CN111379029B - Rapid preparation of NiSn4Method for single crystal phase - Google Patents

Rapid preparation of NiSn4Method for single crystal phase Download PDF

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CN111379029B
CN111379029B CN202010337787.6A CN202010337787A CN111379029B CN 111379029 B CN111379029 B CN 111379029B CN 202010337787 A CN202010337787 A CN 202010337787A CN 111379029 B CN111379029 B CN 111379029B
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single crystal
nisn
crystal phase
sheet
phase
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CN111379029A (en
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陈捷狮
杨明远
曾志
杨瑾
张泽强
尹志康
孟玄
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Shanghai University of Engineering Science
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64—Flat crystals, e.g. plates, strips or discs

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Internal Circuitry In Semiconductor Integrated Circuit Devices (AREA)

Abstract

The invention relates to a method for rapidly preparing NiSn4The method of single crystal phase uses a single crystal Ni sheet as a bonding pad, and the single crystal Ni sheet and Sn-based solder are refluxed at 220-260 ℃ to prepare NiSn4A single crystalline phase; the NiSn4The thickness of the single crystal phase is more than or equal to 3 mu m, and the area is not less than 4 mu m2(ii) a The NiSn4The shape of the single crystal phase is a large plate shape instead of a traditional column shape; the NiSn4The single crystal phase is along<001>Directionally growing compounds, rather than disorientation of the direction of growth; the NiSn4The single crystal phase is generated at the interface and is flat, not upright. Large-scale NiSn prepared by the invention4The single crystal phase can be used as a diffusion barrier layer in electronic micro-connection, and the electromigration reliability of an interconnection structure in electronic packaging is improved. The invention has the advantages of rapid preparation, reliable quality, easy control, little influence of external environment conditions on the preparation process, and the prepared NiSn4The thickness of the single crystal phase is controllable.

Description

Rapid preparation of NiSn4Method for single crystal phase
Technical Field
The invention belongs to the technical field of metal material phase preparation, and relates to a method for quickly preparing NiSn4A single crystal phase method.
Background
As mobile electronic devices have developed to be miniaturized and multifunctional, higher demands and challenges are placed on the performance of the interconnection pads. At present, three-dimensional packaging is often adopted in electronic packaging, the plane form of the traditional packaging is broken through, in three-dimensional lamination interconnection, the space and the size of welding spots are both sharply reduced, and Sn-based solder in the welding spots can react with metal of a welding pad in the welding process and is partially converted into intermetallic compounds (IMCs). During the subsequent service of the solder joint, the IMCs at the interface will grow and transform further. A uniform thickness of the IMCs layer is necessary for better interconnection of the solder joints, but an excessively thick layer of IMCs can cause cracking of the interconnection interface due to the brittle and hard nature, resulting in solder joint failure. At the interface, the IMCs layer thus acts as the sole interconnect medium, the growth and transformation of which are critical to the reliability and service performance of the solder joint.
In electronic packaging, soldering of Cu-containing pads with Sn-based solder often uses a thin Ni buffer layer as a diffusion barrier layer to prevent formation of excessively thick Cu at the interface6Sn5And (3) a layer. However, the Ni buffer layer also reacts with the Sn solder to form an IMCs layer. At present, a polycrystal Ni plate is often adopted as the Ni buffer layer, and stable Ni is formed at the interface3Sn4And (3) a layer. NiSn is also known to be present in the Sn/polycrystalline Ni system4Phase, however, NiSn4Phase at all temperatures against tin solid solution and Ni3Sn4The phases are all metastable, thus producing NiSn4Is relatively difficult. Currently, the most commonly used NiSn4The phase is prepared by solid-phase reaction diffusion coupling method, in which Sn solder is electroplated on a polycrystalline Ni pad, and then aged at room temperature for 10 days to 5 months to obtain NiSn4The phase thickness is only a few microns, the preparation is very difficult, and NiSn generated by taking a polycrystalline Ni sheet as a bonding pad4The phase is metastable at high temperatures because grain boundary diffusion of the polycrystals provides a significant amount of Ni problems that can transform to form Ni at the interface3Sn4And (4) phase(s). Finally, a large piece of NiSn4The semiconductor material can be used as a barrier layer for interface element diffusion, and further improves the electromigration reliability of an interconnection structure in electronic packaging.
In summary, the conventional NiSn4The preparation of the phases is slow and unstable, and rapid and stable preparation cannot be carried out. Therefore, there is an urgent need to develop a NiSn which is fast in preparation, reliable in quality, easy to control, and little in influence of external environmental conditions on the preparation process4Method for the preparation of the phases.
Disclosure of Invention
The invention aims to solve the problem of NiSn in the prior art4Slow phase preparation, small size and instabilityTo provide a method for rapidly preparing NiSn4Method of single crystal phase, NiSn prepared4The single crystal phase is stable and large in size.
One of the purposes of the invention is to provide a method for rapidly preparing NiSn4A single crystal phase method, namely refluxing for a short time (10 s-30 min) at 220-260 ℃ to prepare stable large-size NiSn4A single crystal phase method.
The second purpose of the invention is to provide a large-size stable NiSn4A single crystalline phase.
The third purpose of the invention is to provide a large-sized NiSn4The single crystal phase can act as a diffusion barrier in electronic micro-interconnects.
The fourth purpose of the invention is to provide a large-sized NiSn4The service life of the single-crystal phase diffusion barrier layer is prolonged by more than 100 times compared with the service life of the traditional barrier-free layer.
The fifth purpose of the invention is to provide a large-sized NiSn4Single crystal phase along<001>And (4) directionally growing.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
rapid preparation of NiSn4The method of single crystal phase comprises the steps of using a single crystal Ni sheet as a bonding pad, and refluxing the single crystal Ni sheet and Sn solder at 220-260 ℃ to prepare NiSn4A single crystalline phase;
the NiSn4The thickness of the single crystal phase is more than or equal to 3 mu m, and the area is not less than 4 mu m2；
The NiSn4The shape of the single crystal phase is a large plate shape instead of a traditional column shape;
the NiSn4The single crystal phase is along<001>Directionally growing compounds, rather than disorientation of the direction of growth;
the NiSn4The single crystal phase is generated at the interface and is flat, not upright.
As a preferred technical scheme:
the rapid preparation of NiSn4A single-crystal phase method, the thickness of the single-crystal Ni sheet is not less than 1 mm. The single-crystal Ni plate, its compositionThe method can be used for developing any type of single crystal Ni sheet in 1-5 generation single crystal sheets in China, but the defect rate of the surface is guaranteed to be not more than 2%; the number of surface grain boundaries does not exceed 1%.
The rapid preparation of NiSn4A method of single crystal phase, the Sn solder is pure Sn (Sn content is not less than 99.99 wt%) solder or Sn-based solder containing Ni, Ag, Cu and Zn elements and having Ni content not more than 0.1wt%, Ag content not more than 3.5wt%, Cu content not more than 3.5wt% and Zn content not more than 0.8 wt%.
The rapid preparation of NiSn4The method of the single crystal phase comprises the steps of carrying out surface pretreatment on the single crystal Ni sheet before refluxing, namely polishing the surface area of a material by using metallographic abrasive paper to remove surface oxides and impurities, putting a sample into an acetone solution, carrying out ultrasonic cleaning, taking out, washing with distilled water and drying.
The rapid preparation of NiSn4A single crystalline phase process, said refluxing being: and heating the single crystal Ni sheet to a reflux temperature, and then placing the Sn brazing filler metal on the single crystal Ni sheet for refluxing for 3 min-3 h. If larger size NiSn is required4For single crystal phase, the reflow time may continue to increase until the desired stop is reached.
The rapid preparation of NiSn4A single crystal phase process, said reflow temperature being controlled using a pre-heat stage of a tin melting furnace.
The rapid preparation of NiSn4The method of single crystal phase comprises the steps of placing the alloy in a nitric alcohol solution after refluxing, and removing the Sn brazing filler metal on the top layer, the residual single crystal Ni sheet and NiSn generated at the interface through ultrasonic vibration4A single crystalline phase.
The rapid preparation of NiSn4The single crystal phase method is characterized in that the nital solution is 5-10% of nital solution by volume ratio.
The rapid preparation of NiSn4Method for single crystal phase, further cutting and separating residual single crystal Ni sheet and NiSn generated at interface4Single crystal phase to obtain NiSn4A single crystalline phase.
Large-scale NiSn prepared by the invention4The single crystal phase can be used as a diffusion barrier layer in electronic micro-connection, so that the electromigration reliability of an interconnection structure in electronic packaging is improved, and the service life of the electromigration resistance of the interconnection structure is prolonged by more than 100 times compared with that of the traditional barrier-free layer.
The invention adopts the single crystal Ni welding plate and Sn-based solder containing pure Sn or trace elements at the temperature of: the stable NiSn can be prepared at 220-260 ℃ by short-time reflux (for example, 10 s-30 min)4The single crystal phase is prepared by a solid-liquid interface reaction, and the method is easy to control and can prepare NiSn in a short time4And (4) phase(s). And NiSn is prepared in the early stage4Single crystal phase, solid phase reaction diffusion couple method, its preparation time can be up to 10 days to 5, etc. different time, and the produced NiSn4The phase thickness is also only a few microns, making preparation very difficult. In addition, since the polycrystalline Ni pad is prepared by reacting with Sn-containing solder at the solid-liquid interface, Ni is generated at the interface because of the problem of Ni content provided by grain boundary diffusion3Sn4,The invention changes the diffusion mode from grain boundary diffusion to intracrystalline diffusion by controlling the bonding pad, and finally NiSn is generated by the interface reaction4And the method has great innovative significance.
The invention takes the single crystal Ni sheet as the bonding pad, the NiSn is generated4The phase is stable in solid-liquid interface reaction, mainly because the single crystal Ni welding disc can control the diffusion flux of Ni atoms, stable NiSn can be generated in the solid-liquid interface reaction4A single crystalline phase. In the previous studies, when a polycrystalline Ni plate is used as a bonding pad, the diffusion flux of polycrystalline Ni atoms is large, and NiSn is generated at low temperature4Phase at high temperature, a large amount of Ni atoms are supplied due to grain boundary diffusion, and NiSn cannot be produced by a solid-liquid interface reaction4Phase but Ni3Sn4。
Advantageous effects
Compared with the prior art, the invention has the outstanding advantages of rapid preparation, reliable quality, easy control, little influence of external environment conditions on the preparation process, and the prepared NiSn4The thickness of the single crystal phase is controllable.
Drawings
FIG. 1 is a schematic view of a Sn/Ni joint after reflow;
FIG. 2 is NiSn4Schematic of the phases;
FIG. 3 shows NiSn at different times of reflow4Top layer topography of the phases.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The invention relates to a method for rapidly preparing NiSn4The single crystal phase method is that, as shown in figure 1, a single crystal Ni sheet is used as a bonding pad and reflows with Sn-based solder at 220-260 ℃, and NiSn can be prepared4Single crystal phase, see fig. 2;
the NiSn4The thickness of the single crystal phase is more than or equal to 3 mu m, and the area is not less than 4 mu m2；
The NiSn4The shape of the single crystal phase is a large plate shape instead of a traditional column shape;
the NiSn4The single crystal phase is along<001>Directionally growing compounds, rather than disorientation of the direction of growth;
the NiSn4The single crystal phase is generated at the interface and is flat, but not upright;
the thickness of the single crystal Ni sheet is not less than 1mm, the components of the single crystal Ni sheet can be any type of single crystal Ni sheet in developed domestic 1-5 generation single crystal sheets, but the defect rate of the surface is not more than 2%; the number of surface grain boundaries does not exceed 1 percent;
the Sn brazing filler metal is pure Sn (the Sn content is not less than 99.99wt percent) brazing filler metal or Sn-based brazing filler metal which contains Ni, Ag, Cu and Zn elements, wherein the Ni content is not more than 0.1wt percent, the Ag content is not more than 3.5wt percent, the Cu content is not more than 3.5wt percent and the Zn content is not more than 0.8wt percent;
before the backflow, performing surface pretreatment on the single crystal Ni sheet, namely polishing the surface area of the material by using metallographic abrasive paper to remove surface oxides and impurities, putting a sample into an acetone solution, cleaning the sample by using ultrasonic waves, taking out the sample, washing the sample by using distilled water and drying the sample by blowing;
the refluxing refers to: heating the single crystal Ni sheet to a reflux temperature, then placing the Sn solder on the single crystal Ni sheet for refluxing for 3 min-3 h, and if the NiSn with larger size is needed4The single crystal phase, the reflux time can be increased continuously until the requirement is reached and stopped;
the reflow temperature is controlled by a preheating platform of the tin melting furnace;
after refluxing, the copper foil is also placed in a nitric acid alcohol solution, and ultrasonic vibration is carried out to remove the top Sn brazing filler metal, the residual single crystal Ni sheet and NiSn generated at the interface4A single crystalline phase;
the nitric acid alcohol solution is 5-10% by volume;
removing the top Sn brazing filler metal, the residual single crystal Ni sheet and NiSn generated at the interface by ultrasonic vibration4After single crystal phase, further cutting and separating residual single crystal Ni sheet and NiSn generated at interface4Single crystal phase to obtain NiSn4A single crystalline phase.
Large-scale NiSn prepared by the invention4The single crystal phase can be used as a diffusion barrier layer in electronic micro-connection, so that the electromigration reliability of an interconnection structure in electronic packaging is improved, and the service life of the electromigration resistance of the interconnection structure is prolonged by more than 100 times compared with that of the traditional barrier-free layer.
The invention is based on a method for quickly generating NiSn4The preparation method of the phase comprises the following specific steps:
(1) performing surface pretreatment on a single crystal Ni substrate material, namely polishing the surface area of the material by using metallographic abrasive paper to remove surface oxides and impurities, putting a sample in acetone, cleaning the sample by using ultrasonic waves, taking out the sample, washing the sample by using distilled water, and drying the sample for later use;
(2) a preheating platform of a tin melting furnace is used for heating the processed monocrystal Ni substrate to the reflux temperature (220-260 ℃),then placing the Sn solder on a monocrystal Ni substrate for refluxing for different times (3min,10min,20min,30min,1h and 3h), and then rapidly preparing the NiSn4Single crystal phase, FIG. 3 shows NiSn at different times of reflow4The top layer appearance of the phase is schematic, and NiSn with different thicknesses can be obtained by controlling the reflow temperature and the reflow time4A single crystalline phase;
(3) placing the prepared sample in 5-10% nitric acid alcohol solution by volume ratio, removing excess Sn solder on the top of the sample by ultrasonic vibration, wherein the interface is NiSn4Single crystal phase, characterization of the treated sample by scanning electron microscopy (different scale characterization requirements) to yield NiSn4The top layer appearance of the phase is analyzed, and NiSn under different reflow times is analyzed4Thickness and orientation of the single crystalline phase.
From the above description, the worker can make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.

Claims (5)

1. Rapid preparation of NiSn4A method of single crystal phase characterized by: the single crystal Ni sheet is used as a bonding pad and reflows with Sn-based brazing filler metal at 220-260 ℃, and NiSn can be prepared4A single crystalline phase;
the refluxing refers to: heating the single crystal Ni sheet to a reflux temperature, and then placing the Sn-based brazing filler metal on the single crystal Ni sheet for refluxing for 3 min-3 h;
the defect rate of the single crystal Ni sheet is not more than 2%; the number of surface grain boundaries does not exceed 1 percent;
the thickness of the single crystal Ni sheet is not less than 1 mm;
the Sn-based solder is pure Sn, namely solder with the Sn content not less than 99.99wt%, or Sn-based solder which contains Ni, Ag, Cu and Zn elements, wherein the Ni content is not more than 0.1wt%, the Ag content is not more than 3.5wt%, the Cu content is not more than 3.5wt% and the Zn content is not more than 0.8 wt%;
after the reflux, the mixture is also placed in nitric acidRemoving the top Sn-based brazing filler metal, the residual single crystal Ni sheet and NiSn generated at the interface in alcohol solution through ultrasonic vibration4A single crystalline phase; further cutting and separating residual single crystal Ni sheet and NiSn generated at interface4Single crystal phase to obtain NiSn4A single crystalline phase;
the NiSn4The thickness of the single crystal phase is more than or equal to 3 mu m, and the area is not less than 4 mu m2；
The NiSn4The shape of the single crystal phase is a large plate;
the NiSn4The single crystal phase is along<001>A directionally growing compound;
the NiSn4The single crystal phase is generated at the interface and is flat.
2. The rapid preparation of NiSn as claimed in claim 14The method for preparing the single crystal phase is characterized in that before the backflow, the surface of the single crystal Ni sheet is pretreated, namely, metallographic abrasive paper is used for polishing the surface area of the material, surface oxides and impurities are removed, a sample is placed in an acetone solution, and the sample is taken out after being cleaned by ultrasonic waves and is washed by distilled water and dried by blowing.
3. The rapid preparation of NiSn as claimed in claim 14A method of single crystal phase, characterized in that the reflow temperature is controlled using a pre-heating stage of a tin melting furnace.
4. The rapid preparation of NiSn as claimed in claim 14The method for single crystal phase is characterized in that the nital solution is 5-10% by volume.
5. The rapid preparation of NiSn as claimed in claim 14Method of single crystal phase, characterized in that said NiSn4The single crystal phase can be used as a diffusion barrier layer in electronic micro-connection, the electromigration reliability of an interconnection structure in electronic packaging is improved, and the electromigration resistance of the interconnection structure is prolonged by more than 100 times compared with the service life of the traditional barrier-free layer.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104701283A (en) * 2015-02-09 2015-06-10 大连理工大学 intermetallic compound filled three-dimensional packaging vertical through hole and preparation method thereof
CN104690383A (en) * 2015-02-09 2015-06-10 大连理工大学 Preparation method and structure of fully intermetallic compound interconnection solder joints
CN104701249A (en) * 2015-02-09 2015-06-10 大连理工大学 Intermetallic compound filled three-dimensional packaging vertical through hole and preparation method thereof
CN104716058A (en) * 2015-02-09 2015-06-17 大连理工大学 Manufacturing method and structure for all-intermetallic compound interconnection welding spot for flip chip
CN110193642A (en) * 2019-06-04 2019-09-03 北京理工大学 A kind of welding procedure that regulation scolding tin connector crystal grain is orientated and organizes
JP2020056090A (en) * 2018-10-04 2020-04-09 三菱マテリアル株式会社 Anticorrosive terminal material, manufacturing method therefor, and anticorrosive terminal and wire terminal part structure

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104701283A (en) * 2015-02-09 2015-06-10 大连理工大学 intermetallic compound filled three-dimensional packaging vertical through hole and preparation method thereof
CN104690383A (en) * 2015-02-09 2015-06-10 大连理工大学 Preparation method and structure of fully intermetallic compound interconnection solder joints
CN104701249A (en) * 2015-02-09 2015-06-10 大连理工大学 Intermetallic compound filled three-dimensional packaging vertical through hole and preparation method thereof
CN104716058A (en) * 2015-02-09 2015-06-17 大连理工大学 Manufacturing method and structure for all-intermetallic compound interconnection welding spot for flip chip
JP2020056090A (en) * 2018-10-04 2020-04-09 三菱マテリアル株式会社 Anticorrosive terminal material, manufacturing method therefor, and anticorrosive terminal and wire terminal part structure
CN110193642A (en) * 2019-06-04 2019-09-03 北京理工大学 A kind of welding procedure that regulation scolding tin connector crystal grain is orientated and organizes

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