CN102485924A - Preparation method of phosphorus-copper anode for integrated circuit - Google Patents
Preparation method of phosphorus-copper anode for integrated circuit Download PDFInfo
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- CN102485924A CN102485924A CN2010105819228A CN201010581922A CN102485924A CN 102485924 A CN102485924 A CN 102485924A CN 2010105819228 A CN2010105819228 A CN 2010105819228A CN 201010581922 A CN201010581922 A CN 201010581922A CN 102485924 A CN102485924 A CN 102485924A
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Abstract
The invention discloses a preparation method of a phosphorus-copper anode for an integrated circuit. The preparation method utilizes high-purity graphite as a material of a crucible and a mold, and comprises the following steps of melting a copper ingot having high purity above 99.99% in a high-vacuum medium-frequency induction melting furnace, adding a phosphorus-copper intermediate alloy having phosphorus content of 6 to 16 wt% into the high-vacuum medium-frequency induction melting furnace at a temperature of 1150 to 1300 DEG C, wherein a weight ratio of the added phosphorus-copper intermediate alloy to the copper ingot having high purity is 1: (50 to 600), carrying out heat preservation at a temperature of 1150 to 1300 DEG C for 20 to 30 minutes, standing for 20 minutes, carrying out graphite mold casting to obtain a phosphorus-copper alloy ingot, cutting off a riser of the phosphorus-copper alloy ingot, carrying out multidirecional forging and rolling, carrying out heat preservation at a temperature of 300 to 600 DEG C for 0.5 to 12 hours, carrying out crystallization, and carrying out surface treatment and machining to obtain the phosphorus-copper anode for an integrated circuit. The phosphorus-copper anode for an integrated circuit has low impurity content, low oxygen content, uniform phosphorus content distribution, and small and uniform crystal particle sizes.
Description
Technical field
The present invention relates to a kind of unicircuit with phosphor-copper anodic preparation method; Be specifically related to a kind of through adding the phosphor bronze alloy melting in the high purity copper; Thereby and, belong to metallic substance and field of metallurgy through the uniform distribution of the corresponding thermal treatment process realization of viscous deformation and adjustment phosphorus content and the effect of crystal grain thinning.
Background technology
Conventional copper electrodeposition obtains broad research at home and abroad.From the acidic solution deposited copper about 200 years history is arranged, still use widely so far at aspects such as engineering, decoration and electronic industries.But the copper deposition technique is applied to the semiconductor microactuator electronic industry, the geometrical shape in the bigger submicron cutting of depth-width ratio is filled still brand-new research field.
Along with the continuous development of unicircuit scale, traditional aluminium interconnection technique is replaced by copper interconnection technology at present.The superfill of copper mainly adopts Damascence technology to electroplate.In the copper-connection process, plating is its main technology.In order to obtain well behaved Cu coating, the phosphorous copper anode that needs purity more to increase.
People such as U.S. Nevers in 1954 add a spot of phosphorus when making anode in fine copper, find that anode surface generates the gluey film of one deck black, and anode dissolution produces copper powder hardly when electroplating, and body refuse is few, and the piece surface copper coating can not produce burr.This is that its hole does not influence cupric ion again freely to be passed through, and has accelerated cupprous oxidation, has stoped cupprous accumulation, has reduced univalent copper ion in the plating bath widely because the black film of phosphorous copper anode has conductivity; Make simultaneously the anodic dissolving gradually approaching again, kept copper content balance in the copper plating bath with the efficient of cathodic deposition.
CN 100453667C discloses a kind of working method of anodic phosphorous copper alloy, and this method adopts main frequency furnace, and bath surface covers charcoal, feeds coal gas and guarantees that environment is a reducing atmosphere, then the method for casting.This method is melting under atmosphere, and vacuum tightness can't guarantee, introduces elements such as C and N easily, and can cause the increase of oxygen level in the alloy; Also all can't satisfy the unicircuit requirement of high purity for the scaling loss of P element and the control of other foreign matter content simultaneously.
Therefore, need provide that a kind of technology is simple, cost is low, have good plating rate simultaneously, can significantly reduce adhering to of particle on the plated body, reduce the unicircuit that pollutes with phosphor-copper anodic preparation method.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art; Adopt the method for vacuum induction melting; Through adopting high purity graphite as crucible and moulding stock; Technological process is to adopt high-purity copper and copper-phosphorus alloy as starting material, pass through prepurging, melting, casting, forging, rolling, thermal treatment and mechanical workout after, prepare unicircuit and use the phosphor-copper anode.
For realizing above-mentioned purpose, the present invention takes following technical scheme:
A kind of unicircuit may further comprise the steps with phosphor-copper anodic preparation method:
(1) raw material selection purity is 99.99% and above high purity copper ingot casting and the phosphor bronze alloy of phosphorous 6～16wt.%;
(2) melting copper: the purity that in the high vacuum medium frequency induction melting furnace, adds oven dry is 99.99% and above high purity copper ingot casting, heats melting;
(3) treat that the casting in bronze ingot melts fully after, add down said phosphor bronze alloys at 1150～1300 ℃, the weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 50～600, melts, mixes;
(4) casting: with the liquation of gained at 1150～1300 ℃ of insulation 20～30min down, leave standstill 20 minutes again after, pour into graphite jig, obtain the phosphor copper ingot casting;
(5) with the phosphor copper ingot casting that obtains, behind the excision ingot casting rising head, remove matte layer, carry out the multiway forging distortion at normal temperatures, deflection reaches more than 60%; Be rolled distortion then, deflection reaches more than 50%; Carry out follow-up thermal treatment after the distortion, pass through surface treatment at last, mechanical workout obtains unicircuit and uses the phosphor-copper anode.
A kind of optimized technical scheme is characterized in that: before melting copper, in the high vacuum medium frequency induction melting furnace, using earlier purity is 99.99% high purity copper ingot casting prepurging 2 times.
A kind of optimized technical scheme is characterized in that: described multiway forging is deformed into the three-dimensional forging deformation.
A kind of optimized technical scheme is characterized in that: described thermal treatment is for being incubated 0.5～12 hour down at 300～600 ℃.Removing stress and recrystallize handles.
A kind of optimized technical scheme is characterized in that: the unicircuit that said mechanical workout obtains uses phosphor-copper anodic profile for circular, square or special-shaped, can be monomer or molectron.
The unicircuit of present method preparation is used the phosphor-copper anode, can guarantee phosphorus content between 100～3000ppm, and be evenly distributed; Oxygen level is at 2～100ppm, and all the other foreign matter content summations obtain crystal grain between 20～500 μ m simultaneously less than 100ppm.
Unicircuit provided by the present invention is divided into two stages with phosphor-copper anodic preparation method, i.e. melting and follow-up viscous deformation and thermal treatment.Wherein, melting is in the melting of high vacuum Medium frequency induction, to carry out.Through adding phosphor bronze alloy melting in the high purity copper, thereby and through the uniform distribution of the corresponding thermal treatment process realization of viscous deformation and adjustment phosphorus content and the effect of crystal grain thinning.Therefore, the phosphor-copper anode that a process for preparing has characteristics such as foreign matter content is low, and oxygen level is low, and phosphorus content is evenly distributed, and crystal grain is tiny, even.
Can provide preparation to be in the phosphor-copper manufacturing method of electrode material of realistic scale to unicircuit with the purposes that phosphor copper has enlarged according to the present invention.Compared with prior art, the present invention has marked improvement, and the unicircuit that provides also has good plating rate technology is simple except that having, cost can accept with phosphor copper, can significantly reduce adhering to of particle on the plated body, reduces and pollutes.
Description of drawings
Fig. 1 is that the unicircuit of embodiment 1 preparation is with phosphor-copper anodic metallograph.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1:
1. the melting of material:
(1) adopt high purity graphite as crucible and moulding stock, the purity that in the high vacuum medium frequency induction melting furnace, adds oven dry is 99.99% high purity copper ingot casting.(2) be warmed up to 1150 ℃ of meltings, treat that copper ingot is all after the fusing, at 1200 ℃ of phosphor bronze alloys that add phosphorous 6wt.%.The weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 600; (3) liquation pours into graphite jig after leaving standstill 20 minutes behind 1200 ℃ of insulation 20min.
2. the viscous deformation of material and thermal treatment
(1), behind the excision ingot casting rising head, removes matte layer with the phosphor copper ingot casting that obtains after the melting.(2) carry out the multiway forging distortion at normal temperature, deflection reaches 60%; (3) be rolled distortion then, deflection reaches 50%.The subsequent heat treatment of (4) carrying out after the distortion is for being incubated 2 hours down at 300 ℃.Through surface treatment, it can be monomer or molectron (following examples are identical therewith) for shapes such as circular, square or abnormity with phosphor-copper anodic profile that mechanical workout obtains unicircuit.
Adopt light-intensity method to carry out P alloying element analysis in the alloy, phosphorus content is 100ppm; Adopt glow discharge mass spectrometry GDMS to analyze all the other metal element content summations less than 100ppm, 0 content that the inertia pulse infrared method is measured is 20ppm, obtains the tissue that crystal grain is 20 μ m simultaneously.
Embodiment 2:
1. the melting of material:
(1) purity that adding is dried in the high vacuum medium frequency induction melting furnace is 99.99% high purity copper ingot casting.(2) be warmed up to 1200 ℃ of meltings, treat that copper ingot is all after the fusing, at 1250 ℃ of phosphor bronze alloys that add phosphorous 12wt.%.The weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 240; (3) liquation pours into graphite jig after leaving standstill 20 minutes behind 1250 ℃ of insulation 20min.
2. the viscous deformation of material and thermal treatment
(1), behind the excision ingot casting rising head, removes matte layer with the phosphor copper ingot casting that obtains after the melting.(2) carry out the three-dimensional forging deformation at normal temperature, deflection reaches 80%; (3) be rolled distortion then, deflection reaches 80%.The subsequent heat treatment of (4) carrying out after the distortion is for being incubated 0.5 hour down at 600 ℃.
Adopt light-intensity method to carry out P alloying element analysis in the alloy, phosphorus content is 400ppm; Adopt glow discharge mass spectrometry GDMS to analyze all the other metal element content summations less than 100ppm, 0 content that the inertia pulse infrared method is measured is 20ppm, obtains the tissue that crystal grain is 50 μ m simultaneously.
Embodiment 3:
1. the melting of material:
(1) purity that adding is dried in the high vacuum medium frequency induction melting furnace is 99.99% high purity copper ingot casting.(2) be warmed up to 1300 ℃ of meltings, treat that copper ingot all after the fusing, adds the phosphor bronze alloy of phosphorous 16wt.%.The weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 50; (3) liquation pours into graphite jig after leaving standstill 20 minutes behind 1300 ℃ of insulation 20min.
2. the viscous deformation of material and thermal treatment
(1), behind the excision ingot casting rising head, removes matte layer with the phosphor copper ingot casting that obtains after the melting.(2) carry out the multiway forging distortion at normal temperature, deflection reaches 80%; (3) be rolled distortion then, deflection reaches 50%.The subsequent heat treatment of (4) carrying out after the distortion is for being incubated 8 hours down at 500 ℃.
Adopt light-intensity method to carry out P alloying element analysis in the alloy, phosphorus content is 3000ppm; Adopt glow discharge mass spectrometry GDMS to analyze all the other metal element content summations less than 100ppm, 0 content that the inertia pulse infrared method is measured is 30ppm, obtains the tissue that crystal grain is 500 μ m simultaneously.
Embodiment 4:
1. the melting of material:
(1) purity that adding is dried in the high vacuum medium frequency induction melting furnace is 99.999% high purity copper ingot casting.(2) be warmed up to 1150 ℃ of meltings, treat that copper ingot is all after the fusing, at 1200 ℃ of phosphor bronze alloys that add phosphorous 14wt.%.The weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 350; (3) liquation pours into graphite jig after leaving standstill 20 minutes behind 1200 ℃ of insulation 30min.
2. the viscous deformation of material and thermal treatment
(1), behind the excision ingot casting rising head, removes matte layer with the phosphor copper ingot casting that obtains after the melting.(2) carry out the multiway forging distortion at normal temperature, deflection reaches 60%; (3) be rolled distortion then, deflection reaches 80%.The subsequent heat treatment of (4) carrying out after the distortion is for being incubated 4 hours down at 450 ℃.
Adopt light-intensity method to carry out P alloying element analysis in the alloy, phosphorus content is 450ppm; Adopt glow discharge mass spectrometry GDMS to analyze all the other metal element content summations less than 10ppm, 0 content that the inertia pulse infrared method is measured is 4ppm, obtains the tissue that crystal grain is 60 μ m simultaneously.
Embodiment 5:
1. the melting of material:
(1) before melting copper, in the high vacuum medium frequency induction melting furnace, using earlier purity is 99.99% high purity copper ingot casting prepurging 2 times.The purity that in the high vacuum medium frequency induction melting furnace, adds oven dry then is 99.9999% high purity copper ingot casting.(2) be warmed up to 1150 ℃ of meltings, treat that copper ingot all after the fusing, adds the phosphor bronze alloy of phosphorous 12wt.%.The weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 240; (3) liquation pours into graphite jig after leaving standstill 20 minutes behind 1150 ℃ of insulation 30min.
2. the viscous deformation of material and thermal treatment
(1), behind the excision ingot casting rising head, removes matte layer with the phosphor copper ingot casting that obtains after the melting.(2) carry out the three-dimensional forging deformation at normal temperature, deflection reaches 60%; (3) be rolled distortion then, deflection reaches 80%.The subsequent heat treatment of (4) carrying out after the distortion is for being incubated 2 hours down at 500 ℃.
Adopt light-intensity method to carry out P alloying element analysis in the alloy, phosphorus content is 500ppm; Adopt glow discharge mass spectrometry GDMS to analyze all the other metal element content summations less than 1ppm, 0 content that the inertia pulse infrared method is measured is 2ppm, obtains the tissue that crystal grain is 200 μ m simultaneously.
Claims (6)
1. a unicircuit may further comprise the steps with phosphor-copper anodic preparation method:
(1) raw material selection purity is 99.99% and above high purity copper ingot casting and the phosphor bronze alloy of phosphorous 6～16wt%;
(2) melting copper: the purity that in the high vacuum medium frequency induction melting furnace, adds oven dry is 99.99% and above high purity copper ingot casting, heats melting;
(3) treat that the casting in bronze ingot melts fully after, add down said phosphor bronze alloys at 1150～1300 ℃, the weight ratio that adds phosphor bronze alloy and high purity copper ingot casting is 1: 50～600, melts, mixes;
(4) casting: with the liquation of gained at 1150～1300 ℃ of insulation 20～30min down, leave standstill 20 minutes again after, pour into graphite jig, obtain the phosphor copper ingot casting;
(5) with the phosphor copper ingot casting that obtains, behind the excision ingot casting rising head, remove matte layer, carry out the multiway forging distortion at normal temperatures, deflection reaches more than 60%; Be rolled distortion then, deflection reaches more than 50%; Carry out follow-up thermal treatment after the distortion, pass through surface treatment at last, mechanical workout obtains unicircuit and uses the phosphor-copper anode.
2. unicircuit according to claim 1 is characterized in that with phosphor-copper anodic preparation method: before melting copper, in the high vacuum medium frequency induction melting furnace, using earlier purity is 99.99% high purity copper ingot casting prepurging 2 times.
3. unicircuit according to claim 1 is characterized in that with phosphor-copper anodic preparation method: described multiway forging is deformed into the three-dimensional forging deformation.
4. unicircuit according to claim 1 is characterized in that with phosphor-copper anodic preparation method: described thermal treatment is for being incubated 0.5～12 hour down at 300～600 ℃.
5. unicircuit according to claim 1 is characterized in that with phosphor-copper anodic preparation method: the unicircuit that said mechanical workout obtains uses phosphor-copper anodic profile for circular, square or special-shaped, is monomer or molectron.
6. unicircuit according to claim 1 is characterized in that with phosphor-copper anodic preparation method: the gained unicircuit is with in the phosphor-copper anode, and phosphorus content is 100～3000ppm, and is evenly distributed; Oxygen level is 2～100ppm, and all the other foreign matter content summations are less than 100ppm, and crystal grain is between 20～500 μ m.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105506340A (en) * | 2014-09-26 | 2016-04-20 | 宁波江丰电子材料股份有限公司 | Preparation method for anode of copper-phosphorus alloy |
| CN106381410A (en) * | 2016-11-28 | 2017-02-08 | 佛山市承安铜业有限公司 | Method, smelting furnace and system for preparing phosphor-copper anode for integrated circuit |
| 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 |
| CN111979435A (en) * | 2020-09-11 | 2020-11-24 | 宁波微泰真空技术有限公司 | Smelting method for preparing copper-phosphorus alloy by using copper-phosphorus intermediate alloy |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1534101A (en) * | 2003-04-01 | 2004-10-06 | 安徽铜都铜业股份有限公司铜材厂 | Processing method of anode phosphorus copper alloy material |
| EP1489203A1 (en) * | 2002-03-18 | 2004-12-22 | Nikko Materials Company, Limited | ELECTROLYTIC COPPER PLATING METHOD, PHOSPHORUS−CONTAINING ANODE FOR ELECTROLYTIC COPPER PLATING, AND SEMICONDUCTOR WAFER PLATED USING THEM AND HAVING FEW PARTICLES ADHERING TO IT |
| 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 |
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2010
- 2010-12-06 CN CN2010105819228A patent/CN102485924B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| EP1489203A1 (en) * | 2002-03-18 | 2004-12-22 | Nikko Materials Company, Limited | ELECTROLYTIC COPPER PLATING METHOD, PHOSPHORUS−CONTAINING ANODE FOR ELECTROLYTIC COPPER PLATING, AND SEMICONDUCTOR WAFER PLATED USING THEM AND HAVING FEW PARTICLES ADHERING TO IT |
| CN1534101A (en) * | 2003-04-01 | 2004-10-06 | 安徽铜都铜业股份有限公司铜材厂 | Processing method of anode phosphorus copper alloy material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105506340A (en) * | 2014-09-26 | 2016-04-20 | 宁波江丰电子材料股份有限公司 | Preparation method for anode of copper-phosphorus alloy |
| CN106381410A (en) * | 2016-11-28 | 2017-02-08 | 佛山市承安铜业有限公司 | Method, smelting furnace and system for preparing phosphor-copper anode for integrated circuit |
| CN106381410B (en) * | 2016-11-28 | 2019-01-22 | 佛山市承安铜业有限公司 | A kind of preparation method and its system of phosphorus-copper anode for integrated circuit |
| 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 |
| CN111979435A (en) * | 2020-09-11 | 2020-11-24 | 宁波微泰真空技术有限公司 | Smelting method for preparing copper-phosphorus alloy by using copper-phosphorus intermediate alloy |
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