CN106986665A - 99.6% Al of thin film integrated circuit2O3The preparation method of ceramic substrate - Google Patents
99.6% Al of thin film integrated circuit2O3The preparation method of ceramic substrate Download PDFInfo
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- CN106986665A CN106986665A CN201710305151.1A CN201710305151A CN106986665A CN 106986665 A CN106986665 A CN 106986665A CN 201710305151 A CN201710305151 A CN 201710305151A CN 106986665 A CN106986665 A CN 106986665A
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- 239000000758 substrate Substances 0.000 title claims abstract description 94
- 239000000919 ceramic Substances 0.000 title claims abstract description 49
- 239000010409 thin film Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 33
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 30
- 239000011521 glass Substances 0.000 claims description 64
- 238000004528 spin coating Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005498 polishing Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 239000002002 slurry Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- 229910052681 coesite Inorganic materials 0.000 claims description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
- 229910052682 stishovite Inorganic materials 0.000 claims description 11
- 229910052905 tridymite Inorganic materials 0.000 claims description 11
- 238000007766 curtain coating Methods 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 7
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 7
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001856 Ethyl cellulose Substances 0.000 claims description 6
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229920001249 ethyl cellulose Polymers 0.000 claims description 6
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 230000002238 attenuated effect Effects 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000003475 lamination Methods 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims 1
- 238000003801 milling Methods 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 1
- 230000003746 surface roughness Effects 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 description 9
- 238000002844 melting Methods 0.000 description 8
- 230000008018 melting Effects 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 5
- 238000013461 design Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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- 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
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/77—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate
- H01L21/78—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices
- H01L21/82—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components
- H01L21/84—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components the substrate being other than a semiconductor body, e.g. being an insulating body
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention provides thin film integrated circuit 99.6%Al2O3The preparation method of ceramic substrate.Thin film integrated circuit 99.6%Al provided by the present invention2O3The preparation method of ceramic substrate can reduce substrate surface roughness, finish and flatness be improved, so that thin film circuit precision, reliability are improved, with important practical value.Meanwhile, thin film integrated circuit 99.6%Al provided by the present invention2O3The preparation method of ceramic substrate has surface roughness small, and flatness is good, the advantages of finish is good, surface is in minute surface.
Description
Technical field
The present invention relates to thin film hybrid IC microwave-medium ceramics substrate field, in particular to film collection
Into circuit 99.6%Al2O3The preparation method of ceramic substrate.
Background technology
99.6%Al2O3Electronic ceramic substrate possesses high temperature resistant, electrical insulation capability height, dielectric loss is low, thermal conductivity is big, change
The advantages of learning strong stability and element similar thermal expansion coefficient, thus it is widely used in thickness/thin film hybrid IC and each
Plant in film component.
But, because 99.6% alumina ceramic substrate hardness is high, crystal grain is big, by working process meron any surface finish
Degree difficulty reaches mirror effect (0.02 μm of <), and even across the ceramic substrate of mechanical thinning and polishing, surface still has micron order
Cavity, causes thin film circuit hole, defect and electrode deterioration, broken string or short circuit easily occur, and have a strong impact on thin film circuit can
By property.With developing rapidly for microwave device, Micrometer-Nanometer Processing Technology is maked rapid progress, the design requirement aluminum oxide of film component
Ceramic substrate has the surface roughness of preferable finish and very little, so as to meet nano level circuit line width.Through mechanical reduction
Though the alumina substrate of polishing can meet the requirement of general circuit design, its line width can not meet nano level thin film circuit will
Ask.Handled accordingly, it would be desirable to which further finishing is done on the alumina ceramic substrate surface after to being thinned again, reduce surface roughness
So as to reach mirror effect.
At present, alumina ceramic substrate is not in addition to surface roughness reaches thin film circuit design requirement, nearly all property
Design requirement can be met, to solve this problem, mainly using traditional cmp method.Chemical machinery is thrown
Although light can reduce the roughness of substrate surface, because alumina substrate hardness is larger, the roughness after polishing also can only
0.04~0.05 μm is reached, mirror effect is not obvious, and the more cost height of the polishing fluid consumed, the long efficiency of polishing time are very
It is low, through experiment statisticses, 1 99.6%Al of polishing2O3The time of ceramic substrate is more than 2h.Simultaneously, although in the prior art
There is the method for depositing thin film in substrate surface using special technological means, however, equipment needed for existing method is expensive, skill
Art is complicated and cost is higher, is not suitable for actual production application.
Therefore, the process of surface treatment and performance indications of existing alumina ceramic substrate are all difficult to meet high performance thin film device
The application demand of part/circuit, urgent need seek a kind of new technology, improve its surface roughness, finish, with meet thin-film device/
Substrate requirements of the circuit to highly reliable, inexpensive apperance quality.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of thin film integrated circuit 99.6%Al2O3The preparation side of ceramic substrate
Method, methods described passes through in 99.6%Al2O3Ceramic substrate surface carries out mirror surface treatment, so as to reduce the table of ceramic substrate
Surface roughness, improves the finish of substrate.
The second object of the present invention is to provide a kind of described thin film integrated circuit 99.6%Al2O3Ceramic substrate, this
The there is provided ceramic substrate of invention has the advantages that surface roughness is small, highly polished, and suitable for nano-level thin-membrane circuit etc.
In precise electronic component.
Third object of the present invention is to provide a kind of comprising the thin film integrated circuit 99.6%Al2O3Ceramic base
The electronic component of piece.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme:
A kind of thin film integrated circuit 99.6%Al2O3The preparation method of ceramic substrate, methods described comprises the following steps:
(a) 99.6%Al2O3It is prepared by ceramic substrate
According to Al2O3, MgO and SiO2Mass ratio is 99.6%:0.3%:0.1% ratio carries out dispensing, then by gained
Material and agate ball and deionized water ball milling mixing, and gained slurry drying is sieved;
Drying and screening resulting material and organic solvent and adhesive are mixed with curtain coating material, then flow casting molding obtains oxygen
Change aluminium green band, gained aluminum oxide green band is obtained into 99.6%Al through lamination, isostatic pressed, cutting and dumping sintering2O3Ceramic base
Piece, is then thinned, polishes, and ultrasonic washing, obtains pending alumina ceramic substrate;
(b) prepared by high softness number glass dust
According to mass percent CaO 10~30%, Al2O30~18.3%, SiO254.93~74.93%, and glass
The ratio of glass additive 10~25% carries out dispensing, resulting material then is obtained into vitreum through high-temperature water quenching, by gained glass
Body vibration is crushed, and glass powder is obtained after then adding decentralized medium ball milling, drying and screening;
(c) prepared by glass paste
Organic carrier is dissolved in a solvent, glass powder is then added into resulting solution, and it is dispersed, obtain glass
Glass slurry;
(d) spin coating
In pending alumina ceramic substrate surface spin-coating glass slurry, then gained substrate is dried;
(e) it is heat-treated
Substrate after drying is placed in Muffle furnace and is heat-treated, the high alumina ceramic-base of surface smoothness is obtained
Piece, as thin film integrated circuit 99.6%Al2O3Ceramic substrate.
Optionally, in the present invention, in step (a), the mass ratio of material, agate ball and deionized water is (1~2):(1
~2):(1~2);
And/or, the rotational speed of ball-mill of ball milling mixing described in step (a) is 350~450rpm, and the time is 5~6h.
Optionally, in the present invention, attenuated polishing described in step (a) is to gained 99.6%Al2O3Ceramic substrate it is two-sided
Carry out attenuated polishing;
It is preferred that, it is thinned, polishes, and the thickness of the pending alumina ceramic substrate of gained is less than 1mm after ultrasonic washing,
Thickness and precision and uniformity are less than ± 3 μm.
Optionally, in the present invention, glass additive described in step (b) is BaO, MgO, ZnO, Sb2O3Or B2O3In
One or more of mixtures.
Optionally, in the present invention, decentralized medium described in step (b) is organic solvent, it is preferred that the decentralized medium is
Ethanol solution;
And/or, the rotating speed of ball milling described in step (b) is 350~450rpm, and the time is 2~4h.
Optionally, in the present invention, the organic carrier of stating of institute is ethyl cellulose, acrylic resin in step (c), or poly- second
Enol butyral;
The solvent is the mixed solvent of terpinol and butyl carbitol;
It is preferred that, the mass ratio of the terpinol, butyl carbitol and organic carrier is (35~48):(33~49):(4
~15).
Optionally, it is the method spin-coating glass slurry using spin coating in the present invention, in step (d);
It is preferred that, the speed of spin coating is 500~1500rpm, and the time is 10~20s, and number of times is 1~6 time.
Optionally, in the present invention, heat treatment described in step (e) specifically includes following steps:By Muffle furnace first by room
Temperature is warming up to 500~600 DEG C, and the heating-up time is controlled in 6~8h;Then 900~1000 DEG C are warming up to again, and heating-up time control exists
2~3h;1150~1300 DEG C are then heated to, the heating-up time is controlled in 80~90min;It is incubated furnace cooling after 30~45min.
Meanwhile, present invention also offers the thin film integrated circuit 99.6%Al as made from the method for the invention2O3Ceramics
Substrate.
Further, present invention also offers include thin film integrated circuit 99.6%Al of the present invention2O3Ceramic substrate
Electronic component.
Compared with prior art, beneficial effects of the present invention are:
In the present invention, by carrying out reduction processing to the aluminium oxide ceramics for sintering porcelain into, removing substrate surface sintering will not
Close and uneven part, and by spin coating and heat treatment mode in substrate surface one layer of uniform glass glazings of formation, so that
Further improve the surface smoothness of substrate;
Meanwhile, CaO-Al of the present invention2O3-SiO2Glass has high softening point, thermal coefficient of expansion and Al2O3It is close
The features such as, for traditional silk screen print method, it is coated using the method for spin coating, thickness pole smooth with surface
Thin and equal first-class advantage;The aluminium oxide ceramics of surface ultra-smooth can be obtained after heat treatment, and this is to essences such as thin film integrated circuits
The design and assembling of close electronic component and further apply, it may have important practical is worth
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 is the 99.6%Al of non-spin-coating glass glaze2O3Ceramic substrate;
Fig. 2 is spin-coated glass-glazed 99.6%Al2O3Ceramic substrate.
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
In view of current deficiency of the existing alumina ceramic substrate in performance and preparation technology, in alumina ceramic substrate
Field related researcher has made intensive studies in terms of substrate surface treatment, and common method is except polishing processes, also table
Finishing coat method, coating technology mainly has chemical vapor deposition (CVD), physical vapour deposition (PVD) (PVD), hot spray process, silk-screen printing
Method, sol-gal process etc., with the development of advanced ceramics glaze technology, glass glaze technology has been applied to the preparation of insulating barrier, electricity
The encapsulation field of sub- device.Glass glaze is to be melted in one layer of substrate surface very thin uniform vitreous substance, with smooth
Light, high mechanical strength, chemical property is stable, the features such as matching good with substrate, but at present both at home and abroad for aluminium oxide ceramics
Substrate surface applies the report of high temp glass glaze seldom, and the present invention also exactly in this context, by correlative study and experiment, is proposed
A kind of small, the highly polished 99.6%Al of surface roughness2O3Ceramic substrate preparation method, specifically, the inventive method is included such as
Lower step:
1st, 99.6%Al2O3It is prepared by ceramic substrate
1.1st, according to Al2O3, MgO and SiO2Mass ratio is 99.6%:0.3%:0.1% ratio carries out dispensing, then will
Resulting material and agate ball and deionized water ball milling mixing;
It is preferred that, the mass ratio of material, agate ball and deionized water is (1~2):(1~2):(1~2);It is furthermore preferred that
The mass ratio of material, agate ball and deionized water is 1:2:1;
It is preferred that, in this step, after each raw material is weighed by proportioning, the ball milling mixing carried out in agate pot;
It is preferred that, the rotational speed of ball-mill of the ball milling mixing is 350~450rpm, and the time is 5~6h;The preferred ball
The rotational speed of ball-mill of mill mixing is 387rpm, and the time is 6h;
After ball milling, gained slurry is poured out, and drying and screening;
It is preferred that, the drying is drying, and gained slurry is dried under the conditions of 90 DEG C of constant temperature through 48h, then crosses 100
Eye mesh screen;
1.2nd, resulting material after drying and screening and organic solvent and adhesive are mixed with curtain coating material, are cast the preparation of material
The preparation technology of conventional curtain coating material is may be referred to, organic solvent used can be the organic solvents, adhesive therefor such as toluene, ethanol
Can be the adhesives such as PVB;
Aluminum oxide green band is made by doctor-blade casting process in curtain coating material, and gained aluminum oxide green band is through lamination, isostatic pressed
And after cutting action processing, obtain square oxidation aluminium bars block, the oxidation aluminium bars block of forming is placed in high temperature sintering furnace and carried out
Dumping is sintered, that is, obtains 99.6%Al2O3Ceramic substrate;
It is preferred that, dump temperature is 600 DEG C, is incubated 4h, sintering temperature is 1580 DEG C, and is incubated 2h;
Then, by gained 99.6%Al2O3Ceramic substrate is through being thinned, polishing, and leakiness is sintered and recessed to remove sample surfaces
Convex uneven part;
It is preferred that, it is described to be thinned, be finished to gained 99.6%Al2O3The two-sided carry out attenuated polishing of ceramic substrate;
After being thinned and polishing, ultrasonic wave cleaning is carried out to ceramic substrate, pending alumina ceramic substrate, gained is obtained
The thickness of substrate is less than 1mm, and thickness and precision and uniformity are less than ± 3 μm, and roughness is less than 0.1 μm;
It is preferred that, the time control of cleaning is in 30min or so;
2nd, prepared by high softness number glass dust
Due to CaO-Al2O3-SiO2Glass has higher fusing point (more than 1100 DEG C), and and 99.6%Al2O3Ceramics
Thermal coefficient of expansion is approached, and thermal coefficient of expansion is 6~8 × 10-6/ DEG C in the range of;Therefore the present invention selectes CaO-Al2O3-SiO2It is glass
Glass glaze, and according to ternary phase diagrams, according to mass percent CaO 10~30%, Al2O30~18.3%, SiO254.93~
74.93%, and glass additive 10~25% ratio carry out dispensing;Further it can also be changed by adjusting glass formula
Become glass softening point, so that suitable for being heat-treated at different temperatures;
It is preferred that, the glass additive is BaO, MgO, ZnO, Sb2O3Or B2O3In one or more of mixing
Thing;
Load weighted material is placed in ball grinder, and ball milling mixing;Then the dispensing after ball milling is loaded into Cinker clew furnace
In corundum crucible, the melting generation glass in high temperature Cinker clew furnace, melting pours into Quenching Treatment in deionized water after finishing, obtains nothing
The transparent vitreum of color, i.e., prepare vitreum using the method for high-temperature water quenching (high-temperature fusion water quenching);By gained vitreum vibration
Crush, glass powder is obtained after then adding decentralized medium ball milling, drying and screening;
It is preferred that, the decentralized medium is organic solvent, it is preferred that the decentralized medium is ethanol solution;
It is preferred that, the rotating speed of the ball milling is 350~450rpm, and the time is 2~4h, and sieving mesh size used is 300
Mesh;It is furthermore preferred that the rotating speed of ball milling is 387rpm, the time is 2~4h, and the mesh stainless steel mesh of descendants 300 is sieved after the drying
Get glass powder;
3rd, prepared by glass paste
It is to be formulated with airborne liquid solution first in this step, it is preferred that be to add organic carrier to be loaded into the molten of beaker
In agent, then, 1~3h of stirring is dissolved in the case of 50~80 DEG C of heating water baths;
It is preferred that, organic solvent used is terpinol and butyl carbitol;It is preferred that, organic carrier used is ethyl cellulose
Element, acrylic resin, or polyvinyl butyral resin;
It is further preferred that terpinol, butyl carbitol and organic carrier (i.e. ethyl cellulose, acrylic resin, or
Polyvinyl butyral resin) mass ratio be (35~45):(33~44):(4~15);
Then, the glass powder prepared by step 2 is placed in dispersed with stirring in beaker by the proportioning of solid content 40%~60%
Uniformly, glass paste is made, obtained glass slurry suspension preferably, is uniformly dispersed, is adapted on alumina ceramic substrate
Carry out spin coating;
4th, spin coating
In pending alumina ceramic substrate surface spin-coating glass slurry, it is preferred that in this step, using the method for spin coating
Spin-coating glass slurry, and make it that substrate surface is smooth, uniform;
It is preferred that, the speed of spin coating is 500~1500rpm, and the time is 10~20s, and number of times is 1~6 time, it is possible to according to
Need the number of times of control spin coating;
Then gained substrate is dried, it is preferred that the drying toasts 3min to place the substrate on hot plate, the temperature of hot plate
Degree control is at 130~200 DEG C;
5th, it is heat-treated
Substrate after drying is placed in Muffle furnace and is heat-treated, after heat treatment, the glass paste of spin coating can be in base
Piece surface forms one layer of glass glaze, and finish is higher, and surface roughness is less than 0.01 μm, and substrate thickness precision is less than ± 2 μm, i.e.,
For thin film integrated circuit 99.6%Al2O3Ceramic substrate;
It is preferred that, heat treatment comprises the following steps:By Muffle furnace first by room temperature to 500~600 DEG C, heating-up time
Control is in 6~8h;Then 900~1000 DEG C are warming up to again, and the heating-up time is controlled in 2~3h;Then heat to 1150~1300
DEG C, the heating-up time is controlled in 80~90min;It is incubated furnace cooling after 30~45min;
It is furthermore preferred that heat treatment heating step is as follows:Muffle furnace is first by room temperature to 600 DEG C, heating-up time control
In 8h;Then 1000 DEG C are warming up to again, and the heating-up time is controlled in 2h;Then heat to 1150~1300 DEG C, heating-up time control
In 80min;It is incubated furnace cooling after 30min.
As the Al prepared by as above method2O3Ceramic substrate surface roughness is small, and substrate thickness precision is high, thus suitable for making
For nano level film circuit board, so as to improve thin film circuit precision, reliability.Likewise, being used as base material or encapsulating material
And be used in other precise electronic components.
Embodiment 1
(1) dispensing, batch mixing
Raw material is according to 99.6%Al2O3- 0.3%MgO-0.1%SiO2Mass ratio carry out dispensing, by load weighted batch mixing,
Agate ball, deionized water are according to 1:2:1 ratio is put into ball milling mixing in agate pot;
Ball milling parameter is:Slurry is poured out after 387rpm, 6h, ball milling, inserts in baking oven and to be dried with 90 DEG C of constant temperature through 48 hours
It is dry, and cross 100 eye mesh screens;
(2) configuration curtain coating material
Organic solvent ethanol and toluene, and adhesive PVB are added in gained alumina powder after drying sieving, is obtained
Curtain coating material;
(3) it is cast, laminates
Using doctor-blade casting process, aluminum oxide green band is made by casting machine in curtain coating material, its thickness is 59 ± 1 μm, then
Lamination is carried out, the number of plies is 9 layers, then carries out obtaining square oxidation aluminium bars block after isostatic pressed and cutting action, thickness is 445 μm,
Size is 61 × 61mm;
(4) dumping, sintering
The oxidation aluminium bars block of forming is inserted into progress air atmosphere sintering in Muffle furnace, heating curve is:Room temperature 10h liters
To 600 DEG C, 4h is incubated, 3h rises to 1300 DEG C, then 2h rises to 1580 DEG C, is incubated 2h, and then 2h is down to furnace cooling after 1000 DEG C,
Obtain sintering into the 99.6%Al of porcelain2O3Ceramic substrate, its thickness is 350 μm, and size is 50.8 × 50.8mm;
(5) it is thinned
Two sides is carried out to the alumina substrate for sintering porcelain into thinned machine to be thinned and polishing, its surface sintering is removed not
Fine and close and uneven part, then ultrasonic wave cleaning 30min, obtain 300 μm of thickness, thickness and precision and uniformity less than ± 3 μm,
Surface roughness is less than 0.1 μm of ceramic substrate, and gained substrate is as shown in Figure 1;
(7) preparation of high temp glass powder
Glass each component raw material is constituted into dispensing in the mass fraction ratio in table 1;It is subsequently placed in ball grinder, ball milling 6h
So that each component is well mixed, after ball milling drying and 40 eye mesh screens are crossed;
The glass formula of table 1
Then the dispensing after ball milling is fitted into the corundum crucible of Cinker clew furnace, the melting generation glass in high temperature Cinker clew furnace,
Melting temperature is 1450 DEG C, and soaking time is 1h;Melting pours into Quenching Treatment in deionized water after finishing, and obtains water white transparency
Vitreum, then vibration is crushed, with alcohol as decentralized medium 387rpm 2~4h of ball milling, and 300 mesh stainless steels are crossed after drying and are sieved
To glass powder;
(8) preparation of glass paste
Ratio according to the form below 2 weighs organic solvent, ethyl cellulose, is placed in beaker, and in 80 DEG C of stirred in water bath
2h is to being completely dissolved, then, and it is uniform that glass powder is placed in into dispersed with stirring in beaker in the ratio of solid content 40%~60%
To glass paste;
The organic carrier of table 2 is matched
Organic solvent | Terpinol | Butyl click must alcohol | Ethyl cellulose |
W% | 44 | 46 | 10 |
(9) spin coating
The glass paste prepared is uniformly spin-coated on by alumina ceramic substrate table made from step (5) by sol evenning machine
Face, spin coating speed is 1000rpm, and the time is 20s, and spin coating number of times is 1 time, after spin coating is complete, and substrate is placed on hot plate and toasted
3min is stand-by;
(10) it is heat-treated
Substrate after spin coating is placed in Muffle furnace and is heat-treated, heat treatment cycle curve is:Room temperature 8h to 600 DEG C, then 2h
1000 DEG C are risen to, the furnace cooling after 80min rises to 1200 DEG C, insulation 30min produces thin film integrated circuit 99.6%Al2O3
Ceramic substrate;
The thickness of gained substrate is 303 μm, i.e. after heat treatment its thickness is 3 μm, thickness to the glass glazings that spin coating is 1 time
Precision is ± 2 μm, and surface roughness is 0.008 μm;
Preferably, its surface texture is as shown in Fig. 2 wherein white portion reaches gained substrate surface finish for substrate surface
Mirror effect back reflection light.
Embodiment 2
Change the component of glass:According to basic components, in CaO-Al2O3-SiO2Glass mutually forms interval change and wherein added
The component and content of agent, such as following table:
The modified glass formula of table 3 is designed
Then dispensing is fitted into the corundum crucible of Cinker clew furnace, melting generation glass, melting temperature in high temperature Cinker clew furnace
1500 DEG C are changed to, soaking time is 1h.Melting pours into Quenching Treatment in deionized water after finishing, and obtains the glass of water white transparency
Body.Glass paste is prepared into after ball milling, then glass paste is uniformly spin-coated on after substrate surface by spin coating and carries out hot place
Reason, heat treatment temperature is changed to 1250 DEG C, and other process conditions are constant, specific operation process be the same as Example 1.
Substrate surface after heat treatment is highly polished, into mirror effect, and surface roughness is 0.007 μm, and substrate thickness is
303 μm, thickness and precision is ± 2 μm.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of thin film integrated circuit 99.6%Al2O3The preparation method of ceramic substrate, it is characterised in that methods described includes
Following steps:
(a) 99.6%Al2O3It is prepared by ceramic substrate
According to Al2O3, MgO and SiO2Mass ratio is 99.6%:0.3%:0.1% ratio carries out dispensing, then by resulting material
With agate ball and deionized water ball milling mixing, and gained slurry drying is sieved;
Drying and screening resulting material and organic solvent and adhesive are mixed with curtain coating material, then flow casting molding obtains aluminum oxide
Green band, 99.6%Al is obtained by gained aluminum oxide green band through lamination, isostatic pressed, cutting and dumping sintering2O3Ceramic substrate,
Then it is thinned, polishes, and ultrasonic washing, obtain pending alumina ceramic substrate;
(b) prepared by high softness number glass dust
According to mass percent CaO 10~30%, Al2O30~18.3%, SiO254.93~74.93%, and glass adds
Plus the ratio of agent 10~25% carries out dispensing, and resulting material then is obtained into vitreum through high-temperature water quenching, gained vitreum is shaken
Milling is broken, and glass powder is obtained after then adding decentralized medium ball milling, drying and screening;
(c) prepared by glass paste
Organic carrier is dissolved in a solvent, glass powder is then added into resulting solution, and it is dispersed, obtain glass paste
Material;
(d) spin coating
In pending alumina ceramic substrate surface spin-coating glass slurry, then gained substrate is dried;
(e) it is heat-treated
Substrate after drying is placed in Muffle furnace and is heat-treated, the high alumina ceramic substrate of surface smoothness is obtained, i.e.,
For thin film integrated circuit 99.6%Al2O3Ceramic substrate.
2. preparation method according to claim 1, it is characterised in that in step (a), material, agate ball and deionized water
Mass ratio be (1~2):(1~2):(1~2);
And/or, the rotational speed of ball-mill of ball milling mixing described in step (a) is 350~450rpm, and the time is 5~6h.
3. preparation method according to claim 1, it is characterised in that attenuated polishing described in step (a) is to gained
99.6%Al2O3The two-sided carry out attenuated polishing of ceramic substrate;
It is preferred that, it is thinned, polishes, and the thickness of the pending alumina ceramic substrate of gained is less than 1mm, thickness after ultrasonic washing
Precision and uniformity are less than ± 3 μm.
4. preparation method according to claim 1, it is characterised in that glass additive described in step (b) be BaO,
MgO, ZnO, Sb2O3Or B2O3In one or more of mixtures.
5. preparation method according to claim 4, it is characterised in that decentralized medium described in step (b) is organic solvent,
It is preferred that, the decentralized medium is ethanol solution;
And/or, the rotating speed of ball milling described in step (b) is 350~450rpm, and the time is 2~4h.
6. preparation method according to claim 1, it is characterised in that organic carrier described in step (c) is ethyl cellulose
Element, acrylic resin, or polyvinyl butyral resin;
The solvent is the mixed solvent of terpinol and butyl carbitol;
It is preferred that, the mass ratio of the terpinol, butyl carbitol and organic carrier is (35~48):(33~49):(4~
15)。
7. preparation method according to claim 1, it is characterised in that be the method spin coating glass using spin coating in step (d)
Glass slurry;
It is preferred that, the speed of spin coating is 500~1500rpm, and the time is 10~20s, and number of times is 1~6 time.
8. preparation method according to claim 1, it is characterised in that heat treatment specifically includes as follows described in step (e)
Step:By Muffle furnace first by room temperature to 500~600 DEG C, the heating-up time is controlled in 6~8h;Then it is warming up to 900 again~
1000 DEG C, the heating-up time is controlled in 2~3h;1150~1300 DEG C are then heated to, the heating-up time is controlled in 80~90min;Protect
Furnace cooling after 30~45min of temperature.
9. thin film integrated circuit 99.6%Al made from the method according to any one of claim 1-82O3Ceramic substrate.
10. comprising thin film integrated circuit 99.6%Al described in claim 92O3The electronic component of ceramic substrate.
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