CN102503378B - Thin chip ceramic substrate and manufacturing method thereof - Google Patents
Thin chip ceramic substrate and manufacturing method thereof Download PDFInfo
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- CN102503378B CN102503378B CN 201110311509 CN201110311509A CN102503378B CN 102503378 B CN102503378 B CN 102503378B CN 201110311509 CN201110311509 CN 201110311509 CN 201110311509 A CN201110311509 A CN 201110311509A CN 102503378 B CN102503378 B CN 102503378B
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Abstract
The invention relates to a thin chip ceramic substrate and a manufacturing method thereof. The thin chip ceramic substrate is prepared from a ceramic raw material, a solvent, a binder, and a plasticizer-dispersant mixture, wherein the ceramic raw materials comprise (by weight percentages) calcined alpha-alumina micropowders of D50 0.5-2.0 mum 96-97, talc powders of average particle size 0.6-5.0 mum 2.0-3.5, and rare earth oxide super micro powders 0.5-1.0; the solvent is an organic mixed solvent 20-40% of the ceramic raw material weight; the binder weight is 4-8% of the ceramic raw material weight; and the plasticizer-dispersant mixture weight is half of the binder weight. The invention adds a rare earth oxide in a substrate, so that physicochemical properties and mechanical properties of the substrate are improved.
Description
Technical field
The invention belongs to electronics novel material manufacturing technology field, relate to a kind of aluminium oxide ceramic substrate, ceramic substrate and manufacture method thereof that especially a kind of plate resistor is used.
Background technology
Alumina-ceramic is Application Areas one of stupalith the most widely, and it is widely used in various domestic ceramicses, fine ceramics etc.At present, alumina-ceramic is also extensively adopted in the ceramic substrate field, and the weight ratio by alumina composition in ceramic product is divided into middle aluminium porcelain, alumina porcelain, 85 porcelain, 90 porcelain, 95 porcelain etc. usually.Mostly plate resistor is the 90 above high alumina content potteries of porcelain with ceramic substrate, and this class pottery has good general performance on mechanical property, heat conductivility, dielectric properties and cost performance.But along with people to miniaturization of electronic products, chip types such as mobile phone, LTCC module, multi-chip module, osophone, become more meticulous and the improving constantly of the demand such as multifunction, especially under the surging promotion such as Mobile Communications Market, Medical Device Market, the electronic devices and components such as plate resistor are rapidly to miniaturization, surface mount future development." size is less, with better function " promoting plate resistor to miniaturization, chip type and high-accuracy future development.Simultaneously, overall characteristic and the accuracy that hinders the thin chip ceramic substrate of base carrier material as sheet proposed more and more harsh requirement, specific requirement is mainly reflected in table 1:
Table 1
Yet 96 porcelain of conventional process techniques can only satisfy the conventional need of table 1 usually, are difficult to satisfy simultaneously the Secretaries such as volume density, bending strength, thermal conductivity, tolerance of dimension, Flatness.
Summary of the invention
Defects for conventional process techniques exists the present invention proposes a kind of thin chip ceramic substrate and manufacture method thereof.
The present invention takes following technical scheme: thin chip ceramic substrate, and it is made by following material: ceramic raw material, solvent, binding agent, plasticising and dispersion mixt, wherein:
The proportioning of ceramic raw material: weight ratio 96-97% and D50 are the calcining Alpha-alumina micro mist of 0.5-2.0 μ m, and weight ratio 2.0-3.5% and mean particle size be at the talcum powder of 0.6-5.0 μ m, the rare earth oxide super-fine powder of weight ratio 0.5-1.0%;
Solvent is organic mixed solvent of the 20-40% of ceramic raw material weight;
Weight of binder is the 4-8% of ceramic raw material weight;
Plasticising and dispersion mixt weight are half of binding agent.This plasticising and dispersion mixt can be mixed by PEG, DOP commonly used, fish oil etc.
(annotate: above-mentioned D50:D refers to that the diameter of powder granule, D50 represent the diameter of 50% of accumulative total, or claims 50% by particle diameter, and D50 claims again median size or meso-position radius.)
Preferably, rare earth oxide is selected from: one or more mixtures of lanthanum-oxides, cerium oxide or praseodymium oxide are selected from as rare earth oxide: lanthanum sesquioxide, cerous oxide, cerium dioxide or Praseodymium trioxide.
Preferably, solvent is toluene-propyl carbinol and/or dehydrated alcohol.
Preferably, binding agent is PVB and/or PVA.
The invention also discloses a kind of manufacture method of thin chip ceramic substrate, it carries out as follows:
Batching: the proportioning of ceramic raw material: weight ratio 96-97% and D50 are the calcining Alpha-alumina micro mist of 0.5-2.0 μ m, and weight ratio 2.0-3.5% and mean particle size be at the talcum powder of 0.6-5.0 μ m, the rare earth oxide super-fine powder of weight ratio 0.5-1.0%;
Wet-milling: adopt the wet ball-milling mode to mix, wherein, solvent is organic mixed solvent of the 20-40% of ceramic raw material gross weight, after once levigate, add again the binding agent of the 4-8% of ceramic raw material gross weight, and weight is half plasticising and dispersion mixt of binding agent, obtains the standby slurry of curtain coating after the secondary mix grinding;
Deaeration-casting method slivering: curtain coating becomes the thin chip ceramic substrate strip of certain thickness, width, carries out vacuum defoamation before curtain coating and processes;
Punch forming: punching becomes the thin chip ceramic substrate blank of certain length and width specification;
Row glue-burns till: make the thin chip ceramic substrate workprint;
Tempering: the thin chip ceramic substrate workprint is carried out 1150-1400 ℃/(1-6) the laminated type temper of hr.
After tempering step, if do not carry out the unit wires impression in the punch forming process, adopt the laser scribing mode to carry out the unit wires etching.As for 0201 and ting model specification more, can obstructed overshoot superzapping trace and adopt the laser scribing mode to carry out the unit wires etching.
Preferably, after deaeration, curtain coating slivering thickness can be selected 0.1-1.2mm as required; The punching size can be selected 0.2-150mm according to using needs.
Preferably, the sticking step of row is the hr of normal temperature to 700 ℃/(2-10), burns till step and be 1500-1700 ℃/(0.1-5) hr, and the product that burn till are made the thin chip ceramic substrate workprint after through the polishing washing.
Preferably, rare earth oxide is selected from: one or more mixtures of lanthanum-oxides, cerium oxide or praseodymium oxide are selected from as rare earth oxide: lanthanum sesquioxide, cerous oxide, cerium dioxide or Praseodymium trioxide; Described solvent is toluene-propyl carbinol and/or dehydrated alcohol; Described binding agent is PVB and/or PVA.
Thin chip ceramic substrate of the present invention has added rare earth oxide, thereby has improved physicochemical property and the mechanical property of substrate in preparing burden, reached following technique effect: compactness 100%, volume density are at 3.75g/cm
3Above, folding strength is more than 350MPa.And in the manufacturing processed of thin chip ceramic substrate of the present invention, by one tempering process, not only improved the flatness of substrate, and control and reduced internal stress and the internal fissure of substrate.
Description of drawings
Fig. 1 is the X-ray diffraction figure as a result of thin chip ceramic substrate.
Embodiment
Below by embodiment, the present invention is elaborated, but application of the present invention is not limited to embodiment.
Embodiment one
Main raw material and ceramic formula: the D50 of 97% weight ratio is the calcining Alpha-alumina micro mist of 1.05 μ m, and the mean particle size of 2.3% weight ratio is at the talcum powder of 2.5 μ m, and the mean particle size of 0.7% weight ratio is 0.87 μ m lanthanum sesquioxide super-fine powder.
Other formula: amount of solvent is 31% of ceramic raw material gross weight, and solvent specifically weight ratio is the mixed solvent of the toluene-propyl carbinol-dehydrated alcohol of 4: 1: 2; Binding agent is 5.7% of ceramic raw material gross weight, adopts polyvinyl butyral acetal; Plasticising and dispersion mixt are according to the mobility adjustment of slurry, and its weight is half of binding agent.
Blending means: the mixing that ball milling 36hr is solvent and ceramic raw material and levigate, secondary ball milling 15-20hr (time can be grown a bit a little) is that mixing, the curtain coating characteristic of other supplementary material regulated and processed.
Deaeration-casting method slivering: under whipped state, after vacuum defoamation 1hr, it is the bar of 0.25mm that curtain coating becomes thickness, and the strip width is divided into 75mm.
Punch forming: punching becomes the blank of 71.5*58.7mm.
Row glue-burns till: the sticking step of row is normal temperature to 700 ℃/6hr, and burning till temperature rate after row is sticking is 110 ℃/hour, and firing temperature is 1600 ℃/3hr, and the product that burn till become the thin chip ceramic substrate workprint after washing through polishing.
Temper: the thin chip ceramic substrate workprint is carried out the laminated type tempering of 1350 ℃/2hr, temperature rate is controlled at 100 ℃/hour.
Laser ablation is optional as required, for 0201 and ting model specification more, and can obstructed overshoot superzapping trace and adopt the laser scribing mode to carry out the unit wires etching.
To the thin chip ceramic substrate that makes, the performance measurement outcome record such as its physics and chemistry, machinery, dielectric are at table 2, and the X-ray fluorescence spectra analytical results is recorded in table 3.
Table 2
| Project | Measurement result |
| Outward appearance and state | Fine and closely woven, white |
| Water-intake rate % | 0 |
| Volume density g/cm3 | 3.762 |
| Bending strength MPa | 382 |
| Linear expansivity (20-800) * 10-6 ℃ | 7.3 |
| Thermal conductivity W/mk, 20 ℃ | 24 |
| Disruptive strength KV/mm | 14 |
| Volume specific resistance Ω cm | 1015 |
| Specific inductivity, 1MHz | 9.5 |
| Dielectric loss angle tangent, 1MHz | 4×10-4 |
| Flat altar degree mm/mm2 | 0.08/300 |
Table 3
Embodiment two
Main raw material and ceramic proportioning: the D50 of 96% weight ratio is the calcining Alpha-alumina micro mist of 1.2 μ m, and the mean particle size of 3.3% weight ratio is at the talcum powder of 3.1 μ m, and the mean particle size of 0.7% weight ratio is 0.65 μ m Praseodymium trioxide super-fine powder.
Other formula: solvent is 27% of ceramic raw material gross weight, is toluene-propyl carbinol by the mixed solvent of 3: 1; Binding agent is 5.5% of ceramic raw material gross weight, and binding agent adopts polyvinyl butyral acetal; Plasticising and dispersion mixt are adjusted flexibly according to the mobility of slurry, weight be binding agent half.
Blending means: the mixing that ball milling 39hr is solvent and ceramic raw material and levigate, secondary ball milling 12-15hr is that mixing, the curtain coating characteristic of other supplementary material regulated and processed.
Deaeration-casting method slivering: under whipped state, after vacuum defoamation 30min, it is the bar of 0.5mm that curtain coating becomes thickness, and the strip width is divided into 87mm.
Punch forming: punching becomes blank substrate in the slim plate type pottery of 83.5*71.2mm.
Row glue-burns till: row's adhering process is normal temperature to 700 ℃/7hr, and burning till temperature rate after row is sticking is 100 ℃/hour, and firing temperature is 1570 ℃/3hr, and the product that burn till become the thin chip ceramic substrate workprint after washing through polishing.
Temper: the thin chip ceramic substrate workprint is carried out the laminated type tempering of 1280 ℃/3hr, temperature rate is controlled at 90 ℃/hour.
Measurement result to the thin chip ceramic substrate that makes is recorded in table 4.
Table 4
| Project | Measurement result |
| Volume density g/cm3 | 3.758 |
| Bending strength MPa | 357 |
| Thermal conductivity W/mk, 20 ℃ | 23 |
| Flat altar degree mm/mm2 | 0.07/420 |
Embodiment three
Main raw material and ceramic formula: the D50 of 96.5% weight ratio is the calcining Alpha-alumina micro mist of 1.9 μ m, and the mean particle size of 2.95% weight ratio is at the talcum powder of 1.2 μ m, and the mean particle size of 0.55% weight ratio is 0.8 μ m cerous oxide super-fine powder.
Other formula: solvent is 38% of ceramic raw material gross weight, is toluene-propyl carbinol by the mixed solvent of 8: 3; Binding agent is 7% of ceramic raw material gross weight, and composition is the PVB of 6: 4 weight ratios: the PVA mixture; Plasticising and dispersion mixt are adjusted flexibly according to the mobility of slurry, weight be binding agent half.
Blending means: the mixing that ball milling 42hr is solvent and ceramic raw material and levigate, secondary ball milling 10-15hr is that mixing, the curtain coating characteristic of other supplementary material regulated and processed.
Deaeration-casting method slivering: under whipped state, after vacuum defoamation 15min, it is the bar of 0.6mm that curtain coating becomes thickness, and the strip width is divided into 86mm.
Punch forming: punching becomes blank substrate in the slim plate type pottery of 83.8*71mm.
Row glue-burns till: the sticking step of row is normal temperature to 700 ℃/8hr, and burning till temperature rate after row is sticking is 100 ℃/hour, and firing temperature is 1650 ℃/90min, and the product that burn till become the thin chip ceramic substrate workprint after washing through polishing.
Temper: the thin chip ceramic substrate workprint is carried out the laminated type tempering of 1380 ℃/2hr, temperature rate is controlled at 80 ℃/hour.
Measurement result to the thin chip ceramic substrate that obtains is recorded in table 5.
Table 5
| Project | Measurement result |
| Volume density g/cm3 | 3.751 |
| Bending strength MPa | 368 |
| Thermal conductivity W/mk, 20 ℃ | 22 |
| Flat altar degree mm/mm2 | 0.06/420 |
Can be found out by the result of showing 2-5 embodiment, thin chip ceramic substrate of the present invention is in the comprehensive integral characteristic optimizing, and several key projects: the lifting of the indexs such as volume density, bending strength, thermal conductivity, Flatness is obvious.
Those of ordinary skill in the art should be familiar with; above-mentioned just explaining to the preferred embodiment of the present invention; and be not limitation of the invention, every in essential scope of the present invention, within all will falling into protection scope of the present invention to variation, the modification of above embodiment.
Claims (9)
1. thin chip ceramic substrate, it is made by following material: ceramic raw material, solvent, binding agent, plasticising and dispersion mixt, wherein:
The proportioning of ceramic raw material: weight ratio 96-97% and D50 are the calcining Alpha-alumina micro mist of 0.5-2.0 μ m, and weight ratio 2.0-3.5% and mean particle size be at the talcum powder of 0.6-5.0 μ m, the rare earth oxide super-fine powder of weight ratio 0.5-1.0%; Described rare earth oxide is selected from: one or more mixtures of lanthanum-oxides, cerium oxide or praseodymium oxide;
Solvent is organic mixed solvent of the 20-40% of ceramic raw material weight;
Weight of binder is the 4-8% of ceramic raw material weight;
Plasticising and dispersion mixt weight are half of weight of binder.
2. thin chip ceramic substrate as claimed in claim 1, it is characterized in that: described rare earth oxide is selected from: one or more mixtures of lanthanum sesquioxide, cerous oxide, cerium dioxide or Praseodymium trioxide.
3. thin chip ceramic substrate as claimed in claim 1, it is characterized in that: described solvent is toluene and propyl carbinol, toluene and dehydrated alcohol or toluene, propyl carbinol and dehydrated alcohol.
4. thin chip ceramic substrate as claimed in claim 1, it is characterized in that: described binding agent is PVB and/or PVA.
5. the manufacture method of thin chip ceramic substrate is characterized in that as follows:
Batching: the proportioning of ceramic raw material: weight ratio 96-97% and D50 are the calcining Alpha-alumina micro mist of 0.5-2.0 μ m, and weight ratio 2.0-3.5% and mean particle size be at the talcum powder of 0.6-5.0 μ m, the rare earth oxide super-fine powder of weight ratio 0.5-1.0%;
Wet-milling: adopt the wet ball-milling mode to mix, wherein, solvent is organic mixed solvent of the 20-40% of ceramic raw material gross weight, after once levigate, add again the binding agent of the 4-8% of ceramic raw material gross weight, and weight is half plasticising and dispersion mixt of binding agent, obtains the standby slurry of curtain coating after the secondary mix grinding;
Deaeration-casting method slivering: carry out vacuum defoamation before curtain coating and process, curtain coating becomes the thin chip ceramic substrate strip;
Punch forming: punching becomes the thin chip ceramic substrate blank;
Row glue-burns till: make the thin chip ceramic substrate workprint;
Tempering: the thin chip ceramic substrate workprint is carried out 1150-1400 ℃/(1-6) the laminated type temper of h.
6. the manufacture method of thin chip ceramic substrate as claimed in claim 5, is characterized in that: after tempering step, if do not carry out the unit wires impression in the punch forming process, adopt the laser scribing mode to carry out the unit wires etching.
7. the manufacture method of thin chip ceramic substrate as claimed in claim 5, it is characterized in that: after described deaeration, curtain coating slivering thickness is 0.1-1.2mm; Described punch forming is of a size of 0.2-150mm.
8. the manufacture method of thin chip ceramic substrate as claimed in claim 5, it is characterized in that: the sticking step of described row is the h of normal temperature to 700 ℃/(2-10), burn till step and be 1500-1700 ℃/(0.1-5) h, through making the thin chip ceramic substrate workprint after the polishing washing.
9. the manufacture method of thin chip ceramic substrate as claimed in claim 5, it is characterized in that: described rare earth oxide is selected from: one or more mixtures of lanthanum-oxides, cerium oxide or praseodymium oxide; Described solvent is toluene and propyl carbinol, toluene and dehydrated alcohol or toluene, propyl carbinol and dehydrated alcohol; Described binding agent is PVB and/or PVA.
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| CN107465395A (en) * | 2014-04-03 | 2017-12-12 | 深圳振华富电子有限公司 | A kind of lamination sheet type ceramic RF low pass filter and preparation method thereof |
| CN104230348B (en) * | 2014-09-05 | 2015-12-09 | 横店集团浙江英洛华电子有限公司 | LED semitransparent ceramics filament support and processing technology thereof |
| CN105906331A (en) * | 2016-05-26 | 2016-08-31 | 郑州中瓷科技有限公司 | Large-size ceramic substrate, and preparation method and production line thereof |
| CN108237441B (en) * | 2016-12-23 | 2020-07-28 | 蓝思科技（长沙）有限公司 | Processing method of 3D curved surface ceramic sheet and 3D curved surface ceramic sheet obtained by same |
| CN115784751B (en) * | 2022-12-05 | 2023-10-10 | 北京理工大学 | Method for preparing high-toughness ceramic based on laser etching technology |
| CN116675520A (en) * | 2023-06-12 | 2023-09-01 | 陕西宝光陶瓷科技有限公司 | Preparation method of 7-13um particle size calcined alpha alumina powder and high-density ceramic |
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