A metal–metal bonding process using metallic copper.pdf

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j m a t e r r e s t e c h n o l . 2 0 1 4 ; 3(2) :114121

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Original Article

A metalmetal bonding process using metallic coppernanoparticles produced by reduction of copper oxidenanoparticles

Yoshio Kobayashi a , , Yuki Abe a , Takafumi Maeda a , Yusuke Yasuda b, Toshiaki Morita ba

Department of Biomolecular Functional Engineering, College of Engineering, Ibaraki University, Hitachi, Ibaraki, Japanb Hitachi Research Laboratory, Hitachi Ltd., Hitachi, Ibaraki, Japan

a r t i c l e i n f o

Article history:Received 20 September 2013Accepted 24 December 2013Available online 6 February 2014

Keywords:Metallic Cu

Copper oxideNanoparticleMetalmetal bonding

a b s t r a c t

Metalmetal bonding was performed using metallic Cu nanoparticles fabricated from CuOnanoparticles. Colloid solutions of CuO nanoparticles were prepared by the reaction of Cu(NO3)2 and NaOH in aqueous solution at reaction temperatures ( T CuOs) of 20, 40, 60 and80 C. CuO single crystallites with a size of ca. 10nm were produced, and they formed leaf-like aggregates. The longitudinal and lateral sizes of the aggregates decreased from 522 to84 nm and from 406 to 23nm, respectively, with an increase in T CuO. Colloid solutions of metallic Cu nanoparticles were prepared by reducing the CuO nanoparticles with hydrazine

in

the presence of cetyltrimethylammonium bromide. The size of the metallic Cu nanopar-ticles decreased from 92 to 73nm with increasing T CuO. Metallic copper discs were bondedwith the metallic Cu nanoparticles by annealing at 400 C and 1.2MPa for 5min in H 2 gas.The shear strength required to separate the bonded discs increased with increasing T CuO. Amaximum shear strength of 39.2MPa was recorded for a T CuO of 80 C.

2014 Brazilian Metallurgical, Materials and Mining Association. Published by ElsevierEditora Ltda. All rights reserved.

1. Introduction

In metalmetal bonding processes, which are importantin many elds, solders or llers have conventionally beenused for efcient bonding [15]. These solders are meltedat high temperatures and spread between metallic surfaces,thus bonding the surfaces together. A decrease in temper-ature solidies the metallic materials and completes themetalmetal bonding.Metallicalloys composedmainly of leadand tin have been used as solders [14]. These metallic alloys

Corresponding author .E-mail: [email protected] (Y. Kobayashi).

melt at temperatures as low as 184 C, lower than the melting points of many other metallic alloys. The lead- and tin-basedalloys diffuse into the materials to be bonded, and then, theycan be bonded at low temperatures. It is well known thatlead is harmful to living bodies, which limits its use. Variouslead-free alloys have been developed as new solders [611].Although low-temperature metalmetal bonding can be per-formedusing the lead-freesolders, there is a serious problem:the bonded materials may break apart when exposed to tem-peratureshigher than their melting pointsdue to remelting of the solders.

2238-7854/$ see front matter 2014 Brazilian Metallurgical, Materials and Mining Association. Published by Elsevier Editora Ltda. All rights reserved.http://dx.doi.org/10.1016/j.jmrt.2013.12.003
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Metallic materials such as Au, Ag and Cu can be used asthe ller because they have excellent electrical and thermalconductivities. However, their melting points are ca. 1000 C,higher than those of the conventional lead- and tin-basedsolders. High-temperature annealing is required during thebonding process to successfully bond metallic materials, andthese high temperatures thermally damage the material nearthe bonding site.

The melting pointsof metallic materialssuchas Au, Ag andCuareca. 1000 C in the bulk state butdecrease as the materialsize is decreased to several nanometers [1216]. This decreasein the melting point decreases the temperature needed forthe metalmetal bonding process. Once the metallic materi-als are bonded with the metallic nanoparticles, they remainbonded even at temperatures higher than the melting pointsof the metallic nanoparticles because the nanoparticles con-vert to a bulk state during bonding. Various researchers havestudied metalmetal bonding using metallic Ag nanoparti-cles as the ller [15,1723]because metallic Ag is chemicallystable. Although Ag nanoparticles work well as a ller formetalmetal bonding, they have some disadvantages: metal-lic Ag is relatively expensive and prone to migration under anapplied voltage, which may damage an electric circuit.

Metallic Cu is promising as a ller for bonding because itis inexpensive and because electric migration does not takeplace as often as it does with metallic Ag. Several researchershave studiedmetalmetal bonding using metallicCu nanopar-ticles [20,24,25]. Our research group has developed a methodfor producing metallic Cu nanoparticles for use as the llerin metalmetal bonding [2630]. Metallic Cu nanoparticles areusually prepared using methods based on the direct reduc-tion of copper ions with reducing reagents in the liquidphase.Copper oxide can also be used as a precursor. Previously, ourresearch group proposed a method for fabricating metallic Cunanoparticles using CuO nanoparticles as the precursor andexamined the metallic Cu nanoparticles as a ller for bonding [31]. We also varied the morphologies of CuO nanoparticlesand CuO-nanoparticle aggregates with several parameterssuch as the reaction temperature [32]. The morphology of metallic Cu particles depended on the morphologies of theCuO nanoparticles and CuO-nanoparticle aggregates as wellas on theconcentrations of chemicals. Themetalmetal bond-ing properties are related to the morphology of the metallicCu nanoparticles. In the present work, metallic Cu nanopar-ticles are fabricated from CuO nanoparticles with variouspreparation parameters and are examined with respect tometalmetal bonding.

2. Experimental work

2.1. Chemicals

The reactants for the production of copper oxide were cop-per (II) nitrate trihydrate (Cu(NO 3)2 3H2O) (77.080.0% (asCu(NO3)2)) and sodium hydroxide solution (NaOH) (5M).Hydrazine monohydrate (>98.0%) and cetyltrimethylammo-nium bromide (CTAB) (99%) were used as a reducing reagentfor copper oxide and as a stabilizer for the resulting metallicCu nanoparticles, respectively. All chemicals were purchased

from Kanto Chemical Co., Inc. and were used as received.Water that was ion-exchanged and distilled with a YamatoWG-250 system was used in all preparations, and it was deae-rated by bubbling with N 2 gas for 30min prior to preparationof the aqueous solutions of Cu(NO 3)2.

2.2. Preparation

Colloid solutions of copper oxide nanoparticles were synthe-sized using a reaction between copper ions and a base, asdescribed in our previous work [31]. An aqueous solution of NaOH was added to an aqueous solution of Cu(NO 3)2 withvigorous stirring at reaction temperatures ( T CuOs) of 20,40,60and 80 C. The reaction times were 3 h at T CuOs of 60 and 80 Cand 24h at T CuOs of 20 and 40 C. The initial concentrationsof Cu(NO3)2 and NaOH were 1.25 10 2 and 2.375 10 2 M,respectively, which resulted in an Na/Cu molar ratio of 1.9 inthe nal solution.

Colloid solutionsof metallic Cu nanoparticles were synthe-sized by reducing thecopper oxide nanoparticles. An aqueoussolution of CTAB was added to the colloid solution of copperoxide nanoparticles. After 30min, hydrazine was added. Boththe additions were performed in air with vigorous stirring at aconstant solution temperature of 30 C, and the reaction timewas 3 h. Initial concentrations of Cu, hydrazine and CTAB inthe nal colloid solution were 1.0 10 2, 0.8 and 5.0 10 3 M,respectively. The resulting nanoparticles were washed rstwith centrifugation at 10,000rpm for 30min, followed by theremovalof thesupernatant, theadditionof water,and shaking of the mixture with a vortex mixer to disperse the nanoparti-cles. This process was performed three times. The powderednanoparticles were obtained by drying the nanoparticles atroom temperature in a vacuum after the nal removal of thesupernatant.

2.3. Characterization

The particles were characterized by transmission electronmicroscopy (TEM) and X-ray diffractometry (XRD). TEM obser-vation was performed with a JEOL JEM-2100 microscopeoperating at 200 kV. Samples for TEM were prepared by drop-ping and evaporating the nanoparticle colloid solution on acollodion-coated copper grid. Dozens of particle diameterswere measured in TEM images to determine an average parti-cle size and a standard deviation. XRD patterns were obtainedwith a Rigaku Ultima IV X-ray diffractometer at 40kV and30mA with Cu K 1 radiation. Samples for XRD were pre-pared by removing the supernatant of the nanoparticlecolloidsolutionwith decantationanddrying the residue at room tem-perature for 24h in a vacuum.

The metalmetal bonding properties of metallic Cunanoparticles were investigated by a method described in ourpreviouswork [21,3335]. The powdered particles, which wereprepared usingthe same processas that usedfortheXRDsam-ples, was spread on a copper stage with a diameter of 10mmand a thickness of 5mm. A copper plate with a diameter of 5mm and a thickness of 2.5mm was placed on top of thepowder sample. The copper stage and plate were pressed at1.2MPa while annealing in H 2 at 400 Cfor5min with a ShinkoSeiki vacuum reow system. After bonding, the copper stage


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and plate were separated by applying a shear strength, whichwasmeasured with a Seishin SS-100KP bond tester. The bond-ing and the measurement of shear strength were performedtwo or three times for each sampleandaveraged to determinethebonding strengthof the nanoparticles. The surface of eachcopper plate was observed by scanning electron microscopy(SEM) with a JEOL JSM-5600LV microscope after the measure-ment of shear strength.

3. Results and discussion

3.1. Morphology of copper oxide nanoparticles

The blue aqueous solution of Cu(NO 3)2 became a black col-loid solution after the addition of the NaOH solution. BecauseCuO is black, this observation implied the production of CuO.Fig. 1 shows the TEM images of the prepared nanoparticles, of which colloid solutions were prepared at various T CuOs. At aT CuO of20 C, leaf-likeaggregates withan averagelongitudinalsize of 522 nm and an average lateral size of 406 nm were pro-duced. A high magnication image (inset of Fig. 1(a)) revealedthat the aggregates appeared to be composed of nanoparti-cles with a size of ca. 10nm, which is only an estimate, asthe outlines of the nanoparticles were not well dened in theTEM images. The addition of NaOH made the pH of the solu-tion approach its isoelectric point (IEP) without exceeding itbecause the Na/Cu ratio of 1.9 was lower than the stoichio-metric ratio of 2 required for complete reaction of NaOH and

Cu2+. This increase in pH decreased the surface charge of the nanoparticles, which resulted in their aggregation. Theaggregate size decreased with increasing T CuO; the longitu-dinal/lateral aggregate sizes (in nm) were 522 43/406 39at 20 C, 208 22/151 9 at 40 C, 75 10/48 9 at 60 C and84 15/23 5 at 80 C. This trend corresponded with our pre-vious work [32], which examined the fabrication of CuOparticles at initial concentrations of 1.0 10 2 M Cu(NO3)2and 1.9 10 2 M NaOH. In our previous work [31], the IEPof CuO particles prepared at 80 C was higher than that of CuO nanoparticles prepared at 20 C. Therefore, at a T CuOof 80 C, the pH did not closely approach the IEP. Conse-quently, electrostatic repulsions between the nanoparticleslimited aggregation, and small aggregates were produced athigh T CuOs.

Fig. 2 shows the XRD patterns of the CuO nanoparticles.For the particles prepared at 20 C, the dominant peaks wereat 12.8 and25.8 . These peaks were assigned to Cu 2(OH)3NO3(JCPDS card No. 15-0014). In addition, several peaks attributedto monoclinic CuO (JCPDS card No. 5-0661) were recordedat 35.6 , 38.8 , and 48.9 . The appearance of Cu 2(OH)3NO3peaks indicated that the T CuO of 20 C was too low for com-plete reaction of Cu(NO 3)2 to CuO. At T CuOs over 20 C, theCu2(OH)3NO3 peaks disappeared, and only the peaks due toCuO were detected. Accordingly, it was found that the purityof CuO nanoparticles increased with increasing T CuO. Appli-cation of the Scherrer equation to the XRD line broadening of the 35.6 peak provided average CuOcrystal sizes of 12.6, 14.3,13.4 and 10.7nm for 20, 40, 60 and 80 C, respectively. There

Fig. 1 TEM images of various nanoparticles. Colloid solutions of samples (a)(d) were prepared with the saltbase reactionat 20, 40, 60, and 80 C.


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10 20

a

b

c

d

30

2 (degree), CuK

I n t e n s

i t y

( a r b . u

n i t s

)

40 50 60 70 80

Fig. 2 XRD patterns of various nanoparticles. Samples(a)(d) were the same as in Fig. 1 . Symbols ( ) and ( ) standfor CuO and Cu 2 (OH)3NO3 , respectively.

was no large difference in crystal size at the T CuOs examined.These crystal sizes of ca. 10nm were similar to the sizes of the nanoparticles composing the aggregates. This similarityindicated that single crystals of CuO formed the aggregates.

3.2. Morphology of metallic copper nanoparticles

Theadditionof hydrazine reddenedthe colloidsolutionofCuOnanoparticles. Since surface plasmon resonance absorptionof metallic Cu nanoparticles results in a red color, the red-dening implied the production of metallic Cu nanoparticles.Fig. 3 shows TEM images of the metallic Cu particles. The par-ticles had rough surfaces. Although someparticles larger than1 m were observed,almostall of thenanoparticles examinedhad sizes in the range of 50150nm. The average particle sizeswere 92 33, 93 33, 101 37 and 73 23nm for T CuOs of 20,40, 60 and 80 C, respectively; the particle size was approxi-mately constant in the T CuO range of 2060 C but decreasedwhen the T CuO was increased to 80 C. As shown in Fig. 1, theaggregate size decreased with increasing T CuO. Accordingly,aggregate size was considered a reection of particle size.

Fig. 4 shows theXRD patterns of themetallic Cu nanoparti-cles. Thepatternsshowed peaks at43.3 ,50.3 and74.2 . Thesepeaks were attributed to cubic metallic Cu (JCPDS card No.4-0836). In addition to the metallic Cu peaks, a faint peak wasdetected at 36.6 in each pattern. This peak was assigned tocubic metallic Cu 2O (JCPDS card No. 5-0667). The detection of Cu2O indicatedthat the nanoparticles were partiallyoxidized.The average crystal sizes of the metallic Cu nanoparticles,

Fig. 3 TEM images of various nanoparticles. Colloid solutions of samples (a)(d) were prepared by reducing the samples(a)(d) in Fig. 1 , respectively.


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1 0 2 0

a

b

c

d

3 0 4 0 5 0

2 (de gree ), C uK

I n t e n s

i t y

( a r b . u n

i t s

)

6 0 7 0 8 0

Fig. 4 XRD patterns of various nanoparticles. Samples(a)(d) were the same as in Fig. 3 . Symbols ( ) and ( ) standfor metallic Cu and Cu 2O, respectively.

which were estimated from the XRD line broadening of the43.3 peak using the Scherrer equation, were 33.1, 31.1, 28.2and 32.6nm at T CuOs of 20, 40, 60 and 80 C, respectively. Theparticle size observed with TEM was larger than the crystal

size, which indicated that the nanoparticles were polycrys-talline.

3.3. Bonding properties of metallic coppernanoparticles

Fig. 5 shows the photographs of the copper plates after themeasurement of shear strength. For all the particles exam-ined, the pressedpowders on theplatesappeared to be faintlyreddish due to the presence of metallic Cu: the powderswere still metallic after the bonding process. This observa-tion implies that themetallic Cu powdersstrongly bondedthecopper discs together.

Fig. 6 shows shear strength as a function of T CuO. All oftheshear strengths measured were over 20MPa, which indicatedthat the copper discs were strongly bonded for all the parti-cles examined and also corresponded to the strong bonding implied in Fig. 5. The shear strength increased with increas-ing T CuO andreached39.2MPa ata T CuO of80 C, whichwas thelargest in thepresentwork.As shown in Fig. 3, the particle sizedecreased with increasing T CuO. Small particles have a largersurface area than large particles if the amount of materialis the same. Therefore, the contact area between the parti-cles and the Cu discs was larger for the small particles, asa result of the larger surface area, than for the large parti-cles. This large contact area for the small particles probablycaused the strong metalmetal bonding. There are other pos-sible causes as well. One possible cause involves impuritiesin the metallic Cu nanoparticles. Our previous work showed

Fig. 5 Photographs of the copper plates after the measurement of shear strength. The powders used were the metallic Cuparticles (a)(d) shown in Fig. 3 .


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50

40

30

20

10

S h e a r s

t r e n g

t h ( M P a

)

020 40 60 80

T CuO (C)

Fig. 6 Shear strength vs. T CuO . The powders used were themetallic Cu particles (a)(d) shown in Fig. 3 .

that thepresenceof Cu 2(OH)3NO3 decreased the bonding abil-ity [31]: during bonding, the elimination of NO 3 and H 2Ofrom Cu 2(OH)3NO3 produced pores that prevented the par-ticles from sintering, thus decreasing the shear strength. Inthe present work, the CuO nanoparticles fabricated at the

low T CuO contained Cu 2(OH)3NO3, while the purity of CuOnanoparticles increased with increasing T CuO, as indicated bythe XRD measurements ( Fig. 2). Because the CuO nanoparti-cles were the precursor of the metallic Cu particles, the purityof the metallic Cu nanoparticles should depend on that of theCuO nanoparticles. The purity of the metallic Cu nanoparti-cles might increase with increasing T CuO, while Cu 2(OH)3NO3might remain in the metallic Cu nanoparticles derived fromthe CuO nanoparticles produced at the low T CuO. Therefore,the metallic Cu nanoparticles derived from the CuO nanopar-ticles producedat thehigh T CuO probablydidnotcontainmuchCu2(OH)3NO3, and elimination of NO 3 and H 2O did not occurduring bonding in the metallic Cu nanoparticles at high T CuO.Thus, no decrease in bonding ability as a result of impuritieswas expected for the high T CuO sample. The other possiblecause of strong metalmetal bonding in the high T CuO sampleinvolves a size effect. Sintering of particles takes place inten-sively for small particles because of the size effect related tothe depression of the melting point. This intensive sintering might have contributed to the strong metalmetal bonding with high T CuO, at which the smaller nanoparticles were pro-duced. These three factors are the possible mechanisms forthe strong bonding achieved by the nanoparticles fabricatedat the T CuO of 80 C.

Fig. 7 shows the SEM images of the surfaces of the copperdiscs separated withshear stress.Somedimplesaccompaniedby sharp tips were observed on the surfaces for the samplesat T CuOs of 20 and 80 C. When the metallic materials are sep-arated with shear stress, dimples often form in the bonded

Fig. 7 SEM images of the copper plates after the measurement of shear strength. The powders used were the metallic Cuparticles (a)(d) shown in Fig. 3 .


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region. Such dimples were produced in materials that under-went a strong bonding process using Ag nanoparticles, asreported by Morisada et al. [20] Therefore, the observation of dimples on the copper disks suggests that they were stronglybonded using the metallic Cu nanoparticles. For the T CuOs of 40 and 60 C, clear dimples were not observed, but the bondedmaterials appeared to be sharply cut off. This sharp cut-off also indicated strong bonding.

4. Conclusions

Colloid solutions of leaf-like aggregates composed of CuOsin-gle crystallites with a size of ca. 10nm were prepared byreacting 1.25 10 2 M Cu(NO3)2 with NaOH in aqueous solu-tion at an Na/Cu ratio of 1.9 and at T CuOsof20,40,60and80 C.The aggregate size decreased from 522 to 84nm for longitudi-nal size and from 406 to 23nm for lateral size with an increasein T CuO from 20 to 80 C. The CuO nanoparticles, with a Cuconcentration of 1.25 10 2 M in the colloid solution, were

reduced with 0.8 M hydrazine in the presence of 5.0 10

3 MCTAB in water at 30 C to produce the metallic Cu nanoparti-cles. Thesize of the metallic Cu nanoparticles decreased from92 to 73nm with an increase in T CuO from 20 to 80 C. Thebonding strengthof theparticles was examined byputting themetallic Cu nanoparticles between two metallic copper discsand then annealing the discs at 400 C ata pressureof 1.2MPafor 5min in H2 gas. The shear strength required to separatethe bonded discs increased with increasing T CuO, reaching amaximum of 39.2MPa at a T CuO of 80 C. Further studies onthe practical use of metallic Cu nanoparticles and the precisebonding mechanism are in progress.

Conicts of interest

The authors declare no conicts of interest.

Acknowledgements

This work was partially supported by Hitachi, Ltd. We expressour thanks to Prof. T. Noguchi at the College of Science of Ibaraki University, Japan for assistance with the TEM obser-vations.

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A metal–metal bonding process using metallic copper.pdf

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