CN105271763B - It is a kind of using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material and preparation method thereof - Google Patents
It is a kind of using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to dielectric ceramic material.A kind of preparation method using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material, it is characterised in that it comprises the following steps：(1) using perlite ore deposit as raw material, devitrified glass raw material is prepared；(2) the devitrified glass raw materials melt water quenching prepared, after mill-drying glass dust；(3) it is compressing to prepare base substrate；(4) it is heat-treated：Base substrate is put into high temperature furnace and is warming up to 850~950 DEG C, heating rate is 5~15 DEG C/min, is incubated 6~10h, cools with stove, obtain low Jie's low bulk cordierite glass-ceramic material.Material prepared by this method has the characteristics of low-k, low-dielectric loss, low thermal coefficient of expansion.
Description
Technical field
The present invention relates to dielectric ceramic material, more particularly to a kind of α-cordierite crystallite glass using perlite as primary raw material
Glass material and preparation method thereof.
Background technology
In recent years, semiconductor technology rapid development drive under, electronic component constantly to miniaturization, it is integrated and high
Frequencyization direction is developed.Selection it is appropriate can with the conductive material ceramics low temperature co-fired at a temperature of no more than 950 DEG C such as silver, from
And make sandwich type element or passive device is embedded in Mulitilayer circuit board, turn into the inevitable requirement of above-mentioned trend, as passive
LTCC (Low Temperature Co-fired Ceramics, the abbreviation of integrated component main medium material
LTCC) also therefore a kind of important development trend is turned into.
The subject matter for restricting LTCC technology successful application at present is to develop the LTCC materials for meeting different application demand.
Low-k can improve the transmission rate of signal；Low-dielectric loss coefficient can reduce the loss in alternating electric field, so development
The LTCC materials of low-k (ε≤10) are how LTCC materials adapt to frequency applications to meet the requirement of high frequency and high speed
One challenge.The thermal coefficient of expansion of material is a most critical factor for influenceing LTCC device reliabilities, should be wanted as far as possible with it
The circuit board of welding matches, and can so reduce thermal mismatching, strengthens the globality of machinery, reduces the change of temperature characterisitic
Change, and the integration capability of increase numerical digit, optics and electronic technology.
Currently the LTCC materials of research and commercialization are mainly based on devitrified glass system, and in actual applications
Achieve huge success.Devitrified glass system LTCC materials mainly by nucleation and crystallisation procedure, become densification
The ceramic material with some strength, as single devitrified glass, its crystallization is difficult to control completely, with heat treatment condition
Change, its character changes greatly, especially dielectric loss.It is relatively low because preparing cost that natural minerals prepare cordierite glass-ceramic
There are larger advantages for development.But the cordierite glass-ceramic prepared at present with natural minerals is because of the introducing of impurity of its mineral itself
It can cause to generate other crystalline phases, cause its dielectric constant and dielectric loss to deteriorate, thermal coefficient of expansion is difficult to control.Therefore with natural
Mineral are that the major defect that raw material prepares cordierite glass-ceramic produces while being generation α-cordierite crystalline phase with other crystalline phases
It is raw, cause dielectric constant, dielectric loss and thermal coefficient of expansion larger, the stability of synthesizer is poor, is unfavorable for producing in enormous quantities.
To sum up, for the application demand of electronic component, LTCC investigations of materials is actively developed and are solved in new material research
Basic theory, key technology and the problems such as technique, the application to promoting LTCC technology, meet electronic equipment to high frequency, broadband,
High-power, low-loss, highly reliable direction are developed, and realize the microwave, miniaturization of millimeter wave electronic circuit, lightweight, integrated
With meaning of crucial importance.
The content of the invention
To solve above-mentioned proposed technical problem, it is an object of the invention to provide one kind using perlite as primary raw material
Low Jie's low bulk cordierite glass-ceramic material and preparation method thereof, material prepared by this method has low-k, low
The characteristics of dielectric loss, low thermal coefficient of expansion.
To achieve the above object, the technical solution adopted by the present invention is：It is a kind of low using perlite as low Jie of primary raw material
Expansion cordierite microcrystal glass material, it is characterised in that by including perlite, oxide (silicon-aluminum-magnesium analysis pure-oxide) preparation
Form, in percentage by weight, perlite addition is 40~60%；The oxide is SiO2、Al2O3And MgO；Raw material
Main chemical compositions are SiO by weight percentage240~60%, Al2O325~35%, MgO 10~18%, alkali metal oxygen
Compound 2~8%, other impurities 0~10%.
Above-mentioned alkali metal oxide is K2O、Na2One or two kinds of mixture by any proportioning in O；Other impurities
For Fe2O3、TiO2, the one or more in CaO etc. press the mixture of any proportioning.
A kind of above-mentioned preparation method using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material, its
It is characterised by that it comprises the following steps：(1) using perlite ore deposit as raw material, devitrified glass raw material is prepared；(2) devitrified glass original is prepared
Expect melt water quenching, glass dust is obtained after mill-drying；(3) it is compressing to prepare base substrate；(4) it is heat-treated：Base substrate is put into high temperature furnace
In be warming up to 850~950 DEG C, heating rate is 5~15 DEG C/min, be incubated 6~10h, cool with stove, obtain low Jie's low bulk α-
Cordierite glass-ceramic, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
By such scheme, devitrified glass raw material is prepared as：In percentage by weight, perlite addition be 40~
60%；Crushed crude pearlite is broken into less than 200 mesh powders, then with SiO2、Al2O3Pure-oxide is analyzed with MgO, it is main by raw material
Chemical composition is SiO by weight percentage240~60%, Al2O325~35%, MgO 10~18%, alkali metal oxide 2
~8%, other impurities 0~10%, mixing.
By such scheme, step (2) the raw materials melt water quenching mill-drying obtains glass dust, is to melt 4 at 1550 DEG C
~6h, (it is corundum ball grinder used in grinding, medium is agate in 6~8h of planetary ball mill wet ball grinding after water quenching drying
Ball), it is 1~3 μm of particle to be ground into average grain diameter, and glass dust is obtained after drying.
By such scheme, the step (3) is compressing, be according to every gram of glass dust choose mass fraction be 5% it is poly-
0.06~0.2mL of glycohol solution ratio, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, pressed in 20~30MPa
4~8min is kept under power, obtains base substrate.
Compared with prior art, the beneficial effects of the invention are as follows：Low temperature co-fired α-violet of the low thermal coefficient of expansion of the present invention
Green stone microcrystal glass material, it can be realized at 850~950 DEG C and sinter and be densified, crystalline phase is single in gained microcrystal glass material
One α-cordierite, and material has less dielectric constant (ε≤10) and dielectric loss, and thermal coefficient of expansion is low, mechanical strength
Height, the cordierite glass-ceramic material prepared better than existing mineral, and good manufacturability, cost are low.It can be applied to ltcc substrate
The electronic devices such as material, resonator and other electronic package material fields, greatly improve the added value of perlite, widen
The application field of perlite.
Embodiment
For a better understanding of the present invention, with reference to the example content that the present invention is furture elucidated, but the present invention is not only
It is limited only to the following examples.
Embodiment 1
Perlite 55g is taken to be crushed to below 200 mesh, addition 45g magnalium silico analysis pure-oxides (SiO2、Al2O3, MgO point
Wei 15.2g, 20.0g, 9.8g), formula main oxides content is：SiO254.1%th, Al2O327.0%th, MgO 10.1%,
K2O 2.3%, Na2O 1.4%, other impurities 5.1%, obtain devitrified glass raw material.
100g devitrified glass raw materials are well mixed, are put into corundum crucible, are placed in 1550 DEG C of meltings, are incubated 4h, then
Water quenching and dried in deionization cold water；Water quenching glass is placed in ball milling in planetary ball mill, ball-milling medium is agate ball, is added
Add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 8h (it is 1~3 μm of particle to be ground into average grain diameter), then at 110 DEG C
Drying obtains glass dust.
Base substrate is made by glass dust is compressing：5g glass dust is weighed, takes the poly-vinyl alcohol solution that mass fraction is 5%
1mL, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, 8min is kept under 28MPa pressure, obtains base substrate.
Base substrate is put into high temperature furnace and is warming up to 925 DEG C, heating rate is 10 DEG C/min, is incubated 6h, cools with stove, obtain
Low Jie's low bulk α-cordierite devitrified glass, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
The performance indications of the devitrified glass are as follows：Dielectric constant is 5.29 (10MHz)；Dielectric loss is 0.0025
(10MHz)；Density is 2.51g/cm3；(20~600 DEG C) of thermal coefficient of expansion is 2.72 × 10-6/℃；Rupture strength is 122MPa.
Embodiment 2
Perlite 42g is taken to be crushed to below 200 mesh, addition 58g magnalium silico analysis pure-oxides (SiO2、Al2O3, MgO point
Wei 22.4g, 24.1g, 11.5g), formula main oxides content is：SiO252.1%th, Al2O329.5%th, MgO 11.6%,
K2O 1.8%, Na2O 1.1%, other impurities 3.9%, obtain devitrified glass raw material.
100g devitrified glass raw materials are well mixed, are put into corundum crucible, are placed in 1550 DEG C of meltings, are incubated 5.5h, so
Water quenching and dried in deionization cold water afterwards；Water quenching glass is placed in ball milling in planetary ball mill, ball-milling medium is agate ball,
Appropriate amount of deionized water wet ball grinding is added, Ball-milling Time is 6h (it is 1~3 μm of particle to be ground into average grain diameter), then at 110 DEG C
Lower drying obtains glass dust.
Base substrate is made by glass dust is compressing：5g glass dust is weighed, takes the poly-vinyl alcohol solution that mass fraction is 5%
1mL, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, 6min is kept under 25MPa pressure, obtains base substrate.
Base substrate is put into high temperature furnace and is warming up to 900 DEG C, heating rate is 8 DEG C/min, is incubated 7h, cools with stove, obtain
Low Jie's low bulk α-cordierite devitrified glass, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
The performance indications of the devitrified glass are as follows：Dielectric constant is 5.72 (10MHz)；Dielectric loss is 0.006
(10MHz)；Density is 2.53g/cm3；(20~600 DEG C) of thermal coefficient of expansion is 2.91 × 10-6/℃；Rupture strength is 118MPa.
Embodiment 3
Perlite 50g is taken to be crushed to below 200 mesh, addition 50g magnalium silico analysis pure-oxides (SiO2、Al2O3, MgO point
Wei 11.4g, 25.3g, 13.3g), formula main oxides content is：SiO246.7%th, Al2O331.7%th, MgO
13.6%th, K2O 2.1%, Na2O 1.3%, other impurities 4.6%, obtain devitrified glass raw material.
100g devitrified glass raw materials are well mixed, are put into corundum crucible, are placed in 1550 DEG C of meltings, are incubated 5h, then
Water quenching and dried in deionization cold water；Water quenching glass is placed in ball milling in planetary ball mill, ball-milling medium is agate ball, is added
Add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 7h (it is 1~3 μm of particle to be ground into average grain diameter), then at 110 DEG C
Drying obtains glass dust.
Base substrate is made by glass dust is compressing：5g glass dust is weighed, takes the poly-vinyl alcohol solution that mass fraction is 5%
1mL, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, 5min is kept under 23MPa pressure, obtains base substrate.
Base substrate is put into high temperature furnace and is warming up to 875 DEG C, heating rate is 6 DEG C/min, is incubated 8h, cools with stove, obtain
Low Jie's low bulk α-cordierite devitrified glass, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
The performance indications of the devitrified glass are as follows：Dielectric constant is 5.68 (10MHz)；Dielectric loss is 0.0043
(10MHz)；Density is 2.58g/cm3；(20~600 DEG C) of thermal coefficient of expansion is 2.60 × 10-6/℃；Rupture strength is 125MPa.
Embodiment 4
Perlite 45g is taken to be crushed to below 200 mesh, addition 55g magnalium silico analysis pure-oxides (SiO2、Al2O3, MgO point
Wei 12.4g, 24.8g, 17.8g), formula main oxides content is：SiO244.2%th, Al2O330.5%th, MgO 18%,
K2O 1.9%, Na2O 1.2%, other impurities 4.2%, obtain devitrified glass raw material.
100g devitrified glass raw materials are well mixed, are put into corundum crucible, are placed in 1550 DEG C of meltings, are incubated 6h, then
Water quenching and dried in deionization cold water；Water quenching glass is placed in ball milling in planetary ball mill, ball-milling medium is agate ball, is added
Add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 6h (it is 1~3 μm of particle to be ground into average grain diameter), then at 110 DEG C
Drying obtains glass dust.
Base substrate is made by glass dust is compressing：5g glass dust is weighed, takes the poly-vinyl alcohol solution that mass fraction is 5%
1mL, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, 7min is kept under 20MPa pressure, obtains base substrate.
Base substrate is put into high temperature furnace and is warming up to 850 DEG C, heating rate is 12 DEG C/min, is incubated 10h, cools with stove, obtain
To low Jie's low bulk α-cordierite devitrified glass, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
The performance indications of the devitrified glass are as follows：Dielectric constant is 5.54 (10MHz)；Dielectric loss is 0.0032
(10MHz)；Density is 2.64g/cm3；(20~600 DEG C) of thermal coefficient of expansion is 2.55 × 10-6/℃；Rupture strength is 126MPa.
Embodiment 5
Perlite 48g is taken to be crushed to below 200 mesh, addition 52g magnalium silico analysis pure-oxides (SiO2、Al2O3, MgO point
Wei 14.5g, 22.3g, 15.2g), formula main oxides content is：SiO248.4%th, Al2O328.5%th, MgO
15.4%th, K2O 2.1%, Na2O 1.2%, other impurities 4.4%, obtain devitrified glass raw material.
100g devitrified glass raw materials are well mixed, are put into corundum crucible, are placed in 1550 DEG C of meltings, are incubated 4.5h, so
Water quenching and dried in deionization cold water afterwards；Water quenching glass is placed in ball milling in planetary ball mill, ball-milling medium is agate ball,
Appropriate amount of deionized water wet ball grinding is added, Ball-milling Time is 7h (it is 1~3 μm of particle to be ground into average grain diameter), then at 110 DEG C
Lower drying obtains glass dust.
Base substrate is made by glass dust is compressing：5g glass dust is weighed, takes the poly-vinyl alcohol solution that mass fraction is 5%
1mL, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, 4min is kept under 30MPa pressure, obtains base substrate.
Base substrate is put into high temperature furnace and is warming up to 875 DEG C, heating rate is 10 DEG C/min, is incubated 8h, cools with stove, obtain
Low Jie's low bulk α-cordierite devitrified glass, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
The performance indications of the devitrified glass are as follows：Dielectric constant is 5.65 (10MHz)；Dielectric loss is 0.0048
(10MHz)；Density is 2.77g/cm3；(20~600 DEG C) of thermal coefficient of expansion is 2.84 × 10-6/℃；Rupture strength is 128MPa.
Embodiment 6
Perlite 58g is taken to be crushed to below 200 mesh, addition 42g magnalium silico analysis pure-oxides (SiO2、Al2O3, MgO point
Wei 9.5g, 21.8g, 10.7g), formula main oxides content is：SiO250.5%th, Al2O329.2%th, MgO
10.9%th, K2O 2.5%, Na2O 1.5%, other impurities 5.4%, obtain devitrified glass raw material.
100g devitrified glass raw materials are well mixed, are put into corundum crucible, are placed in 1550 DEG C of meltings, are incubated 5h, then
Water quenching and dried in deionization cold water；Water quenching glass is placed in ball milling in planetary ball mill, ball-milling medium is agate ball, is added
Add appropriate amount of deionized water wet ball grinding, Ball-milling Time is 8h (it is 1~3 μm of particle to be ground into average grain diameter), then at 110 DEG C
Drying obtains glass dust.
Base substrate is made by glass dust is compressing：5g glass dust is weighed, takes the poly-vinyl alcohol solution that mass fraction is 5%
1mL, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, 6min is kept under 26MPa pressure, obtains base substrate.
Base substrate is put into high temperature furnace and is warming up to 900 DEG C, heating rate is 5 DEG C/min, is incubated 7h, cools with stove, obtain
Low Jie's low bulk α-cordierite devitrified glass, crystalline phase is single α-cordierite crystalline phase in microcrystal glass material.
The performance indications of the devitrified glass are as follows：Dielectric constant is 5.93 (10MHz)；Dielectric loss is 0.0096
(10MHz)；Density is 2.44g/cm3；(20~600 DEG C) of thermal coefficient of expansion is 3.02 × 10-6/℃；Rupture strength is 116MPa.
It in summary it can be seen, outstanding feature of the invention and significant progress are effective natural non-metallic ore deposits using rich production
Source of the thing perlite sial element as devitrified glass element, its impurity can reduce sintering temperature and promote α-cordierite crystalline phase
Separate out.Technology of preparing of the present invention is reasonable, and raw material sources enrich, and technological process is simple, greatly improves the extra price of perlite
Value.
Each raw material cited by the present invention, and bound, the section value of each raw material of the present invention, and technological parameter
Bound, the section value of (such as temperature, time) can realize the present invention, embodiment numerous to list herein.
Above example is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the field those of ordinary skill possessed knowledge, that is made within the spirit and principles in the present invention is any
Modification, equivalent substitute and improvement etc., it all should cover within the scope of the claimed technical scheme of the present invention.
Claims (7)
1. a kind of low Jie's low bulk cordierite glass-ceramic material using perlite as primary raw material, it is characterised in that by including treasure
Zhu Yan, oxide are prepared, and in percentage by weight, perlite addition is 40~60%；The oxide is SiO2、
Al2O3And MgO；Raw material main chemical compositions are SiO by weight percentage240~60%, Al2O325~35%, MgO 10~
18%th, alkali metal oxide 2~8%, other impurities 0~10%.
A kind of 2. low Jie's low bulk cordierite glass-ceramic material using perlite as primary raw material according to claim 1
Material, it is characterised in that the alkali metal oxide is K2O、Na2One or two kinds of mixture by any proportioning in O.
A kind of 3. low Jie's low bulk cordierite glass-ceramic material using perlite as primary raw material according to claim 1
Material, it is characterised in that other impurities Fe2O3、TiO2, the one or more in CaO press the mixture of any proportioning.
It is 4. as claimed in claim 1 a kind of using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material
Preparation method, it is characterised in that it comprises the following steps：(1) using perlite ore deposit as raw material, devitrified glass raw material is prepared；(2) make
Standby devitrified glass raw materials melt water quenching, after mill-drying glass dust；(3) it is compressing to prepare base substrate；(4) it is heat-treated：Will
Base substrate, which is put into high temperature furnace, is warming up to 850~950 DEG C, and heating rate is 5~15 DEG C/min, is incubated 6~10h, cools with stove, obtain
To low Jie's low bulk cordierite glass-ceramic material.
5. according to a kind of preparation using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material of claim 4
Method, it is characterised in that described devitrified glass raw material is prepared as：In percentage by weight, perlite addition is 40
~60%；Crushed crude pearlite is broken into less than 200 mesh powders, then with SiO2、Al2O3Pure-oxide is analyzed with MgO, by raw material master
It is SiO by weight percentage to want chemical composition240~60%, Al2O325~35%, MgO 10~18%, alkali metal oxide
2~8%, other impurities 0~10%, mixing.
6. according to a kind of preparation using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material of claim 4
Method, it is characterised in that step (2) the raw materials melt water quenching mill-drying obtains glass dust, be 1550 DEG C melt 4~
6h, after water quenching drying, in planetary ball mill 6~8h of wet ball grinding, it is 1~3 μm of particle to be ground into average grain diameter, after drying
To glass dust.
7. according to a kind of preparation using perlite as low Jie's low bulk cordierite glass-ceramic material of primary raw material of claim 4
Method, it is characterised in that the step (3) is compressing, is to choose the polyethylene that mass fraction is 5% according to every gram of glass dust
0.06~0.2mL of alcoholic solution ratio, glass dust and poly-vinyl alcohol solution ground and mixed is uniform, under 20~30MPa pressure
4~8min is kept, obtains 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 |
| CN106747357B (en) * | 2016-12-22 | 2019-12-06 | 广东风华高新科技股份有限公司 | Low-temperature co-fired ceramic and preparation method thereof |
| 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 |
| 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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| CN1304894A (en) * | 2001-01-18 | 2001-07-25 | 清华大学 | Process for preparing cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor |
| CN1489965A (en) * | 2002-09-13 | 2004-04-21 | 舱壁玻璃公司 | Ceramic heating apparatus and producing method thereof |
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| US4897509A (en) * | 1987-04-27 | 1990-01-30 | Corning Incorporated | Glass-ceramics for electronic packaging |
| CN1304894A (en) * | 2001-01-18 | 2001-07-25 | 清华大学 | Process for preparing cordierite-base microcrystal glass-ceramics medium material used for multi-layer inductor |
| CN1489965A (en) * | 2002-09-13 | 2004-04-21 | 舱壁玻璃公司 | Ceramic heating apparatus and producing method thereof |
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