CN105271763A - Low-dielectric low-expanded cordierite glass-ceramic material taking perlite as main raw materials and preparation method thereof - Google Patents
Low-dielectric low-expanded cordierite glass-ceramic material taking perlite as main raw materials and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a dielectric ceramic material and a preparation method of a low-dielectric low-expanded cordierite glass-ceramic material taking perlite as main raw materials. The preparation method is characterized by comprising the following steps that 1, perlite ore is taken as the raw materials to prepare glass-ceramic raw materials; 2, the prepared glass-ceramic raw materials are fused, quenched with water, ground and dried to obtain glass powder; 3, compression moulding is performed to prepare green bodies; 4, heat treatment is performed, wherein the green bodies are placed in a high temperature furnace, the temperature is increased to 850 DEG C-950 DEG C, the temperature increasing rate is 5-15 DEG C/min, heat preservation is performed for 6-10 h, the temperature is lowered along with the furnace, and then the low-dielectric low-expanded cordierite glass-ceramic material is obtained. The material prepared through the method has the advantages of being low in dielectric constant, dielectric loss and thermal expansion coefficient.
Description
Technical field
The present invention relates to dielectric ceramic material, particularly a kind of take perlite as α-cordierite microcrystal glass material of main raw material and preparation method thereof.
Background technology
In recent years, under the drive of semiconductor technology develop rapidly, electronic devices and components are constantly to miniaturization, integrated and high frequency future development.Select suitable to be no more than pottery low temperature co-fired at the temperature of 950 DEG C with electro-conductive materials such as silver, thus make sandwich type element or passive device is imbedded in Mulitilayer circuit board, become the inevitable requirement of above-mentioned trend, therefore LTCC (LowTemperatureCo-firedCeramics is called for short LTCC) as passive integration element main medium material also becomes a kind of important development trend.
The subject matter of current restriction LTCC technology successful Application is to develop the LTCC material meeting different application demand.Low-k can improve the transfer rate of signal; Low-dielectric loss coefficient can reduce the loss in alternating electric field, so the LTCC material of development low-k (ε≤10) is the challenge how LTCC material adapts to frequency applications to meet the requirement of high frequency and high speed.The thermal expansivity of material is the most critical factor affecting LTCC device reliability, should match with its circuit card that will weld as far as possible, thermal mismatching can be reduced like this, strengthen the globality of machinery, reduce the change of temperature profile, and increase the integration capability of numerical digit, optics and electronic technology.
To study at present and commercial LTCC material is mainly main with microcrystallite body, and achieving huge success in actual applications.Devitrified glass system LTCC material, mainly by nucleation and crystallisation procedure, becomes the fine and close stupalith with some strength, as single devitrified glass, its crystallization is difficult to control completely, along with the change of heat-treat condition, its Character change is comparatively large, especially dielectric loss.Natural mineral prepares cordierite glass-ceramic has larger advantages for development because preparation cost is lower.But cordierite glass-ceramic prepared by current natural mineral can cause generating other crystalline phases because of the introducing of the impurity of its mineral own, cause its specific inductivity and dielectric loss to worsen, thermal expansivity is difficult to control.Therefore with natural mineral be the main drawback that cordierite glass-ceramic prepared by raw material be and generate α-cordierite crystalline phase while produce with other crystalline phases, cause specific inductivity, dielectric loss and thermal expansivity larger, the poor stability of synthesizer, is unfavorable for producing in enormous quantities.
To sum up, for the application demand of electronic devices and components, actively develop LTCC investigation of materials and solve the problems such as basic theory, gordian technique and the technique in new material research, to the application promoting LTCC technology, meet electronics to high frequency, broadband, high-power, low-loss, highly reliable future development, realize microwave, the miniaturization of millimeter wave electronic circuit, lightweight, integrated there is meaning of crucial importance.
Summary of the invention
For solving above-mentioned proposed technical problem, the object of the present invention is to provide a kind of take perlite as low Jie's low bulk cordierite glass-ceramic material of main raw material and preparation method thereof, and material prepared by the method has the feature of low-k, low-dielectric loss, low thermal coefficient of expansion.
For achieving the above object, the technical solution used in the present invention is: a kind of take perlite as low Jie's low bulk cordierite glass-ceramic material of main raw material, it is characterized in that by comprising perlite, oxide compound (silicon-aluminum-magnesium analytical pure oxide compound) is prepared from, according to weight percent meter, perlite addition is 40 ~ 60%; Described oxide compound is SiO
2, Al
2o
3and MgO; Raw material main chemical compositions is SiO by weight percentage
240 ~ 60%, Al
2o
325 ~ 35%, MgO10 ~ 18%, alkalimetal oxide 2 ~ 8%, other impurity 0 ~ 10%.
Above-mentioned alkalimetal oxide is K
2o, Na
2a kind of or two kinds of mixtures by any proportioning in O; Other impurity are Fe
2o
3, TiO
2, one or more mixtures by any proportioning in CaO etc.
Above-mentioned a kind of take perlite as the preparation method of low Jie's low bulk cordierite glass-ceramic material of main raw material, it is characterized in that it comprises the following steps: (1) for raw material, prepares devitrified glass raw material with perlite ore deposit; (2) prepare the shrend of devitrified glass raw materials melt, after mill-drying, obtain glass powder; (3) base substrate is prepared in compression moulding; (4) thermal treatment: base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 850 ~ 950 DEG C, temperature rise rate is 5 ~ 15 DEG C/min, and insulation 6 ~ 10h, lowers the temperature with stove, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
By such scheme, being prepared as of devitrified glass raw material: according to weight percent meter, perlite addition is 40 ~ 60%; Perlite powder is broken into and is less than 200 order powders, then with SiO
2, Al
2o
3with MgO analytical pure oxide compound, be SiO by weight percentage by raw material main chemical compositions
240 ~ 60%, Al
2o
325 ~ 35%, MgO10 ~ 18%, alkalimetal oxide 2 ~ 8%, other impurity 0 ~ 10%, mixing.
By such scheme, described step (2) raw materials melt shrend mill-drying obtains glass powder, at 1550 DEG C of melting 4 ~ 6h, after shrend is dried, at planetary ball mill wet ball grinding 6 ~ 8h, (grinding used is corundum ball grinder, medium is agate ball), grinding to form median size is 1 ~ 3 μm of particle, obtains glass powder after oven dry.
By such scheme, described step (3) compression moulding chooses according to every gram of glass powder the ratio that massfraction is the polyvinyl alcohol solution 0.06 ~ 0.2mL of 5%, by glass powder and polyvinyl alcohol solution ground and mixed even, under 20 ~ 30MPa pressure, keep 4 ~ 8min, obtain base substrate.
Compared with prior art, the invention has the beneficial effects as follows: the low temperature co-fired α-cordierite microcrystal glass material of low thermal coefficient of expansion of the present invention, sintering can be realized and densification at 850 ~ 950 DEG C, in gained microcrystal glass material, crystalline phase is single α-cordierite, and material has less specific inductivity (ε≤10) and dielectric loss, thermal expansivity is low, physical strength is high, be better than cordierite glass-ceramic material prepared by existing mineral, and good manufacturability, cost is low.Can be applicable to electron device and other electronic package material fields such as ltcc substrate material, resonator, greatly improve perlitic added value, widened perlitic Application Areas.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with example, but the present invention is not only confined to the following examples.
Embodiment 1
Get perlite 55g and be crushed to below 200 orders, add 45g magnalium silico analysis pure-oxide (SiO
2, Al
2o
3, MgO is respectively 15.2g, 20.0g, 9.8g), formula main oxides content is: SiO
254.1%, Al
2o
327.0%, MgO10.1%, K
2o2.3%, Na
2o1.4%, other impurity 5.1%, obtain devitrified glass raw material.
100g devitrified glass raw material is mixed, puts into corundum crucible, be placed in 1550 DEG C of meltings, insulation 4h, then shrend drying in deionization cold water; Shrend glass is placed in planetary ball mill ball milling, and ball-milling medium is agate ball, and add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 8h (grinding to form median size is 1 ~ 3 μm of particle), then dries at 110 DEG C and obtains glass powder.
Base substrate is made in glass powder compression moulding: take 5g glass powder, get the polyvinyl alcohol solution 1mL that massfraction is 5%, glass powder and polyvinyl alcohol solution ground and mixed is even, under 28MPa pressure, keep 8min, obtain base substrate.
Base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 925 DEG C, temperature rise rate is 10 DEG C/min, insulation 6h, and with stove cooling, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
The performance index of this devitrified glass are as follows: specific inductivity is 5.29 (10MHz); Dielectric loss is 0.0025 (10MHz); Density is 2.51g/cm
3; Thermal expansivity (20 ~ 600 DEG C) is 2.72 × 10
-6/ DEG C; Folding strength is 122MPa.
Embodiment 2
Get perlite 42g and be crushed to below 200 orders, add 58g magnalium silico analysis pure-oxide (SiO
2, Al
2o
3, MgO is respectively 22.4g, 24.1g, 11.5g), formula main oxides content is: SiO
252.1%, Al
2o
329.5%, MgO11.6%, K
2o1.8%, Na
2o1.1%, other impurity 3.9%, obtain devitrified glass raw material.
100g devitrified glass raw material is mixed, puts into corundum crucible, be placed in 1550 DEG C of meltings, insulation 5.5h, then shrend drying in deionization cold water; Shrend glass is placed in planetary ball mill ball milling, and ball-milling medium is agate ball, and add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 6h (grinding to form median size is 1 ~ 3 μm of particle), then dries at 110 DEG C and obtains glass powder.
Base substrate is made in glass powder compression moulding: take 5g glass powder, get the polyvinyl alcohol solution 1mL that massfraction is 5%, glass powder and polyvinyl alcohol solution ground and mixed is even, under 25MPa pressure, keep 6min, obtain base substrate.
Base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 900 DEG C, temperature rise rate is 8 DEG C/min, insulation 7h, and with stove cooling, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
The performance index of this devitrified glass are as follows: specific inductivity is 5.72 (10MHz); Dielectric loss is 0.006 (10MHz); Density is 2.53g/cm
3; Thermal expansivity (20 ~ 600 DEG C) is 2.91 × 10
-6/ DEG C; Folding strength is 118MPa.
Embodiment 3
Get perlite 50g and be crushed to below 200 orders, add 50g magnalium silico analysis pure-oxide (SiO
2, Al
2o
3, MgO is respectively 11.4g, 25.3g, 13.3g), formula main oxides content is: SiO
246.7%, Al
2o
331.7%, MgO13.6%, K
2o2.1%, Na
2o1.3%, other impurity 4.6%, obtain devitrified glass raw material.
100g devitrified glass raw material is mixed, puts into corundum crucible, be placed in 1550 DEG C of meltings, insulation 5h, then shrend drying in deionization cold water; Shrend glass is placed in planetary ball mill ball milling, and ball-milling medium is agate ball, and add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 7h (grinding to form median size is 1 ~ 3 μm of particle), then dries at 110 DEG C and obtains glass powder.
Base substrate is made in glass powder compression moulding: take 5g glass powder, get the polyvinyl alcohol solution 1mL that massfraction is 5%, glass powder and polyvinyl alcohol solution ground and mixed is even, under 23MPa pressure, keep 5min, obtain base substrate.
Base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 875 DEG C, temperature rise rate is 6 DEG C/min, insulation 8h, and with stove cooling, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
The performance index of this devitrified glass are as follows: specific inductivity is 5.68 (10MHz); Dielectric loss is 0.0043 (10MHz); Density is 2.58g/cm
3; Thermal expansivity (20 ~ 600 DEG C) is 2.60 × 10
-6/ DEG C; Folding strength is 125MPa.
Embodiment 4
Get perlite 45g and be crushed to below 200 orders, add 55g magnalium silico analysis pure-oxide (SiO
2, Al
2o
3, MgO is respectively 12.4g, 24.8g, 17.8g), formula main oxides content is: SiO
244.2%, Al
2o
330.5%, MgO18%, K
2o1.9%, Na
2o1.2%, other impurity 4.2%, obtain devitrified glass raw material.
100g devitrified glass raw material is mixed, puts into corundum crucible, be placed in 1550 DEG C of meltings, insulation 6h, then shrend drying in deionization cold water; Shrend glass is placed in planetary ball mill ball milling, and ball-milling medium is agate ball, and add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 6h (grinding to form median size is 1 ~ 3 μm of particle), then dries at 110 DEG C and obtains glass powder.
Base substrate is made in glass powder compression moulding: take 5g glass powder, get the polyvinyl alcohol solution 1mL that massfraction is 5%, glass powder and polyvinyl alcohol solution ground and mixed is even, under 20MPa pressure, keep 7min, obtain base substrate.
Base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 850 DEG C, temperature rise rate is 12 DEG C/min, insulation 10h, and with stove cooling, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
The performance index of this devitrified glass are as follows: specific inductivity is 5.54 (10MHz); Dielectric loss is 0.0032 (10MHz); Density is 2.64g/cm
3; Thermal expansivity (20 ~ 600 DEG C) is 2.55 × 10
-6/ DEG C; Folding strength is 126MPa.
Embodiment 5
Get perlite 48g and be crushed to below 200 orders, add 52g magnalium silico analysis pure-oxide (SiO
2, Al
2o
3, MgO is respectively 14.5g, 22.3g, 15.2g), formula main oxides content is: SiO
248.4%, Al
2o
328.5%, MgO15.4%, K
2o2.1%, Na
2o1.2%, other impurity 4.4%, obtain devitrified glass raw material.
100g devitrified glass raw material is mixed, puts into corundum crucible, be placed in 1550 DEG C of meltings, insulation 4.5h, then shrend drying in deionization cold water; Shrend glass is placed in planetary ball mill ball milling, and ball-milling medium is agate ball, and add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 7h (grinding to form median size is 1 ~ 3 μm of particle), then dries at 110 DEG C and obtains glass powder.
Base substrate is made in glass powder compression moulding: take 5g glass powder, get the polyvinyl alcohol solution 1mL that massfraction is 5%, glass powder and polyvinyl alcohol solution ground and mixed is even, under 30MPa pressure, keep 4min, obtain base substrate.
Base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 875 DEG C, temperature rise rate is 10 DEG C/min, insulation 8h, and with stove cooling, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
The performance index of this devitrified glass are as follows: specific inductivity is 5.65 (10MHz); Dielectric loss is 0.0048 (10MHz); Density is 2.77g/cm
3; Thermal expansivity (20 ~ 600 DEG C) is 2.84 × 10
-6/ DEG C; Folding strength is 128MPa.
Embodiment 6
Get perlite 58g and be crushed to below 200 orders, add 42g magnalium silico analysis pure-oxide (SiO
2, Al
2o
3, MgO is respectively 9.5g, 21.8g, 10.7g), formula main oxides content is: SiO
250.5%, Al
2o
329.2%, MgO10.9%, K
2o2.5%, Na
2o1.5%, other impurity 5.4%, obtain devitrified glass raw material.
100g devitrified glass raw material is mixed, puts into corundum crucible, be placed in 1550 DEG C of meltings, insulation 5h, then shrend drying in deionization cold water; Shrend glass is placed in planetary ball mill ball milling, and ball-milling medium is agate ball, and add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 8h (grinding to form median size is 1 ~ 3 μm of particle), then dries at 110 DEG C and obtains glass powder.
Base substrate is made in glass powder compression moulding: take 5g glass powder, get the polyvinyl alcohol solution 1mL that massfraction is 5%, glass powder and polyvinyl alcohol solution ground and mixed is even, under 26MPa pressure, keep 6min, obtain base substrate.
Base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 900 DEG C, temperature rise rate is 5 DEG C/min, insulation 7h, and with stove cooling, obtain low Jie's low bulk α-cordierite devitrified glass, in microcrystal glass material, crystalline phase is single α-cordierite crystalline phase.
The performance index of this devitrified glass are as follows: specific inductivity is 5.93 (10MHz); Dielectric loss is 0.0096 (10MHz); Density is 2.44g/cm
3; Thermal expansivity (20 ~ 600 DEG C) is 3.02 × 10
-6/ DEG C; Folding strength is 116MPa.
In summary it can be seen, outstanding feature of the present invention and significant progress effectively utilize the rich natural non-metallic mineral perlite sial element produced as the source of devitrified glass element, and its impurity can reduce sintering temperature and promote that α-cordierite crystalline phase is separated out.Technology of preparing of the present invention is reasonable, abundant raw material source, and technical process is simple, greatly improves perlitic value added.
Each raw material cited by the present invention, and the bound of each raw material of the present invention, interval value, and the bound of processing parameter (as temperature, time etc.), interval value can realize the present invention, do not enumerate embodiment at this.
Above embodiment is only for illustration of the preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; in the ken that described exercising ordinary skill possesses; the any amendment done within the spirit and principles in the present invention, equivalent to substitute and improvement etc., it all should be encompassed within the technical scheme scope of request of the present invention protection.
Claims (7)
1. be low Jie's low bulk cordierite glass-ceramic material of main raw material with perlite, it is characterized in that by comprising perlite, Preparation forms, according to weight percent meter, perlite addition is 40 ~ 60%; Described oxide compound is SiO
2, Al
2o
3and MgO; Raw material main chemical compositions is SiO by weight percentage
240 ~ 60%, Al
2o
325 ~ 35%, MgO10 ~ 18%, alkalimetal oxide 2 ~ 8%, other impurity 0 ~ 10%.
2. according to claim 1 a kind of take perlite as low Jie's low bulk cordierite glass-ceramic material of main raw material, it is characterized in that, described alkalimetal oxide is K
2o, Na
2a kind of or two kinds of mixtures by any proportioning in O.
3. according to claim 1 a kind of take perlite as low Jie's low bulk cordierite glass-ceramic material of main raw material, it is characterized in that, other impurity are Fe
2o
3, TiO
2, one or more mixtures by any proportioning in CaO.
4. a kind of as claimed in claim 1 take perlite as the preparation method of low Jie's low bulk cordierite glass-ceramic material of main raw material, it is characterized in that it comprises the following steps: (1) for raw material, prepares devitrified glass raw material with perlite ore deposit; (2) the devitrified glass raw materials melt shrend prepared, obtains glass powder after mill-drying; (3) base substrate is prepared in compression moulding; (4) thermal treatment: base substrate is put into High Temperature Furnaces Heating Apparatus and be warming up to 850 ~ 950 DEG C, temperature rise rate is 5 ~ 15 DEG C/min, insulation 6 ~ 10h, with stove cooling, obtains low Jie's low bulk cordierite glass-ceramic material.
5. be the preparation method of low Jie's low bulk cordierite glass-ceramic material of main raw material with perlite according to claim 4 one kind, it is characterized in that, being prepared as of described devitrified glass raw material: according to weight percent meter, perlite addition is 40 ~ 60%; Perlite powder is broken into and is less than 200 order powders, then with SiO
2, Al
2o
3with MgO analytical pure oxide compound, be SiO by weight percentage by raw material main chemical compositions
240 ~ 60%, Al
2o
325 ~ 35%, MgO10 ~ 18%, alkalimetal oxide 2 ~ 8%, other impurity 0 ~ 10%, mixing.
6. be the preparation method of low Jie's low bulk cordierite glass-ceramic material of main raw material with perlite according to claim 4 one kind, it is characterized in that, described step (2) raw materials melt shrend mill-drying obtains glass powder, at 1550 DEG C of melting 4 ~ 6h, after shrend is dried, at planetary ball mill wet ball grinding 6 ~ 8h, grinding to form median size is 1 ~ 3 μm of particle, obtains glass powder after oven dry.
7. be the preparation method of low Jie's low bulk cordierite glass-ceramic material of main raw material with perlite according to claim 4 one kind, it is characterized in that, described step (3) compression moulding, choose according to every gram of glass powder the ratio that massfraction is the polyvinyl alcohol solution 0.06 ~ 0.2mL of 5%, by glass powder and polyvinyl alcohol solution ground and mixed even, under 20 ~ 30MPa pressure, keep 4 ~ 8min, obtain base substrate.
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| CN105731807A (en) * | 2016-02-01 | 2016-07-06 | 中国人民解放军第四军医大学 | Method for preparing dental restoration material lithium disilicate glass ceramic by means of adhesive |
| CN106747357A (en) * | 2016-12-22 | 2017-05-31 | 广东风华高新科技股份有限公司 | LTCC and preparation method thereof |
| CN107188407A (en) * | 2017-02-16 | 2017-09-22 | 山东炳坤腾泰陶瓷科技股份有限公司 | Wiring board glass substrate and preparation method that a kind of utilization alkali-free glass fibre waste silk makes |
| CN110256060A (en) * | 2019-07-09 | 2019-09-20 | 嘉兴佳利电子有限公司 | A kind of high frequency low-k low-temperature co-burning ceramic material and preparation method |
| CN110655392A (en) * | 2019-10-24 | 2020-01-07 | 信阳师范学院 | Microcrystalline surface porous heat-insulating ceramic composite material taking low-grade potassium feldspar as raw material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105731807A (en) * | 2016-02-01 | 2016-07-06 | 中国人民解放军第四军医大学 | Method for preparing dental restoration material lithium disilicate glass ceramic by means of adhesive |
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| CN107188407A (en) * | 2017-02-16 | 2017-09-22 | 山东炳坤腾泰陶瓷科技股份有限公司 | Wiring board glass substrate and preparation method that a kind of utilization alkali-free glass fibre waste silk makes |
| CN107188407B (en) * | 2017-02-16 | 2020-06-19 | 江苏炳坤腾泰陶瓷科技股份有限公司 | Circuit board glass substrate manufactured by using alkali-free glass fiber waste silk and preparation method |
| CN110256060A (en) * | 2019-07-09 | 2019-09-20 | 嘉兴佳利电子有限公司 | A kind of high frequency low-k low-temperature co-burning ceramic material and preparation method |
| CN110256060B (en) * | 2019-07-09 | 2021-10-08 | 嘉兴佳利电子有限公司 | High-frequency low-dielectric-constant low-temperature co-fired ceramic material and preparation method thereof |
| CN110655392A (en) * | 2019-10-24 | 2020-01-07 | 信阳师范学院 | Microcrystalline surface porous heat-insulating ceramic composite material taking low-grade potassium feldspar as raw material and preparation method thereof |
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