CN102276151B - Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch - Google Patents
Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title abstract description 18
- 238000000034 method Methods 0.000 title abstract description 12
- 239000002241 glass-ceramic Substances 0.000 title abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 72
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- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
The invention discloses a technological method for preparing LTCC amorphous glass ceramic powder with a microwave plasma torch. The technological method comprises the following steps: mixing raw materials of glass, ball milling, drying, and granulating into particles with diameters of 1-3mm, and sintering into ceramic balls at 650-850DEG C; and rapidly fusing the hot ceramic balls into glass droplets through the microwave plasma torch with the temperature of 3000-5000DEG C, falling into deionized water, chilling to obtain an amorphous glass ceramic material with the particle size of 15-500mum, carrying out wet ball milling, and drying to a product the LTCC amorphous glass ceramic powder. According to the invention, methods for fusing glass with platinum and ceramic crucibles in traditional technologies are abandoned, and the glass droplets are in a suspending state in the process of fusing with the microwave plasma torch and do not contact with any vessels, so the technological method of the invention which has the advantages of guarantee of the glass purity, convenient operation, uniform glass chilling, obvious effect better than the traditional technologies, good product consistency, and good economy is in favor of the large scale production.
Description
Technical field
The present invention relates to the preparation method of LTCC amorphous glass porcelain powder, especially adopt microwave plasma torch to prepare the processing method of LTCC amorphous glass porcelain powder, belong to electronic material and device technology field.
Background technology
LTCC (Low Temperature Co-fired Ceramic LTCC) technology is a kind of novel electron material and device application technology, that the low-temperature sintered ceramics powder is made the accurate and fine and close green band of thickness, utilize laser boring on the green band, the machinery punching, micropore slip casting, the techniques such as accurate conductor paste printing are made needed circuitous pattern, and with a plurality of passive components (as low appearance value electric capacity, resistance, wave filter, impedance transducer, coupling mechanism etc.) imbed in multilayer ceramic substrate, then overlap together, internal and external electrode can use respectively silver, copper, the metals such as gold, at 900 ℃ of lower sintering, make the non-interfering high-density circuit of three-dimensional space, also can be made into the three-dimensional circuit substrate of built-in passive element, can mount IC and active part on its surface, make passive/active integrated functional module, can be further with circuit miniaturization and densification, be particularly suitable for high frequency communication assembly.
The low sintering stupalith of can realizing that uses at present mainly comprises devitrified glass system, glass-ceramic compound system and amorphous glass system.Wherein devitrified glass system, glass+ceramics compound system are the emphasis of people's research in recent years, have developed (Mg, Ca) TiO
3, BaO-TiO
2System, ZnO-TiO
2System, BaO-Nd
20
3-TiO
2System, (Zr, Sn) TiO
3, (Ba, Nb) TiO
3Many LTCC material systems such as system and borosilicate system.Wherein, the subject matter that faces at present of low-k LTCC material is high-performance (low-k, low-dielectric loss, high mechanical strength) and the contradiction of sintering temperature and low.LTCC is except rational glass-ceramic formulating of recipe, and its preparation technology and glass smelting method are also very important.Traditional technology is through mixing and ball milling with frit, obtain the frit presoma, insert platinum or the ceramic crucible high-temperature fusion becomes glass metal, then with cold quenching in the cold deionized water of glass metal impouring, obtain fragments of glass, again fragments of glass pulverized or added ceramic packing ball milling, drying at last, making LTCC porcelain powder.The cold quenching effect of this technique is inhomogeneous, and working temperature is high, and labour intensity is large, the employing platinum crucible has high input, and during high temperature melting, the platinum loss that can dissociate, cause LTCC porcelain powder production cost high, and the employing ceramic crucible, glass can corrode ceramic crucible when founding, introduce impurity, affected the purity of LTCC porcelain powder, the consistence of product is difficult to assurance, and the ceramic crucible thermal shock performance is poor simultaneously, often be full of cracks, fragmentation, cause a large amount of crucible wastes, produce industrial waste ballast, increased product cost.
Now, international mature production also can provide several specific inductivity to mainly contain three of DuPont, Ferro and Heraeus less than 10 raw material band, the domestic tracking development that still is in, and most LTCC products depend on these raw material bands of import.Along with the modularization of following electronic component and the surplus of electronic terminal product, the competition of Costco Wholesale must be fiercer, the raw material design of domestic manufacturer's original adoption directly must be difficult to satisfy the requirement of rate war from the way of external packing import, this shows, break away from the dependence to external LTCC porcelain and device, the LTCC porcelain that exploitation is national and advanced person's process for producing has great importance for the development of CHINESE INDUSTRIES.
Summary of the invention
The present invention is intended to the deficiency for traditional technology, abandons with platinum crucible or ceramic crucible melten glass operation, and a kind of processing method of utilizing microwave plasma torch to prepare LTCC amorphous glass porcelain powder is provided.This technique cold quenching effect is even, and production cost is low, and the LTCC amorphous glass porcelain powder purity that makes is high.
Technical problem to be solved by this invention is achieved through the following technical solutions.
A kind of microwave plasma torch prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that processing step is as follows:
A, batching, mixing, ball milling
With frit according to Al
2O
3, 5 ~ 50wt%; SiO
2, 0 ~ 60wt%; B
2O
33H
2O, 0 ~ 40wt%; MgO, 0 ~ 15wt%; ZrO
2, 0 ~ 15wt%; H
3PO
4, 0 ~ 25wt%; Sb
2O
3, 0 ~ 5wt%; BaO, 0 ~ 40wt%; CaO, 0 ~ 35wt%; K
2O, 0 ~ 5wt%; Na
2O, 0 ~ 5wt% weighing mixes, and adds solvent and zirconia ball, adopts wet ball grinding 20 ~ 24 hours;
Described solvent is deionized water or dehydrated alcohol.
The weight proportion of described glass raw material, solvent, zirconia ball is 1:1:1 ~ 1:2:4.
B, oven dry, granulation, sintering
After the glass raw material discharging after ball milling, grind to form in 100 ~ 120 ℃ of oven dry the powder that particle diameter is 10 ~ 40 μ m, add the high polymer binder aqueous solution of 5 ~ 15wt%, mix, granulation, after binder removal, became the porcelain ball in 1 ~ 2 hour in 650 ~ 850 ℃ of sintering;
Described high polymer binder is selected from polyvinyl butyral acetal (PVB) or polyvinyl alcohol (PVA), and the concentration of its aqueous solution is 8 ~ 12wt%.
Described granulation refers to: adopt the rotating-expressing type granulator granulation to become the particle of φ 1 ~ 3mm.
Described binder removal refers to: particle is warmed up to 250 ℃ of insulations 2 hours with the heat-up rate of 1 ℃/min, then is warmed up to 500 ℃ of insulations 4 hours.
C, microwave plasma torch melting, cold quenching
Red-hot porcelain ball after sintering is packed in the charging hopper of microwave plasma torch system, and make the porcelain ball freely fall into the microwave plasma torch of 3000 ~ 5000 ℃ with the flow of 80 ~ 120g/min, rapid melting becomes glass metal to be dropped in deionized water, and obtaining particle diameter after cold quenching is the amorphous glass porcelain of 15～500 μ m;
The homo(io)thermism of described charging hopper is at 780 ~ 850 ℃.
The temperature of described deionized water remains on below 45 ℃.
D, pulverizing, drying
After airflow milling was pulverized, then with wet ball grinding, oven dry obtained LTCC amorphous glass porcelain powder product with the amorphous glass porcelain.
microwave plasma torch of the present invention system comprises the charging hopper, Magnetron microwave supply, circulator, tuner, the microwave reaction cavity, cold rinse bank and condensing works, it is characterized in that: the charging hopper is positioned at the upper end of device, charging hopper outlet at bottom position is provided with the mass flow controller, charging hopper surrounding is coated with adiabator layer on the outside, the adiabator layer place is provided with heating unit, the bottom of charging hopper is the microwave reaction cavity, the bottom of microwave reaction cavity is cold rinse bank and condensing works, be provided with temperature control unit in cold rinse bank, be provided with gas jet in both sides, microwave reaction cavity upper end, the centre is plasma body, one side of plasma body is the tuner that can produce waveguide, opposite side is the Magnetron microwave supply that produces discharge, also be provided with infrared thermometer between microwave reaction cavity and cold rinse bank.
Compared with prior art, advantage of the present invention is as follows:
1, the present invention has abandoned the method for using platinum, ceramic crucible melten glass in the traditional technology, and platinum crucible is expensive, the platinum loss that can dissociate during high temperature melting, and cost is high; And ceramic crucible at high temperature can be introduced impurity by glass corrosion, makes thus the purity of LTCC porcelain powder be affected, the consistence of product is difficult to assurance, and the ceramic crucible thermal shock performance is poor simultaneously, often be full of cracks, fragmentation, cause a large amount of crucible wastes, produce industrial waste ballast, increased product cost.
2, because glass metal grain of the present invention is to be in vacant state, do not contact any vessel in the microwave plasma torch melting process, thereby fully guaranteed the purity of glass porcelain, and easy to operate.
3, also be provided with infrared thermometer between microwave reaction cavity of the present invention and cold rinse bank, in order to measuring the temperature of melten glass material, and then regulate waveguide, perhaps control flow and the flow velocity of Ceramic Balls and realize temperature control.The glass cold quenching is even, and good product consistency has economy preferably, is conducive to scale operation.
Description of drawings
Fig. 1 is the microwave plasma torch system schematic.
Embodiment
Embodiment one
A kind of microwave plasma torch prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that processing step is as follows:
A, batching, mixing, ball milling
With raw material A l
2O
3(99%), SiO
2(99%), B
2O
33H
2O(99%), MgO(99%), ZrO
2(99%), H
3PO
4(80%) be mixed with glass raw material according to weight percentage 28.58%, 25.47%, 35.21%, 6.90%, 0.50%, 3.34% respectively, weighing is sequentially for first claiming the raw material that quality is large, claim that again quality is little, add deionized water and zirconia ball, glass raw material and deionized water, zirconic weight proportion are 1:1:1, adopt wet ball grinding 24 hours;
B, oven dry, granulation, sintering
After the glass raw material discharging after ball milling, grind to form the powder of 10 ~ 40 μ m in 100 ℃ of oven dry, add polyvinyl butyral acetal (PVB) aqueous solution of 10wt% as binding agent, the concentration of this aqueous solution is 10wt%, after mixing, adopt the rotating-expressing type granulator granulation to become the particle of φ 2mm, after binder removal, became the porcelain ball in 1 hour in 850 ℃ of sintering;
Described binder removal refers to: particle is warmed up to 250 ℃ of insulations 2 hours with the heat-up rate of 1 ℃/min, then is warmed up to 500 ℃ of insulations 4 hours;
C, microwave plasma torch melting, cold quenching
Red-hot porcelain ball after sintering is packed in the charging hopper of microwave plasma torch system, the homo(io)thermism of charging hopper is at 800 ℃, and make the porcelain ball freely fall into the microwave plasma torch of 4500 ℃ with the flow of 80g/min, it is that in the deionized water of 20 ~ 50 ℃, obtaining particle diameter after cold quenching is the amorphous glass porcelain of 15～500 μ m that rapid melting becomes glass metal to be dropped into temperature;
D, pulverizing, drying
After airflow milling was pulverized, then with wet ball grinding, frit, deionized water ratio were 1:1 with the amorphous glass porcelain, and Ball-milling Time is 12 hours.Discharging, oven dry obtain LTCC amorphous glass porcelain powder product.
1, this product detects through laser particle size analyzer, and D50 equals 1.12 μ m;
2, this product is tested after granulation, compacting disk, binder removal, sintering, back of the body silver, and wherein dielectric properties adopts the Agilent4284A-LCR test, and the high-frequency dielectric performance adopts Agilent8753ES and matched clamp test:
The dielectric properties of this material are: under 1MHz,
ε r =6.6,
Tan δ=4.8 * 10
-4Under 3GHz,
ε r =6.5,
Tan δ=5.8 * 10
-3
Embodiment two
A kind of microwave plasma torch prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that processing step is as follows:
A, batching, mixing, ball milling
With raw material A l
2O
3(99%), SiO
2(99%), B
2O
33H
2O(99%), MgO(99%), ZrO
2(99%), H
3PO
4(80%), Sb
2O
3(99%), BaO (99%) is mixed with glass raw material according to weight percentage 8.94%, 52.34%, 24.89%, 2.44%, 1.86%, 1.52%, 0.13%, 7.88% respectively, weighing is sequentially for first claiming the raw material that quality is large, claim that again quality is little, add deionized water and zirconia ball, glass raw material and dehydrated alcohol, zirconic weight proportion are 1:1:2, adopt wet ball grinding 22 hours;
B, oven dry, granulation, sintering
After the glass raw material discharging after ball milling, grind to form the powder of 10 ~ 40 μ m in 120 ℃ of oven dry, add polyvinyl butyral acetal (PVB) aqueous solution of 5wt% as binding agent, the concentration of this aqueous solution is 12wt%, after mixing, adopt the rotating-expressing type granulator granulation to become the particle of φ 1mm, after binder removal, became the porcelain ball in 1 hour in 830 ℃ of sintering;
Described binder removal refers to: particle is warmed up to 250 ℃ of insulations 2 hours with the heat-up rate of 1 ℃/min, then is warmed up to 500 ℃ of insulations 4 hours.
C, microwave plasma torch melting, cold quenching
Red-hot porcelain ball after sintering is packed in the charging hopper of microwave plasma torch system, the homo(io)thermism of charging hopper is at 780 ℃, and make the porcelain ball freely fall into the microwave plasma torch of 4400 ℃ with the flow of 100g/min, it is that in the deionized water of 20 ~ 50 ℃, obtaining particle diameter after cold quenching is the amorphous glass porcelain of 15～500 μ m that rapid melting becomes glass metal to be dropped into temperature;
D, pulverizing, drying
After airflow milling was pulverized, then with wet ball grinding, frit, deionized water ratio were 1:1 with the amorphous glass porcelain, and Ball-milling Time is 12 hours.Discharging, oven dry obtain LTCC amorphous glass porcelain powder product.
1, this product detects through laser particle size analyzer, and D50 equals 1.36 μ m;
2, this product is tested after granulation, compacting disk, binder removal, sintering, back of the body silver, and wherein dielectric properties adopts the Agilent4284A-LCR test, and high-frequency dielectric performance 5 adopts Agilent8753ES and matched clamp test:
The dielectric properties of this material are: under 1MHz,
ε r =5.5,
Tan δ=7.8 * 10
-4Under 3GHz,
ε r =5.3,
Tan δ=6.2 * 10
-3
Embodiment three
A kind of microwave plasma torch prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that processing step is as follows:
A, batching, mixing, ball milling
With chemical feedstocks BaO(99%), SiO
2(99%), B
2O
33H
2O(99%), MgO(99%), CaO(99%), ZrO
2(99%) be mixed with glass raw material according to weight percentage 8.03%, 28.56%, 17.08%, 4.94%, 22.86%, 18.53% respectively, weighing is sequentially for first claiming the raw material that quality is large, claim that again quality is little, add deionized water and zirconia ball, glass raw material and deionized water, zirconic weight proportion are 1:2:4, adopt wet ball grinding 20 hours;
B, oven dry, granulation, sintering
After the glass raw material discharging after ball milling, grind to form the powder of 10 ~ 40 μ m in 120 ℃ of oven dry, polyvinyl alcohol (PVA) aqueous solution % that adds 15wt%) as binding agent, this concentration of aqueous solution is 8wt%, after mixing, adopt the rotating-expressing type granulator granulation to become the particle of φ 3mm, after binder removal, became the porcelain ball in 1 hour in 820 ℃ of sintering;
Described binder removal refers to: particle is warmed up to 250 ℃ of insulations 2 hours with the heat-up rate of 1 ℃/min, then is warmed up to 500 ℃ of insulations 4 hours;
C, microwave plasma torch melting, cold quenching
Red-hot porcelain ball after sintering is packed in the charging hopper of microwave plasma torch system, the homo(io)thermism of charging hopper is at 850 ℃, and make the porcelain ball freely fall into the microwave plasma torch of 4000 ℃ with the flow of 120g/min, it is that in the deionized water of 20 ~ 40 ℃, obtaining particle diameter after cold quenching is the amorphous glass porcelain of 15～500 μ m that rapid melting becomes glass metal to be dropped into temperature;
D, pulverizing, drying
After airflow milling was pulverized, then with wet ball grinding, frit, deionized water ratio were 1:1 with the amorphous glass porcelain, and Ball-milling Time is 12 hours.Discharging, oven dry obtain LTCC amorphous glass porcelain powder product.
1, this product is after mixing according to weight ratio 1:1 with alpha-type aluminum oxide, and ball milling is dried, and grinds and obtains mixing uniformly the porcelain powder, and laser particle size analyzer detects, and D50 equals 1.23 μ m;
2, mix the porcelain powder and test after granulation, compacting disk, binder removal, sintering, back of the body silver, wherein dielectric properties adopts the Agilent4284A-LCR test, and the high-frequency dielectric performance adopts Agilent8753ES and matched clamp test:
The dielectric properties of this material are: under 1MHz,
ε r =8.2,
Tan δ=4.7 * 10
-4Under 3GHz,
ε r =8.0,
Tan δ=3.6 * 10
-3
Claims (7)
1. a microwave plasma torch prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that processing step is as follows:
A, batching, mixing, ball milling
With frit according to Al
2O
35 ~ 50wt%, SiO
20 ~ 60wt%, B
2O
33H
2O 0 ~ 40wt%, MgO 0 ~ 15wt%, ZrO
20 ~ 15wt%, H
3PO
40 ~ 25wt%, Sb
2O
30 ~ 5wt%, BaO 0 ~ 40wt%, CaO 0 ~ 35wt%, K
2O 0 ~ 5wt%, Na
2O 0 ~ 5wt% weighing mixes, and adds solvent and zirconia ball, adopts wet ball grinding 20 ~ 24 hours;
The weight proportion of described glass raw material, solvent, zirconia ball is 1:1:1 ~ 1:2:4;
B, oven dry, granulation, sintering
After the glass raw material discharging after ball milling, grind to form in 100 ~ 120 ℃ of oven dry the powder that particle diameter is 10 ~ 40 μ m, add the high polymer binder aqueous solution of 5 ~ 15wt%, mix, be a granulated into the particle of φ 1 ~ 3mm, after binder removal, became the porcelain ball in 1 ~ 2 hour in 650 ~ 850 ℃ of sintering;
C, microwave plasma torch melting, cold quenching
Red-hot porcelain ball after sintering is packed in the charging hopper of microwave plasma torch system, and make the porcelain ball freely fall into the microwave plasma torch of 3000 ~ 5000 ℃ with the flow of 80 ~ 120g/min, rapid melting becomes glass metal to be dropped in deionized water, and obtaining particle diameter after cold quenching is the amorphous glass porcelain of 15～500 μ m;
D, pulverizing, drying
The amorphous glass porcelain after airflow milling is pulverized, then is obtained LTCC amorphous glass porcelain powder product with wet ball grinding, oven dry.
2. microwave plasma torch according to claim 1 prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that solvent described in steps A is deionized water or dehydrated alcohol.
3. microwave plasma torch according to claim 1 prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that described in step B, high polymer binder is selected from polyvinyl butyral acetal or polyvinyl alcohol, and the concentration of its aqueous solution is 8 ~ 12wt%.
4. microwave plasma torch according to claim 1 prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that described in step B, granulation refers to: adopt the rotating-expressing type granulator granulation to become the particle of φ 1 ~ 3mm.
5. microwave plasma torch according to claim 1 prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that described in step B, binder removal refers to: particle is warmed up to 250 ℃ of insulations 2 hours with the heat-up rate of 1 ℃/min, then is warmed up to 500 ℃ of insulations 4 hours.
6. microwave plasma torch according to claim 1 prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that the homo(io)thermism of the hopper of charging described in step C is at 780 ~ 850 ℃.
7. microwave plasma torch according to claim 1 prepares the processing method of LTCC amorphous glass porcelain powder, it is characterized in that the temperature of deionized water described in step C remains on below 45 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110125584 CN102276151B (en) | 2011-05-16 | 2011-05-16 | Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110125584 CN102276151B (en) | 2011-05-16 | 2011-05-16 | Technological method for preparing LTCC (low temperature co-fired ceramic) amorphous glass ceramic powder with microwave plasma torch |
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| Publication Number | Publication Date |
|---|---|
| CN102276151A CN102276151A (en) | 2011-12-14 |
| CN102276151B true CN102276151B (en) | 2013-05-08 |
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| CN103360793A (en) * | 2012-03-27 | 2013-10-23 | 重庆市锦艺硅材料开发有限公司苏州分公司 | Low-dielectric constant filler and preparation technology thereof |
| CN104496424A (en) * | 2014-12-02 | 2015-04-08 | 佛山铭乾科技有限公司 | Glass ceramic and preparation method thereof |
| CN107555764B (en) * | 2017-09-22 | 2021-08-06 | 中国建材国际工程集团有限公司 | Preparation method of glass batch |
| CN112573831A (en) * | 2020-12-08 | 2021-03-30 | 赣州中瓷科技有限公司 | Glass bead for fixing filament of incandescent lamp and preparation process thereof |
| CN114049983B (en) * | 2021-12-27 | 2022-04-08 | 西安宏星电子浆料科技股份有限公司 | Chip resistor paste with high resistance concentration and preparation method thereof |
| CN115180806A (en) * | 2022-08-03 | 2022-10-14 | 南京高新经纬电气有限公司 | Glass state material manufacturing process |
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| US5258335A (en) * | 1988-10-14 | 1993-11-02 | Ferro Corporation | Low dielectric, low temperature fired glass ceramics |
| CN1189410C (en) * | 2002-07-12 | 2005-02-16 | 清华大学 | Formula and prepn process of glass ceramics for HF chip inductor |
| KR100522135B1 (en) * | 2003-04-02 | 2005-10-18 | 한국과학기술연구원 | Low dielectric constant, low temperature fired ceramics |
| CN101215157B (en) * | 2008-01-11 | 2011-08-17 | 清华大学 | Fluorine silicon aluminum doping glass-base low-temperature cofired ceramic material and preparing method thereof |
| CN101913850A (en) * | 2010-07-06 | 2010-12-15 | 电子科技大学 | Preparation method of high-magnetic-conductivity low-temperature-sintering Z-shaped hexagonal ferrite material |
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