CN102527747A - Method for preparing copper-molybdenum-copper laminar composite material - Google Patents

Abstract

The invention relates to a method for preparing a copper-molybdenum-copper laminar composite material, and belongs to the technical field of connection of different metals. The method is mainly characterized by comprising the following steps of: rolling molybdenum plates and copper plates which are prepared by using powder metallurgy into different thicknesses, annealing at a high temperature to remove internal stress, performing surface polishing and cleaning on the molybdenum plates and the copper plates of different thicknesses ratios, drying, then stacking the plates in a hydrogen tunnel furnace, and thus compounding the plates into the laminar composite plates at a high temperature under the action of certain pressure. Compared with the explosion cladding or roll cladding method adopted by the conventional molybdenum-copper composite plates, the method has the advantages that: the environment is safer, the processing flow is simpler and environment-friendly, the thickness ratio of the molybdenum plates to the copper plates can be accurately ensured, the laminar composite material with a good composite interface can be obtained, and the composite material can be used as an electronic encapsulation material or a heat sink material and applied in the technical field of electronic information.

Description

A kind of preparation method of copper molybdenum copper laminar composite

Technical field

The present invention relates to the preparation method of a kind of CMC (copper molybdenum copper) laminar composite, belong to dissimilar metal interconnection technique field.The laminar composite that the present invention makes can be used as a kind of electronic package material or heat sink material is applied to electronic information technical field.

Background technology

Cu has high conduction and heat conductivility, is widely used in the Electronic Packaging field, but because its thermal coefficient of expansion is excessive, does not match with a lot of semi-conducting materials, possibly cause the defective of product structure or function aspects.The thermal coefficient of expansion of Mo is low; Heat-conductivity conducting property is good, and itself and the compounded CMC of Cu (copper molybdenum copper) laminar composite are integrated both advantages, and the heat-conductivity conducting performance improves a lot than traditional pure Mo; And can be through changing Cu, Mo, Cu thickness ratio; With some crucial electronic materials, be complementary like silicon, GaAs, aluminium oxide, beryllium oxide, aluminium nitride, enjoy the favor of electronic industry.

Particularly in today of electronic technology high speed development; The application density of semiconductor integrated circuit is increasing, and electronic technology develops towards the direction of high density, high-power, miniaturization and high-performance, high reliability, and the CMC laminar composite is at HB-LED; Many substrates group substrate material; Heat sink heat radiation, fields such as radar Aero-Space have a wide range of applications.

The method of making the CMC laminar composite at present mainly contains blast composite algorithm and roll-bonding method.But explode compound dangerous height, big to surrounding environment influence, the coarse bad mechanical property of quality of item needs following process to handle.The CMC stratified material interface quality that roll-bonding method obtains is better, but because the physical and mechanical properties of Cu and Mo differs greatly, molybdenum plate can produce cracking and layering; And, being difficult to obtain desirable thickness proportion because the roll-force of molybdenum and copper is different, this has also influenced product quality.

In order to address the above problem, the present invention adopts the high temperature solid-state complex method to prepare CMC (copper molybdenum copper) laminar composite, utilizes year piece pressure copper that high temperature is softening down to be pressed in the gully on molybdenum surface; The activation energy that continuous high temperature provides, the weak chemical bond that causes molybdenum copper surface atom to be torn originally overcomes potential barrier, produces electron interaction between atom, forms firm metallic bond, obtains good compound interface.

Summary of the invention

The object of the present invention is to provide a kind of Electronic Packaging that is applicable to, the composite of heat sink heat dissipation element.

The present invention is the preparation method of a kind of CMC (copper molybdenum copper) laminar composite, it is characterized in that having following preparation process and step:

A. the molybdenum board material that powder metallurgy is made is rolling to the thickness that needs, and carries out The high temperature anneal, and annealing temperature is 800 ~ 900 ℃, removes the internal stress in the sheet material;

B. will reach the thickness ratio of CMC according to designing institute, red copper sheet material is rolling to needed thickness, carry out The high temperature anneal, annealing temperature is 800 ~ 950 ℃ of internal stress of removing in the sheet material;

C. be cut into onesize according to the size of needs two copper coins and molybdenum plate;

D. with fine sandpaper polishing copper coin surface, remove the oxide layer on surface;

E. gained sheet material is put into industrial degrease liquid, soaked 5 minutes, taking-up is cleaned, and cleans oven dry once more with ethanol;

F. with molybdenum plate and alternately stack of copper coin, load briquetting, on-load pressure is 20 ~ 100Kpa;

G. range upon range of sheet material is pushed in the hydrogen furnace and heat, heating rate is about 5 ℃/s, and holding temperature is 850 ~ 1050 ℃, and temperature retention time is 60 ~ 100 minutes;

H. product cools off with stove, and product remains in the nitrogen atmosphere always in the cooling procedure, takes out after being cooled to be lower than 100 ℃.

The present invention is compound good to utilizing the high temperature composite algorithm to prepare CMC laminar composite interface; Its outstanding feature is:

product in hydrogen furnace, produce; Compound interface non-oxidation or other nuisance generate, and interface binding power is higher;

single sheet material rolling with respect to laminar composite; Process is controlled easily, and yield rate is high;

but the thickness of the thickness of laminar composite and refractory metal and copper coin material than regulated at will, can satisfy the demand of different field and different product.

Description of drawings

Fig. 1 embodiment of the invention 1 makes the micro-metallograph of example interface;

Fig. 2 embodiment of the invention 2 makes the micro-metallograph of example interface;

Fig. 3 embodiment of the invention 2 makes sample copper coin and the compound back of molybdenum plate survey map;

Fig. 4 inventive embodiments 1 makes sample molybdenum copper interface energy spectrum composition analysis line sweep figure;

Fig. 5 inventive embodiments 2 makes sample molybdenum copper interface energy spectrum composition analysis line sweep figure.

The specific embodiment

Below in conjunction with embodiment the present invention is elaborated:

Embodiment 1

A. the molybdenum board material that powder metallurgy is made is rolling to 0.5mm, carries out The high temperature anneal, and annealing temperature is 850 ℃, removes the internal stress in the sheet material;

B. red copper sheet material is rolling to 0.8mm, carries out The high temperature anneal, annealing temperature is 800 ℃, removes the internal stress in the sheet material;

C. adopt line cutting technology molybdenum board material and copper coin material to be cut into the square of 30 * 26mm;

D. use sand papering copper surface No. 5, remove the oxide layer on surface;

E. gained sheet material is put into the liquid that deoils, soaked 5 minutes, taking-up is cleaned, and cleans oven dry once more with ethanol;

F. with molybdenum plate and alternately stack of copper coin, load briquetting, on-load pressure is 20Kpa;

G. range upon range of sheet material is pushed in the hydrogen furnace and heat, heating rate is about 5 ℃/s, and holding temperature is at 1050 ℃, and temperature retention time was at 60 minutes;

H. product cools off with stove, and product remains in the nitrogen atmosphere always in the cooling procedure, takes out after being cooled to be lower than 100 ℃.

Embodiment 2

A. the molybdenum board material that powder metallurgy is made is rolling to 0.1mm, carries out The high temperature anneal, and annealing temperature is 950 ℃, removes the internal stress in the sheet material;

B. red copper sheet material is rolling to 0.91mm, carries out The high temperature anneal, annealing temperature is 850 ℃, removes the internal stress in the sheet material;

C. adopt line cutting technology molybdenum board material and copper coin material to be cut into the square of 40 * 30mm;

D. use sand papering copper surface No. 5, remove the oxide layer on surface;

E. gained sheet material is put into the liquid that deoils, soaked 5 minutes, taking-up is cleaned, and cleans oven dry once more with ethanol;

F. with molybdenum plate and alternately stack of copper coin, load briquetting, on-load pressure is 100Kpa;

G. range upon range of sheet material is pushed in the hydrogen furnace and heat, heating rate is about 5 ℃/s, and holding temperature is at 850 ℃, and temperature retention time was at 100 minutes;

H. product cools off with stove, and product remains in the nitrogen atmosphere always in the cooling procedure, takes out after being cooled to be lower than 100 ℃.

Product cools off with stove, and product remains in the nitrogen atmosphere always in the cooling procedure, takes out after being cooled to be lower than 100 ℃.

The CMC laminar composite that utilizes method of the present invention to obtain, the interface between the out-phase metal combine good (like accompanying drawing 1 and accompanying drawing 2).

Measurement through the digital metallographic microscope of KEYENCE VHX-100K; The thickness that can find out compound front and back molybdenum plate and copper coin does not almost change, and the CMC laminar composite of producing through the present invention can well guarantee molybdenum plate and copper plate thickness ratio and intrinsic consistent (like accompanying drawing 3 and subordinate list 1).

Table oneMeasured value after molybdenum plate and copper coin are compound

Unit (μ m)	1	2	3	4	Mean value
						Cu1	917.01	917.1	914.84	910.61	914.89
Cu2	914.84	912.81	914.9	912.75	913.825
						Mo	101.44	101.41	97.96	98.96	99.9425

Through adopting the X-ray energy spectrometer in the JSM-6700F awkward silence at a meeting emission scan Electronic Speculum that molybdenum copper linkage interface place is carried out line sweep, find not produce between the interface the bad intermediate diffusion layer of performance (like accompanying drawing 4 and accompanying drawing 5).

Claims (1)

1. the preparation method of a copper molybdenum copper laminar composite is characterized in that this method has following preparation process:

A. the molybdenum board material that powder metallurgy is made is rolling to the thickness that needs, and carries out The high temperature anneal, and annealing temperature is 800 ~ 950 ℃, removes the internal stress in the sheet material;

B. will reach the thickness ratio of copper molybdenum copper according to designing institute, red copper sheet material is rolling to needed thickness, carry out The high temperature anneal, annealing temperature is 800 ~ 900 ℃, removes the internal stress in the sheet material;

C. be cut into onesize according to the size of needs two copper coins and molybdenum plate;

D. with fine sandpaper polishing copper coin surface, remove the oxide layer on surface;

E. gained sheet material is put into industrial degrease liquid, soaked 5 minutes, taking-up is cleaned, and cleans oven dry once more with ethanol;

F. with molybdenum plate and alternately stack of copper coin, load briquetting, on-load pressure is 20 ~ 100Kpa;

G. range upon range of sheet material is pushed in the hydrogen furnace and heat, heating rate is about 5 ℃/s, and holding temperature is 850 ~ 1050 ℃, and temperature retention time is 60 ~ 100 minutes;

H. product cools off with stove, and product remains in the nitrogen atmosphere always in the cooling procedure, takes out after being cooled to be lower than 100 ℃.

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