CN110462074A - Copper sheet material and its manufacturing method for the insulating substrate with copper sheet - Google Patents
Copper sheet material and its manufacturing method for the insulating substrate with copper sheet Download PDFInfo
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- CN110462074A CN110462074A CN201880022820.7A CN201880022820A CN110462074A CN 110462074 A CN110462074 A CN 110462074A CN 201880022820 A CN201880022820 A CN 201880022820A CN 110462074 A CN110462074 A CN 110462074A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/02—Alloys based on copper with tin as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/08—Alloys based on copper with lead as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
- C04B2237/40—Metallic
- C04B2237/407—Copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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Abstract
Copper sheet material for the insulating substrate with copper sheet of the invention has following composition: being selected from Al, Be, Cd, Mg, Pb, Ni, P, total content of metal component in Sn and Cr is 0.1~2.0ppm, the content of copper is 99.96 mass % or more, and with following rolling texture: the crystalline orientation distribution function Eulerian angles (φ 1 that will be parsed by the texture using EBSD, Φ, φ 2) indicate when, in φ 2=0 °, φ 1=0 °, the average value of orientation density in the range of Φ=0 °~90 ° is 3.0 more than or lower than 35.0, and in φ 2=35 °, 1=45 °~55 ° φ, the maximum value of orientation density in the range of Φ=65 °~80 ° is 1.0 more than or lower than 30.0.
Description
Technical field
The present invention relates to the copper sheet material for the insulating substrate with copper sheet, in particular to suitable for power device with copper sheet
The copper sheet material and its manufacturing method of insulating substrate.
Background technique
In general, power device generates a large amount of hot, associated with it material due to using high voltage, high current
Deterioration becomes project.Therefore, in recent years, by using the excellent ceramic substrate of insulating properties and thermal diffusivity is engaged with copper sheet and
At the insulating substrate with copper sheet, come cope with insulation, heat dissipation.
In the joint method of ceramic substrate and copper sheet, mainly used via silver be the engagements such as solder joint method,
Or the joint method for utilizing the eutectic reaction of copper to engage not via solder, it is required to 700 DEG C or more of high-temperature heat treatment.
In addition, aluminium nitride, aluminium oxide, silicon nitride etc. have been used in ceramic substrate, their thermal expansion coefficient and the copper for constituting copper sheet
Thermal expansion coefficient it is different.Therefore, when at high temperature engaging ceramic substrate with copper sheet, due to the difference of thermal expansion coefficient, exist
The tendency of big deformation is generated in insulating substrate entirety.In addition, copper sheet material has high for ceramic substrate and copper sheet material
Coefficient of thermal expansion then applies tensile stress to ceramic substrate so if being heat-treated, and applies compression stress to copper sheet material.By
This, not only insulating substrate overall deformation, generates change in size, and be easy to happen the removing etc. of ceramic substrate Yu copper sheet material.Into
And the copper of the high-purity for copper sheet material crystal grain at a high temperature of 700 DEG C or more is grown significantly, homogenizing for tissue becomes tired
It is difficult.Accordingly, there exist associativities to reduce, starting point such problems as intercrystalline failure when deforming.
For example, in patent document 1, as the fine copper plate for heat-radiating substrate, disclose by 99.90 mass % of purity with
On fine copper constitute and define X-ray diffraction intensity ratio fine copper plate.In addition, in patent document 2, as being suitable for
The copper alloy plate of heat transmission electronic component and high current electronic component etc., it is 350MPa or more and right for disclosing tensile strength
The copper alloy plate that the accumulation degree of the crystalline orientation of specified position is controlled.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 2014-189817 bulletin
Patent document 2: No. 5475914 bulletins of Japanese Patent No.
Summary of the invention
Subject to be solved by the invention
But fine copper plate disclosed in Patent Document 1 generates bumps by being etched in surface due to being difficult to, therefore, it is considered that with
The excellent adhesion of other components still about the engagement with other components at high temperature, is absolutely not studied.In addition,
It for copper alloy plate disclosed in Patent Document 2, about heat resistance, is studied, but only considered and utilize 200 DEG C, 30
The heat resistance of the heat treatment of minute.In addition, for copper alloy plate disclosed in Patent Document 2, tensile strength be 350MPa with
On, not yet to the range that should be used as the 150~330MPa suitable for the copper sheet material of the insulating substrate with copper sheet.
Therefore, the purpose of the present invention is to provide continuous lower, anti-from rolling direction to plate width direction longitudinal modulus of elasticity
Tensile strength and conductivity it is excellent and be heat-treated at high temperature (such as 700 DEG C or more and 800 DEG C or less carry out 10 points
It is more than clock and heat treatment below in 5 hours) when inhibit grain growth the copper sheet material and its system for the insulating substrate with copper sheet
Make method.
Means for solving the problems
Present inventor have discovered that by the longitudinal modulus of elasticity of control copper sheet material, and inhibit at a high temperature of 700 DEG C or more
Grain growth, thus in the engagement of copper sheet material and ceramic substrate reduce due to the thermal expansion coefficient of copper sheet material and ceramic substrate it
The bearing strength test of the entirety of substrate caused by difference, in addition, being able to suppress the heterogeneity and knot organized caused by the growth of crystal grain
The reduction of conjunction property.
That is, of the invention mainly consisting of is described.
(1) a kind of copper sheet material for the insulating substrate with copper sheet, which is characterized in that there is following composition: selected from Al, Be, Cd,
Total content of metal component in Mg, Pb, Ni, P, Sn and Cr is 0.1~2.0ppm, the content of copper be 99.96 mass % with
On, and with following rolling texture: the crystalline orientation distribution function parsed by the texture using EBSD is used into Euler
Angle (φ 1, Φ, φ 2) indicate when, φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value
For 3.0 more than or lower than 35.0, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation it is close
The maximum value of degree is 1.0 more than or lower than 30.0.
(2) described in (1) be used for the insulating substrate with copper sheet copper sheet material, wherein the content of the copper be 99.99 mass % with
On, and the average value of longitudinal modulus of elasticity be 115GPa hereinafter, the longitudinal modulus of elasticity rolling direction, plate width direction and
It is measured on direction between them.
(3) the copper sheet material of the insulating substrate with copper sheet is used for described in (1) or (2), wherein average crystallite particle diameter to be 3 μm~100
μm。
(4) the copper sheet material of the insulating substrate with copper sheet is used for described in any one of (1)~(3), wherein be subjected in 700~
At 800 DEG C after 10 minutes~5 hours thermal process in the state of, average crystallite particle diameter be 50 μm~200 μm.
(5) the copper sheet material of the insulating substrate with copper sheet is used for described in any one of (1)~(4), wherein tensile strength 150
~330MPa, and conductivity is 95%IACS or more.
(6) a kind of manufacturing method of the copper sheet material for the insulating substrate with copper sheet is use described in any one of (1)~(5)
In the manufacturing method of the copper sheet material of the insulating substrate with copper sheet, it includes:
For ingot bar obtained from the casting of the copper raw material with the composition homogenize the heat treatment that homogenizes of heat treatment
Process；
The hot-rolled process of hot rolling is carried out after this homogenizes heat treatment procedure；
Cooling cooling process is carried out after the hot-rolled process；
The face cutting process of face cutting is carried out to the two sides of the material to be rolled after the cooling process；
The first cold rolling process of the cold rolling that general working rate is 75% or more is carried out after the face cutting process；
It is 1~100 DEG C/sec, reaches that temperature is 100~500 DEG C, the retention time is in heating rate after first cold rolling process
1~900 second and cooling velocity implement the first annealing operation of heat treatment under conditions of being 1~50 DEG C/sec；
The second cold rolling process of the cold rolling that general working rate is 60~95% is carried out after first annealing operation；
Heating rate is 10~100 DEG C/sec, to reach temperature be 200~550 DEG C, retention time after second cold rolling process
For 10~3600 seconds and cooling velocity be 10~100 DEG C/sec under conditions of implement heat treatment the second annealing operation；
The finishing rolling step further rolled after second annealing operation；
Implement the final annealing process of final heat treatment after the finishing rolling step；
The surface film oxide removal step of pickling and grinding is carried out after the final annealing process.
The effect of invention
In accordance with the invention it is possible to a kind of copper sheet material and its manufacturing method for the insulating substrate with copper sheet is provided, it is described
Continuous lower, tensile strength and conductivity are excellent and in high temperature from rolling direction to plate width direction longitudinal modulus of elasticity for copper sheet material
Under press down when being heat-treated (such as carrying out 10 minutes or more and heat treatment below in 5 hours at 700 DEG C or more and 800 DEG C or less)
Grain growth processed.
Detailed description of the invention
Fig. 1 is the figure for indicating the result parsed using EBSD to the rolling texture of copper sheet material of the invention, and (A) is φ
2=0 ° of sectional view, (B) are the sectional view of φ 2=35 °.
Specific embodiment
The preferred embodiment of copper sheet material of the invention described further below.It should be noted that the numerical value for using "~" to indicate
Range Representation includes range of the numerical value documented by the front and back of "~" as lower limit value and upper limit value.
Copper sheet material of the invention has following composition: the metal component in Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr
Total content be 0.1~2.0ppm, the content of copper is 99.96 mass % or more, and there is following rolling texture: will be by
When the crystalline orientation distribution function Eulerian angles (φ 1, Φ, φ 2) parsed using the texture of EBSD are indicated, φ 2=0 °,
φ 1=0 °, Φ=0 °~90 ° range in the average value of orientation density be 3.0 more than or lower than 35.0, and in φ 2=
35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in the maximum value of orientation density be 1.0 more than or lower than 30.0.
So-called copper product, expression (will have before processing defined composition), and copper raw material is processed as defined shape (example
Such as plate, item, foil, stick, line).Wherein, so-called " plate " refers to specific thickness, stable in shape and in face direction
The material of upper extension broadly includes web.In the present invention, the thickness of copper sheet material is not particularly limited, preferably 0.05~
7.0mm, more preferably 0.1~6.0mm.
[at being grouped as]
The content of copper is 99.96 mass % or more, preferably 99.99 mass % or more.If the content of copper is lower than 99.96 matter
% is measured, then thermal conductivity reduces, and cannot get desired thermal diffusivity.In addition, in Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr
Metal component total content be 0.1~2.0ppm, preferably 0.1~1.0ppm.To total content of these metal components
Lower limit value be not particularly limited, consider inevitable impurity, be 0.1ppm.On the other hand, if these metal components
Total content is more than 2.0ppm, then cannot get desired orientation density.In addition, in copper sheet material, in addition to copper and selected from Al,
Other than metal component in Be, Cd, Mg, Pb, Ni, P, Sn and Cr, as remainder, inevitable impurity can be contained.No
What evitable impurity indicated inevitably to contain in manufacturing process contains horizontal impurity.
GDMS method is able to use in the quantitative analysis of the above-mentioned metal component other than copper.So-called GDMS method, is Glow
The abbreviation of Discharge Mass Spectrometry (glow discharge spectrometry), specifically by using solid sample as
Cathode sputters specimen surface using glow discharge, touches the neutral particle released with the intracorporal Ar of plasma, electronics
It hits, to make its ionization, by measuring number of ions with mass analyzer, to parse atomic secondary element contained in metal
The technology of ratio.
[rolling texture]
Copper sheet material of the invention has rolling texture, which is indicated using Eulerian angles (φ 1, Φ, φ 2) by using
Crystalline orientation distribution function (the ODF:crystal orientation distribution that the texture of EBSD parses
When function), φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value be 3.0 or more and
Lower than 35.0, preferably 15 hereinafter, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation it is close
The maximum value of degree is 1.0 more than or lower than 30.0, preferably 10 or more.Rolling direction is set as the direction RD, by plate width direction (with
The orthogonal direction in the direction RD) it is set as the direction TD, it, will be with the direction RD when the direction vertical with rolling surface (face RD) is set as the direction ND
It is expressed as Φ for the orientation rotation of axis, φ 1 will be expressed as by the rotation of the orientation of axis of the direction ND, it will be using the direction TD as the orientation of axis
Rotation is expressed as φ 2.Orientation density be quantitatively parse texture in crystalline orientation there are uses when ratio and dispersity
Parameter, carry out EBSD and X-ray diffraction, the determination data of the positive pole figure based on 3 kinds or more of (100), (110), (112) etc.,
It is calculated by using the crystalline orientation distribution analytic method of Series Expansion Method.It is being parsed by the texture using EBSD, by φ 2
It is fixed in the sectional view of predetermined angular, the distribution of the orientation density in the face RD is shown.
Fig. 1 (A) and (B) are the result for indicating to parse the rolling texture of copper sheet material of the invention using EBSD
Figure.Fig. 1 (A) is the sectional view of φ 2=0 °, and Fig. 1 (B) is the sectional view of φ 2=35 °.Crystalline orientation is distributed to random state
Being set as orientation density is 1, will be indicated as several times gather with contour relative to it.In Fig. 1 (A) and (B), white portion
Indicate that orientation density is high, black portions indicate that orientation density is low, and the part of grey indicates that, closer to white, orientation density is higher.
In the present invention, by φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value
For 3.0 more than or lower than 35.0, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation it is close
The maximum value of degree is 1.0 more than or lower than 30.0, to inhibit the growth of crystal grain for 700 DEG C or more of high temperature.If
The average value of orientation density in the range of Φ=0 ° is lower than 3.0, then at a high temperature of 700 DEG C or more, crystal grain is grown significantly
To 300 μm of partial size or more, the load becomes large when causing associativity to reduce, thermally expanding.On the other hand, if in the range of Φ=0 °
The average value of orientation density is 35.0 or more, then the strength reduction of plate, as the copper sheet material for the insulating substrate with copper sheet
In the case where use, becomes easy and be deformed.In addition, if φ 2=35 °, φ 1=45 °~55 °, Φ=65 °~80 °
The maximum value of orientation density in range is 30.0 or more, then the strength reduction of plate, as the insulation base with copper sheet
In the case where the copper sheet material use of plate, becomes easy and be deformed.It should be noted that φ 2=0 °, φ 1=0 °, Φ=0 °~90 °
Range in orientation density it is high on the whole, but φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in take
It is locally high to density.Therefore, for the former, it is specified that average value, for the latter, it is specified that maximum value.
So-called EBSD method is the abbreviation of Electron BackScatter Diffraction (electron backscatter diffraction),
Specifically the crystallization of the reflective electron generated when using in scanning electron microscope (SEM) to sample irradiating electron beam takes
To analytic technique.When being parsed using EBSD, measuring area and scanning step can determine according to the grain size of sample.To survey
When crystal grain after fixed is parsed, such as it is able to use the analysis software OIM Analysis (trade name) of TSL company manufacture.In
Information obtained in parsing using the crystal grain of EBSD includes electron beam intrusion sample until the information of the depth of tens nm.Plate
The measurement site in thick direction is preferably set to from specimen surface to 1/8 times~1/2 times of plate thickness of position.
[longitudinal modulus of elasticity]
The average value of longitudinal modulus of elasticity is preferably 115GPa hereinafter, more preferably 110GPa or less.In addition, longitudinal modulus of elasticity
The lower limit value of average value be preferably 80GPa or more.Longitudinal elasticity is measured on the direction RD, the direction TD and direction between them
Modulus.Specifically, obtain the average value of longitudinal modulus of elasticity in the following way: calculating rotates every time from the direction RD to the direction TD
After defined angle (such as 10 °), longitudinal modulus of elasticity in all directions, their average value is calculated.If upper
The average value for stating the longitudinal modulus of elasticity of range measurement is more than 115Gpa, what is be heat-treated to engage with insulating substrate
In the case of, there is the raised tendency of bearing strength test that thermal expansion generates.
[average crystallite particle diameter]
In copper sheet material of the invention, average crystallite particle diameter is preferably 3 μm~100 μm, more preferably 10 μm~90 μm or less.If
Average crystallite particle diameter is lower than 3 μm, not can be carried out sufficient crystalline orientation control sometimes.On the other hand, if average crystallite particle diameter
More than 100 μm, then there is the tendency of tensile strength reduction.In addition, the shape after being heated 10 minutes~5 hours at 700~800 DEG C
Under state, average crystallite particle diameter is preferably 50 μm~200 μm, more preferably 120 μm or more.If being averaged in the state of after heated
Crystallization particle diameter is more than 200 μm, then the load becomes large when the reduction, thermal expansion of associativity.It should be noted that crystallization particle diameter can pass through
EBSD in the face RD of copper sheet material parses measurement.For the crystallization particle diameter in the state of after heated, also can to copper sheet material into
It is measured after row heat treatment using same method.
[characteristic]
In copper sheet material of the invention, tensile strength is preferably 150~330MPa, preferably 190MPa or more.If tensile strength
Lower than 150MPa, then intensity is insufficient, if tensile strength is more than 330MPa, there are the tendencies that elongation, processability reduce.
In addition, conductivity is preferably 95%IACS or more.If conductivity is lower than 95%, thermal conductivity is reduced, and result has heat dissipation
Property deterioration tendency.
Copper sheet material of the invention can engage with well known ceramic substrate and laminated body is made.To copper sheet material and ceramic substrate
Joint method be not particularly limited, in general, copper sheet material is engaged at a high temperature of 700 DEG C or more with ceramic substrate.With regard to this hair
For bright copper sheet material, due to being heat-treated (such as 700 DEG C or more and 800 DEG C or less, 10 minutes or more and 5 at high temperature
Heat treatment hour below) when crystal grain growth inhibited, therefore, engaged with ceramic substrate and the case where laminated body is made
Under, removing etc. is not susceptible in the bonding part with ceramic substrate.Therefore, copper sheet material of the invention is as with the exhausted of copper sheet
The copper sheet material of edge substrate is excellent.
[manufacturing method of copper sheet material]
Next, being illustrated to an example of the manufacturing method of copper sheet material of the invention.
In the manufacturing method of copper sheet material of the present invention, at melting, casting process [process 1], the heat that homogenizes
Science and engineering sequence [process 2], hot-rolled process [process 3], cooling process [process 4], face cutting process [process 5], the first cold rolling process
[process 6], the first annealing operation [process 7], the second cold rolling process [process 8], the second annealing operation [process 9], finishing rolling step
[process 10], final annealing process [process 11], surface film oxide removal step [process 12], successively carry out by these process structures
At processing.In the present invention, particularly, by suitably controlling the first cold rolling process [process 6] and the first annealing operation [work
Sequence 7] and the second annealing operation [process 9] condition, to obtain longitudinal modulus of elasticity from the direction RD of copper sheet material to the direction TD
The continuously excellent copper sheet material of reduction, in turn tensile strength and conductivity.
Firstly, melting, in casting process [process 1], by that will have the copper raw material of above-mentioned composition to melt, cast, from
And obtain ingot bar.That is, copper raw material has total content of the metal component in Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr
Content for 0.1~2.0ppm, copper is the composition of 99.96 mass % or more.It is right in the heat treatment procedure that homogenizes [process 2]
In obtained ingot bar, carry out keeping 700~1000 DEG C of temperature, the heat treatment that homogenizes of 10 minutes~20 hours retention time.In
In hot-rolled process [process 3], hot rolling is carried out in such a way that general working rate becomes 10~90%.In cooling process [process 4], with
10 DEG C/sec or more of cooling velocity carries out cooling (chilling).In face cutting process [process 5], material after cooling (is rolled
Prepared material) two sides difference face cut about 1.0mm.The oxidation film of plate surface is removed as a result,.
In the first cold rolling process [process 6], the cold rolling that general working rate is 75% or more is carried out, is preferably carried out multiple.In
In first cold rolling process [process 6], if general working rate is lower than 75%, it cannot get desired rolling texture.
In the first annealing operation [process 7], heating rate be 1~100 DEG C/sec, reach temperature and be 100~500 DEG C,
Retention time be 1~900 second and cooling velocity be 1~50 DEG C/sec under conditions of implement heat treatment.If in above-mentioned condition
Except, then it cannot get desired rolling texture.
In the second cold rolling process [process 8], the cold rolling that general working rate is 60~95% is carried out.
In the second annealing operation [process 9], heating rate is 10~100 DEG C/sec, to reach temperature be 200~550
DEG C, the retention time be 10~3600 seconds and cooling velocity be 10~100 DEG C/sec under conditions of implement heat treatment.If upper
It states other than condition, then cannot get desired rolling texture.
In finishing rolling step [process 10], the cold rolling that general working rate is 10~60% is carried out.In final annealing process [process
11] in, implement heat treatment under conditions of reaching temperature and being 125~400 DEG C.In surface film oxide removal step [process 12]
In, in order to remove and clean the oxidation film of plate surface, carry out pickling and grinding.It should be noted that in the rolling process
Working modulus R (%) is defined by the formula.
R=(t0-t)/t0 × 100
In formula, t0 is the plate thickness before rolling, and t is the plate thickness after rolling.
Embodiment
The present invention is explained in detail below based on embodiment, but the present invention is not limited to these.
(embodiment 1~13 and comparative example 1~17)
Firstly, by with being melted shown in table 1 at the copper raw material that is grouped as, and cast, to obtain ingot bar [process
1].For obtained ingot bar, keep 700~1000 DEG C of temperature, at the heat that homogenizes of 10 minutes~20 hours retention time
It manages [process 2].Then, after carrying out hot rolling [process 3] in such a way that general working rate becomes 10~90%, with 10 DEG C/sec or more
Cooling velocity carries out chilling [process 4].By the two sides difference face cutting about 1.0mm [process 5] of material after cooling.Next,
After carrying out the first cold treatment [process 6] with general working rate shown in table 2, and with heating rate shown in table 2, arrival temperature
Degree, retention time and cooling velocity carry out the first annealing [process 7].Next, carrying out second with general working rate shown in table 2
Cold rolling [process 8].With heating rate shown in table 2, reach temperature, retention time and cooling velocity progress the second annealing [work
Sequence 9] after, finish rolling [process 10] is carried out with general working rate shown in table 2.Reach temperature be 125~400 DEG C under conditions of into
After row final annealing [process 11], pickling and grinding [process 12] are carried out, is made copper sheet material (test material).
(measuring method and evaluation method)
The quantitative analysis > of < metal component
For each test material of production, parsed using VG 9000 (VG Scientific Ltd. manufacture).By each test
The content (ppm) of Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr contained in material, Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr
Total content (ppm) of (" metal component " is abbreviated as in table 1) and the content (quality %) of Cu are shown in Table 1.It should be noted that
Sometimes with inevitable impurity in each test material.In addition, the metal component is not detected in the "-" expression in table 1.
< orientation density >
Orientation density is measured using OIM5.0HIKARI (manufacture of TSL company), using EBSD method.Measurement area is set as comprising 200
A above crystal grain, 1600 μm of 800 μ m range, is set as 0.1 μm for scanning step.Make in the parsing of crystal grain after measurement
The analysis software OIM Analysis (trade name) manufactured with TSL company.By parsing obtained crystalline orientation distribution function
It is indicated with Eulerian angles.The range (" range A " is denoted as in table 3) of φ 1=0 °, Φ=0 °~90 ° are calculated by the sectional view of φ 2=0 °
In orientation density average value.In addition, in the sectional view of the φ 2=35 ° indicated with Eulerian angles, reading φ 1=45 °~
55 °, the maximum value of orientation density in the ranges (being denoted as " range B " in table 3) of Φ=65 °~80 °.For each test material,
The maximum value of orientation density in the average value of orientation density in range A and range B is shown in Table 3.
< average crystallite particle diameter >
Average crystallite particle diameter is measured using method same as orientation density.Whole crystal grain as contained in measurement range calculates
Average crystallite particle diameter.The average crystallite particle diameter of each test material is shown in Table 3.
< longitudinal modulus of elasticity >
By each test material, the direction RD, the direction TD, from the direction RD to the direction TD every on 10 ° of postrotational directions, take respectively
Obtain the strip test film of wide 20mm, long 200mm.Firstly, being answered on the length direction of test film using cupping machine imparting
Power.Moreover, using 80% deflection of deflection when surrendering as maximum displacement, and providing will be until the maximum displacement
The displacement of 10 equal parts.The proportionality constant that deformation with stress are calculated at this 10 points, using the average value of each proportionality constant as longitudinal bullet
The average value of property modulus.It is that 115GPa situation below is evaluated as " good " by the average value of longitudinal modulus of elasticity, will will be more than
The situation of 115GPa is evaluated as " bad ".For each test material, the average value of longitudinal modulus of elasticity is shown in Table 3.
< conductivity >
Conductivity is calculated by the numerical value of resistivity, the resistivity in the thermostat for being held in 20 DEG C (± 0.5 DEG C) by adopting
It is measured with four-terminal method.It should be noted that distance is set as 100mm between terminal.In the case where conductivity is 95%IACS or more
It is evaluated as " good ", is evaluated as " bad " in the case where being lower than 95%IACS.The conductivity of each test material is shown in table 3
In.
< tensile strength >
The test film of 3 JIS Z2201-13B is cut out by the direction RD of each test material.According to JIS Z2241, each examination is measured
The tensile strength for testing piece calculates its average value.It is " good that tensile strength is that 150MPa or more and 330MPa situation below are evaluated as
It is good ", tensile strength is lower than the situation of 150MPa or is evaluated as " bad " more than the situation of 330MPa.By the anti-of each test material
Tensile strength is shown in Table 3.
< heat resistance >
For each test material, after implementing heat treatment in 5 hours at 800 DEG C with the tube furnace under argon atmospher or nitrogen atmosphere, adopt
Average crystallite particle diameter is measured with method same as the measuring method of above-mentioned average crystallite particle diameter.Average crystallite after heat treatment
Partial size be in 200 μm of situations below by Evaluation of Heat Tolerance be " good ", be by Evaluation of Heat Tolerance more than 200 μm
" bad ".For each test material, the average crystallite particle diameter after heat treatment is shown in Table 3.In general, more for a long time
Ground is heat-treated, and crystallization particle diameter is more grown.That is, being for average crystallite particle diameter after carrying out heat treatment in 5 hours at 800 DEG C
200 μm of test materials below, carry out 10 minutes or more at 700~800 DEG C and in the case where heat treatment within 5 hours,
Obvious average crystallite particle diameter is 200 μm or less.
[table 1]
[table 2]
[table 3]
As shown in table 1 and table 3, in embodiment 1~13, have selected from Al, Be, Cd, Mg, Pb, Ni, P, Sn and
The composition that total content of metal component in Cr is 0.1~2.0ppm, the content of copper is 99.96 mass % or more.In addition, In
In embodiment 1~13, the crystalline orientation distribution function Eulerian angles (φ 1, Φ, φ that will be parsed by the texture using EBSD
2) when indicating, with following rolling texture: φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density it is flat
Mean value be 3.0 more than or lower than 35.0, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation
The maximum value of density is 1.0 more than or lower than 30.0.Therefore, the average value of the longitudinal modulus of elasticity on from the direction RD to the direction TD
Down to 115GPa hereinafter, tensile strength is 150~330MPa, and conductivity is up to 95%IACS or more.In addition, at 800 DEG C
It is lower to carry out the average crystallite particle diameter after being heat-treated 5 hours as 200 μm hereinafter, therefore, it is known that the growth of crystal grain is inhibited.
And in Comparative Examples 1 and 2,4,6,8, the conjunction of the metal component in Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr
Meter content has been more than 2.0ppm, and φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value
Lower than 3.0.Therefore, the average value of the longitudinal modulus of elasticity from the direction RD to the direction TD is respectively more than 115GPa.In addition, 800
Therefore average crystallite particle diameter after carrying out heat treatment in 5 hours at DEG C, confirmed the growth of crystal grain respectively more than 200 μm respectively.
In comparative example 3,7, total content point of the metal component in Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr
Not up to 150.0ppm, 130.0ppm, φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density be averaged
Value be respectively 2.3,0.1, it is lower, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation it is close
The maximum value of degree is up to 31.0,37.0 respectively.Therefore, the average value difference of the longitudinal modulus of elasticity on from the direction RD to the direction TD
Up to 135GPa, 150GPa.In addition, carried out at 800 DEG C 5 hours heat treatment after average crystallite particle diameter difference it is larger, be 368
μm, 399 μm, it is thus identified that the growth of crystal grain.
In comparative example 5, total content of the metal component in Al, Be, Cd, Mg, Pb, Ni, P, Sn and Cr is up to
2=0 ° of 250.0ppm, φ, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value it is lower, be 0.8, and
φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation density maximum value it is higher, be 35.0.Cause
This, the average crystallite particle diameter after heat treatment in 5 hours is carried out at 800 DEG C is larger, is 456 μm, it is thus identified that the growth of crystal grain.
In comparative example 9, the content of copper is 99.00 mass %, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °
The maximum value of orientation density in~80 ° of range is up to 31.0.Therefore, conductivity is down to 93.4%IACS.In addition, 800
Average crystallite particle diameter after carrying out heat treatment in 5 hours at DEG C is larger, is 400 μm, it is thus identified that the growth of crystal grain.
In the comparative example 10,12,14,17, φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density
Average value difference is lower, is 1.9,2.5,2.9,2.9.Therefore, the average value of the longitudinal modulus of elasticity from the direction RD to the direction TD
It is higher respectively, it is 129GPa, 143GPa, 153GPa, 128GPa.In addition, carrying out being averaged after heat treatment in 5 hours at 800 DEG C
Crystallization particle diameter difference is larger, is 402 μm, 420 μm, 400 μm, 399 μm, confirmed the growth of crystal grain respectively.
In comparative example 11, φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value it is high
Up to 42.5.Therefore, tensile strength is lower, is 145MPa.In addition, carrying out the average crystallite grain after heat treatment in 5 hours at 800 DEG C
Diameter is larger, is 275 μm, it is thus identified that the growth of crystal grain.
In comparative example 13, φ 2=35 °, φ 1=45 °~55 °, Φ=65 °~80 ° range in orientation density
Maximum value is up to 39.0.Therefore, the average value of the longitudinal modulus of elasticity on from the direction RD to the direction TD is up to 165GPa, and tension is strong
Degree is also up to 385MPa.In addition, the average crystallite particle diameter carried out after heat treatment in 5 hours at 800 DEG C is larger, and it is 435 μm, confirmation
The growth of crystal grain.
In comparative example 15, φ 2=35 °, φ 1=45 °~55 °, Φ=65 °~80 ° range in orientation density
Maximum value is up to 31.0.Therefore, the average value of the longitudinal modulus of elasticity on from the direction RD to the direction TD is up to 129GPa.In addition,
Average crystallite particle diameter after carrying out heat treatment in 5 hours at 800 DEG C is larger, is 380 μm, it is thus identified that the growth of crystal grain.
In comparative example 16, φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation density average value compared with
It is low, be 2.7, and φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 ° range in orientation density maximum value it is high
Up to 32.0.Therefore, the average value of the longitudinal modulus of elasticity on from the direction RD to the direction TD is up to 130GPa.In addition, at 800 DEG C
Average crystallite particle diameter after carrying out heat treatment in 5 hours is larger, is 432 μm, it is thus identified that the growth of crystal grain.
As known from the above, from rolling direction to plate width direction, longitudinal modulus of elasticity is continuously reduced copper sheet material of the invention,
In turn, tensile strength and conductivity are excellent.In addition, when copper sheet material of the invention due to being heat-treated at high temperature crystal grain life
Length is inhibited, therefore in the case where engaging with ceramic substrate, is not susceptible to removing etc. in the bonding part with ceramic substrate.
Therefore, copper sheet material of the invention is excellent as the copper sheet material for the insulating substrate with copper sheet.
Claims (6)
1. a kind of copper sheet material for the insulating substrate with copper sheet, which is characterized in that have following composition: selected from by Al, Be,
Total content of metal component in the group of Cd, Mg, Pb, Ni, P, Sn and Cr composition is 0.1~2.0ppm, the content of copper is
99.96 mass % or more, and with following rolling texture: it indicates using Eulerian angles (φ 1, Φ, φ 2) by using EBSD's
When the crystalline orientation distribution function that texture parses, φ 2=0 °, φ 1=0 °, Φ=0 °~90 ° range in orientation
The average value of density is 3.0 more than or lower than 35.0, and the model in φ 2=35 °, 1=45 °~55 ° φ, Φ=65 °~80 °
The maximum value of orientation density in enclosing is 1.0 more than or lower than 30.0.
2. the copper sheet material according to claim 1 for the insulating substrate with copper sheet, wherein the content of the copper is
99.99 mass % or more, and the average value of longitudinal modulus of elasticity is 115GPa hereinafter, the longitudinal modulus of elasticity is in rolling side
It is measured on direction to, plate width direction and between them.
3. the copper sheet material according to claim 1 or 2 for the insulating substrate with copper sheet, wherein average crystallite particle diameter 3
μm~100 μm.
4. the copper sheet material described in any one of claim 1 to 3 for the insulating substrate with copper sheet, wherein be subjected to
At 700~800 DEG C after 10 minutes~5 hours thermal process in the state of, average crystallite particle diameter be 50 μm~200 μm.
5. the copper sheet material according to any one of claims 1 to 4 for the insulating substrate with copper sheet, wherein tension is strong
Degree is 150~330MPa, and conductivity is 95%IACS or more.
It is institute according to claim 1~any one of 5 6. a kind of manufacturing method of the copper sheet material for the insulating substrate with copper sheet
The manufacturing method for the copper sheet material for the insulating substrate with copper sheet stated, it includes:
Homogenize the heat treatment that homogenizes of heat treatment for by ingot bar obtained from the casting of the copper raw material with the composition
Process；
The hot-rolled process of hot rolling is carried out after this homogenizes heat treatment procedure；
Cooling cooling process is carried out after the hot-rolled process；
The face cutting process of face cutting is carried out to the two sides of the material to be rolled after the cooling process；
The first cold rolling process of the cold rolling that general working rate is 75% or more is carried out after the face cutting process；
It is 1~100 DEG C/sec, reaches that temperature is 100~500 DEG C, the retention time is in heating rate after first cold rolling process
1~900 second and cooling velocity implement the first annealing operation of heat treatment under conditions of being 1~50 DEG C/sec；
The second cold rolling process of the cold rolling that general working rate is 60~95% is carried out after first annealing operation；
Heating rate is 10~100 DEG C/sec, to reach temperature be 200~550 DEG C, retention time after second cold rolling process
For 10~3600 seconds and cooling velocity be 10~100 DEG C/sec under conditions of implement heat treatment the second annealing operation；
The finishing rolling step further rolled after second annealing operation；
Implement the final annealing process of final heat treatment after the finishing rolling step；
The surface film oxide removal step of pickling and grinding is carried out after the final annealing process.
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| JP2017069734 | 2017-03-31 | ||
| PCT/JP2018/013002 WO2018181593A1 (en) | 2017-03-31 | 2018-03-28 | Copper sheet material for copper sheet-provided insulating substrate and production method therefor |
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| JP (1) | JP6678757B2 (en) |
| KR (1) | KR102326618B1 (en) |
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| CN114502755A (en) * | 2020-01-15 | 2022-05-13 | 古河电气工业株式会社 | Copper plate material, method for producing same, and insulating substrate with copper plate material |
| CN115210394A (en) * | 2020-03-06 | 2022-10-18 | 三菱综合材料株式会社 | Pure copper plate |
| CN115244196A (en) * | 2020-03-06 | 2022-10-25 | 三菱综合材料株式会社 | Pure copper plate, copper-ceramic junction body, and insulated circuit board |
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| KR20200104858A (en) | 2018-01-10 | 2020-09-04 | 후루카와 덴키 고교 가부시키가이샤 | Insulated wire |
| KR102343189B1 (en) * | 2018-03-29 | 2021-12-24 | 후루카와 덴끼고교 가부시키가이샤 | Insulation substrate and method for manufacturing the same |
| CN111051546B (en) * | 2018-03-29 | 2021-09-14 | 古河电气工业株式会社 | Insulating substrate and method for manufacturing same |
| CN115896532A (en) * | 2018-12-13 | 2023-04-04 | 三菱综合材料株式会社 | Pure copper plate |
| KR20220146466A (en) * | 2020-03-06 | 2022-11-01 | 미쓰비시 마테리알 가부시키가이샤 | Pure copper plate, copper/ceramic bonded body, insulated circuit board |
| JP7342924B2 (en) * | 2020-10-23 | 2023-09-12 | 三菱マテリアル株式会社 | Slit copper materials, parts for electronic and electrical equipment, bus bars, heat dissipation boards |
| JP7342923B2 (en) * | 2020-10-23 | 2023-09-12 | 三菱マテリアル株式会社 | Slit copper materials, parts for electronic and electrical equipment, bus bars, heat dissipation boards |
| WO2022085718A1 (en) * | 2020-10-23 | 2022-04-28 | 三菱マテリアル株式会社 | Slit copper material, component for electronic/electric devices, bus bar, and heat dissipation substrate |
| US20230313342A1 (en) * | 2020-10-23 | 2023-10-05 | Mitsubishi Materials Corporation | Slit copper material, part for electric/electronic device, bus bar, heat dissipation substrate |
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| KR102326618B1 (en) | 2021-11-16 |
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| JP6678757B2 (en) | 2020-04-08 |
| KR20190134455A (en) | 2019-12-04 |
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