATERIAL 
               
            
           
           
               
               
               
            
               
                   
                 SCM 
                 SUP 
               
            
           
           
               
               
            
               
                   
                 THERMAL TREATMENT 
               
            
           
           
               
               
               
               
               
               
               
               
            
               
                   
                   
                   
                   
                   
                   
                 ANNEALING 
                 ANNEALING 
               
               
                   
                   
                   
                 ANNEALING 
                   
                   
                 QUENCHING 
                 QUENCHING 
               
               
                   
                 ANNEALING 
                 ANNEALING 
                 VACUUM 
                 ANNEALING 
                 ANNEALING 
                 AND 
                 AND 
               
               
                   
                 — 
                 — 
                 CARBURIZATION 
                 — 
                 — 
                 HV 500 
                 HV 450 
               
               
                   
               
               
                 SHOT MATERIAL 
                 RCW03PS 
                 FeCrB80 
                 RCW03PS 
                 — 
                 RCW03PS 
                 RCW03PS 
                 RCW03PS 
               
            
           
           
               
               
               
               
            
               
                 SHOT TECHNIQUE 
                 AIR TYPE 
                 — 
                 AIR PRESSURE 
               
            
           
           
               
               
               
               
               
               
               
               
            
               
                 PROJECTION 
                 0.1 
                 0.1 
                 0.1 
                 — 
                 0.1 
                 0.1 
                 0.1 
               
               
                 PRESSURE [MPa] 
                   
                   
                   
                   
                   
                   
                   
               
               
                 JETTING TIME [min] 
                 6 
                 1 
                 5 
                 — 
                 3 
                 3 
                 3 
               
               
                 RESIDUAL STRESS 
                 −35 
                 −24 
                 11 
                 −31 
                 −32 
                 −32 
                 −31 
               
               
                 [MPa] 
                   
                   
                   
                   
                   
                   
                   
               
               
                 HALF-WIDTH [deg] 
                 2.51 
                 2.55 
                 2.69 
                 2.5 
                 2.52 
                 2.54 
                 2.48 
               
               
                 COUNT RATE  
                 23.233 
                 23.133 
                 20.600 
                 23.900 
                 23.733 
                 23.367 
                 23.900 
               
               
                 [kcount/s] 
                   
                   
                   
                   
                   
                   
                   
               
               
                 DIFFRACTION RING 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 MATERIAL 
                   
               
            
           
           
               
               
               
               
               
               
               
            
               
                   
                   
                   
                   
                   
                 STRAIN-FREE 
                   
               
               
                   
                 SPCC 
                 SPHC 
                 S10C 
                 SUP 
                 IRON POWDER 
                   
               
            
           
           
               
               
               
            
               
                   
                 THERMAL TREATMENT 
                   
               
            
           
           
               
               
               
               
               
               
               
            
               
                   
                 ANNEALING 
                 ANNEALING 
                 ANNEALING 
                 ANNEALING 
                 ANNEALING 
                   
               
               
                   
               
               
                 SHOT MATERIAL 
                 RCW03PS 
                 RCW03PS 
                 RCW03PS 
                 SB25 
                 — 
                   
               
               
                 SHOT TECHNIQUE 
                 AIR TYPE 
                 AIR TYPE 
                 AIR TYPE 
                 IMPELLER TYPE 
                 — 
                   
               
               
                 PROJECTION 
                 0.1 
                 0.1 
                 0.1 
                 — 
                 — 
                   
               
               
                 PRESSURE [MPa] 
                   
                   
                   
                   
                   
                   
               
               
                 JETTING TIME [min] 
                 1 
                 1 
                 1 
                 — 
                 — 
                   
               
               
                 RESIDUAL STRESS 
                 11 
                 52 
                 30 
                 −30 
                 −1 
                   
               
               
                 [MPa] 
                   
                   
                   
                   
                   
                   
               
               
                 HALF-WIDTH [deg] 
                 2.32 
                 2.36 
                 2.49 
                 2.5 
                 2.88 
                   
               
               
                 COUNT RATE 
                 16.178 
                 15.143 
                 20.529 
                 23.633 
                 20.733 
                   
               
               
                 [kcount/sec.] 
                   
                   
                   
                   
                   
                   
               
               
                 DIFFRACTION RING 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                 
                   
                 
                   
               
               
                   
               
            
           
           
               
               
               
            
               
                   
                 MATERIAL 
                   
               
            
           
           
               
               
               
               
               
               
               
            
               
                   
                   
                   
                   
                   
                 STRAIN-FREE 
                   
               
               
                   
                 SPCC 
                 SPHC 
                 S10C 
                 SUP 
                 IRON POWDER 
                   
               
            
           
           
               
               
               
            
               
                   
                 THERMAL TREATMENT 
                   
               
            
           
           
               
               
               
               
               
               
               
            
               
                   
                 ANNEALING 
                 ANNEALING 
                 ANNEALING 
                 ANNEALING 
                 ANNEALING 
                   
               
               
                   
               
               
                 SHOT MATERIAL 
                 RCW03PS 
                 RCW03PS 
                 RCW03PS 
                 SB25 
                 — 
                   
               
               
                 SHOT TECHNIQUE 
                 AIR TYPE 
                 AIR TYPE 
                 AIR TYPE 
                 IMPELLER TYPE 
                 — 
                   
               
               
                 PROJECTION 
                 0.1 
                 0.1 
                 0.1 
                 — 
                 — 
                   
               
               
                 PRESSURE [MPa] 
                   
                   
                   
                   
                   
                   
               
               
                 JETTING TIME [min] 
                 5 
                 5 
                 5 
                 — 
                 — 
                   
               
               
                 RESIDUAL STRESS 
                 18 
                 −12 
                 −32 
                 −26 
                 7 
                   
               
               
                 [MPa] 
                   
                   
                   
                   
                   
                   
               
               
                 HALF-WIDTH [deg] 
                 2.36 
                 2.5 
                 2.51 
                 2.45 
                 2.88 
                   
               
               
                 COUNT RATE 
                 20.633 
                 11.363 
                 17.400 
                 25.333 
                 20.988 
                   
               
               
                 [kcount/sec.] 
                   
                   
                   
                   
                   
                   
               
               
                 DIFFRACTION RING