CN102409147B - Heat treatment method for target material - Google Patents
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- CN102409147B CN102409147B CN2011103592515A CN201110359251A CN102409147B CN 102409147 B CN102409147 B CN 102409147B CN 2011103592515 A CN2011103592515 A CN 2011103592515A CN 201110359251 A CN201110359251 A CN 201110359251A CN 102409147 B CN102409147 B CN 102409147B
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Abstract
The present invention provides a heat treatment method for a target material. The method comprises: providing a target material, wherein the target material is a copper-phosphorus alloy; preheating sand; coating the target material by the sand; carrying out a heat treatment for the target material. Compared to the prior art, with the present invention, the heating method of the sand bath preheating is adopted, such that the uniform heating of the target material is ensured, the uniformity of the target material organization structure is achieved, and the electroplating requirements are met.
Description
Technical field
The present invention relates to field of semiconductor manufacture, relate in particular to heat treatment method of target material.
Background technology
Electroplating (Electroplating) utilizes electrolysis principle to plate the process of other metal or alloy of skim on some metallic surface.It utilizes electrolysis principle to make the surface attachment layer of metal film of metal or other material product, thereby play, prevents from corrosion from improving the effects such as wear resistance, electroconductibility, reflective and having improved aesthetic appearance.
In filling the coating bath of 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 comprised 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, be moved on negative electrode and form coating in the effect of potential difference.The metal of anode forms metal ion and enters electroplate liquid, the concentration of the metal ion be plated with maintenance.At present, can select high purity copper phosphorus alloy target as anode.
The making processes of metal targets generally comprises: the steps such as melting, homogenizing processing, viscous deformation processing, thermal treatment, on the basis of strict control target purity, by selecting different viscous deformation processing, heat-treat condition, the grain orientation of adjustment target, grain-size etc., finally meet the requirement of sputter procedure.
Especially, thermal treatment is technique indispensable in Target Design and the course of processing, and this technique is often combined closely with viscous deformation processing, mainly for realizing the recrystallize of metallic substance, makes the homogeneous microstructure of material.The thermal treatment of aluminium target of take is example, and different thermal treatment temps, soaking time, type of heating, can obtain different metal material tissue structures.Equally, also applicable for high purity copper phosphorus alloy target.
Electroplate the film formed and need to meet certain uniformity requirement, and high purity copper phosphorus alloy target internal organizational structure can affect the homogeneity of film.The inner grain size of high purity copper phosphorus alloy target, grain orientation all can affect the homogeneity of film.Therefore, the inner grain size of electroplating technology requirement high purity copper phosphorus alloy target is suitable, grain orientation is suitable.
If adopting traditional technology heat-treats the copper-phosphorus alloy target, heat treating method as the application number disclosed a kind of aluminium target of Chinese patent application that is 200910140622.3, the application aforesaid method, can cause inconsistent due to the inequality of being heated in the processed weave construction of copper-phosphorus alloy target on diameter and thickness direction.Apply the target product of this method production for electroplating, there is very large negative effect, even can not meet the plating requirement.
Summary of the invention
The object of the present invention is to provide a kind of heat treatment method of target material, in the solution prior art, target because the inequality of being heated causes weave construction inhomogeneous, causes applying this target and makes the problem of the poor effect of electroplating technology as anode in thermal treatment process.
For addressing the above problem, the invention provides a kind of heat treatment method of target material, comprising: target is provided, and the material of described target is copper-phosphorus alloy; The preheating sand; The sand of preheating is coated to described target, described target is heat-treated.
Optionally, described sand is to be filled in thermal treatment unit, and described target is in described sand is submerged in heating after described sand again.
Optionally, the step that also comprises the Heating temperature of the described target of sensing.
Optionally, the Heating temperature of the described target of described sensing comprises by the surface temperature sensor and carries out sensing.
Optionally, described target had carried out plastic deformation process before thermal treatment.
Optionally, the Heating temperature of described preheating sand is 700 ℃～750 ℃.
Optionally, described thermal treatment process design parameter is: Heating temperature is 650 ℃～750 ℃, and is incubated 45min～90min at this temperature.
Optionally, the purity range of described target is 4N5～6N.
Optionally, described thermal treatment unit is constant temperature oven.
Optionally, described sand material is silicon carbide, aluminum oxide or quartz sand, specification be No. 45, No. 60, No. 70, No. 80 with No. 90 in any.
Compared with prior art, heat treatment method of target material provided by the present invention, adopted first preheating sand, then in sand target to be heated submerged after preheating and the mode of heating, by the sand after heating, heat is conducted to target to be heated, guarantee target energy thermally equivalent, make the weave construction of the target after thermal treatment even, meet and electroplate requirement.
The heat treating method of applying above-mentioned target has been accelerated the rate of heating of product, has shortened the heat treatment time of product, and has improved the Stability and veracity of thermal treatment process, thereby can obtain and meet performance requriements and stay-in-grade product.
And the application aforesaid method can a plurality of targets of laser heating, realize the batch thermal treatment process of product, the batch production speed of product significantly improves, and then has shortened the fabrication cycle of product.
The accompanying drawing explanation
Fig. 1 is the schematic flow sheet of an embodiment of application heat treatment method of target material of the present invention;
Fig. 2 and Fig. 3 are the target that is applied in above-mentioned embodiment and the structural representation of heating unit;
The schematic diagram that Fig. 4 is the copper-phosphorus alloy target after thermal treatment;
Fig. 5 is the copper-phosphorus alloy target crystalline grains schematic diagram after thermal treatment.
Embodiment
The present inventor finds, in existing heat treatment method of target material, when target is heat-treated, in diameter and the weave construction on thickness direction of target, can cause inconsistent due to the inequality of being heated.Therefore, the present inventor proposes a kind of heat treatment method of target material, comprising: target is provided, and described target is copper-phosphorus alloy; Heating energy coats the sand of described target; Described target is heat-treated.
In an embodiment of the present invention, provide a kind of heat treatment method of target material, as shown in Figure 1, comprise step:
S10, provide target, and described target is copper-phosphorus alloy;
S11, preheating is filled in the sand in thermal treatment unit;
S12, submerge described target in the sand of preheating, and described target is heat-treated.
Below in conjunction with accompanying drawing, the heat treating method shown in above-mentioned Fig. 1 is elaborated.
At first perform step S10, provide target 10, as shown in Figure 2.In the present embodiment, described target 10 can be highly purified copper-phosphorus alloy.Particularly, described target purity is 4N5,5N or 6N, and wherein, described 4N5 means that purity is that 99.995%, 5N means that purity is 99.999%, and 6N means that purity is 99.9999%.
In addition, before execution step S10, target 10 has carried out plastic deformation process.Described plastic deformation process is that the metal materials and parts are placed in to the technique that the overflow mould of squeezing device (for example forging press, air hammer or rolling press) carries out extrusion molding.The shape and size of overflow mould have determined the cross section of product.Described extruding can adopt the forward hot extrusion, and the direction of extrusion of squeezing device is consistent with the flow direction of metal materials and parts, and extruding is to carry out at a certain temperature simultaneously.By reasonable control extrusion temperature and the suitable extrusion ratio of setting, can accurately control the compact dimensions precision of target, produce the target that meets the plastic deformation process requirement, realize reducing the purpose of target crystalline grains size, crystal grain thinning and reduction target material surface roughness.The ratio of total cross-sectional area of the goods after total cross-sectional area that described extrusion ratio refers to the goods before extruding and extruding.
In actual applications, the shape of target 10, according to the actual requirement of applied environment, sputtering equipment, can be any in circle, rectangle, annular, taper shape or other analogous shapes (comprising regular shape and irregularly shaped), and its thickness can not wait for 1mm to 100mm.As shown in Figure 2, the present embodiment is circular target.
Then perform step S11, preheating is filled in the sand in thermal treatment unit.In the present embodiment, described thermal treatment unit can be the constant temperature oven shown in Fig. 3 for example, and it has chamber 20, has installed sand 30 in chamber 20 additional.Wherein, the sand 30 installed additional can be to be partially filled chamber 20, also can fill completely whole chamber 20.Like this, by the operation constant temperature oven, can the sand 30 installed additional in chamber 20 be preheated.
Because the composition of sand 30 and kind can affect itself rate of heating, uniformity coefficient and to the heat-conducting effect of the target 10 that coats.Therefore, the selection of the material of sand 30 is also an important factor.In actual applications, the material of sand 30 can be to be selected from silicon carbide, aluminum oxide or quartz sand, any in can No. 45, No. 60, No. 70, No. 80 or No. 90 of its size specification.
In the present embodiment, sand 30 is specially silicon carbide (SiC).The raw materials such as quartz sand for silicon carbide, refinery coke (or coal tar), wood chip (while producing green silicon carbide need to salt) form through pyrotic smelting in resistance furnace.Silicon carbide is hot good conductor, there are high temperature resistant, good heat conductivility and the characteristics of thermostability, utilize these characteristics, just silicon carbide can be positioned over to heating source (in the present embodiment, constant temperature oven for example) with heating object (in the present embodiment, for example target 10) between, as the indirect heating material of high temperature.
Constant temperature oven first carries out preheating to sand 30, and preheating temperature is controlled at 700 ℃～750 ℃.Preheating temperature is too low, and the long heat treatment efficiency that makes of heat treatment time is low; Preheating temperature is too high, surpasses the thermal treatment temp of expection, and in target, crystal grain is easily grown up, and size can surpass scope.
Then perform step S12, described target is submerged in the sand of preheating, described target is heat-treated.Specifically comprise: utilize the heat conductivility that sand 30 is good, it is heated to thing as centre, by the sand 30 after preheating, carry out heat conduction, indirectly, to target 10 heating, heat-treat.
Here, target 10 is inserted in the chamber 20 of constant temperature oven, as shown in Figure 3, specifically refer to target 10 is submerged in sand 30 with certain degree of depth, make the periphery of target 10 to be coated by sand 30.The described degree of depth can be made accommodation according to the heat characteristic of constant temperature oven, the structure of chamber or the filling situation of sand, preferably, target 10 can be placed on the zone of energy thermally equivalent, for example is placed on the geometric centre zone in sand 30 space that forms of filling.
Practice shows, grain-size and orientation thereof have a great impact the performance of target, are mainly manifested in:, along with the increase of grain-size, the film deposition rate zone reduces (1); (2) in suitable grain size range, plasma impedance when target is used is lower, and film deposition rate is high and uniformity of film is good; (3), in suitable grain size range, grain orientation is more evenly better; (4) when the target crystalline grains size surpasses suitable grain size range, for improving the performance of target, must the strict grain orientation of controlling target.In the present embodiment, the inner grain size of the copper-phosphorus alloy target obtained through above-mentioned heat treating method is 70 μ m～100 μ m.The inside grain-size of the copper-phosphorus alloy target obtained through above-mentioned heat treating method is in this scope, and the copper-phosphorus alloy target after thermal treatment is electroplated as anode, and electroplating quality is stable.
The schematic diagram that Fig. 4 is the copper-phosphorus alloy target after thermal treatment.As shown in Figure 4, the copper-phosphorus alloy target after this thermal treatment is circular, and this copper-phosphorus alloy target is equally divided into to three fan-shaped parts, is respectively PartA, Part B, Part C.The PartA of copper-phosphorus alloy target of take is partly example, near the part at PartA long arc edge, is Side A, and the centre portions that is the copper-phosphorus alloy target near Part A short arc edge is Center A.Same, the part at close Part B long arc edge is Side B, the centre portions that is the copper-phosphorus alloy target 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 the copper-phosphorus alloy target near Part C short arc edge is Center C.
Fig. 5 is the copper-phosphorus alloy target crystalline grains schematic diagram after thermal treatment.Table 1 is the copper-phosphorus alloy target crystalline grains size after thermal treatment.Table 1 is the grain-size numerical value that three fan-shaped part PartA of copper-phosphorus alloy target after thermal treatment, Part B, Part C (being Center A, Side A, Center B, Side B, Center C, Side C position) detected.The detection size is that X-axis, Y-axis and three directions of Z axis of copper-phosphorus alloy crystal grain from Fig. 5 are measured.In conjunction with Fig. 4, Fig. 5 and table 1, draw, the inner grain-size of the copper-phosphorus alloy target obtained through above-mentioned heat treating method is all in the scope of 70 μ m～100 μ m, the grain structure even structure, the above-mentioned copper-phosphorus alloy target after thermal treatment is electroplated as anode, and electroplating quality is stable.
Table 1 is the copper-phosphorus alloy target crystalline grains size after thermal treatment
The grain-size of target and grain orientation need to be adjusted and be controlled by thermal treatment process, guarantee the homogeneity of target on weave construction.
In the present embodiment, described thermal treatment process design parameter is: Heating temperature is 650 ℃～750 ℃, and is incubated 45min～90min at this temperature.Heating temperature is too low, and in target, the crystal grain recrystallize is insufficient; Heating temperature is too high, and in target, crystal grain is easily grown up, and size can surpass scope; Soaking time is too short, and in target, crystal grain is heated not, and recrystallize is insufficient; Soaking time is long, and in target, crystal grain is easily grown up, and size can surpass scope.In actual applications, can before heat-treating, 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, such as 750 ℃ of * 45min or 650 ℃ of * 90min etc.
In addition, in the present embodiment, for guaranteeing the stability of Heating temperature, the present invention also disposes the surface temperature sensor (not indicating) for sensing temperature.Described surface temperature sensor both can be embedded in sand 30, also can be directly arranged in the surface of target 10.When described surface temperature sensor senses that described Heating temperature is undergone mutation or surpass specialized range, can immediately be shown that Current Temperatures numerical value produces alarm message even simultaneously, for heat temperature or soaking time are made adjustment in good time, guarantee the stability of thermal treatment process.Wherein, described adjustment can specifically comprise such as the Heating temperature of adjusting (improve or reduce) described constant temperature oven, adjustment (extend or shorten) soaking time or adjust target 10 there be not implantation site etc. in sand 30.
Visible, in the present invention, because the periphery of target 10 is coated by the sand 30 after preheating, therefore by sand 30, heat is conducted to target 10, can, so that target 10 can thermally equivalents, guarantee the homogeneity of target on weave construction.
Follow-up, after thermal treatment, can also comprise heat treated target 10 is carried out to cooling step.Cooling target 10 can be described target 10 to be put into to 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.Due to described process for cooling and subsequent step and prior art indifference, be well known to those skilled in the art, therefore do not repeat them here.
After described target 10 thermal treatments, need to pass through the techniques such as roughing, precision work again, make satisfactory target product, wherein roughing refers to that contour turning, precision work refer to product size turning.
Below in conjunction with preferred embodiment, the present invention is further introduced.
Example:
Below take processing step and the result that the copper-phosphorus alloy target of 4N5 or 5N heat-treats in heat treatment method of target material of the present invention as example illustrates:
(1) provide the copper-phosphorus alloy target after plastic deformation process.The described copper-phosphorus alloy target through plastic deformation process has the weave construction of better grain size.
(2) sand is preheated in constant temperature oven to 700 ℃.What described sand adopted is No. 45 silicon carbide (45#SiC).
(3) the copper-phosphorus alloy target the is submerged sand inside of the prior preheating of constant temperature oven, make the periphery of described copper-phosphorus alloy target all be coated by sand.
(4) the copper-phosphorus alloy target is heat-treated.Specifically comprise: Heating temperature is 750 ℃, and is incubated 60min at this temperature.
(5) the copper-phosphorus alloy target after thermal treatment is carried out to roughing.
(6) the copper-phosphorus alloy target after roughing is carried out to precision work.
See through above steps, the final acquisition meets the copper-phosphorus alloy target product of electroplating requirement.
Heat treatment method of target material provided by the present invention, due to the mode that has adopted pre-arenation, target is submerged in the sand of preheating, using sand as the indirect heating material, heat is conducted to target to be heated, guarantee target energy thermally equivalent, make the weave construction of the target after thermal treatment realize homogeneity, and apply this target product as anode, can improve the efficiency of follow-up electroplating technology.
The actual intensification effect of direct sensing blank, for example with the surface temperature sensor, measure the temperature of target, indirectly control the temperature of target than the Heating temperature by controlling constant temperature oven, the temperature of target and soaking time have obtained controlling better, have therefore guaranteed the Stability and veracity of thermal treatment process.
In sum, the heat treating method of applying above-mentioned target has been accelerated the rate of heating of product, has shortened the heat treatment time of product, and has improved the Stability and veracity of thermal treatment process, thereby can obtain and meet performance requriements and stay-in-grade product.
And, the application aforesaid method can a plurality of targets of laser heating, realize the batch thermal treatment process of target product, after the thermal treatment that completes last target, because the Heating temperature of constant temperature oven can be warming up to the preheating temperature of sand very soon, that is to say, shortened the warm up time of constant temperature oven, and after making like this, the heat treatment time of a target has shortened.Therefore, the batch production speed of target product significantly improves, and then has shortened the fabrication cycle of target product.
The above, be only preferred embodiment of the present invention, not the present invention done to any pro forma restriction.Any those of ordinary skill in the art, do not breaking away from technical solution of the present invention scope situation, all can utilize method and the technology contents of above-mentioned announcement to make many possible changes and modification to technical solution of the present invention, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical scheme of the present invention,, all still belong in the scope of technical solution of the present invention protection any simple modification made for any of the above embodiments, equivalent variations and modification according to technical spirit of the present invention.
Claims (6)
1. a heat treatment method of target material, is characterized in that, comprising:
The target of processing through the forward hot extrusion technique is provided, and the material of described target is copper-phosphorus alloy;
Adopt constant temperature oven preheating sand, the Heating temperature of described preheating sand is 700 ℃～750 ℃;
The sand of preheating is coated to described target, described target is heat-treated in constant temperature oven, described thermal treatment process design parameter is: Heating temperature is 650 ℃～750 ℃, and be incubated 45min～90min at this temperature, after thermal treatment, the grain-size of described target is 70 μ m～100 μ m.
2. heat treatment method of target material according to claim 1, is characterized in that, described sand is to be filled in constant temperature oven, and described target is in described sand is submerged in heating after described sand again.
3. heat treatment method of target material according to claim 1 and 2, is characterized in that, also comprises the step of the Heating temperature of the described target of sensing.
4. heat treatment method of target material according to claim 3, is characterized in that, the Heating temperature of the described target of described sensing comprises by the surface temperature sensor carries out sensing.
5. heat treatment method of target material according to claim 1, is characterized in that, the purity range of described target is 4N5～6N.
6. heat treatment method of target material according to claim 1, is characterized in that, described sand material is silicon carbide, aluminum oxide or quartz sand, specification be No. 45, No. 60, No. 70, No. 80 with No. 90 in any.
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| CN106702120B (en) * | 2015-07-13 | 2018-08-28 | 宁波江丰电子材料股份有限公司 | Heat treatment method of target material |
| CN107663619A (en) * | 2016-07-28 | 2018-02-06 | 宁波江丰电子材料股份有限公司 | The processing method of alloy |
| CN116479487A (en) * | 2023-06-07 | 2023-07-25 | 宁波科宁达工业有限公司 | Electroplated magnet and method for preparing same |
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| CN101649438B (en) * | 2009-05-12 | 2011-08-03 | 宁波江丰电子材料有限公司 | Heat treatment method of target material |
| CN101624694B (en) * | 2009-08-11 | 2011-01-26 | 宁波江丰电子材料有限公司 | Target heat treatment method |
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Effective date of registration: 20160420 Address after: 315400 Zhejiang city in Ningbo Province, the State Science and Technology Industrial Park Road No. 198. Patentee after: NINGBO JIANGFENG ELECTRONIC MATERIAL CO., LTD. Address before: 315400 Ningbo City, Yuyao Province Economic Development Zone, state science and Technology Industrial Park Road, No. 198, No. Patentee before: Yuyao Kang Fute Electron Material Co., Ltd |