CN102503137A - Calcium-aluminum-boron-silicon glass and fused quartz low-temperature co-fired ceramic material and preparation method thereof - Google Patents
Calcium-aluminum-boron-silicon glass and fused quartz low-temperature co-fired ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a calcium-aluminum-boron-silicon glass and fused quartz low-temperature co-fired ceramic material and a preparation method thereof. In the ceramic material, the calcium-aluminum-boron-silicon low-melting-point glass phase accounts for 50-70% of the total material mass. The preparation method comprises the steps of: weighing raw materials according to the molar percentages of oxides required by the low-melting-point glass phase, maintaining the temperature at 1500-1600 DEG C for 3-5 hours, directly pouring the molten glass into deionized water to obtain glass slag, and ball-milling to obtain glass powder with average granularity of 1-3 mu m; ball-milling fused quartz to obtain fused quartz powder with average granularity of 3-5 mu m; uniformly mixing 50-70wt% of low-melting-point glass phase and high-melting-point ceramic filling phase, adding a polyvinyl alcohol adhesive accounting for 3wt% of the mixed material, granulating and carrying out dry pressing to obtain blank sheets; and sintering to obtain the low-temperature co-fired ceramic material. The obtained low-temperature co-fired ceramic material has low sintering temperature, and can be co-fired with gold, silver, copper and other conductor materials; the obtained material is high in densification degree, low porosity and lower in thermal expansion coefficient; and the process flow is simple and the cost is low.
Description
Technical field
The present invention relates to low-temperature co-burning ceramic material of a kind of low thermal coefficient of expansion and preparation method thereof, belong to the electronic package material field.
Background technology
Along with developing rapidly of microelectronics, electronic circuit develops to microminiaturized, integrated direction day by day.And that the development of Electronic Packaging technology does not form with it is supporting, becomes the bottleneck that restriction microelectronics continues development.(a kind of new Electronic Packaging technology as rising in recent years has received domestic and international scientific research personnel's extensive attention and research to LTCC for Low Temperature Cofired Ceramics, LTCC) technology.It relates to circuit layout, wide spectrums such as microwave technology, Materials science.Especially the material technology that plays a key effect has obtained paying attention to widely.
The LTCC technology mainly has the technical superiority of following several respects: (1) LTCC can be directly and metal in atmosphere, burn altogether, reduced process procedure.The gold and silver, copper etc. that (2) can adopt lower melting point, high conductivity are as conductor material.Therefore reduce cost, can obtain good performance again.(3) substrate flexible design.Comprising wiring flexibly, dielectric-constant adjustable, advantage such as the number of plies is variable.
Studying and main flow LTCC material that put into production mainly is divided into two types at present, i.e. sytull system and glass+ceramic systems.Sytull is that the LTCC material mainly is nucleation and the crystallisation process through glass, obtains fine and close stupalith.Its shortcoming is that crystallisation process is difficult to control, and material property is difficult to prediction, dielectric loss especially, and process window is narrow, and device stability is relatively poor, is unfavorable for producing in enormous quantities.
By comparison, glass+ceramic systems material has following advantage: (1) is mechanical property better.Because the mechanical property that the adding of phase has improved material is filled in the minimizing of amount of glass, pottery.(2) lower thermal expansivity, specific inductivity and dielectric loss.(3) easy to operate, easy to control.Can adjust the character of both ratio control gained materials through selecting suitable glass, ceramic phase for use
Through research for many years, the LTCC technology is increasingly mature, and domesticly still is in the starting stage.At present, the thermomechanical property of material is the principal element that influences the LTCC device reliability, and wherein most critical is thermal expansivity.LTCC packaged material and contained silicon substrate chip material thermal expansivity (3.5 * 10
-6/ ℃) coupling can reduce mechanical stress, thereby guarantee the thermostability of system.Therefore exploitation has the LTCC material of low thermal coefficient of expansion, and to realizing the miniaturized of microelectronic product, high-performance and safety are significant.Simultaneously, LTCC material (＜1000 ℃) at a lower temperature reaches higher density, and generally speaking, the void content of material should be less than 5%.
Summary of the invention
The objective of the invention is to develop a kind of low-temperature co-burning ceramic material with low thermal coefficient of expansion.It is simple that another object of the present invention provides a kind of technology, this preparation methods with low cost.
Technology of the present invention is following:
A kind of calcium aluminium borosilicate is glass+fused quartz low-temperature co-burning ceramic material, low-temperature co-burning ceramic material comprise low melting glass mutually with the filling of HMP pottery mutually, wherein to account for the massfraction of overall material mutually be 50～70% to calcium aluminium borosilicate low melting glass.
Described low-temperature co-burning ceramic material, low melting glass mutually in the molar content of each oxide compound following:
The preparation method of described low-temperature co-burning ceramic material of the present invention, step is following:
(1) raw material of low melting glass is prepared: the molar content by mutually required each oxide compound of low melting glass takes by weighing raw material, and mixes;
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 3～5 hours down at 1500～1600 ℃, the fused glass metal is directly poured in the deionized water, obtain the glass slag; Ball milling makes the glass powder that mean particle size is 1～3 μ m;
(3) the HMP pottery is filled the preparation of phase: behind the fused quartz powder ball milling, obtain the fused quartz powder that mean particle size is 3～5 μ m;
(4) forming materials: with the low melting glass of 50～70% weight percents mutually with the HMP pottery fill mix mutually after, 3% polyvinyl alcohol adhesive of the weight of adding mixing material is processed the base sheet after the granulation dry-pressing;
(5) sintering: gained base sheet at 900～1000 ℃ of following sintering, is made low-temperature co-burning ceramic material.
The ball-to-powder weight ratio of said ball milling is 3: 1, and ball-milling medium is a deionized water.
Described sintering process is, do not separate out under the situation of silicon-dioxide crystalline phase guaranteeing, is warming up to temperature requiredly, is incubated after 1 hour, in stove, naturally cools to room temperature.
The invention has the advantages that: the low-temperature co-burning ceramic material sintering temperature is low, at (900～1000) ℃ realization sintering, therefore can burn altogether with conductor materials such as gold and silver, copper; Gained material densification degree is high, and void content is low, and is as shown in Figure 1; Technical process is simple, and is with low cost; The gained material has lower thermal expansivity.
Description of drawings
Fig. 1 is the SEM figure of low-temperature co-burning ceramic material among the embodiment 3 among the present invention.
Embodiment
Embodiment 1:
In the specific embodiment of the invention, the mole percent level of each oxide compound is following in the calcium aluminium borosilicate glass:
The preparation method of low-temperature co-burning ceramic material in the present embodiment may further comprise the steps:
(1) raw material of low melting glass is prepared: the molar content by above-mentioned each oxide compound takes by weighing lower melting point calcium aluminium borosilicate glass desired raw material, and mixes.
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 4 hours down at 1500 ℃; The fused glass metal is directly poured in the deionized water, obtained the glass slag, (ball-to-powder weight ratio is 3: 1 behind the ball milling; Ball-milling medium is a deionized water), make the glass powder that mean particle size is 3 μ m.
(3) the HMP pottery is filled the preparation of phase: with (ball-to-powder weight ratio is 3: 1, and ball-milling medium is a deionized water) behind the fused quartz powder ball milling of buying, obtain the fused quartz powder that mean particle size is 4 μ m
(4) forming materials: with the low melting glass of 70wt% mutually with the HMP pottery fill mix mutually after, adding 3wt% polyvinyl alcohol adhesive is processed the base sheet after the granulation dry-pressing.
(5) sintering: gained base sheet at 900 ℃ of following sintering, is incubated after 1 hour, in stove, naturally cools to room temperature, make low-temperature co-burning ceramic material.
The thermal expansivity of obtained low-temperature co-burning ceramic material is 4.70 * 10 in the present embodiment
-6/ ℃.The void content of this material is 18.6%.
Embodiment 2:
In the specific embodiment of the invention, the mole percent level of each oxide compound is following in the calcium aluminium borosilicate glass:
The preparation method of low-temperature co-burning ceramic material in the present embodiment may further comprise the steps:
(1) raw material of low melting glass is prepared: the molar content by above-mentioned each oxide compound takes by weighing lower melting point calcium aluminium borosilicate glass desired raw material, and mixes.
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 4 hours down at 1550 ℃; The fused glass metal is directly poured in the deionized water, obtained the glass slag, (ball-to-powder weight ratio is 3: 1 behind the ball milling; Ball-milling medium is a deionized water), make the glass powder that mean particle size is 1 μ m.
(3) the HMP pottery is filled the preparation of phase: with (ball-to-powder weight ratio is 3: 1, and ball-milling medium is a deionized water) behind the fused quartz powder ball milling of buying, obtain the fused quartz powder that mean particle size is 3 μ m
(4) forming materials: with the low melting glass of 70wt% mutually with the HMP pottery fill mix mutually after, add 3% polyvinyl alcohol adhesive of the weight of material after mixing, process the base sheet after the granulation dry-pressing.
(5) sintering: gained base sheet at 900 ℃ of following sintering, is incubated after 1 hour, in stove, naturally cools to room temperature, make low-temperature co-burning ceramic material.
The thermal expansivity of obtained low-temperature co-burning ceramic material is 6.2 * 10 in the present embodiment
-6/ ℃.The void content of this material is 1.1%.
Embodiment 3:
In the specific embodiment of the invention, the mole percent level of each oxide compound is following in the calcium aluminium borosilicate glass:
The preparation method of low-temperature co-burning ceramic material in the present embodiment may further comprise the steps:
(1) raw material of low melting glass is prepared: the molar content by above-mentioned each oxide compound takes by weighing lower melting point calcium aluminium borosilicate glass desired raw material, and mixes.
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 5 hours down at 1550 ℃; The fused glass metal is directly poured in the deionized water, obtained the glass slag, (ball-to-powder weight ratio is 3: 1 behind the ball milling; Ball-milling medium is a deionized water), make the glass powder that mean particle size is 1.5 μ m.
(3) the HMP pottery is filled the preparation of phase: with (ball-to-powder weight ratio is 3: 1, and ball-milling medium is a deionized water) behind the fused quartz powder ball milling of buying, obtain the fused quartz powder that mean particle size is 4 μ m
(4) forming materials: with the low melting glass of 70wt% mutually with the HMP pottery fill mix mutually after, adding 3wt% polyvinyl alcohol adhesive is processed the base sheet after the granulation dry-pressing.
(5) sintering: gained base sheet at 900 ℃ of following sintering, is incubated after 1 hour, in stove, naturally cools to room temperature, make low-temperature co-burning ceramic material.
The thermal expansivity of obtained low-temperature co-burning ceramic material is 4.80 * 10 in the present embodiment
-6/ ℃.The void content of this material is 2.2%.The SEM figure of this instance sees accompanying drawing 1.
Embodiment 4:
In the specific embodiment of the invention, the mole percent level of each oxide compound is following in the calcium aluminium borosilicate glass:
The preparation method of low-temperature co-burning ceramic material in the present embodiment may further comprise the steps:
(1) raw material of low melting glass is prepared: the molar content by above-mentioned each oxide compound takes by weighing lower melting point calcium aluminium borosilicate glass desired raw material, and mixes.
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 3 hours down at 1600 ℃; The fused glass metal is directly poured in the deionized water, obtained the glass slag, (ball-to-powder weight ratio is 3: 1 behind the ball milling; Ball-milling medium is a deionized water), make the glass powder that mean particle size is 3 μ m.
(3) the HMP pottery is filled the preparation of phase: with (ball-to-powder weight ratio is 3: 1, and ball-milling medium is a deionized water) behind the fused quartz powder ball milling of buying, obtain the fused quartz powder that mean particle size is 5 μ m
(4) forming materials: with the low melting glass of 70wt% mutually with the HMP pottery fill mix mutually after, adding 3wt% polyvinyl alcohol adhesive is processed the base sheet after the granulation dry-pressing.
(5) sintering: gained base sheet at 900 ℃ of following sintering, is incubated after 1 hour, in stove, naturally cools to room temperature, make low-temperature co-burning ceramic material.
The thermal expansivity of obtained low-temperature co-burning ceramic material is 7.95 * 10 in the present embodiment
-6/ ℃.The void content of this material is 2.9%.
Embodiment 5:
In the specific embodiment of the invention, the mole percent level of each oxide compound is following in the calcium aluminium borosilicate glass:
The preparation method of low-temperature co-burning ceramic material in the present embodiment may further comprise the steps:
(1) raw material of low melting glass is prepared: the molar content by above-mentioned each oxide compound takes by weighing lower melting point calcium aluminium borosilicate glass desired raw material, and mixes.
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 4 hours down at 1550 ℃; The fused glass metal is directly poured in the deionized water, obtained the glass slag, (ball-to-powder weight ratio is 3: 1 behind the ball milling; Ball-milling medium is a deionized water), make the glass powder that mean particle size is 1 μ m.
(3) the HMP pottery is filled the preparation of phase: with (ball-to-powder weight ratio is 3: 1, and ball-milling medium is a deionized water) behind the fused quartz powder ball milling of buying, obtain the fused quartz powder that mean particle size is 3 μ m
(4) forming materials: with the low melting glass of 50wt% mutually with the HMP pottery fill mix mutually after, adding 3wt% polyvinyl alcohol adhesive is processed the base sheet after the granulation dry-pressing.
(5) sintering: gained base sheet at 1000 ℃ of following sintering, is incubated after 1 hour, in stove, naturally cools to room temperature, make low-temperature co-burning ceramic material.
The thermal expansivity of obtained low-temperature co-burning ceramic material is 4.95 * 10 in the present embodiment
-6/ ℃.The void content of this material is 4.4%.
Embodiment 6:
In the specific embodiment of the invention, the mole percent level of each oxide compound is following in the calcium aluminium borosilicate glass:
The preparation method of low-temperature co-burning ceramic material in the present embodiment may further comprise the steps:
(1) raw material of low melting glass is prepared: the molar content by above-mentioned each oxide compound takes by weighing lower melting point calcium aluminium borosilicate glass desired raw material, and mixes.
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 5 hours down at 1550 ℃; The fused glass metal is directly poured in the deionized water, obtained the glass slag, (ball-to-powder weight ratio is 3: 1 behind the ball milling; Ball-milling medium is a deionized water), make the glass powder that mean particle size is 1.5 μ m.
(3) the HMP pottery is filled the preparation of phase: with (ball-to-powder weight ratio is 3: 1, and ball-milling medium is a deionized water) behind the fused quartz powder ball milling of buying, obtain the fused quartz powder that mean particle size is 4 μ m
(4) forming materials: with the low melting glass of 60wt% mutually with the HMP pottery fill mix mutually after, adding 3wt% polyvinyl alcohol adhesive is processed the base sheet after the granulation dry-pressing.
(5) sintering: gained base sheet at 950 ℃ of following sintering, is incubated after 1 hour, in stove, naturally cools to room temperature, make low-temperature co-burning ceramic material.
The thermal expansivity of obtained low-temperature co-burning ceramic material is 4.75 * 10 in the present embodiment
-6/ ℃.The void content of this material is 1.3%.
A kind of calcium aluminium borosilicate that the present invention proposes is glass+fused quartz system low-temperature co-burning ceramic material and preparation method thereof; Be described through embodiment; Person skilled obviously can be changed or suitably change and combination content as herein described in not breaking away from content of the present invention, spirit and scope, realizes the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as and are included in spirit of the present invention, scope and the content.
Claims (5)
1. a calcium aluminium borosilicate is glass+fused quartz low-temperature co-burning ceramic material; It is characterized in that low-temperature co-burning ceramic material comprise low melting glass mutually with the filling of HMP pottery mutually, wherein to account for the massfraction of overall material mutually be 50～70% to calcium aluminium borosilicate low melting glass.
2. low-temperature co-burning ceramic material according to claim 1 is characterized in that, low melting glass mutually in the molar content of each oxide compound following:
3. the preparation method of low-temperature co-burning ceramic material according to claim 1 and 2, its characterization step is following:
(1) raw material of low melting glass is prepared: the molar content by mutually required each oxide compound of low melting glass takes by weighing raw material, and mixes;
(2) preparation of low melting glass: with the above-mentioned mixture that the mixes crucible of packing into; Be incubated 3～5 hours down at 1500～1600 ℃, the fused glass metal is directly poured in the deionized water, obtain the glass slag; Ball milling makes the glass powder that mean particle size is 1～3 μ m;
(3) the HMP pottery is filled the preparation of phase: behind the fused quartz powder ball milling, obtain the fused quartz powder that mean particle size is 3～5 μ m;
(4) forming materials: with the low melting glass of 50～70% weight percents mutually with the HMP pottery fill mix mutually after, 3% polyvinyl alcohol adhesive of the weight of adding mixing material is processed the base sheet after the granulation dry-pressing;
(5) sintering: gained base sheet at 900～1000 ℃ of following sintering, is made low-temperature co-burning ceramic material.
4. the preparation method of the low-temperature co-burning ceramic material of stating according to claim 3 is characterized in that the ball-to-powder weight ratio of said ball milling is 3: 1, and ball-milling medium is a deionized water.
5. the preparation method of the low-temperature co-burning ceramic material of stating according to claim 3 is characterized in that described sintering process is, does not separate out under the situation of silicon-dioxide crystalline phase guaranteeing, is warming up to temperature requiredly, is incubated after 1 hour, in stove, naturally cools to room temperature.
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| CN103086703A (en) * | 2013-01-30 | 2013-05-08 | 云南云天化股份有限公司 | Material and method for preparing low-temperature co-fired ceramic with high anti-bending strength |
| CN103979941A (en) * | 2014-05-07 | 2014-08-13 | 云南云天化股份有限公司 | Low-temperature co-fired ceramic and preparation method thereof |
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| 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 |
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| CN108996902A (en) * | 2018-09-19 | 2018-12-14 | 深圳市晶特智造科技有限公司 | A kind of low-temperature co-burning ceramic material and preparation method thereof |
| CN111470778A (en) * | 2019-01-24 | 2020-07-31 | 上海晶材新材料科技有限公司 | Calcium barium silicon aluminum glass-based low-dielectric low-temperature co-fired ceramic material and preparation method thereof |
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