CN109437863A - A kind of high intensity HTCC ceramic material and preparation method thereof - Google Patents
A kind of high intensity HTCC ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high intensity HTCC ceramic materials and preparation method thereof, are related to high-temperature co-fired ceramics shell production field.High-intensitive HTCC ceramic material includes: micron grade aluminum oxide 60%~90%, submicron order aluminium oxide 0.1%~30%, kaolin 3%~5%, talcum powder 3%~5%, chrome green 1%~3%, molybdenum trioxide 1%~3%, yttrium oxide 0.1%~1% according to weight percent.Preparation method includes: to mix in proportion each component in raw material；Curtain coating auxiliary agent drying and moulding is added；Sinter fine and close ceramic material at 1500 DEG C~1600 DEG C.The present invention passes through the introducing of submicron order aluminium oxide, reduces the porosity of ceramic material, improves the consistency and bending strength of ceramic material.
Description
Technical field
The invention belongs to high temperature multilayer co-firing ceramic shell manufacture technology field, in particular to a kind of high intensity HTCC ceramics
Material and preparation method thereof.
Background technique
As integrated circuit is gradually to extensive and ultra-large development, in order to meet weaponry, space flight and aviation
Demand, it is necessary to develop small in size, light-weight all kinds of device ceramic package shells.Portable hyundai electronics high at the same time produce
Product also need to realize slim small and exquisite surface mount, band in addition to having the characteristics such as low conduction impedance, low switching losses, low thermal resistance
Dynamic middle small scale integrated circuit and semi-conductor discrete device ceramic shell Xiang Geng little, thinner, the better chip-scale of heat dissipation performance
Encapsulation development.
For the application for adapting to current small hermetic ceramic shell, it is necessary to improve density and the intensity of ceramic material to realize
Slimming, lightweight.The package casing mechanical strength of traditional ceramics material production is relatively low, in constant acceleration, mechanical punching
The accidental ceramic matrix fracture in test such as hit, to occur encapsulating the failure phenomenons such as gas leakage, wiring open circuit；In the machine system limit
Accidental cause ceramics micro-crack in test, to cause lead to fall off, weld the failure phenomenons such as frame layering.In addition, traditional ceramics material system
The package casing consistency of work is insufficient, is easy occur the failure phenomenons such as internal steam is exceeded, hydrogen content is exceeded because of outgassing.
Summary of the invention
In order to solve the problems in the prior art, the present invention provides a kind of high intensity HTCC ceramic material and its preparation sides
Method.
To achieve the above object, the invention adopts the following technical scheme:
A kind of high intensity HTCC ceramic material, composed of the following components according to weight percent:
The micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 1~10 μm, specific surface area be 0.5~
3m2/g。
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 0.1~1 μm, specific surface area be 3~
10m2/g。
The kaolin, talcum powder, chrome green, molybdenum trioxide and yttrium oxide median be 1~10 μm.
The preparation method of above-mentioned high-intensitive HTCC ceramic material, comprising the following steps:
A, each component in raw material is mixed in proportion；
B, curtain coating auxiliary agent drying and moulding is added；
C, fine and close ceramic material is sintered at 1500 DEG C~1600 DEG C.
In the step a, incorporation time be 12~for 24 hours.
In the step b, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In the step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
In the step b, drying temperature is 25 DEG C~105 DEG C.
In the step c, sintering time is 2~6h.
Compared with prior art, the invention has the following advantages:
1, the present invention passes through the introducing of submicron order aluminium oxide, reduces the grain size of ceramic material, increases crystal boundary
Quantity extends crack propagation path in fracture process, the fracture toughness and work to break of ceramic material is improved, to improve
The bending strength of material；
2, the present invention passes through the introducing of submicron order aluminium oxide, so that little crystal grain is effectively filled between big crystal grain, drop
The low porosity of ceramic material, improve ceramic material at porcelain density；
3, the present invention passes through the introducing of submicron order aluminium oxide, improves the sintering activity of ceramic material, makes it lower
At a temperature of densification saved the energy at porcelain, and extend the service life of sintering furnace.
Detailed description of the invention
Fig. 1 is the surface sem analysis figure using the made ceramic material of the method for the present invention；
Fig. 2 is the surface sem analysis figure using the made ceramic material of conventional method.
Specific embodiment
Below with reference to embodiment, the present invention will be further explained.
Embodiment 1
A kind of high intensity HTCC ceramic material, includes: micron grade aluminum oxide 85%, submicron order oxygen according to weight percent
Change aluminium 5%, kaolin 3%, talcum powder 3%, chrome green 2%, molybdenum trioxide 1.5%, yttrium oxide 0.5%；
Wherein: the micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 1~10 μm, specific surface area is
0.5~3m2/g。
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 0.1~1 μm, specific surface area be 3~
10m2/g。
The kaolin, talcum powder, chrome green, molybdenum trioxide, yttrium oxide median be 1~10 μm.
A kind of high intensity HTCC ceramic material preparation method, comprising the following steps:
A) each component in raw material is mixed in proportion into 12h；
B) curtain coating auxiliary agent is added in 35 DEG C~105 DEG C drying and mouldings；
C) it is sintered 2h at 1600 DEG C and fine and close ceramic material is made；
Wherein, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
Using the major technique of high intensity HTCC ceramic material made from raw material component proportion in embodiment 1 and preparation method
Index is as follows:
At porcelain color: black,
At porcelain density >=3.83g/cm3,
Bending strength >=500MPa.
Embodiment 2
A kind of high intensity HTCC ceramic material, includes: micron grade aluminum oxide 80%, submicron order oxygen according to weight percent
Change aluminium 10%, kaolin 3%, talcum powder 3%, chrome green 2%, molybdenum trioxide 1.5%, yttrium oxide 0.5%；
Wherein: the micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 1~5 μm, specific surface area is
0.5~2m2/g。
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 0.1~0.5 μm, specific surface area 3
~5m2/g。
The kaolin, talcum powder, chrome green, molybdenum trioxide, yttrium oxide median be 1~5 μm.
A kind of high intensity HTCC ceramic material preparation method, comprising the following steps:
A) each component in raw material is mixed in proportion into 16h；
B) curtain coating auxiliary agent is added in 30 DEG C~100 DEG C drying and mouldings；
C) it is sintered 2h at 1580 DEG C and fine and close ceramic material is made；
Wherein, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
Using the major technique of high intensity HTCC ceramic material made from raw material component proportion in embodiment 2 and preparation method
Index is as follows:
At porcelain color: black,
At porcelain density >=3.83g/cm3,
Bending strength >=500MPa.
Embodiment 3
A kind of high intensity HTCC ceramic material, includes: micron grade aluminum oxide 75%, submicron order oxygen according to weight percent
Change aluminium 15%, kaolin 3%, talcum powder 3%, chrome green 2%, molybdenum trioxide 1.5%, yttrium oxide 0.5%；
Wherein: the micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 5~10 μm, specific surface area 2
~3m2/g；
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 0.5~1 μm, specific surface area be 6~
10m2/g；
The kaolin, talcum powder, chrome green, molybdenum trioxide, yttrium oxide median be 3~10 μm.
A kind of high intensity HTCC ceramic material preparation method, comprising the following steps:
A) each component in raw material is mixed in proportion for 24 hours；
B) curtain coating auxiliary agent is added in 25 DEG C~95 DEG C drying and mouldings；
C) it is sintered 2h at 1560 DEG C and fine and close ceramic material is made.
Wherein, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
Using the major technique of high intensity HTCC ceramic material made from raw material component proportion in embodiment 3 and preparation method
Index is as follows:
At porcelain color: black,
At porcelain density >=3.83g/cm3,
Bending strength >=500Mpa.
Embodiment 4
A kind of high intensity HTCC ceramic material, includes: micron grade aluminum oxide 60%, submicron order oxygen according to weight percent
Change aluminium 30%, kaolin 4%, talcum powder 3%, chrome green 1%, molybdenum trioxide 1.9%, yttrium oxide 0.1%；
Wherein: the micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 4 μm, specific surface area 2m2/
g；
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 1 μm, specific surface area 6m2/g；
The kaolin, talcum powder, chrome green, molybdenum trioxide, yttrium oxide median be 4 μm.
A kind of high intensity HTCC ceramic material preparation method, comprising the following steps:
A) each component in raw material is mixed in proportion for 24 hours；
B) curtain coating auxiliary agent is added in 25 DEG C of drying and mouldings；
C) it is sintered 6h at 1500 DEG C and fine and close ceramic material is made.
Wherein, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
Using the major technique of high intensity HTCC ceramic material made from raw material component proportion in embodiment 4 and preparation method
Index is as follows:
At porcelain color: black,
At porcelain density >=3.83g/cm3,
Bending strength >=500Mpa.
Embodiment 5
A kind of high intensity HTCC ceramic material, includes: micron grade aluminum oxide 90%, submicron order oxygen according to weight percent
Change aluminium 0.1%, kaolin 3%, talcum powder 4%, chrome green 1%, molybdenum trioxide 1%, yttrium oxide 0.9%；
Wherein: the micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 1 μm, specific surface area is
0.5m2/g；
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 0.6 μm, specific surface area 3m2/g；
The kaolin, talcum powder, chrome green, molybdenum trioxide, yttrium oxide median be 1 μm.
A kind of high intensity HTCC ceramic material preparation method, comprising the following steps:
A) each component in raw material is mixed in proportion into 18h；
B) curtain coating auxiliary agent is added in 95 DEG C of drying and mouldings；
C) it is sintered 5h at 1580 DEG C and fine and close ceramic material is made.
Wherein, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
Using the major technique of high intensity HTCC ceramic material made from raw material component proportion in embodiment 5 and preparation method
Index is as follows:
At porcelain color: black,
At porcelain density >=3.83g/cm3,
Bending strength >=500Mpa.
Embodiment 6
A kind of high intensity HTCC ceramic material, includes: micron grade aluminum oxide 70%, submicron order oxygen according to weight percent
Change aluminium 13.5%, kaolin 5%, talcum powder 5%, chrome green 3%, molybdenum trioxide 3%, yttrium oxide 0.5%；
Wherein: the micron grade aluminum oxide be α phase, purity be greater than 99.8, median be 10 μm, specific surface area 3m2/
g；
The submicron order aluminium oxide be α phase, purity be greater than 99.8, median be 1 μm, specific surface area 10m2/g；
The kaolin, talcum powder, chrome green, molybdenum trioxide, yttrium oxide median be 10 μm.
A kind of high intensity HTCC ceramic material preparation method, comprising the following steps:
A) each component in raw material is mixed in proportion into 12h；
B) curtain coating auxiliary agent is added in 105 DEG C of drying and mouldings；
C) it is sintered 2h at 1600 DEG C and fine and close ceramic material is made.
Wherein, according to mass percent, it is composed of the following components to be cast auxiliary agent:
In step b, the mass ratio of the raw material of curtain coating auxiliary agent and HTCC ceramic material is 3:7.
Using the major technique of high intensity HTCC ceramic material made from raw material component proportion in embodiment 6 and preparation method
Index is as follows:
At porcelain color: black,
At porcelain density >=3.83g/cm3,
Bending strength >=500Mpa.
Using high intensity HTCC ceramic material surfaces SEM made from raw material component proportion in embodiment 1-6 and preparation method
Analysis chart is shown in Fig. 1, it can be seen that little crystal grain is effectively filled between big crystal grain from 1 figure, intercrystalline is tightly combined, after tested
The bending strength of ceramic material has reached 500MPa.
Fig. 2 is shown in using ceramic material surfaces sem analysis figure prepared by conventional method, as can be seen from the figure partial particulate is in
Existing subgrain is grown up, and there are holes for intercrystalline, and the bending strength of ceramic material is less than 400MPa after tested.
The above is only a preferred embodiment of the present invention, it should be pointed out that: for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of high intensity HTCC ceramic material, it is characterised in that: composed of the following components according to weight percent:
2. high intensity HTCC ceramic material according to claim 1, it is characterised in that: the micron grade aluminum oxide be α phase,
Purity be greater than 99.8, median be 1~10 μm, specific surface area is 0.5~3m2/g。
3. high intensity HTCC ceramic material according to claim 1, it is characterised in that: the submicron order aluminium oxide is α
Phase, purity be greater than 99.8, median be 0.1~1 μm, specific surface area is 3~10m2/g。
4. high intensity HTCC ceramic material according to claim 1, it is characterised in that: the kaolin, talcum powder, three oxygen
The median for changing two chromium, molybdenum trioxide and yttrium oxide is 1~10 μm.
5. the preparation method of high intensity HTCC ceramic material according to claim 1 to 4, which is characterized in that including with
Lower step:
A, each component in raw material is mixed in proportion；
B, curtain coating auxiliary agent drying and moulding is added；
C, fine and close ceramic material is sintered at 1500 DEG C~1600 DEG C.
6. a kind of preparation method of high intensity HTCC ceramic material according to claim 5, it is characterised in that: the step
In a, incorporation time be 12~for 24 hours.
7. a kind of preparation method of high intensity HTCC ceramic material according to claim 5, it is characterised in that: the step
In rapid b, according to mass percent, it is composed of the following components to be cast auxiliary agent:
8. a kind of preparation method of high intensity HTCC ceramic material according to claim 5 or 7, it is characterised in that: described
Step b in, curtain coating auxiliary agent and HTCC ceramic material raw material mass ratio be 3:7.
9. a kind of preparation method of high intensity HTCC ceramic material according to claim 5, it is characterised in that: the step
In b, drying temperature is 25 DEG C~105 DEG C.
10. a kind of preparation method of high intensity HTCC ceramic material according to claim 5, it is characterised in that: the step
In rapid c, sintering time is 2~6h.
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| CN201811624190.9A CN109437863A (en) | 2018-12-28 | 2018-12-28 | A kind of high intensity HTCC ceramic material and preparation method thereof |
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| CN201811624190.9A CN109437863A (en) | 2018-12-28 | 2018-12-28 | A kind of high intensity HTCC ceramic material and preparation method thereof |
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| CN112850733A (en) * | 2021-03-01 | 2021-05-28 | 江苏省宜兴电子器件总厂有限公司 | HTCC packaging tube shell glass pigment, preparation method and application |
| CN116332627A (en) * | 2023-02-14 | 2023-06-27 | 西安航科创星电子科技有限公司 | Low-thermal expansion coefficient high-temperature co-fired ceramic (HTCC) material and preparation method thereof |
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| CN112850733B (en) * | 2021-03-01 | 2023-06-09 | 江苏省宜兴电子器件总厂有限公司 | HTCC packaging tube shell glass pigment, preparation method and application |
| CN116332627A (en) * | 2023-02-14 | 2023-06-27 | 西安航科创星电子科技有限公司 | Low-thermal expansion coefficient high-temperature co-fired ceramic (HTCC) material and preparation method thereof |
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