CN107001147A - Ceramic matrix and its manufacture method - Google Patents
Ceramic matrix and its manufacture method Download PDFInfo
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- CN107001147A CN107001147A CN201580066723.4A CN201580066723A CN107001147A CN 107001147 A CN107001147 A CN 107001147A CN 201580066723 A CN201580066723 A CN 201580066723A CN 107001147 A CN107001147 A CN 107001147A
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/111—Fine ceramics
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/12—Mountings, e.g. non-detachable insulating substrates
- H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
- H01L23/15—Ceramic or glass substrates
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/12—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using thick film techniques, e.g. printing techniques to apply the conductive material or similar techniques for applying conductive paste or ink patterns
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2224/00—Indexing scheme for arrangements for connecting or disconnecting semiconductor or solid-state bodies and methods related thereto as covered by H01L24/00
- H01L2224/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
- H01L2224/10—Bump connectors; Manufacturing methods related thereto
- H01L2224/15—Structure, shape, material or disposition of the bump connectors after the connecting process
- H01L2224/16—Structure, shape, material or disposition of the bump connectors after the connecting process of an individual bump connector
- H01L2224/161—Disposition
- H01L2224/16151—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
- H01L2224/16221—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked
- H01L2224/16225—Disposition the bump connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive the body and the item being stacked the item being non-metallic, e.g. insulating substrate with or without metallisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/0001—Technical content checked by a classifier
- H01L2924/0002—Not covered by any one of groups H01L24/00, H01L24/00 and H01L2224/00
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2924/00—Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
- H01L2924/15—Details of package parts other than the semiconductor or other solid state devices to be connected
- H01L2924/161—Cap
- H01L2924/1615—Shape
- H01L2924/16195—Flat cap [not enclosing an internal cavity]
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Production Of Multi-Layered Print Wiring Board (AREA)
Abstract
The present invention relates to ceramic matrix and its manufacture method.The crystalline phase of ceramic matrix is with Al2O3And ZrO2For main crystalline phase, in addition, Mn is included3Al2(SiO4)3Or MgAl2O4, and bending strength is more than 650Ma, Young's modulus is below 300GPa.
Description
Technical field
The present invention relates to a kind of ceramic matrix, the ceramics system encapsulation of the element such as being related to suitable for internally installing oscillator
The ceramic matrix and its manufacture method of body, high frequency electric road plate etc..
Background technology
As existing ceramic matrix, for example with aluminum oxide (Al2O3) and zirconium oxide (ZrO2) be principal component ceramic base
Body, it is known that in No. 2883787 publications of Japanese Patent Publication No., No. 3176815 publications of Japanese Patent Publication No. and Japanese Patent Publication No. 4717960
The ceramic matrix of record.
In No. 2883787 publications of Japanese Patent Publication No., a kind of ceramic matrix is recorded, it includes 70~90 mass % oxidation
Aluminium and 10~30 mass % zirconium oxide are as principal component, and yttrium (Y), 0.5~2.0 mass % comprising 0.5~2.0 mass %
Calcium (Ca), 0.5~2.0 mass % magnesium (Mg), 0.5~2.0 mass % cerium (Ce) be used as additive.
In No. 3176815 publications of Japanese Patent Publication No., a kind of ceramic matrix is recorded, it includes 82~97 mass % oxidation
Aluminium and 2.5~17.5 mass % zirconium oxide are as principal component, and yttrium (Y) comprising 0.1~2.0 mass %, 0.02~0.5 matter
Amount % calcium (Ca), 0.02~0.4 mass % magnesium (Mg) is used as additive.
In No. 4717960 publications of Japanese Patent Publication No., a kind of include as the aluminum oxide of principal component, as accessory ingredient is recorded
PSZ, the ceramic matrix of magnesia.On the ceramic matrix, the content of PSZ is relative to powder
For the gross weight of body material in the range of 1~30wt%, the content of magnesia is for the gross weight of powder body material
In the range of 0.05~0.50wt%, the mole fraction of the yttria in PSZ is 0.015~0.035
In the range of.
The content of the invention
Generally, in ceramic matrix, as bending strength is raised, Young's modulus can also be raised.If Young's modulus is raised,
It is unlikely to deform and can becomes fragile, therefore, easily crack, additionally, there are the problems such as easily occurring chipping in chip separation.
It is provided with the packaging body purposes of oscillator etc., by the way that ceramic mouldings and metal film are burnt till simultaneously, can obtains
It is formed with the ceramic matrix of electrode layer, wiring layer.In this case, if the Young's modulus rise of ceramic matrix, is being carried
Easily because being cracked to resistant to bending stresses in the small-sized and slim packaging body purposes of wearable device, IC-card etc..
But, above-mentioned No. 2883787 publications of Japanese Patent Publication No., No. 3176815 publications of Japanese Patent Publication No. and Japanese Patent
In No. 4717960, although bending strength is illustrated, but any consideration is not made to Young's modulus.
The present invention considers this problem and implemented, it is therefore intended that provide a kind of ceramic matrix and its manufacture method, should
Ceramic matrix is also adapted to high frequency electric road plate, and its bending strength is high, also, Young's modulus is low, and can be achieved at low cost makes
With the miniaturization of the product (ceramic packaging body, high frequency electric road plate etc.) of ceramic matrix.
The involved ceramic matrix of [1] first invention is characterised by that its crystalline phase is with Al2O3And ZrO2For main crystalline phase,
In addition, comprising Mn3Al2(SiO4)3Or MgAl2O4, and bending strength is more than 650Ma, Young's modulus is below 300GPa.
In [2] first inventions, preferably bending strength is 650MPa~1100MPa, and Young's modulus is 240GPa~300GPa.
In [3] first inventions, preferably dielectric loss angle tangent is 200 × 10 in 1MHz- 4Hereinafter, relative dielectric constant
For 10~15.
In [4] first inventions, it is preferable over 1250~1500 DEG C of temperature and is sintered.
In [5] first inventions, preferably comprise：By Al2O3Conversion is calculated as 70.0~90.0 mass % Al, by ZrO2Conversion
It is calculated as 10.0~30.0 mass % Zr, Al2O3And ZrO2Add up to 100 mass % in the case of, comprising：Based on MnO conversions
For 2.0~7.0 mass % Mn, by SiO2Conversion is calculated as 2.0~7.0 mass % Si, is calculated as 0.5~2.0 matter by BaO conversions
Measure % Ba, being converted by MgO is calculated as 0~2.0 mass % Mg.Mn, Ba, Mg can also use carbonate.
The manufacture method of the involved ceramic matrix of [6] second inventions is characterised by, including following process：Make shaping
The formed body production process of body and by the formed body in 1250~1500 DEG C of firing process burnt till, the formed body contains
Have by Al2O3Conversion is calculated as 70.0~90.0 mass % Al, by ZrO2Conversion is calculated as 10.0~30.0 mass % Zr, Al2O3
And ZrO2Add up to 100 mass % in the case of, containing by MnO2Conversion is calculated as 2.0~7.0 mass % Mn, by SiO2Change
Calculate to convert for 2.0~7.0 mass % Si, by BaO and be calculated as 0.5~2.0 mass % Ba, be calculated as 0~2.0 by MgO conversions
Quality % Mg.
In [7] second inventions, it can be additionally included in formation on the formed body after the formed body production process and include
The process of the conductor layer of metal, in the firing process, burns till to the formed body for being formed with the conductor layer.
In [8] second inventions, the firing process can enter in hydrogen content is more than 5% hydrogen and the forming gas of nitrogen
OK.
According to ceramic matrix and its manufacture method involved in the present invention, following effect is played.
(a) bending strength is high, also, Young's modulus is low.
(b) it is also adapted to high frequency electric road plate.
(c) chipping incidence during chip separation is also small.
(d) when carrying as encapsulation body component etc., it is difficult to destroy because of bending stress.
(e) during soldering, it is not likely to produce crackle.
(f) yield rate can be improved, product (ceramic packaging body, the height for having used ceramic matrix can be achieved at low cost
Frequency circuit board etc.) miniaturization.
Brief description of the drawings
Fig. 1 is the section for representing the first configuration example (the first packaging body) using the ceramic matrix involved by present embodiment
Figure.
Fig. 2 be by the manufacture method of the manufacture method of the ceramic matrix involved by present embodiment and the first packaging body together
The process block diagram of expression.
Fig. 3 is the section for representing the second configuration example (the second packaging body) using the ceramic matrix involved by present embodiment
Figure.
Fig. 4 be by the manufacture method of the manufacture method of the ceramic matrix involved by present embodiment and the second packaging body together
The process block diagram of expression.
Embodiment
Hereinafter, 1~Fig. 4 of reference picture, the embodiment example to ceramic matrix and its manufacture method involved in the present invention is entered
Row explanation.It should illustrate, "~" that number range is represented in this specification is to be used as lower limit as the numerical value that will be recorded before and after it
Implication that value and higher limit are included and use.
The crystalline phase of ceramic matrix involved by present embodiment is with Al2O3And ZrO2For main crystalline phase, in addition, bag
Containing Mn3Al2(SiO4)3Or MgAl2O4。
Specifically, preferably comprise：By Al2O3Conversion is calculated as 70.0~90.0 mass % Al, by ZrO2Conversion is calculated as
10.0~30.0 mass % Zr, Al2O3And ZrO2Add up to 100 mass % in the case of, comprising：It is calculated as by MnO conversions
2.0~7.0 mass % Mn, by SiO2Conversion is calculated as 2.0~7.0 mass % Si, is calculated as 0.5~2.0 matter by BaO conversions
Measure % Ba, being converted by MgO is calculated as 0~2.0 mass % Mg.Thereby, it is possible to improve bending strength, also, low poplar can be realized
Family name's modulus.
The ceramic matrix is to make the Al for example containing 70.0~90.0 mass %2O3Powder, 10.0~30.0 mass %
ZrO2Powder, 2.0~7.0 mass % MnO powder, by SiO2Conversion is calculated as 2.0~7.0 mass % Si, 0.5~2.0 matter
Measure after % BaO powder, the formed body of 0~2.0 mass % MgO powder, formed body is burnt till at 1250~1500 DEG C
And make.
Now, it is as shown in table 1 below, on Al2O3, preferred feedstock (Al2O3Powder) particle mean size be 0.3~2.5 μm, and
Al during sintered body is made2O3Crystallization particle diameter be 0.7~3.0 μm.In addition, on ZrO2, preferred feedstock (ZrO2Powder) be averaged
Granularity is 0.05~1.0 μm, and ZrO when being made sintered body2Crystallization particle diameter be 0.05~1.0 μm.
Table 1
It should illustrate, the particle mean size of raw material refers to：Utilize Measurement of particle size distribution by laser diffraction (HORIBA
System, LA-920) determine in obtained volume reference size distribution, the throughput accumulation from small particle side (accumulation passes through a point rate)
50% particle diameter.
Crystallization particle diameter when sintered body is made is obtained as follows.That is, sintered body is being shot using scanning electron microscope
It is micro- to adjust scanning electron by 500~1000 or so crystalline particles are photographed in captured whole image during surface
The multiplying power of mirror.Also, image processing software is used, arbitrary 100 particles crystallized above in captured image are changed respectively
Calculate as positive round, using being averaged for its particle diameter, calculate crystallization particle diameter.
MnO powder and SiO2Powder is the sintering aid as principal component, in addition, being to realize burning to generate glass phase
The reduction of junction temperature and add.BaO powder is to suppress to generate the MnAl that uprises of hardness2O4And add.MgO powder is
In order to generate spinel crystal phase, the i.e. MgAl with the feature such as resistant to chemical etching, electrical loss is few2O4And add.As electric
Characteristic, preferably dielectric loss angle tangent are 200 × 10 in 1MHz- 4Below.More preferably 20 × 10- 4Below.Thus,
Can also by ceramic matrix be applied to high frequency electric road plate, therefore it is preferred that.In addition, relative dielectric constant is preferably 10~15.
It should illustrate, below 1.0 mass % Mo (molybdenum) oxides or W (tungsten) oxides or Cr can be included as needed
(chromium) oxide is used as colouring agent.
Thus, it is possible to be sintered in temperature for 1250~1500 DEG C of low temperature, it is 650MPa that can realize bending strength
Above, Young's modulus is below 300GPa ceramic matrix.Specifically, can realize bending strength for 650MPa~
1100MPa, Young's modulus are 240GPa~300GPa ceramic matrix.
Generally, in ceramic matrix, as bending strength is raised, Young's modulus can also be raised.If Young's modulus is raised,
It is unlikely to deform and can becomes fragile, therefore, easily crack, additionally, there are the problems such as easily occurring chipping in chip separation.
But, the ceramic matrix involved by present embodiment is also adapted to high frequency electric road plate, even if bending strength is
More than 650MPa, Young's modulus still as little as below 300GPa, therefore, chipping incidence during chip separation are also small, are being used as envelope
When filling the carrying such as body component, it is difficult to destroy because of bending stress, in soldering, is not likely to produce crackle, it is possible to increase finished product
Rate, can be achieved at low cost the miniaturization for the product (ceramic packaging body, high frequency electric road plate etc.) for having used ceramic matrix.
It should illustrate, by making Al content by Al2O3Conversion is calculated as 70.0~90.0 mass %, the Al generated2O3's
Measure to be optimal, even if firing temperature rises, can also suppress Al2O3Crystallization particle diameter increase, therefore, easily realize bending strength
Raising.
By making Zr content by ZrO2Conversion is calculated as 10.0~30.0 mass %, easily improves bending strength, also, energy
Enough suppress Young's modulus rise, in addition, dielectric constant increase and pyroconductivity reduction can be suppressed.
2.0~7.0 mass % are calculated as by making Mn content be converted by MnO, the amount of generated glass phase can be suppressed
Reduction, easily realize the densification at 1250~1500 DEG C, in addition, can suppress generated glass softening temperature reduce with
And porosity increase.And then, bending strength reduction can be suppressed.
By making Si content by SiO2Conversion is calculated as 2.0~7.0 mass %, can suppress the amount of generated glass phase
Reduction, easily realize the densification at 1250~1500 DEG C, in addition, can suppress generated glass softening temperature reduce with
And porosity increase.And then, bending strength reduction can be suppressed.
0.5~2.0 mass % is calculated as by making Ba content be converted by BaO, easily suppresses MnAl2O4Generation, can press down
Intensity decreases processed.In addition, the high temperature of sintering temperature can be suppressed, so that suppress the grain growth of aluminum oxide and zirconium oxide, also,
Being capable of inhibition strength reduction.
0~2.0 mass % is calculated as by making Mg content be converted by MgO, the high temperature of sintering temperature can be suppressed, so that
Suppress the grain growth of aluminum oxide and zirconium oxide, further, it is possible to which inhibition strength is reduced.
Therefore, by containing Al, Zr, Mn, Si, Ba, Mg with above-mentioned ratio, the firing temperature of porcelain, energy can be optimized
The enough intensity for improving generated glass phase, as a result, bending strength is raised, and Young's modulus is reduced, and can promote to have used pottery
The miniaturization of the product (ceramic packaging body etc.) of porcelain basal body.Further, it is possible to be made under low firing temperature, be conducive into
Originally cheaper.And then, chipping incidence when chip separation is carried out using such as compression roller can be reduced, it is possible to increase production
Rate.Electrical characteristic (dielectric loss angle tangent) can also be suppressed in low-level.In addition, if (i) addition MgO or (ii) knot
There is MgAl in crystalline phase2O4And in the absence of Mn3Al2(SiO4)3Or above-mentioned (1) and (ii), then dielectric loss angle tangent is relatively low, example
Such as it is suitable for high frequency electric road plate.
Herein, 1~Fig. 4 of reference picture, 2 of ceramic packaging body to having used the ceramic matrix involved by present embodiment
Configuration example is illustrated.
Ceramic packaging body (hereinafter referred to as the first packaging body 10A) involved by first configuration example has by this as shown in Figure 1
The multilayer board 12 that ceramic matrix involved by embodiment is constituted is with same as the ceramic matrix structure involved by present embodiment
Into lid 14.
Multilayer board 12 be at least by the first substrate 16a of tabular, the second substrate 16b of tabular and framework 18 in this order
It is laminated and constitutes.In addition, the multilayer board 12 has：Formed second substrate 16b upper surfaces upper surface electrode 20, formed
Lower surface electrode 22 in first substrate 16a lower surfaces, form internal layer electrode 24 internally, by the internal layer electrode 24 and following table
The first through hole 26a of the electrical connection of face electrode 22, the second through hole 26b for electrically connecting internal layer electrode 24 and upper surface electrode 20.
In addition, in first packaging body 10A, it is empty in the collecting surrounded by second substrate 16b upper surface and framework 18
Between in 28, quartz crystal unit 30 is electrically connected to upper surface electrode 20 via conductor layer 32.And then, in order to protect quartz crystal unit 30, lid
Body 14 is hermetically sealed in the upper surface of framework 18 via glassy layer 34.
In above-mentioned first packaging body 10A, the example that quartz crystal unit 30 is mounted with receiving space 28 is given, except this
In addition, at least one or more in resistor, wave filter, capacitor, semiconductor element can also be installed.In the present embodiment,
Dielectric loss angle tangent is 200 × 10 in 1MHz- 4Hereinafter, preferably 20 × 10- 4Hereinafter, therefore, it also is suitable as high frequency use
Circuit board.
Also, because the first packaging body 10A multilayer board 12 and lid 14 are constituted as the pottery involved by present embodiment
Porcelain basal body is constituted, so bending strength is more than 650MPa, Young's modulus is below 300GPa.If bending strength is 650MPa
Hereinafter, Young's modulus is more than 300GPa, then is unlikely to deform and can become fragile as described above, therefore, easily occur in chip separation
Chipping.Additionally, it is possible to apply thermal stress when lid 14 is sealed and during secondary installing and destroy.Or, it is possible to because of operation
When and impact after being carried as encapsulation body component etc. etc. and destroy.
As long as bending strength is more than 650MPa, Young's modulus is below 300GPa, it becomes possible to avoid such destruction wind
Danger.Even if in addition, not carrying out surface grinding to ceramic matrix functions as the first packaging body 10A multilayer board 12 and lid 14,
Also it can prevent from destroying when hermetic sealing lid 14, the first packaging body 10A manufacturing cost can be improved
And reliability.It should illustrate, " bending strength " refers to 4 bending strengths, be to be based on the JISR1601 (bend tests of fine ceramics
Method) value that determines at room temperature.
Also, can be 1250 in temperature because the ceramic matrix involved by present embodiment has above-mentioned composition
It is sintered in a low temperature of~1500 DEG C.Therefore, by by the presoma (formed body before burning till) of ceramic matrix, electrode (on
Surface electrode 20, lower surface electrode 22, internal layer electrode 24) and through hole 26 (first through hole 26a, the second through hole 26b) burn till simultaneously,
Multilayer board 12 can be made, manufacturing process can be simplified.
Next, according to such as the first packaging body 10A manufacture method, reference picture 2, the manufacture method to ceramic matrix is entered
Row explanation.
First, in Fig. 2 step S1a, the Al containing 70.0~90.0 mass % is prepared2O3Powder, 10.0~30.0 matter
Measure % ZrO2Powder, 2.0~7.0 mass % MnO powder, by SiO2Conversion be calculated as 2.0~7.0 mass % Si, 0.5~
The mixed-powder of 2.0 mass % BaO powder, 0~2.0 mass % MgO powder, in step S1b, prepares organic principle
(bonding agent), in step S1c, prepares solvent.
Al2O3The particle mean size of powder is preferably 0.3~2.5 μm.ZrO2The particle mean size of powder is preferably 0.05~1.0 μ
m.If within the range, obtaining uniform porcelain, therefore it is preferred that, further, it is possible to improve intensity, Neng Goushi by being densified
Existing Al2O3And ZrO2The agglutinating property of itself is improved.
The particle mean size of MnO powder is preferably 0.5~4.0 μm.SiO2The particle mean size of powder is preferably 0.1~2.5 μm.
The particle mean size of BaO powder is preferably 0.5~4.0 μm.The particle mean size of MgO powder is preferably 0.1~1.0 μm.
For these MnO powder, SiO2Powder, BaO powder, MgO powder, if in preferred scope, can carry
The dispersiveness of high particle, homogenizes composition, further, it is possible to realize the raising of intensity.
The organic principle (bonding agent) prepared in step S1b can enumerate resin, surfactant, plasticizer etc..Make
For resin, for example, polyvinyl butyral resin, as surfactant, for example, tertiary amine, as plasticizer,
For example, phthalic acid ester (such as phthalic acid diisononyl esters：DINP).
The solvent prepared in step S1c can enumerate alcohol series solvent, fragrant family solvent etc.., can as alcohol series solvent
To enumerate such as IPA (isopropanol), as fragrant family solvent, for example, toluene.
Then, in following step S2, after mixing organic principle and solvent, being dispersed in above-mentioned mixed-powder,
In step s3, it is used as by forming method known to extrusion, doctor blade method, rolling process, injection etc. before ceramic matrix
Drive the ceramic mouldings (also referred to as ceramic band) of body.Organic principle, solvent are added for example in mixed-powder, slurry is modulated into
Afterwards, the ceramic band of specific thickness is made by doctor blade method.Or, organic principle is added in mixed-powder, by extrusion forming,
Calendering formation etc. and the ceramic band for making specific thickness.
In step s 4, ceramic band is cut off and is processed into desired shape, make the large area of first substrate
First band, the second band of the large area of second substrate, the 3rd band and the 4th band of lid of framework, and then, by making
Formed with the punch press process of mould, microbit processing, Laser Processing etc. for forming first through hole 26a and the second through hole 26b
Through hole.
Next, in step s 5, by methods such as silk-screen printing, intaglio printings, to make as described above
One band and the second conductor paste with printing coating for forming upper surface electrode 20, lower surface electrode 22, internal layer electrode 24, enter
And, as needed, conductor paste is filled into through hole.
Conductor paste preferably as conductor composition using in the refractory metal such as W (tungsten), Mo (molybdenum) it is at least one kind of,
Al wherein with the addition of with such as 1~20 mass %, particularly below 8 mass % ratio2O3Powder or SiO2Powder or with pottery
The conductor paste of porcelain basal body identical powder.Thereby, it is possible to which the conducting resistance of conductor layer is being maintained into low-level raising simultaneously
The adhesion of alumina sintered body and conductor layer, can prevent a problem that electrodeposited coating is lacked.
Then, in step s 6, the first band for being coated with conductor paste and the second band and the 3rd band of framework will be printed
Contraposition, carries out stacking crimping, makes layered product.
Then, in the step s 7, the segmentation groove formed on the two sides of layered product for splitting chip is cut for example, by knife.
In following step S8, by layered product and the 4th band in the hydrogen and the shaping gas of nitrogen that hydrogen content is more than 5%
Body atmosphere, such as H2/N2With 1250~1500 DEG C in=30%/70% forming gas atmosphere (25~47 DEG C of fogger temperature)
Temperature range burnt till.Thus, stacking raw sheet (the polyelectron part base that layered product and conductor paste are burnt till simultaneously is made
Plate).Burnt till by this, crystalline phase as described above can be made with Al2O3And ZrO2For main crystalline phase, in addition, comprising
Mn3Al2(SiO4)3Or MgAl2O4Ceramic matrix, i.e. polyelectron part substrate.
Because the atmosphere burnt till is forming gas atmosphere as described above, thus, it is possible to prevent the metal in conductor paste
Oxidation.The preferred said temperature scope of firing temperature.Densification can be promoted, further, it is possible to improve bending strength.In addition, energy
Enough shrinkage factors for reducing the first band for constituting layered product, the second band and the 3rd band are uneven, additionally it is possible to realize dimensional accuracy improve, with
And cost rate is improved.Due to firing temperature need not be improved, so cost correspondingly need not be spent in equipment.
In addition, Al when sintered body is made2O3Crystallization particle diameter be preferably 0.7~3.0 μm, ZrO during sintered body is made2
Crystallization particle diameter be preferably 0.05~1.0 μm.If within the range, obtaining uniform porcelain, therefore it is preferred that, further, it is possible to
Intensity is improved by being densified, Al is realized2O3And ZrO2The agglutinating property of itself is improved.
Next, in step s 9, carrying out electroplating processes to above-mentioned polyelectron part substrate, being formed at the polyelectron portion
The conductor layer formation of part substrate surface is by least one kind of electrodeposited coating constituted in Ni, Co, Cr, Au, Pd and Cu, in polyelectron portion
Part substrate surface forms multiple upper surface electrodes 20 and multiple lower surface electrodes 22.
Then, in step slo, it is pushed against polyelectron part substrate being divided into multiple (chip separations) with compression roller etc.,
Make multiple multilayer boards 12 with receiving space 28.In step s 11, in each receiving space 28 of multiple multilayer boards 12
It is interior, quartz crystal unit 30 is installed on upper surface electrode 20 via conductor layer 32 respectively.
Then, in step s 12, in the upper surface of each multilayer board 12, with the ceramics for being formed with glass for sealing layer 34
Lid 14 processed is hermetic sealed (lid engagement), so as to complete internally to be provided with multiple first encapsulation of quartz crystal unit 30
Body 10A.
In first packaging body 10A manufacture method (manufacture method of ceramic matrix), knot as described above can be made
Crystalline phase is with Al2O3And ZrO2For main crystalline phase, in addition, include Mn3Al2(SiO4)3Or MgAl2O4, be also adapted to high frequency use
Circuit board, bending strength are the ceramic matrix that more than 650MPa, Young's modulus are below 300GPa.In addition, can be in low burning
Chipping incidence when chip separation is made at a temperature of is also small, can improve yield rate, can be achieved at low cost and use
The ceramic matrix of the miniaturization of the product (ceramic packaging body, high frequency electric road plate etc.) of ceramic matrix.
Next, reference picture 3 and Fig. 4, to ceramic packaging body (hereinafter referred to as the second packaging body involved by the second configuration example
10B) illustrate.
Second packaging body 10B have as shown in Figure 3 with above-mentioned first packaging body 10A almost same compositions, but with
Lower aspect is different.
That is, metal cap body 40 is hermetically sealed in the frame of multilayer board 12 using the high-temperature sealing materials such as silver solder 42
On body 18.
In addition, there is bonding layer 44 between the upper surface of the framework 18 of multilayer board 12 and high-temperature sealing material 42.Should
Bonding layer 44 the upper surface of framework 18 have by formed with the identical material of upper surface electrode 20 metal layer 46, formed
Such as nickel (Ni) electrolysis electrodeposited coating 48, formation on the metal layer 46 are electrolysed for example golden (Au) nothing on electrodeposited coating 48 in the Ni
It is electrolysed electrodeposited coating 50.
Metal cap body 40 is formed as 0.05~0.20mm of thickness tabular, by Fe-Ni alloy plate or iron-nickel-cobalt
Alloy sheets are constituted.In the lower surface (whole face or the part corresponding to framework 18) of the metal cap body 40, it is formed with as high temperature
The solders such as the silver-copper eutectic solder of encapsulant 42.Thickness is 5~20 μm or so.
Specifically, following composite plate is punched into regulation shape with blanking die and made by metal cap body 40, and this is answered
Plywood is that the lower surface that the solder foils such as silver-copper solder are overlapped into Fe-Ni alloy plate or iron-nickel-cobalt alloy sheets is gone forward side by side
What row rolled and constituted.
As high-temperature sealing material 42, solder 1 (85Ag-15Cu), (72Ag- of solder 2 shown in table 2 below can be used
28Cu), solder 3 (67Ag-29Cu-4Sn) etc..
Table 2
Ni is electrolysed electrodeposited coating 48 and Au electroless platings layer 50 as raising high-temperature sealing material 42 to metal layer 46
The layer of wetability plays a role.
Next, reference picture 4, the manufacture method to the second packaging body 10B is illustrated.Should illustrate, for Fig. 2 weights
Multiple process, is omitted the description.
First, in Fig. 4 step S101, the mixed-powder, organic principle and solvent for making ceramic band are prepared.It is accurate
Standby mixed-powder, organic principle and solvent is identical with above-mentioned steps S1a, step S1b and step S1c, so omitting its repetition
Explanation.
Then, in step s 102, after mixing organic principle and solvent, being dispersed in above-mentioned mixed-powder, in step
In S103, ceramic matrix presoma is used as by forming method known to extrusion, doctor blade method, rolling process, injection etc.
Ceramic mouldings (ceramic band).
In step S104, ceramic band is cut off and desired shape is processed into, first substrate 16a big face is made
The second band, the 3rd band of framework 18 of long-pending first band, second substrate 16b large area, and then, by microbit plus
Work, Laser Processing etc. form the through hole for forming first through hole 26a and the second through hole 26b.
On the other hand, in step S105, material powder, organic principle and the solvent of conductor paste are prepared.The original of preparation
Feed powder end can enumerate at least one kind of in the metal dusts such as W (tungsten), Mo (molybdenum), nickel (Ni) and wherein with such as 1 as described above
~20 mass %, particularly below 8 mass % ratio are properly added Al2O3Powder or SiO2Powder or with ceramic base body phase
Mixed-powder obtained from same powder.The organic principle of preparation can enumerate resin (such as ethyl cellulose), surface-active
Agent etc..The solvent of preparation can enumerate terpinol (terpineol) etc..
Then, in step s 106, organic principle and solvent are mixed, are dispersed in above-mentioned mixed-powder, modulate conductor
Paste.
Next, in step s 107, by the methods such as silk-screen printing, intaglio printing to make as described above
One band the~the three band printing coated conductor paste.
Then, in step S108, first band~3rd for being coated with conductor paste will be printed with aligning, stacking is crimped, system
Make layered product.
Then, in step S109, the segmentation ditch formed on the two sides of layered product for splitting chip is cut for example, by knife
Groove.
In following step S110, by layered product in H2/N2=30%/70% forming gas atmosphere (fogger temperature
Degree 25~47 DEG C) in burnt till with 1250~1500 DEG C of temperature range.Thus, make layered product and conductor paste is burnt simultaneously
Into stacking raw sheet (polyelectron part substrate).There are the polyelectron part substrate multiple frameworks 18 to be aligned to integral shape
Shape.In addition, being burnt till by this, conductor paste turns into electrode (upper surface electrode 20 etc.), metal layer 46.
In following step S111, the surface (pre-treatment) of metal layer 46 is at least cleaned with alkali, acid etc..That is, exist
Carry out after alkali cleaning, carry out sour cleaning.In preceding processing, alkali and acid can be diluted to appropriate concentration and be used.In addition, preceding
The temperature handled at 20 DEG C~70 DEG C or so implements a few minutes~dozens of minutes.
In step S112, handled by carrying out Ni electrolysis or electroless plating, Ni electricity is formed on metal layer 46
(the thickness of coating 48：1.0~5.0 μm).
In step S113, Au electrolysis or electroless plating 50 (thickness of layer are formed on Ni electrodeposited coating 48：0.05~
0.3μm)。
Then, in step S114, it is pushed against polyelectron part substrate being divided into multiple (chip separations) with compression roller etc.,
Multiple multilayer boards 12 with receiving space 28 are made respectively.Then, in step sl 15, in each of multiple multilayer boards 12
In receiving space 28, quartz crystal unit 30 is installed on upper surface electrode 20 via conductor layer 32 respectively.
Then, in step S116, make upper surface (bonding layer 44) side of high-temperature sealing material 42 and framework 18 opposed and
The metal cap body 40 for making the back side form high-temperature sealing material 42 is covered in framework 18.Then, a pair of rolls electricity of seam welder is made
Pole is while contact is in the opposite outer peripheral edge of metal cap body 40, rotation, and by flowing through electric current between the roller electrode on one side,
Make the part melting of high-temperature sealing material 42, thus metal cap body 40 is hermetically sealed in framework 18.It is used as sealing
When atmosphere, in N2Sealed in gas or vacuum.Thus, completion is internally provided with multiple second envelopes of quartz crystal unit 30
Fill body 10B.
Embodiment
For embodiment 1~12, comparative example 1 and 2, it is thus identified that the Al of ceramic matrix2O3And ZrO2Crystalline phase in addition, machine
Tool characteristic (bending strength (rupture strength) and Young's modulus), electrical characteristic (relative dielectric constant and dielectric loss angle tangent).
(embodiment 1)
Prepare material powder.Material powder is the Al of 1.70 μm of average grain diameter2O3The ZrO of powder, 0.50 μm of average grain diameter2
Powder, the MnO powder of 1.0 μm of average grain diameter, the SiO of 1.0 μm of average grain diameter2The BaO powder of powder, 1.0 μm of average grain diameter.
By the ratio (Al shown in material powder according to the form below 32O3Powder：78.60 mass %, ZrO2Powder：21.40 matter
Measure %, MnO powder：3.04 mass %, SiO2Powder：2.78 mass %, BaO powder：0.77 mass %) mixing, mixed
Powder.In obtained mixed-powder, the polyvinyl butyral resin, tertiary amine and phthalic acid ester as organic principle are mixed
(phthalic acid diisononyl esters：DINP), mix, spread as the IPA (isopropanol) and toluene of solvent and modulate slurry, so
Afterwards, the ceramic band of 60~270 μm of thickness is produced by doctor blade method.By obtained ceramic band in firing temperature (maximum temperature)
1440℃、H2+N2Forming gas atmosphere in burnt till, produce the ceramic matrix involved by embodiment 1.By burning simultaneously
Into and form conductor.As ceramic matrix, make for confirming the first ceramic matrix of crystalline phase, for confirming bending strength
The second ceramic matrix, the 3rd ceramic matrix for confirming Young's modulus and (normal with respect to dielectric for determining electrical characteristic
Number and dielectric loss angle tangent) the 4th ceramic matrix.Embodiment explained below 2~12 and comparative example 1 and 2 are similarly.
(embodiment 2)
In material powder, it is 2.81 mass % to make MnO powder, makes SiO2Powder is 2.57 mass %, makes the BaO powder be
0.71 mass %, it is 0.54 mass % to make MgO powder, in addition, and the institute of embodiment 2 is made in the same manner as the above embodiments 1
The ceramic matrix being related to.
(embodiment 3)
In material powder, make Al2O3Powder is 89.30 mass %, makes ZrO2Powder be 10.70 mass %, except this with
Outside, the ceramic matrix involved by embodiment 3 is made in the same manner as the above embodiments 2.
(embodiment 4)
In material powder, it is 3.34 mass % to make MnO powder, makes SiO2Powder is 2.04 mass %, makes the BaO powder be
0.71 mass %, it is 0.54 mass % to make MgO powder, in addition, and the institute of embodiment 4 is made in the same manner as the above embodiments 1
The ceramic matrix being related to.
(embodiment 5)
In material powder, it is 2.27 mass % to make MnO powder, makes SiO2Powder is 3.11 mass %, makes the BaO powder be
0.71 mass %, it is 0.54 mass % to make MgO powder, in addition, and the institute of embodiment 5 is made in the same manner as the above embodiments 1
The ceramic matrix being related to.
(embodiment 6)
In material powder, it is 2.44 mass % to make MnO powder, makes SiO2Powder is 2.23 mass %, makes the BaO powder be
1.42 mass %, it is 0.54 mass % to make MgO powder, in addition, and the institute of embodiment 6 is made in the same manner as the above embodiments 1
The ceramic matrix being related to.
(embodiment 7)
In material powder, it is 2.57 mass % to make MnO powder, makes SiO2Powder is 2.35 mass %, makes the BaO powder be
0.64 mass %, it is 1.07 mass % to make MgO powder, also, makes firing temperature (maximum temperature) be 1470 DEG C, in addition,
The ceramic matrix involved by embodiment 7 is made in the same manner as the above embodiments 1.
(embodiment 8)
In material powder, it is 4.36 mass % to make MnO powder, makes SiO2Powder is 4.00 mass %, makes the BaO powder be
1.11 mass %, it is 0.83 mass % to make MgO powder, also, makes firing temperature (maximum temperature) be 1390 DEG C, in addition,
The ceramic matrix involved by embodiment 8 is made in the same manner as the above embodiments 1.
(embodiment 9)
In material powder, make Al2O3Powder is 70.00 mass %, makes ZrO2Powder be 30.00 mass %, except this with
Outside, the ceramic matrix involved by embodiment 9 is made in the same manner as the above embodiments 8.
(embodiment 10)
In material powder, make Al2O3The particle mean size of powder is 0.50 μm, and it is 1390 to make firing temperature (maximum temperature)
DEG C, in addition, the ceramic matrix involved by embodiment 10 is made in the same manner as the above embodiments 2.
(embodiment 11)
In material powder, it is 6.04 mass % to make MnO powder, makes SiO2Powder is 5.53 mass %, makes the BaO powder be
1.53 mass %, it is 1.15 mass % to make MgO powder, also, makes firing temperature (maximum temperature) be 1310 DEG C, in addition,
The ceramic matrix involved by embodiment 11 is made in the same manner as the above embodiments 10.
(embodiment 12)
In material powder, make Al2O3Powder is 70.00 mass %, makes ZrO2Powder be 30.00 mass %, except this with
Outside, the ceramic matrix involved by embodiment 12 is made in the same manner as the above embodiments 10.
(comparative example 1)
In material powder, make Al2O3Powder is 75.80 mass %, makes ZrO2Powder is 24.20 mass %, makes MnO powder
End is 0.00 mass % (without), makes SiO2Powder is 0.60 mass %, and it is 0.00 mass % (without) to make BaO powder,
It is 0.10 mass % to make MgO powder, also, makes firing temperature (maximum temperature) be 1500 DEG C, in addition, with above-mentioned implementation
The ceramic matrix of example 1 similarly involved by comparison example 1.
(comparative example 2)
In material powder, make Al2O3Powder is 80.00 mass %, makes ZrO2Powder is 20.00 mass %, also, is made
Firing temperature (maximum temperature) is 1580 DEG C, in addition, in the same manner as above-mentioned comparative example 1 involved by comparison example 2
Ceramic matrix.
(evaluation)
The confirmation ＞ of ＜ crystalline phases
Each first ceramic matrix of embodiment 1~12 and comparative example 1 and 2 is identified by X-ray diffraction.As
Whether the determinating reference of crystalline phase is included, for the intensity of the main peak (104 crystal face) of aluminum oxide, with more than 3%
Main peak intensity.Namely based on the main peak relative to aluminum oxide intensity have more than 3% main peak intensity position (peak position) and
Miller indices and lattice constant etc., confirm included crystalline phase.
＜ bending strengths ＞
4 bending strength tests based on JISR1601, at room temperature to each of embodiment 1~12 and comparative example 1~2
Second ceramic matrix is measured.
＜ Young's modulus ＞
Static modulus of elasticity test method based on JISR1602, at room temperature to embodiment 1~12 and comparative example 1~
2 each 3rd ceramic matrix is measured.
＜ relative dielectric constants ＞
Using JISC2138 electrostatic capacity, when frequency at room temperature is 1MHz, to embodiment 1~12 and ratio
Each 3rd ceramic matrix compared with example 1~2 is measured.
＜ dielectric loss angle tangents ＞
Using JISC2138 electrostatic capacity, when frequency at room temperature is 1MHz, to embodiment 1~12 and ratio
Each 3rd ceramic matrix compared with example 1~2 is measured.
The detailed content of embodiment 1~12 and comparative example 1 and 2 is shown in table 3, evaluation result is shown in table 4.In table 4,
The relative dielectric constant of electrical characteristic is recited as to " dielectric loss angle tangent is recited as " tan δ " by ε r ".
Table 3
Table 4
For embodiment 1~12, bending strength (rupture strength) is more than 650MPa, Young's modulus be 300GPa with
Under.In addition, the Al of sintered body2O3Crystallization particle diameter be 0.7~3.0 μm, ZrO2Crystallization particle diameter be 0.05~1.0 μm.
Also, for embodiment 1, as crystalline phase, except Al3O4And ZrO2In addition, Mn is only observed3Al2(SiO4)3。
Because this relation, electrical characteristic, particularly dielectric loss angle tangent are 170, poorer than other embodiments 2~12.On machinery
Characteristic, bending strength is up to 720MPa, Young's modulus as little as 268GPa, obtains good result.
For embodiment 12, the bending strength in mechanical property is 1030MPa, as a result best in embodiment 1~12.
For embodiment 9, the Young's modulus in mechanical property is 249GPa, as a result best in embodiment 1~12.For embodiment 3
And 10, the dielectric loss angle tangent in electrical characteristic is 17 and 15, as a result best in embodiment 1~12.
For embodiment 2,4~8,11, the scope of the bending strength in mechanical property is 700~910MPa, mechanical property
In Young's modulus scope be 255~300GPa, as a result well.The scope of dielectric loss angle tangent in electrical characteristic is also
20~40, as a result well.
It should illustrate, for embodiment 6, as crystalline phase, except Al3O4And ZrO2In addition, it was further observed that MgAl2O4And
BaAl2Si2O8。
On the other hand, for comparative example 1 and 2, as crystalline phase, except Al3O4And ZrO2In addition, it is not observed other
Crystalline phase.On mechanical property, for comparative example 1, bending strength ratio embodiment 10 is high, is 970MPa, still, and Young's modulus is high
Up to 336GPa.It is 650MPa although bending strength ratio embodiment 1 is low, Young's modulus is up to 324GPa for comparative example 2.
It should illustrate, ceramic matrix and its manufacture method involved in the present invention is not limited to above-mentioned embodiment, not take off
On the premise of present subject matter, it is of course possible to constituted using various.
Claims (8)
1. a kind of ceramic matrix, it is characterised in that
The crystalline phase of the ceramic matrix is with Al2O3And ZrO2For main crystalline phase, in addition, Mn is included3Al2(SiO4)3Or
MgAl2O4,
And the bending strength of the ceramic matrix is more than 650Ma, Young's modulus is below 300GPa.
2. ceramic matrix according to claim 1, it is characterised in that
The bending strength of the ceramic matrix is 650MPa~1100MPa, and Young's modulus is 240GPa~300GPa.
3. ceramic matrix according to claim 1, it is characterised in that
The dielectric loss angle tangent of the ceramic matrix is 200 × 10 in 1MHz- 4Hereinafter, relative dielectric constant is 10~15.
4. ceramic matrix according to claim 1, it is characterised in that
The ceramic matrix is sintered for 1250~1500 DEG C in temperature.
5. ceramic matrix according to claim 1, it is characterised in that
The ceramic matrix is included：By Al2O3Conversion is calculated as 70.0~90.0 mass % Al, by ZrO2Conversion is calculated as 10.0~
30.0 mass % Zr, Al2O3And ZrO2Add up to 100 mass % in the case of, comprising：2.0~7.0 are calculated as by MnO conversions
Quality % Mn, by SiO2Conversion be calculated as 2.0~7.0 mass % Si, by BaO convert be calculated as 0.5~2.0 mass % Ba,
Converted by MgO and be calculated as 0~2.0 mass % Mg.
6. a kind of manufacture method of ceramic matrix, it is characterised in that including following process：
The formed body production process of formed body is made, the formed body contains by Al2O3Conversion is calculated as 70.0~90.0 mass %'s
Al, by ZrO2Conversion is calculated as 10.0~30.0 mass % Zr, Al2O3And ZrO2Add up to 100 mass % in the case of, contain
Have and be calculated as 2.0~7.0 mass % Mn, by SiO by MnO conversions2Conversion is calculated as 2.0~7.0 mass % Si, converted by BaO
It is calculated as 0.5~2.0 mass % Ba, being converted by MgO is calculated as 0~2.0 mass % Mg；
By the formed body in 1250~1500 DEG C of firing process burnt till.
7. the manufacture method of ceramic matrix according to claim 6, it is characterised in that
After the formed body production process, the process that the conductor layer comprising metal is formed on the formed body is additionally included in,
In the firing process, the formed body for being formed with the conductor layer is burnt till.
8. the manufacture method of ceramic matrix according to claim 6, it is characterised in that
The firing process is carried out in hydrogen content is more than 5% hydrogen and the forming gas of nitrogen.
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| CN110483088A (en) * | 2019-09-10 | 2019-11-22 | 四川广通碳复合材料有限公司 | A kind of leaching copper carbon slipper and preparation method thereof |
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| WO2023163066A1 (en) * | 2022-02-28 | 2023-08-31 | 京セラ株式会社 | Ceramic wiring board, electronic device and electronic module |
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| JPWO2016098767A1 (en) | 2017-09-28 |
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| JP6632995B2 (en) | 2020-01-22 |
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