TWI294465B - - Google Patents

Description

1294465 IX. Description of the Invention: The present invention relates to titanium copper excellent in strength, electrical conductivity, and bending workability, and a method for producing the same. [Prior Art] With the miniaturization and weight reduction of electronic equipment, electrical and electronic components such as connectors have been continuously reduced in size and weight (thinner and narrower). When the connector is thinned and narrowly pitched, the contact area and the conductivity are reduced due to the reduction of the cross-sectional area due to the reduced cross-sectional area of the contact. Therefore, the metal material for the joint is required to be higher. The strength of the 盥 conductivity. Further, as the parts are miniaturized, the metal material used may be subjected to severe bending work, and therefore the metal material must have good bending workability. Regarding high-strength copper alloys, the use amount of the age-hardening type copper alloy has been increasing in recent years. Age hardening type copper alloy will be solution treated

The supersaturated solid solution is subjected to aging treatment so that fine precipitates are dispersed in the alloy. Among the steel alloys of the day-effect hardening type, in particular, a copper alloy containing ruthenium (hereinafter referred to as "Iron copper") has high mechanical strength and excellent bending workability, and is widely used for various terminals and connections S of electronic equipment.

Titanium copper which has been put into practical use in the industry is JIS, and the grade brake is Jib Cl 990, and the alloy contains 2. 9~3. 5mass% of the ii 〇7 mouth R Shi Shizhou J Shi βΒ τ as Japanese Patent Special Open 7-258803 As described in the examples of the patent publications (Patent Document 1) and JP-A-2002-356726 (Patent Document 8), sufficient strength cannot be obtained when the T1 content is too low. 5 1294465 Age-hardening type high strength like titanium copper The copper alloy may be high bismuth copper (JIS C1 720). Compared with high bismuth copper, titanium copper has the same performance in strength and bending workability, but is excellent in stress relaxation resistance, such as a weathering test fixture (burn). - in socket) and other applications requiring heat resistance, titanium copper is more suitable than bismuth copper. On the other hand, in terms of electrical conductivity, titanium copper is 10~16% IACS, and its conductivity is higher than that of high bismuth copper. %IACS is poor. Therefore, bismuth copper is used for applications requiring electrical conductivity. However, in the case of yttrium high copper, the bismuth compound is toxic and its manufacturing process is complicated by the high cost 'so the titanium copper Need to keep rising. If there is solid solution of titanium in copper, the conductivity By reducing the amount of Ti in the form of a cu_ Τι intermetallic compound phase, the amount of solid solution titanium can be reduced to increase the conductivity. In the specification of Japanese Patent Application No. 2003-78751 (Patent Document 3), the pair contains 2_5 to 4. The titanium oxide of 5 mass% titanium is used to adjust the amount of precipitation of the Cu_n intermetallic compound phase to improve the electrical conductivity. However, as a result of analyzing the bending workability of the copper disclosed in the specification, the bending workability is remarkably deteriorated. It is confirmed that a large amount of Cu_Tf metal = compound phase precipitates as a crack origin, which is confirmed by a large amount of precipitated Cu-Tf metal. In particular, when there is a Cu-Ti intermetallic compound phase having a diameter exceeding 2 #m, f. The curvature of the workability (4) is optimized by the crystal grain # and the final calendering degree, and the strength and bending workability of the titanium copper can be considered (for example, see Patent Document 2). However, the current technology In addition, it is not possible to achieve the improvement of the overall strength of the titanium-copper strength, the bending workability, and the electrical conductivity. [Patent Document 1] JP-A-H07-258803 (Patent Document 2) JP-A-2002-356726, No. 1,294,465 Patent Document 3] The present invention provides a titanium copper which is excellent in strength, electrical conductivity, and bending workability. The inventors of the present invention have excellent strength and excellent bending workability. Titanium copper, which is not inferior to the conductivity of sorghum copper, has been intensively studied and found to be optimal by adjusting the size and area ratio of Ti and Cu-Ti intermetallic compound phases and the average crystal grain size. Titanium copper having desired strength, electrical conductivity and bending workability can be obtained. The reason why the copper and titanium shown in Patent Document 3 is deteriorated in bending workability is a large amount of precipitated coarse Cu-Ti intermetallic compound phase. According to the present invention, the Ti concentration can be reduced, the coarse Cu-Ti intermetallic compound phase can be reduced, and the structure and production conditions can be further optimized to obtain desired strength and bending workability at a low Ti concentration. (1) The titanium copper excellent in strength, electrical conductivity, and bending workability of the present invention is a copper alloy composed of 1·5 to 2·3 mass% of Ti, a residual part of Cu, and unavoidable impurities, and is 0.2% safe. The stress limit is 750 MPa or more, the conductivity is 17% iacs or more, and the minimum bending radius (MBR, mm) and plate thickness (t, where no crack occurs) when the W bending test described in JIS H3130 is performed in the direction perpendicular to the rolling direction. The relationship between mm ratio (MBR/t) and 0.2% safety limit stress (YS, MPa) has a relationship of MBR/tSO. 〇4xYS _ 30. (2) The above-mentioned titanium copper is a Cu-Ti intermetallic compound having a thickness of 1.5 to 2·3 mass% of Ti, a residual part of Cu, and a copper alloy composed of unavoidable impurities, which is observed in a cross section perpendicular to the rolling direction. The phase diameter is 2. 0 // m or less, and the blocking resistance is in contact with the rolling direction 7 1294465. Therefore, the 0.2% safety limit stress must be 750MPa or more. A better 0.2% safety limit stress is 8 〇〇 MPa or more. (3) Bending processability center When the material is applied to various terminals and connectors, the balance of the 〇·2% safety limit stress “bow bending processability is very important. The inventors have focused on the Τ丨 concentration of 1·5+~2.3. Titanium copper with a maSS% and a conductivity of 17% ucs or more, and the relationship between the 安全·2% safety limit stress and the bending workability required for the recent electric actuator is determined by the analysis of the material for the connector. One of the requirements is that, in order to achieve the balance between strength and bending workability, in accordance with recent requirements, titanium copper must satisfy the minimum crack occurrence when the boundary bending test described in US H3130 is performed in the direction perpendicular to the rolling direction. Bending radius (臓, ^ mm) 0nbm(MBR/t)^ 〇.2%^^P^^(YS, MPa)fa1 has the relationship of MBR/tS〇.〇4xYS~ 30. (4) If the titanium content is correct Titanium steel is subjected to aging treatment, and spinodine decomposition (spin〇dai decompositiGn) is generated to produce a titanium concentration adjustment structure in the base material, whereby a very high titanium content can be obtained, and it is difficult to obtain a pa. The above 0.2% safety limit stress. On the other hand, the content is more than the amount, When it is produced under the conditions that the conductivity m is equal to or higher than that, the coarse Cu_Tl intermetallic compound phase having a diameter exceeding 2/m is precipitated, which deteriorates the bending workability of the material. Therefore, the titanium copper of the present invention is deteriorated. The Ti-containing shirt is h 5~2·3 %%, and the ratio = 1.6~2.Qmass%. Titanium copper in this Ti concentration range has been used up to date. Although it has been mentioned in the patent literature towel, it is still not possible. The strength 'bending property, 'the gross rate is improved in a well-balanced manner. For example, 'Special opening--356726'! 9 1294465 The embodiment discloses an alloy having a Ti content of 1. 7 mass%, and the conductivity of the alloy is 2 〇·3% ucs. It is equivalent to the alloy of the present invention, but its 2% safety limit stress is only 71 MPa. The second embodiment of JP-A-2002-356726 discloses an alloy having a Ti content of 1·5 mass% and 2.3 mass%, but The 0.2% safety limit stresses are 72〇MPa and U8〇Mpa, respectively, and the electrical conductivity is 26.4% IACS and 10.2% IACS, respectively, and cannot meet the requirements of strength and conductivity at the same time. (5) Cu-Ti intermetallic phase Diameter

By depositing Ti in the form of a Cu-Ti intermetallic phase, the Ti phase can be reduced and the conductivity can be improved. However, when the straight line of the smallest circle of the Cu-Ti intermetallic compound phase (the maximum diameter of the cu-Ti intermetallic compound phase) exceeds 2.0/zm in the cross section perpendicular to the rolling direction, the material will be bent. The starting point of the crack during processing is deteriorated, and the bending workability is deteriorated. Therefore, the diameter of the Cu-Ti intermetallic compound phase is set to be 2/zm or less. (6) Area ratio of Cu-Ti intermetallic phase In order to increase the conductivity of titanium and copper, it is quite important to analyze Ti to minimize the reduction of Ti ϊ: That is, the conductivity can be increased by increasing the amount of the cu-Ti intermetallic compound phase. Further, by depositing a fine Cu_Ti intermetallic compound phase, it is possible to increase the strength of the material. The inventors have found that the titanium-copper having a Ti content of 1. 5~2. 3mass% is observed in a cross section perpendicular to the rolling direction. The diameter of the Cu-Ti intermetallic compound phase is 0. 02~2. The area ratio (S%) and the Ti content ([Ti]mass%) can obtain a conductivity of 17% IACS or more as long as the relationship of &8·1χ[Ti]-ιι·5 is satisfied. On the other hand, even if the Cu_Ti intermetallic compound precipitated is in the range of 2·0 // m or less, if s exceeds 7.5%, the bending workability of the material is deteriorated, so that the 〇2 prescribed by the present invention is retained. It is difficult to balance the % safety limit stress with the curvature of 1294465. Then, the area ratio S of the Cu-Ti intermetallic compound phase is 8.1 χ [ Τι] - 11 · 5 $ Ss7 · 5. Further, it has been found that as long as the Ti contains 1·5 to 2.0 mass% and satisfies the relationship of 81χ[Ti]-9.5<%7·5, the safety limit stress of the present invention can be satisfied. The relationship with the bending workability and the conductivity of 20% IACS or more is obtained. (7) Average crystal grain size

When the average crystal grain size of the cross section perpendicular to the rolling direction (measured by the cutting method of η Η 050 1) exceeds 1 〇, the effect of the strength between the materials obtained by refining the crystal grains is not good, so it is difficult Obtain the above, 2/0 Anwang limit stress. Further, if the average crystal grain size is adjusted to less than 2 " m ', the non-recrystallized portion may remain, and if there is no recrystallized portion remaining, f: workability may be deteriorated. Thus, the titanium-copper system of the present invention has an average crystal grain size of a cross section of the direction of the money of 2 to 10 m. (8) The heat of the manufacturing method 2 The hydrazine is sequentially subjected to the dissolution casting and casting of the raw materials, and the lyophilization, solution treatment, and solid-state release before treatment are performed; the aging treatment is carried out under appropriate conditions, It can be a piece. Titanium copper of the invention characteristics. The following describes the manufacturing of each step. When the material is recrystallized, the strain will become the core due to the strain of the grain ▲. The more cold-rolling processing before solution treatment, the more the re-crystallized grains are introduced by Jiang Gue, and the inhibition of crystal grains is inhibited by Yang.

1294465 A fine crystal grain size can thus be obtained. When the cold rolling degree before the solution treatment is set to 89% or more, an average crystal grain size of 10/zm or less can be obtained. The solid solution treatment of the solid solution of the titanium and copper is generally carried out at a temperature equal to or higher than the temperature at which a Ti is equal to a T1 / □. However, if the solution treatment is carried out in this temperature range, the crystal grain size will exceed 1 〇//m. The inventors of the present invention obtained a solution treatment temperature range in which a crystal grain size of 2 to 1 Å/m was stably obtained by an experiment. That is, when the solution treatment temperature τ (. ^ in D. > [6580 / Π · 35 - ln [Ti]}] - 273 (χ represents Ti content), the crystal grain size will exceed l 〇 / / ra It is difficult to obtain a safety limit stress of 75 〇 MPa or more. Also, when the solution treatment temperature τ is at T < 658 〇 / {7 · 35 - ln [Ti] - 333, the crystal grain size will be low. At 2//m, the bending processability difference of the material is determined accordingly, and the temperature T of the fixation treatment is set at [658〇/{7·35 - ln[Ti]}] 333 一丁一[ 6580/{ 7.35 - 111 [1^]}] A range of 273, the crystal grain size of 2 to 1 〇 can be obtained. Also, when the heating temperature from the solution treatment to the average cooling rate of the intermuscular material is lower than 3G ( Rc / sec, in the material cooling, the intermetallic phase with a diameter of more than 2 〇 _ will precipitate out of the grain boundary, so when bending stress is applied to the material, it will easily crack at the grain boundary. Based on this, it will be solid. The average cooling rate of the melting treatment is set to be less than c/sec. Further, the cooling method at this time is not particularly limited, and water cooling is generally used in most cases. _> Cold-drying processing after the treatment; the cold-rolling degree after the solidification and glutenization treatment is not hardened to achieve high strength, and it is difficult to obtain the full-limit stress, and the strain introduced by the rolling is small, and it is impossible to process by 10%. 750 750 MPa or more 〇 2% aging treatment step 12 1294465 The intermetallic compound phase precipitation rate is slow, difficult to obtain long. The above conductivity. When the degree of processing exceeds 70%, the ductility will be obvious - The warpage property is deteriorated, and it is difficult to obtain the relationship between the 0.2% female full stress and the bending workability of the present invention. Based on this, the cold-drying degree after the treatment is set to 10 to 7 G%. The relationship between Wenwang's limit of force and 'bow processability' is preferably 40 to 65% of the cold rolling degree after solution treatment.

In order to precipitate the Cu-buti intermetallic compound phase defined by the present invention, for example, the aging conditions are adjusted as follows. (1) Heating temperature The heating temperature is less than 35 (TC), the Cu-Ti intermetallic compound phase is insufficiently precipitated, and the 〇2% safety limit stress of 750 MPa or more cannot be obtained, and the above conductivity is obtained. Further, when the heating temperature exceeds 450° In the case of C, since the Cu_Ti intermetallic compound phase will be coarsened, the (four) degree and the bending workability will be deteriorated. Based on this, the heating temperature is set to 35 〇 to 45 (rc. The heating temperature here refers to the material used to heat the material. (2) Holding time at heating temperature When the holding time at the heating temperature is less than 5 hours, the precipitation of the Cu-Ti intermetallic compound phase is insufficient, and it is difficult to obtain a conductivity of 17% IACS or more. When the holding time exceeds 2 hrs, the Cu-Ti intermetallic compound phase will be coarsened, so the strength and bending workability will be deteriorated. Based on this, the holding time at the heating temperature is set to 5 to 2 hrs. Keeping the day-to-day guard refers to the time from the temperature of the material to the temperature of the furnace until the start of cooling. 13 1294465 (3) Average cooling rate

In the aging treatment, if the average cold portion speed from the heating temperature to 2 〇 (rc is 5 (TC/hour is fast, the precipitation of the Cu-Ti intermetallic compound phase is insufficient, it is difficult to obtain a conductivity of 17% IACS or more. When the average cooling rate is less than HTC/hour, the Cu-Ti intermetallic compound phase precipitates significantly. The area ratio of the Cu-Ti intermetallic compound phase with a diameter of 0.02 to 2.0 (4) will exceed 17. The bending and curing properties are deteriorated. Therefore, the average cooling rate from the heating temperature to 20 ITC at the time of the aging treatment is set to 1 〇 5 (rc / hr. [Example] _ using electrolytic copper as a raw material" is melt-cast by a high-frequency vacuum melting furnace. Ingots of various compositions (width 6Gmmx thick Hi heat-dried into 8_thick. After that, the cold rolling, solution treatment after solution treatment, cold rolling and aging treatment after solution treatment are carried out under the conditions shown in Table! It is necessary to change the average crystal grain size, the size and area ratio of the Cu_Ti intermetallic compound phase, and the solution treatment is maintained for 1 minute after the temperature of the test material reaches the surface temperature, and then cooled. Speed Cooling, 嗔 翕 翕 、, into ^, 飞 卩 卩 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺 贺The thermocouple is smelted on the test material, and the temperature of the test material reaches the step (room temperature) as the average cooling rate. During the aging treatment, the temperature of the test material is determined by controlling the furnace temperature to change the cold speed. The average cooling rate from the heating temperature to the range of c. 14 1294465 , for each of the alloys thus obtained, the 〇· 2% safety limit stress, electrical conductivity, bending workability (MBR/t), and cross section perpendicular to the rolling direction were evaluated. The average crystal grain size, the size of the Cu-Ti intermetallic compound phase, and the area ratio. The 0.2% safety limit stress is measured by a tensile tester in accordance with JIS Z2241. The conductivity is based on the JIS H0505 4-terminal method. The measurement was carried out. The evaluation of the mold and the % curvature was carried out. (Bei, a rectangular sample having a width of 1 mm and a length of 5 〇 was used (the longitudinal direction of the sample was the vertical direction of the rolling direction), and the bending was performed at various bending radii. Bending test (JIS H3130), and This extension copper association technical standard JBMA T3〇7: • The evaluation criteria are compared to evaluate the appearance of the convex portion of the curved portion, and the ratio of the minimum bending radius (mm) to the thickness (mm) without cracking is obtained (MBR/t) The average crystal grain size (//m) is measured by etching the cross section perpendicular to the rolling direction (water (100 ml) - FeC13 (5 g) - HCl (10 ml)) to scan the electron microscope The crystal grain of the etched surface was observed, and the crystal grain size was calculated by the cutting method (JIS H0501). The Cu-Ti intermetallic compound phase precipitated in the alloy was observed by fe-SEM (XL30SFEG, manufactured by FEI Corporation, Japan). The section perpendicular to the rolling direction of the material was ground with a water-resistant abrasive paper of #150, and then mirror-polished with a polishing agent mixed with a silicone resin having a particle diameter of 4 〇 nm, and the obtained "material was subjected to slave plating. Each of the alloys has a reflection electron image of the field of view 1 〇〇# at a magnification of 10,000 times, and changes the field of view to observe five parts. Then, using an image analysis device, the phase of the Cu-Ti containing intermetallic compound in the observation field is obtained. The diameter and area ratio of the small circle. Regarding the evaluation of the size of the Cu-Ti intermetallic compound phase, the alloy having a diameter exceeding 2·〇μιη is evaluated as another, • there will be no diameter exceeding 2.0//m. The alloy was evaluated as ◦. Regarding the evaluation of the area of 15 1294465, the Cu-Ti intermetallic compound phase with a diameter of 〇·02~2.0//m was used as the object of measurement. The total area of the Cu-Ti intermetallic compound phase was divided by observation. The total area of the field of view, the obtained value is the area ratio of the Cu-T i intermetallic compound phase. Table 2 shows the evaluation results of the respective alloys. Inventive Example 1 to 丨〇, which satisfies the Ti content and crystal grain size specified in the present invention, Cu-Ti intermetallicization The size and area ratio of the phase show a conductivity of 1 7% I ACS or more, a 0.2% safety limit stress of 75 OMPa or more, and the relationship between 〇·2% safety limit stress (YS) and MBR/t also satisfies the present invention. In particular, the Ti content is in the range of 丨.5 to 2. 〇mass%, and the area ratio s of the Cu-Ti intermetallic compound phase satisfies the invention example 2 of & ιχ[Ti] -11·5SSS7.5. 4, 7, and 10, the electrical conductivity is more than 2% IACS. Further, the Ti content is in the range of L6 to 2.0 mass%, and the calendering degree after the solution treatment is 4G 65% Fan® inventive examples 2 and 5' Compared to the other examples, when the 〇·2% safety limit stress is equivalent, it shows better bending workability (MBR/t), and when the bending workability is equivalent, it shows a higher 〇·2% safety limit stress.

On the other hand, in Comparative Example 11, since 丁, 、, and 11 / Chen are too low, a 0.2% safety limit stress of 750 MPa or more cannot be obtained. In Comparative Example 12, since the Ti concentration is too high, a coarseness of 2 〇 or more is precipitated.

The Cu-h intermetallic compound phase and the area ratio of the Cu_Ti intermetallic compound phase are outside the scope of the present invention, and the bending workability of the present invention cannot be obtained. Further, in Comparative Example 13, since the degree of processing before the solution treatment was low, the +-average crystal grain size after the solution treatment was more than 12%, and the safety limit stress was not reached. In Comparative Example U, since the solution treatment temperature is lower than the range of the present invention, the Q portion remains, and the size and area ratio of the Cu-Tl intermetallic compound phase exceed 16 1294465, which is within the scope of the present invention, and the present invention cannot be obtained. Bending workability. 2%。 。 5% MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa MPa Safety limit stress. In Comparative Example 16, since the average cooling rate after the solution treatment was slow, a coarse Cu-Ti intermetallic compound phase of 2.0 / zm or more was precipitated, and the bending workability prescribed by the present invention could not be obtained.

In Comparative Example 17, since the calendering degree after the solution treatment was too low, a 0.2% safety limit stress of 750 MPa or more could not be obtained, and the precipitation rate of the Ti treated by the aging treatment was slow, and the area ratio of the Cu-Ti intermetallic compound phase was lower. The range of the present invention does not provide conductivity of 17% IACS or more. In Comparative Example 18, since the degree of calendering after the solution treatment was too high, the bending workability prescribed by the present invention could not be obtained. In Comparative Example 19, since the heating temperature at the time of the aging treatment was too low, the 0.2% safety limit stress of 750 MPa or more could not be obtained due to insufficient aging treatment, and the area ratio of the Cu-Ti intermetallic compound phase was lower than the range of the present invention, and Conductivity of 17% IACS or more was obtained. In Comparative Example 20, the heating temperature of the aging treatment was too high, and the Cu-Ti intermetallic compound phase was coarsened due to overaging, and the relationship between the 0.2% safety limit stress and the bending workability was not satisfied. In Comparative Example 21, since the heat retention time of the aging treatment was short, the area ratio of the Cu-Ti intermetallic compound phase was lower than the range of the present invention, and the conductivity of 17% IACS or more was not obtained. In Comparative Example 22, since the heating retention time of the aging treatment was too long, the Cu_Ti intermetallic compound phase was coarsened due to the overaging effect 17 1294465, and the # method satisfies the relationship between the 0.2% safety limit stress and the bending workability specified in the present invention. . In Comparative Example 23, since the average cooling rate of the aging treatment was fast, the area ratio of the Cu-Ti intermetallic compound phase was lower than the range of the present invention, and the conductivity of 17% IACS or more was not obtained. In Comparative Example 24, since the average cooling rate of the aging treatment was slow, the area ratio of the Cu-Ti intermetallic compound phase exceeded the range of the present invention, and the bending workability prescribed by the present invention could not be obtained.

18 1294465

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Claims (1)

1294465 X. Patent application scope · 1· A titanium steel excellent in strength, electrical conductivity, and bending workability is a copper alloy containing ~2.3 mass% Ti, a residual portion of Cu, and unavoidable impurities, 0.2% The safety limit stress (YS) is 750 MPa or more, and the electrical conductivity (^^ is 17% IACS or more 'when the w bending test described in JIS H3130 is performed in the direction perpendicular to the rolling direction, the minimum bending radius (MBR) is not generated. The relationship between 〇 and plate thickness (t, ratio (MBR/t) and 0.2% safety limit stress (YS, MPa) has MBR/t. 〇4xYS -3 0. 2 · Titanium copper, which is excellent in strength, conductivity, and bending workability, is a copper alloy composed of 1.5 to 2.3 mass% of Ti, a residual part of Cu, and an unavoidable impurity. The diameter of the Cu-Τι intermetallic compound phase observed in the cross section perpendicular to the rolling direction is 2 〇//m or less, and the diameter of the Cu-Ti metal of the G.G2~2.G/zm is observed in the cross section perpendicular to the rolling direction. The area ratio (S%) of the inter-compound phase and the Ti content ([Ti], mass%) are the cross-sections that satisfy the relationship of 8·1χ[Ti]-丨丨·μ%·· 5 and perpendicular to the direction of the extension. The average crystal grain size (measured by the Yichuan leg 〇 1 method) is 2 to 10 // m. d• A method for manufacturing titanium and copper, which is to carry out hot rolling, cold-drying/solidification treatment, cold rolling and aging treatment of ingots to produce copper, which is characterized by 'the cold rolling degree before solution treatment” # 89%以上,Solution treatment ΤΓΟ^ [ 6580/( 7. 35^ΐη[ τη }] ^333,1, [6580/丨7· 35-In[ Τι]丨]—273 'The average of solution treatment The cooling rate is 30〇c/t or more, and the cold-drying degree before the defensive treatment is ~·, the force at the aging is.../the degree of the dish is 350~450 C, and the heating retention time is 5~2〇, aging treatment The average cooling rate from the heating temperature (four) is 〖(一)代/小时. 22 1294465 十一,图: no twenty three