CN102517621B - Method for preparing anode made of copper-phosphorus alloy - Google Patents
Method for preparing anode made of copper-phosphorus alloy Download PDFInfo
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- CN102517621B CN102517621B CN201110460344.7A CN201110460344A CN102517621B CN 102517621 B CN102517621 B CN 102517621B CN 201110460344 A CN201110460344 A CN 201110460344A CN 102517621 B CN102517621 B CN 102517621B
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Abstract
A method for preparing an anode made of a copper-phosphorus alloy comprises the following steps in sequence: conducting first heat treatment on an ingot and forging in sequence for three times; conducting second heat treatment on the ingot after the last time of forging; conducting cold rolling on the ingot to form a blank; conducting third heat treatment on the blank; and machining the blank after the third heat treatment, so as to form the anode made of the copper-phosphorus alloy. According to the method, the combination of repeated plastic deformation with a specific deformation rate and annealing treatment under specific temperature is mainly adopted, and the deformation rate of the plastic deformation, the temperature during the annealing treatment, and the time of the annealing treatment are controlled strictly, so that the anode meeting the requirements on internal grain size and grain orientation for electroplating can be produced.
Description
Technical field
The present invention relates to field of electroplating, the preparation method of the copper-phosphorus alloy anode in the galvanic anode that particularly a kind of semi-conductor is used.
Background technology
Electroplating (Electroplating) utilizes electrolysis principle on some metallic surface, to plate the process of other metal or alloy of skim.It utilizes electrolysis principle to make the surface attachment layer of metal film of metal or other material product, prevents from corrosion from improving the effects such as wear resistance, electroconductibility, reflective and having improved aesthetic appearance thereby play.
In the coating bath that fills electroplate liquid, with the unplated piece through cleaning and special pre-treatment, as negative electrode, metal lining is as anode, and the two poles of the earth connect with negative pole and the positive pole of direct supply respectively.Electroplate liquid is made up of the aqueous solution of salt, buffer reagent, pH adjusting agent and the additive etc. of the compound that contains metal lining, conduction.After energising, the metal ion in electroplate liquid, is moved to and on negative electrode, forms coating in the effect of potential difference.The metal of anode forms metal ion and enters electroplate liquid, with the concentration of the metal ion that keeps being plated.At present, can select high purity copper-phosphorus alloy as anode.
The making processes of copper-phosphorus alloy anode generally comprises: be smelted into the steps such as ingot casting, homogenizing processing, viscous deformation processing, thermal treatment, on the strict basis of controlling galvanic anode purity, by selecting different viscous deformation processing, heat-treat condition, grain orientation, the grain-size etc. of adjusting copper-phosphorus alloy anode, finally meet the requirement of electroplating process.
But the method for the crystal grain thinning of copper-phosphorus alloy anode is also immature at present, therefore the grain orientation of copper-phosphorus alloy anode of the prior art, grain-size can not meet plating requirement, make the metallic film of unicircuit even not.
Therefore, utilize existing installation, copper-phosphorus alloy anode of how producing grain orientation, the satisfied plating requirement of grain-size just becomes those skilled in the art's problem demanding prompt solution.
Summary of the invention
The object of the invention is to utilize existing installation, produce grain orientation, the satisfied copper-phosphorus alloy anode requiring of electroplating of grain-size, the plating performance of copper-phosphorus alloy anode is improved.
For achieving the above object, the invention provides a kind of preparation method of copper-phosphorus alloy anode, comprising:
Ingot casting is carried out to the first thermal treatment, then forge, carry out successively described forging and described the first thermal treatment, altogether carry out three times;
Described ingot casting to the first thermal treatment and after forging carries out the second thermal treatment;
Described ingot casting after the second thermal treatment is carried out to cold rolling formation blank;
Described blank after cold rolling is carried out to the 3rd thermal treatment;
Described the 3rd heat treated blank is carried out to mechanical workout, form copper-phosphorus alloy anode.
Optionally, described the first thermal treatment temp is 850 DEG C～950 DEG C.
Optionally, the deformation rate of each described forging is 50%～70%.
Optionally, for the third time forge after, before the second thermal treatment, described ingot casting is carried out to cooling process for the first time.
Optionally, described the second thermal treatment temp is 650 DEG C～750 DEG C, and soaking time is 55min～65min.
Optionally, after described the second thermal treatment, cold rolling before, carry out cooling process for the second time.
Optionally, described cold rolling deformation rate is 80%～90%.
Optionally, described the 3rd heat treated temperature is 650 DEG C～750 DEG C, and soaking time is 55min～65min.
Optionally, in the 30s after described the 3rd thermal treatment, described blank is carried out to cooling process for the third time fast.
Optionally, in described the 3rd thermal treatment, the tolerance of thermal treatment temp is ± 5 DEG C.
Compared with prior art, the technical program has the following advantages:
(1) under the processing mode of the technical program and processing parameter, be that copper-phosphorus alloy ingot casting of 2000 μ m left and right is made as copper-phosphorus alloy anode that grain-size is 70 μ m～100 μ m by grain-size, enable to meet and electroplate requirement.
(2) be 50%～70% 850 DEG C～950 DEG C deformation rates of carrying out forging for three times, forging at every turn, can better improve weave construction and the mechanical property of copper-phosphorus alloy ingot casting, copper-phosphorus alloy cast structure makes original thick dendritic crystal grain and columnar grain smash to become small grains after three forging method thermal processing distortions, original segregation in copper-phosphorus alloy ingot casting, loose, pore, slag inclusion etc. are compacted and seam, its tissue becomes tightr, has improved plasticity and the mechanical property of copper-phosphorus alloy ingot casting.
(3) adopt the cold-rolling treatment of repeatedly rolling on rolling press, just the shape of the copper-phosphorus alloy ingot casting through cold-rolling treatment is become to thinner copper-phosphorus alloy blank.Because the plasticity of the copper-phosphorus alloy ingot casting through cold-rolling treatment is better, meet processing requirement, therefore do not need to carry out the crystal grain of the next above-mentioned processing copper-phosphorus alloy of the further refinement ingot casting of recrystallize processing in hot rolling.
The deformation rate of each calendering is 8%～10%, total deformation rate is 80%～90% cold rolling mode, realizing total calendering degree can meet the structure properties of copper-phosphorus alloy inside as inhomogeneity improvement degree, and the thickness of the final copper-phosphorus alloy blank forming meets the needs of galvanic anode, and each deformation rate is all smaller, avoid copper-phosphorus alloy, in the process of this strong viscous deformation of calendering, crackle or other defect occur.
(4) copper-phosphorus alloy ingot casting is carried out to the first thermal treatment, the first heat treated mode is for to be heated to 850 DEG C～950 DEG C by copper-phosphorus alloy ingot casting.In this temperature range, the crystal orientation of the final copper-phosphorus alloy ingot casting forming distributes can meet forging requirement.
(5) the described ingot casting after cooling process is for the first time carried out to the second thermal treatment, the second heat treated mode is to be slowly warmed up to 650 DEG C～750 DEG C, insulation 55min～65min, then naturally cooling.Making the element output solid-state diffusion in copper-phosphorus alloy, alleviate the ununiformity of chemical composition, is mainly the ununiformity that alleviates the chemical composition in crystal particle scale, can also eliminate the unrelieved stress after copper-phosphorus alloy inside forges.
(6) copper-phosphorus alloy is carried out to the 3rd heat treatment mode for being slowly warmed up to 650 DEG C～750 DEG C, insulation 55min～65min, can make copper-phosphorus alloy interior tissue carry out recrystallize, further make copper-phosphorus alloy blank crystal grain become equi-axed crystal more uniformly, further reduce the demixing phenomenon of copper-phosphorus alloy interior tissue, eliminate strain-hardening, recover plasticity and the deformability of copper-phosphorus alloy blank, can also keep metal or alloy surface-brightening.
Brief description of the drawings
Fig. 1 is process flow diagram of the present invention.
Fig. 2 to Fig. 4 is the schematic diagram of the copper-phosphorus alloy ingot casting before three forging procesies are carried out in the present invention and after carrying out.
Fig. 5 and Fig. 6 are the schematic diagram of cold-rolling process in the present invention.
Fig. 7 is the schematic diagram of the last copper-phosphorus alloy anode forming of the present invention.
Fig. 8 is the schematic diagram of copper-phosphorus alloy blank in cold rolling step in the embodiment of the present invention.
Fig. 9 is the schematic diagram of copper-phosphorus alloy anode of the present invention.
Figure 10 is copper-phosphorus alloy anode crystal grain schematic diagram of the present invention.
Embodiment
The present invention is mainly by the method for the heat treatment phase combination under viscous deformation and the specified temp of certain variations rate repeatedly, and strictly control the deformation rate of viscous deformation, heat treated temperature, time realize making to meet and electroplate the grain orientation of use, copper-phosphorus alloy anode of grain-size.
The research that contriver is wholwe-hearted and practice repeatedly improve the method that obtains optimum making copper-phosphorus alloy anode, and its technical process as shown in Figure 1, wherein mainly comprises the following steps:
Step S11, carries out the first thermal treatment to ingot casting, then forges, and carries out successively described the first thermal treatment and described forging, altogether carries out three times;
Step S12, the described ingot casting to the first thermal treatment and after forging carries out cooling process for the first time;
Step S13, carries out the second thermal treatment to the described ingot casting after cooling process for the first time;
Step S14, carries out cold rolling formation blank to the described ingot casting after the second thermal treatment;
Step S15, carries out the 3rd thermal treatment to described blank after cold rolling;
Step S16, carries out mechanical workout to described the 3rd heat treated blank, forms copper-phosphorus alloy anode.
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.Set forth detail in the following description so that fully understand the present invention.But the present invention can be different from alternate manner described here and implements with multiple, and those skilled in the art can do similar popularization without prejudice to intension of the present invention in the situation that.Therefore the present invention is not subject to the restriction of following public embodiment.
Execution step S11, carries out the first thermal treatment to ingot casting, then forges, and carries out successively described the first thermal treatment and described forging, altogether carries out three times.
The general purity requirement of copper-phosphorus alloy of semiconductor copper-phosphorus alloy anode is more than 4N (99.99%), the content that is copper-phosphorus in copper-phosphorus alloy is more than 99.99%, for example, be 4N5 (99.995%) or 5N (99.999%).In the present embodiment, be preferably copper-phosphorus alloy ingot casting of 4N5 (99.995%), the grain-size of copper-phosphorus alloy ingot casting is now 2000 μ m left and right.Described copper-phosphorus alloy ingot casting can be the right cylinder that 235mm～245mm, height h1 are 20mm～50mm for diameter, and its size is determined according to the size of default copper-phosphorus alloy anode of producing.
The present embodiment, the cross section of copper-phosphorus alloy ingot casting is circular, in other embodiments, described copper-phosphorus alloy ingot casting can be also other shapes, as rectangle, square, annular, other rule or irregular shapes.
Copper-phosphorus alloy ingot casting is carried out to the first thermal treatment, and the first heat treated mode is for to be heated to 850 DEG C～950 DEG C by copper-phosphorus alloy ingot casting.In this temperature range, the crystal orientation of the final copper-phosphorus alloy ingot casting forming distributes can meet forging requirement.The words of excess Temperature, can cause the grain-size of generation of recrystallize larger, make the last copper-phosphorus alloy anode forming can not meet the requirement of plating, and temperature is too low or do not carry out heat treated words for the first time, follow-up forging will be carried out not too easily, be not fine for the effect of improving copper-phosphorus alloy inside ingot aspect of performance, and in forging process, easily there is crackle in copper-phosphorus alloy ingot casting.
Then the described ingot casting after the first thermal treatment is forged for the first time.
The described embodiment forging is for the first time for utilizing air hammer to carry out multidirectional strike to copper-phosphorus alloy ingot casting, comprise along with the circumferential direction of high purity copper-phosphorus alloy ingot casting, high purity copper-phosphorus alloy ingot casting being impacted, or be that the upper surface that utilizes air hammer to face toward high purity copper-phosphorus alloy ingot casting impacts.Along circumferential direction, copper-phosphorus alloy ingot casting is impacted the height of copper-phosphorus alloy ingot casting is increased, and cross-sectional area reduces, and the upper surface of copper-phosphorus alloy ingot casting is impacted the height of copper-phosphorus alloy ingot casting is reduced, and cross-sectional area increases.
Summary after contriver repeatedly puts into practice, to forge the degree of the deformation rate of copper-phosphorus alloy ingot casting being weighed to forging, described deformation rate represents with Δ H, it is defined as:
ΔH＝|h1-h2|/h1
In the present embodiment, wherein, h1 forges the height of copper-phosphorus alloy ingot casting before for the first time, and h2 is the height that has forged for the first time rear copper-phosphorus alloy ingot casting.
In the present embodiment, adopt two kinds of forging modes utilizing air hammer to impact and utilize air hammer to impact the upper surface of copper-phosphorus alloy ingot casting along the circumferential direction of copper-phosphorus alloy ingot casting to copper-phosphorus alloy ingot casting to hocket.
Described being forged to for the first time compressed forging, and the copper-phosphorus alloy ingot casting forging after finishing is for the first time the first forging intermediate, and described first forges intermediate and forge for the first time compared with previous copper-phosphorus alloy ingot casting, and its deformation rate reaches 50%～70%.Before and after described forging for the first time, as shown in Figure 2, in the present embodiment, the described first height that forges intermediate is h2 to copper-phosphorus alloy ingot casting situation.
Then the first forging intermediate is carried out to the first thermal treatment again.The first heat treated mode is for to be heated to 850 DEG C～950 DEG C by copper-phosphorus alloy ingot casting.
Then first after the first thermal treatment again being forged to intermediate forges for the second time.Described be forged to for the second time stretch forge, copper-phosphorus alloy ingot casting after end is the second forging intermediate, described second forges intermediate and forges for the second time compared with previous copper-phosphorus alloy ingot casting (described first forges intermediate), the height h2 of the first forging intermediate is stretched, its deformation rate reaches 50%～70%, before and after described forging for the second time, as shown in Figure 3, in the present embodiment, the described second height that forges intermediate is h3 to copper-phosphorus alloy ingot casting situation.
Then the second forging intermediate is carried out to the first thermal treatment for the third time.The first heat treated mode is for to be heated to 850 DEG C～950 DEG C by copper-phosphorus alloy ingot casting.
Then second after the first thermal treatment being forged to intermediate forges for the third time.Described being forged to for the third time compressed forging, and the copper-phosphorus alloy ingot casting after finishing is for forging body, and described process of forging is for the third time identical with the process of forging for the first time.Described forging body, compared with forging for the third time previous copper-phosphorus alloy ingot casting (second forges intermediate), compresses the height h3 of the second forging intermediate, and its deformation rate reaches 50%～70%.Before and after described forging for the second time, as shown in Figure 4, in the present embodiment, the height of described forging body is h4 to copper-phosphorus alloy ingot casting situation.
In this step, the first heat treated temperature is greater than the recrystallization temperature of copper-phosphorus alloy ingot casting, so three forgings carrying out in this step are all forge hot, the advantage of in the present embodiment, copper-phosphorus alloy ingot casting being carried out to three forge hots comprises following three aspects::
1, can reduce the resistance to deformation of copper-phosphorus alloy ingot casting, thereby reduce the copper-phosphorus alloy ingot casting required forging force of when distortion being forged, the dynamics that forging and stamping are applied reduces greatly;
2, improve the plasticity of copper-phosphorus alloy ingot casting, especially in the present invention when the lower temperature the more crisp copper-phosphorus alloy ingot casting that is difficult to forging and stamping particularly important;
3, in the present embodiment, the number of times forging is that three times, each deformation rate of forging are 50%～70%, can better improve like this weave construction and the mechanical property of copper-phosphorus alloy ingot casting, copper-phosphorus alloy cast structure makes original thick dendritic crystal grain and columnar grain smash to become small grains after three forging method thermal processing distortions, original segregation in copper-phosphorus alloy ingot casting, loose, pore, slag inclusion etc. are compacted and seam, its tissue becomes tightr, has improved plasticity and the mechanical property of copper-phosphorus alloy ingot casting.The degree of forging is inadequate, and for the effect of improving of copper-phosphorus alloy inside ingot tissue, and the degree of grain refining is inadequate, the performance of copper-phosphorus alloy anode of the final formation of impact.And deformation rate is too large, because copper-phosphorus alloy is hard and crisp, there is crackle in work in-process easily.
Then perform step S12, the described ingot casting after forging is carried out to cooling process for the first time.
Cooling copper-phosphorus alloy ingot casting can be the described forging body of last forge hot to be put into water carry out cooling water-cooling pattern, but not as limit, process for cooling can be also the mode of air-cooled or air cooling.Why cool to room temperature, be cooled to room temperature, can make the poor maximization of cooling temperature, and cooling energy maximizes, and is conducive to the crystal grain homogenizing more of copper-phosphorus alloy ingot casting after forge hot.Due to described process for cooling and prior art indifference, be well known to those skilled in the art, therefore do not repeat them here.
Then perform step S13, the described ingot casting after cooling process is for the first time carried out to the second thermal treatment.
Described ingot casting after cooling process is for the first time carried out to the second thermal treatment, and the second heat treated mode is to be slowly warmed up to 650 DEG C～750 DEG C, insulation 55min～65min, then naturally cooling.
The second heat treated main purpose is:
(1) make the element in copper-phosphorus alloy produce solid-state diffusion, alleviate the ununiformity of chemical composition, alleviate the ununiformity of the chemical composition in crystal particle scale.
(2) eliminate the unrelieved stress after copper-phosphorus alloy inside forges, stable dimensions, hardness and the fragility of attenuating copper-phosphorus alloy, increase its plasticity-, reduces distortion and crackle tendency in subsequent technique.
(3) because 650 DEG C～750 DEG C of temperature in this step are higher than 450 DEG C～600 DEG C of the recrystallization temperatures of copper-phosphorus alloy, and insulation 55min～65min.So in current heat treatment process, primary recrystallization also can be carried out in copper-phosphorus alloy inside, further dwindle the size of crystal grain after above-mentioned forging and can make the uniform crystal particles of dwindling.Heating temperature is too low, and in copper-phosphorus alloy ingot casting, crystal grain recrystallize is insufficient or without recrystallize phenomenon; Heating temperature is too high, and in copper-phosphorus alloy ingot casting, crystal grain is easily grown up, and size can surpass scope; Soaking time is too short, and in copper-phosphorus alloy ingot casting, crystal grain is heated inhomogeneously, and recrystallize is insufficient; Soaking time is long, and in copper-phosphorus alloy ingot casting, crystal grain is easily grown up, and size can surpass scope.In actual applications, can be at the concrete numerical value that carries out presetting before the second thermal treatment above-mentioned each parameter, wherein, described Heating temperature and soaking time can be set according to certain corresponding relation, for example 700 DEG C of * 60min etc.
Then perform step S14, the described ingot casting after the second thermal treatment is carried out to cold rolling formation blank.
Also comprise copper-phosphorus alloy ingot casting is carried out to cooling for the second time process before cold rolling carrying out, described cooling copper-phosphorus alloy ingot casting for the second time can be described copper-phosphorus alloy ingot casting to be put into water carry out cooling water-cooling pattern, but not as limit, process for cooling can be also the mode of air-cooled or air cooling.Be cooled to room temperature.Due to described process for cooling and prior art indifference, be well known to those skilled in the art, therefore do not repeat them here.
Then carry out cold rolling to copper-phosphorus alloy ingot casting.As shown in Figure 5, Figure 6, described cold rolling mode is between two rollers 8 of rolling press (calender), the upper and lower surface of being pushed copper-phosphorus alloy ingot casting that thickness is h4 originally by roller 8, the thickness that dwindles copper-phosphorus alloy ingot casting is h5, and launches its sectional area.Through calendering repeatedly, finally the extension of copper-phosphorus alloy ingot casting being become to thickness is the metal nahlock (as shown in Figure 7) of h, forms copper-phosphorus alloy blank.The thickness h of copper-phosphorus alloy blank that general calendering forms is afterwards 25mm～35mm.
The deformation rate of the copper-phosphorus alloy ingot casting in the present embodiment is all 8%～10%, and copper-phosphorus alloy blank that final calendering forms is compared with the copper-phosphorus alloy ingot casting before calendering, and its deformation rate is 80%～90%.In order to make the various piece of the copper-phosphorus alloy blank after calendering more even more consistent, preferably, described copper-phosphorus alloy ingot casting is often once rolled, all can carry out again calendering next time after rotating same preset angles to the copper-phosphorus alloy ingot casting after calendering.In the present embodiment, described preset angles is between 30 °～150 °.
Please first referring to Fig. 8, direction in Fig. 8 shown in four-headed arrow is the direction that copper-phosphorus alloy ingot casting directly rolls, direction shown in unidirectional arrow is the direction that copper-phosphorus alloy ingot casting is rotated, and 1～8th shown in Fig. 8, for the convenient mark of determining the angle to being rotated after described copper-phosphorus alloy ingot casting calendering and set.For instance, if some o'clock on copper-phosphorus alloy ingot casting has rotated to 8 position from 3 inverse position hour hands, can know that described copper-phosphorus alloy ingot casting has been rotated counterclockwise 135 ° in calender line.If rotated to 2 position from 3 inverse position hour hands at some o'clock on copper-phosphorus alloy ingot casting, can know that described copper-phosphorus alloy ingot casting has been rotated counterclockwise 45 ° in calender line, in the present embodiment, after every pair of copper-phosphorus alloy ingot casting once rolls, the rotation that equal angular is carried out to it in capital is more even to guarantee the copper-phosphorus alloy ingot casting after calendering, the great angle of rotation of concrete employing, is determined by practical situation.In the present embodiment, preferably, described preset angles is 135 °.
In actual applications, every calendering calendering amount once can correspondingly be adjusted according to actual demand, to make copper-phosphorus alloy ingot casting to be calendered to the size that meets copper for semi-conductor-phosphorus alloy anode in optimum mode.
Calender line of the present invention does not need the temperature of described copper-phosphorus alloy ingot casting to monitor in real time.Adopt calendering process of the present invention, when the temperature of the copper-phosphorus alloy ingot casting after thermal treatment from preset value close to time, the attenuation of copper-phosphorus alloy ingot casting, more easily calendering, make copper-phosphorus alloy ingot casting at the above calendering formation of preset temperature value, to save the step of copper-phosphorus alloy ingot casting being carried out to Real-Time Monitoring.
The calendering of this step just becomes thinner copper-phosphorus alloy blank by the shape through above-mentioned processing copper-phosphorus alloy ingot casting.Because the plasticity through above-mentioned processing copper-phosphorus alloy ingot casting is better, meet processing requirement, therefore do not need to carry out the crystal grain of the next above-mentioned processing copper-phosphorus alloy of the further refinement ingot casting of recrystallize processing in hot rolling.
In the present embodiment, described to above-mentioned copper-phosphorus alloy ingot casting cold rolling effect can also eliminate the defect of microstructure, be compacted at short textures such as high temperature and pressure-acting bubble, crackles, thereby make the copper-phosphorus alloy blank forming organize more closely knitly, mechanical property also improves.This improvement is mainly reflected in along in rolling direction, is no longer isotropic body to a certain extent thereby make copper-phosphorus alloy.
This step adopts repeatedly calendering, and control the deformation rate of each calendering 8%～10%, total deformation rate is 80%～90% mode, realizing total calendering degree can meet the structure properties of copper-phosphorus alloy inside as inhomogeneity improvement degree, and the thickness of the final copper-phosphorus alloy blank forming meets the needs of copper-phosphorus alloy anode, and each deformation rate is all smaller, avoid copper-phosphorus alloy, in the process of this strong viscous deformation of calendering, crackle or other defect occur.
Then, execution step S15, carries out the 3rd thermal treatment to described blank after cold rolling.
The embodiment of this step is at the temperature of 650 DEG C～750 DEG C, insulation 55min～65min.
Copper-phosphorus alloy blank is carried out to the 3rd thermal treatment can make copper-phosphorus alloy interior tissue carry out recrystallize, can further make copper-phosphorus alloy blank crystal grain become equi-axed crystal more uniformly, further reduce the demixing phenomenon of copper-phosphorus alloy interior tissue, eliminate strain-hardening, the plasticity and the deformability that recover copper-phosphorus alloy blank, can also keep metal or alloy surface-brightening.
Heating temperature is too low, and in copper-phosphorus alloy blank, crystal grain recrystallize is insufficient or without recrystallize phenomenon; Heating temperature is too high, and in copper-phosphorus alloy blank, crystal grain is easily grown up, and size can surpass scope; Soaking time is too short, and in copper-phosphorus alloy blank, crystal grain is heated inhomogeneously, and recrystallize is insufficient; Soaking time is long, and in copper-phosphorus alloy blank, crystal grain is easily grown up, and size can surpass scope.In actual applications, can before carrying out recrystallization annealing, preset the concrete numerical value of above-mentioned each parameter, wherein, described Heating temperature and soaking time can be set according to certain corresponding relation, for example 700 DEG C of * 60min etc.
It is the final recrystallization annealing to copper-phosphorus alloy ingot casting in process of the present invention that copper-phosphorus alloy blank is carried out to the 3rd thermal treatment.The grain size that copper-phosphorus alloy ingot casting forms in this step annealing process and distributing be the grain size of final copper-phosphorus alloy anode and distribution (grain-size be 70 μ m～100 μ m).So the temperature of the annealing of this step is wanted meticulous control.In implementation process, temperature tolerance only allows for ± and 5 DEG C.
Finally, execution step S16, carries out mechanical workout to described the 3rd heat treated blank, forms copper-phosphorus alloy anode.
Described the 3rd heat treated blank is carried out to described mechanical workout and comprise the technique such as roughing, precision work, make to meet and electroplate the copper-phosphorus alloy anode product requiring, wherein roughing refers to that contour turning, precision work refer to product size turning, comprises all astragal cuttings, upper and lower surface grinding machine processing.Copper-phosphorus alloy anode surface form accuracy is met and electroplate requirement.
And by contriver's continuous practice, through copper-phosphorus alloy anode of obtaining in processing step above as shown in Figure 9, its compactness and uniformity coefficient can meet the requirement of plating, there will not be demixing phenomenon.As shown in Figure 9, copper-phosphorus alloy anode is circular, and this copper-phosphorus alloy anode is equally divided into three fan-shaped parts, is respectively Part A, Part B, Part C.Taking the Part A part of copper-phosphorus alloy anode as example, be Side A near the part at Part A long arc edge, the centre portions that is copper-phosphorus alloy anode near Part A short arc edge is Center A.Same, be Side B near the part at Part B long arc edge, the centre portions that is copper-phosphorus alloy anode near Part B short arc edge is Center B; Part near Part C long arc edge is Side C, and the centre portions that is copper-phosphorus alloy anode near Part C short arc edge is Center C.
Figure 10 is copper-phosphorus alloy anode crystal grain schematic diagram of making in above-mentioned steps.Copper-phosphorus alloy anode the grain-size of table 2 for making in above-mentioned steps.Table 1 is the grain-size numerical value that copper-phosphorus alloy anode three fan-shaped part Part A, Part B, Part C (being Center A, Side A, Center B, Side B, Center C, Side C position) detected.Detection size is that X-axis, Y-axis and three directions of Z axis of copper-phosphorus alloy crystal grain from Figure 10 are measured.Draw in conjunction with Fig. 9, Figure 10 and table 1, the copper-phosphorus alloy anode interior grain-size obtaining through above-mentioned viscous deformation and heat treating method is all in the scope of 70 μ m～100 μ m and grain structure even structure.
Table 1
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; can utilize method and the technology contents of above-mentioned announcement to make possible variation and amendment to technical solution of the present invention; therefore; every content that does not depart from technical solution of the present invention; any simple modification, equivalent variations and the modification above embodiment done according to technical spirit of the present invention, all belong to the protection domain of technical solution of the present invention.
Claims (3)
1. a preparation method for copper-phosphorus alloy anode, is characterized in that, comprising:
Ingot casting is carried out to the first thermal treatment, then forge, carry out successively described the first thermal treatment and described forging, altogether carry out three times, described the first thermal treatment temp is 850 DEG C～950 DEG C, and the deformation rate of described forging is 50%～70%;
Ingot casting after described forging is carried out to cooling process for the first time;
Described ingot casting after cooling process is for the first time carried out to the second thermal treatment, and described thermal treatment temp is for the second time 650 DEG C～750 DEG C, and soaking time is 55min～65min;
Described ingot casting after the second thermal treatment is carried out to cooling process for the second time;
The ingot casting of cooling process is for the second time carried out repeatedly to cold rolling formation blank, and each cold rolling deformation rate is 8%～10%, and described cold rolling total deformation rate is 80%～90%;
Described blank after cold rolling is carried out to the 3rd thermal treatment, and described the 3rd heat treated temperature is 650 DEG C～750 DEG C, and soaking time is 55min～65min;
Described the 3rd heat treated blank is carried out to mechanical workout, form copper-phosphorus alloy anode.
2. the preparation method of copper-phosphorus alloy anode as claimed in claim 1, is characterized in that, in the 30s after described the 3rd thermal treatment, described blank is carried out to cooling process for the third time fast.
3. the preparation method of copper-phosphorus alloy anode as claimed in claim 1, is characterized in that, in described the 3rd thermal treatment, the tolerance of thermal treatment temp is ± 5 DEG C.
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| US10760156B2 (en) | 2017-10-13 | 2020-09-01 | Honeywell International Inc. | Copper manganese sputtering target |
| US11035036B2 (en) | 2018-02-01 | 2021-06-15 | Honeywell International Inc. | Method of forming copper alloy sputtering targets with refined shape and microstructure |
| WO2020013898A1 (en) | 2018-07-10 | 2020-01-16 | Commscope Technologies Llc | Orientation adjustable mounts and related methods of locking into alignment |
| CN109338443A (en) * | 2018-11-20 | 2019-02-15 | 有研亿金新材料有限公司 | A kind of Cu-P anode preparation process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385557A (en) * | 2001-03-13 | 2002-12-18 | 三菱综合材料株式会社 | Copper phosphide anode for electroplating |
| CN1458292A (en) * | 2002-05-14 | 2003-11-26 | 同和矿业株式会社 | Copper base alloy with improved punchin and impacting performance and its preparing method |
| CN1630567A (en) * | 2001-07-02 | 2005-06-22 | 勃拉希·威尔曼股份有限公司 | Manufacture of fine-grained electroplating anodes |
| CN101168808A (en) * | 2007-11-21 | 2008-04-30 | 苏州有色金属研究院有限公司 | Method for producing Cu-Ti alloy used for injection moulding die |
| CN101586198A (en) * | 2009-06-26 | 2009-11-25 | 中南大学 | A process for preparing aluminum oxide dispersion strengthened copper with high strength and high conductivity |
Family Cites Families (2)
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| US20030155050A1 (en) * | 2001-09-21 | 2003-08-21 | Industrial Technology Research Institute | High-strength and high-conductivity Cu-(Ni, Co, Fe)-Si copper alloy for use in leadframes |
| JP4869415B2 (en) * | 2010-02-09 | 2012-02-08 | 三菱伸銅株式会社 | Pure copper plate manufacturing method and pure copper plate |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1385557A (en) * | 2001-03-13 | 2002-12-18 | 三菱综合材料株式会社 | Copper phosphide anode for electroplating |
| CN1630567A (en) * | 2001-07-02 | 2005-06-22 | 勃拉希·威尔曼股份有限公司 | Manufacture of fine-grained electroplating anodes |
| CN1458292A (en) * | 2002-05-14 | 2003-11-26 | 同和矿业株式会社 | Copper base alloy with improved punchin and impacting performance and its preparing method |
| CN101168808A (en) * | 2007-11-21 | 2008-04-30 | 苏州有色金属研究院有限公司 | Method for producing Cu-Ti alloy used for injection moulding die |
| CN101586198A (en) * | 2009-06-26 | 2009-11-25 | 中南大学 | A process for preparing aluminum oxide dispersion strengthened copper with high strength and high conductivity |
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