CN103943601A - Interconnection line with copper-graphene complex phase and preparation method of interconnection line - Google Patents
Interconnection line with copper-graphene complex phase and preparation method of interconnection line Download PDFInfo
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- CN103943601A CN103943601A CN201410194333.2A CN201410194333A CN103943601A CN 103943601 A CN103943601 A CN 103943601A CN 201410194333 A CN201410194333 A CN 201410194333A CN 103943601 A CN103943601 A CN 103943601A
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- copper
- interconnection line
- complex phase
- graphene
- graphite alkene
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Abstract
The invention discloses an interconnection line with a copper-graphene complex phase. A copper layer and a copper-graphene complex phase conducting layer are sequentially arranged on an insulating substrate from bottom to top. A preparation method of the interconnection line includes the steps: depositing one copper layer on the washed insulating substrate by a chemical plating method; imaging the copper layer by a photoetching method; performing electroplating on the copper layer in electroplating liquid with graphene nano-sheets by an electroplating method. The copper-graphene complex phase serves as the conducting layer, and electrical conductivity, heat conductivity, oxidation resistance, mechanical performance and corrosion resistance of the interconnection line are improved.
Description
Technical field
The present invention relates to a kind of interconnection line, especially a kind of interconnection line with copper-graphite alkene complex phase and preparation method thereof.
Background technology
Existing interconnection line generally has insulated substrate, metal layer and conductive layer from bottom to top.Wherein, conductive layer is mainly copper.Copper is easy to diffusion, and a little less than current carrying capacity, deelectric transferred performance is poor, conventionally improves the performance such as deelectric transferred of copper by increase the method such as diffusion barrier layer of layer of copper between insulated substrate and metal layer.The resistance of diffusion barrier layer is conventionally very large, and thermal diffusion performance is also poor, and its thickness is conventionally also larger, and this has reduced the conductivity of interconnection line on the one hand, and one side has increased the size of interconnecting construction.
In addition, the antioxygenic property of copper is poor, in order to improve the antioxygenic property of copper, conventionally need to be at surperficial re-plating one deck tin of copper, thus the oxidation of copper stoped, and the conductivity of tin is poor, this had both reduced the conductivity of interconnection line, increase device size, hindered the trend toward miniaturization of device, increased again the triviality of technique.
Summary of the invention
The object of the present invention is to provide a kind of technique simple, and possess interconnection line with copper-graphite alkene complex phase of excellent conductivity, thermal conductivity, antioxygenic property, mechanical performance and corrosion resistance and preparation method thereof.
The interconnection line with copper-graphite alkene complex phase of the present invention has successively copper layer and copper-graphite alkene complex phase conductive layer from bottom to top on insulated substrate.
Above-mentioned insulated substrate can be PET or Si/SiO
2substrate.
The preparation method with the interconnection line of copper-graphite alkene complex phase, comprises the following steps:
1) insulated substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) copper facing on the insulated substrate processed;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, surfactant and hydrochloric acid, stir, obtain copper electrolyte, concentration of copper sulfate in copper electrolyte is 150-250g/L, sulfuric acid concentration is 40-110 g/L, and chlorine ion concentration is 50-120 ppm, and surfactant concentration is 0.1-2g/L;
5) electroplate liquid of graphene-containing configuration: graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 0.01-4g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, adjusting temperature is 10-40
oc, current density are 0.5-16A/dm
2, under stirring condition, electroplate 1-120min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Above-mentioned surfactant can be neopelex or lauryl sodium sulfate.Described graphene nanometer sheet is single or multiple lift.
The beneficial effect that the present invention has compared with background technology: the present invention, using copper-graphite alkene complex phase as conductive layer, can improve conductivity, thermal conductivity, antioxygenic property, mechanical performance and the corrosion resistance of interconnection line, is conducive to the miniaturization of device.Preparation technology of the present invention is simple.
Brief description of the drawings
The schematic diagram of Fig. 1 interconnection line with copper-graphite alkene complex phase of the present invention.
Embodiment
Further illustrate the present invention below in conjunction with embodiment.
As shown in Figure 1, the interconnection line with copper-graphite alkene complex phase of the present invention has successively copper layer 2 and copper-graphite alkene complex phase conductive layer 3 from bottom to top on insulated substrate 1.
Embodiment 1
1) by Si/SiO
2substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) Si/SiO that processes
2copper facing on substrate;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, neopelex and hydrochloric acid, stir, obtain plating solution, concentration of copper sulfate in plating solution is 150g/L, sulfuric acid concentration is 40 g/L, and chlorine ion concentration is 100ppm, and neopelex concentration is 0.1g/L;
5) electroplate liquid of graphene-containing configuration: single-layer graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 0.01g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, regulating temperature is 10
oc, current density are 16A/dm
2, under stirring condition, electroplate 120min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Embodiment 2
1) by Si/SiO
2substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) Si/SiO that processes
2copper facing on substrate;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, lauryl sodium sulfate and hydrochloric acid, stir, obtain plating solution, concentration of copper sulfate in plating solution is 250g/L, sulfuric acid concentration is 110 g/L, and chlorine ion concentration is 50 ppm, and lauryl sodium sulfate concentration is 2g/L;
5) electroplate liquid of graphene-containing configuration: multi-layer graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 4g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, regulating temperature is 40
oc, current density are 0.5A/dm
2, under stirring condition, electroplate 60min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Embodiment 3
1) by Si/SiO
2substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) Si/SiO that processes
2copper facing on substrate;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, neopelex and hydrochloric acid, stir, obtain plating solution, concentration of copper sulfate in plating solution is 220g/L, sulfuric acid concentration is 80g/L, and chlorine ion concentration is 120 ppm, and neopelex concentration is 1.5g/L;
5) electroplate liquid of graphene-containing configuration: single-layer graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 1g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, regulating temperature is 30
oc, current density are 8A/dm
2, under stirring condition, electroplate 1min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Embodiment 4
1) by Si/SiO
2substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) Si/SiO that processes
2copper facing on substrate;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, neopelex and hydrochloric acid, stir, obtain plating solution, concentration of copper sulfate in plating solution is 200g/L, sulfuric acid concentration is 90 g/L, and chlorine ion concentration is 100ppm, and neopelex concentration is 2g/L;
5) electroplate liquid of graphene-containing configuration: multi-layer graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 2g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, regulating temperature is 20
oc, current density are 1A/dm
2, under stirring condition, electroplate 50min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Embodiment 5
1) pet substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) copper facing on the pet substrate processed;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, neopelex and hydrochloric acid, stir, obtain plating solution, concentration of copper sulfate in plating solution is 180g/L, sulfuric acid concentration is 65 g/L, and chlorine ion concentration is 100ppm, and neopelex concentration is 1.2g/L;
5) electroplate liquid of graphene-containing configuration: single-layer graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 3g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, regulating temperature is 25
oc, current density are 2A/dm
2, under stirring condition, electroplate 30min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Embodiment 6
1) pet substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) copper facing on the pet substrate processed;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, lauryl sodium sulfate and hydrochloric acid, stir, obtain plating solution, concentration of copper sulfate in plating solution is 200g/L, sulfuric acid concentration is 70g/L, and chlorine ion concentration is 100ppm, and lauryl sodium sulfate concentration is 1.2g/L;
5) electroplate liquid of graphene-containing configuration: multi-layer graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 3g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, regulating temperature is 28
oc, current density are 3A/dm
2, under stirring condition, electroplate 20min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
Claims (5)
1. there is an interconnection line for copper-graphite alkene complex phase, it is characterized in that on insulated substrate (1), having successively copper layer (2) and copper-graphite alkene complex phase conductive layer (3) from bottom to top.
2. the interconnection line with copper-graphite alkene complex phase according to claim 1, is characterized in that: described insulated substrate (1) is PET or Si/SiO
2substrate.
3. a method of preparing the interconnection line with copper-graphite alkene complex phase as claimed in claim 1, is characterized in that comprising the following steps:
1) insulated substrate is put into acetone ultrasonic cleaning, and with deionized water rinsing;
2) use the method for chemical plating through step 1) copper facing on the insulated substrate processed;
3) use the method for photoetching to step 2) copper layer pattern, interconnection line figure is transferred on copper layer;
4) copper electrolyte configuration: copper sulphate water is dissolved, add successively therein sulfuric acid, surfactant and hydrochloric acid, stir, obtain copper electrolyte, concentration of copper sulfate in copper electrolyte is 150-250g/L, sulfuric acid concentration is 40-110 g/L, and chlorine ion concentration is 50-120 ppm, and surfactant concentration is 0.1-2g/L;
5) electroplate liquid of graphene-containing configuration: graphene nanometer sheet is first used to a small amount of step 4) copper electrolyte wetting and ultrasonic after, join again in remaining copper electrolyte, the concentration of graphene nanometer sheet is 0.01-4g/L, fully stirs, and obtains the electroplate liquid of graphene-containing;
6) electroplate: taking phosphorus bronze sheet as anode, step 2) the patterned copper layer of gained is as negative electrode, is placed in step 5) the electroplate liquid of graphene-containing nanometer sheet, adjusting temperature is 10-40
oc, current density are 0.5-16A/dm
2, under stirring condition, electroplate 1-120min, obtaining conductive layer is the interconnection line of copper-graphite alkene complex phase.
4. the preparation method of the interconnection line with copper-graphite alkene complex phase according to claim 3, is characterized in that: described surfactant is neopelex or lauryl sodium sulfate.
5. the preparation method of the interconnection line with copper-graphite alkene complex phase according to claim 3, is characterized in that: described graphene nanometer sheet is single or multiple lift.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106793533A (en) * | 2017-01-16 | 2017-05-31 | 厦门大学 | A kind of printed circuit board and conductive membrane preparation method with copper Graphene complex phase pattern conductive film |
| CN108677172A (en) * | 2018-04-18 | 2018-10-19 | 重庆材料研究院有限公司 | A kind of Zero-discharge non-pollution graphene electroless copper plating method |
| CN110344099A (en) * | 2019-07-18 | 2019-10-18 | 桂林电子科技大学 | A kind of preparation method of high thermal conductivity graphene composite thin film material |
| CN110846662A (en) * | 2019-11-12 | 2020-02-28 | 四川轻化工大学 | Copper/graphene-plated magnesium alloy composite material and preparation method thereof |
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| CN103606514A (en) * | 2013-12-03 | 2014-02-26 | 西安电子科技大学 | Chemical corrosion transfer method based on GaN substrate CVD epitaxial growth graphene |
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| CN102859032A (en) * | 2010-02-26 | 2013-01-02 | 独立行政法人产业技术总合研究所 | Carbon film laminate |
| US20140120270A1 (en) * | 2011-04-25 | 2014-05-01 | James M. Tour | Direct growth of graphene films on non-catalyst surfaces |
| CN102849961A (en) * | 2011-07-01 | 2013-01-02 | 中央研究院 | Method for growing carbon film or inorganic material film on substrate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106793533A (en) * | 2017-01-16 | 2017-05-31 | 厦门大学 | A kind of printed circuit board and conductive membrane preparation method with copper Graphene complex phase pattern conductive film |
| CN108677172A (en) * | 2018-04-18 | 2018-10-19 | 重庆材料研究院有限公司 | A kind of Zero-discharge non-pollution graphene electroless copper plating method |
| CN110344099A (en) * | 2019-07-18 | 2019-10-18 | 桂林电子科技大学 | A kind of preparation method of high thermal conductivity graphene composite thin film material |
| CN110846662A (en) * | 2019-11-12 | 2020-02-28 | 四川轻化工大学 | Copper/graphene-plated magnesium alloy composite material and preparation method thereof |
| CN110846662B (en) * | 2019-11-12 | 2021-12-17 | 四川轻化工大学 | Copper/graphene-plated magnesium alloy composite material and preparation method thereof |
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Application publication date: 20140723 |