CN108503230A - A kind of package substrate composite material and preparation method - Google Patents
A kind of package substrate composite material and preparation method Download PDFInfo
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- CN108503230A CN108503230A CN201810376514.5A CN201810376514A CN108503230A CN 108503230 A CN108503230 A CN 108503230A CN 201810376514 A CN201810376514 A CN 201810376514A CN 108503230 A CN108503230 A CN 108503230A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/02—Pretreated ingredients
- C03C1/026—Pelletisation or prereacting of powdered raw materials
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/04—Particles; Flakes
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/16—Microcrystallites, e.g. of optically or electrically active material
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2214/00—Nature of the non-vitreous component
- C03C2214/30—Methods of making the composites
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Abstract
The present invention provides a kind of package substrate composite material and preparation methods.It is made of following steps：By carbon nanohorn, giantreed charcoal and silicon powder mixed grinding；Guar gum, polyethylene glycol and deionized water stirring, dry, sieving is added；Deionized water, absolute ethyl alcohol and water-soluble polyacrylamide ball milling is added, spray drying forms composite spheroidal particle；It is encapsulated with plastic film after dry-pressing formed, cold isostatic compaction；It is placed in graphite crucible and is sintered to obtain powder A；By silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and deionized water mixing and ball milling；It is sieved after drying, is sintered to obtain glass powder；By powder A, glass powder and deionized water mixing and ball milling, sieving；Lubricant, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added to continue to grind；Compression moulding；Sintering, cooling to obtain the final product.The package substrate composite material of the present invention has higher dielectric constant, very low dielectric loss value and good mechanical property, bending strength high.
Description
Technical field
The present invention relates to package substrate fields, and in particular to a kind of package substrate composite material and preparation method.
Background technology
With the fast development of science and technology, panoramic electronic product, equipment and system are continuously emerged in large numbers.It is each from each row
The automatic control system of industry, the various electric appliances used to family, without not comprising a large amount of electronic circuit.Various electronic components and
Its sensor makes rapid progress, and plays irreplaceable role in national economy and each field of national defence, in people's lives
It has been more and more widely used.In current information and era of knowledge-driven economy, electronic industry has become the important warp of countries in the world
Ji growth point, pushes global economy to flourish.At the same time, the minimizing of electronic product, integrated and digitlization are to envelope
Fill the requirement standard of substrate also further harsh.Package substrate carries, consolidates electronic component, between chip and printed circuit board
Electrical connection is provided by the circuitous pattern of substrate surface or inside, while can be with mechanical support, insulation, heat radiation protection core
Piece is significant to the development of electronic industry.Dielectric constant height is worked out, the good package substrate of mechanical property becomes it in weight
Weight.
Invention content
Technical problems to be solved：The object of the present invention is to provide a kind of package substrate composite materials, have higher Jie
Electric constant, very low dielectric loss value and good mechanical property, bending strength are high.
Technical solution：A kind of package substrate composite material is prepared by following component with parts by weight：Silica 50-
70 parts, 18-25 parts of carbon nanohorn, 1-2 parts of giantreed charcoal, 10-15 parts of spodumene, 10-15 parts of silicon powder, 3-5 parts of Fluorspar Powder,
30-40 parts of boric acid, 2-3 parts of barium carbonate, 2-3 parts of lubricant, 0.2-0.5 parts of guar gum, 0.1-0.3 parts of polyethylene glycol, acrylic acid
10-20 parts, 2-4 parts of polyvinylpyrrolidone, 2-4 parts of phlogopite crystallite, 4-8 parts of water-soluble polyacrylamide, absolute ethyl alcohol 28-
40 parts.
Further, a kind of package substrate composite material, is prepared by following component with parts by weight：Silica 60
Part, 22 parts of carbon nanohorn, 1.5 parts of giantreed charcoal, 13 parts of spodumene, 13 parts of silicon powder, 4 parts of Fluorspar Powder, 35 parts of boric acid, carbonic acid
2.5 parts of barium, 2.5 parts of lubricant, 0.3 part of guar gum, 0.2 part of polyethylene glycol, 15 parts of acrylic acid, 3 parts of polyvinylpyrrolidone, gold
3 parts of mica crystallite, 6 parts of water-soluble polyacrylamide, 34 parts of absolute ethyl alcohol.
Further, the lubricant be castor oil, calcium sulfonate complex grease, glyceryl tristearate or beeswax in one kind or
It is several.
The preparation method of above-mentioned package substrate composite material includes the following steps：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, 22-24h is ground at rotating speed 170-180rpm using planetary ball mill,
In, ratio of grinding media to material 25:1；
(2) guar gum, polyethylene glycol and 50-70 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
15-18h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50-70 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
60-80min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 130-150 DEG C, and outlet temperature is
75-90 DEG C, pressure 0.08-0.1MPa；
(4) it is encapsulated, is placed in the oil cylinder of cold isostatic compaction machine, in the pressure of 250-270MPa with plastic film after dry-pressing formed
Lower pressurize 1-2min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 50-70 parts of deionized waters are mixed, is put into ball grinder
Ball milling 5-6h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3-4h in ball grinder, cross 40 mesh sieve, wherein mixing
Powder, water, ball mass ratio be 1:1:5；
(9) lubricant, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3-4h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Further, the preparation method of the giantreed charcoal is：
The first step：It is dried after giantreed is cleaned, is crushed to 40 mesh, be put into air dry oven in 105 DEG C of dry 5-8h；
Second step：10 parts of giantreed powder, 25 parts of pyrophosphoric acids and 30 parts of deionized waters are mixed, stirs evenly, impregnates 4- at room temperature
5h；
Third walks：Filtering, is transferred in Muffle furnace, the carbonization-activation 1h at 350-600 DEG C；
4th step：It is cooled to room temperature, is washed with distilled water to neutrality, be put into baking oven the drying at 100 DEG C, be ground to grain size ＜
20 μm to obtain the final product.
Advantageous effect：
1. the ceramic composition added in the present invention, which can enter in glass network, forms tetrahedron, increases bond energy, improve material
Mechanical performance.
2. barium carbonate is network outer body substance, it is added in system and has suspension, has the function of reducing viscosity, in a certain range
The densification of interior acceleration of sintering body improves the dielectric constant and bending strength of material of the present invention on the whole.
It is 6.26 3. material of the present invention has higher dielectric constant, very low dielectric loss value, only 4.65 × 10-3, together
When have good anti-bending strength, reach as high as 169.49MPa.
Specific implementation mode
Embodiment 1
A kind of package substrate composite material is prepared by following component with parts by weight：50 parts of silica, carbon nanohorn 18
Part, 1 part of giantreed charcoal, 10 parts of spodumene, 10 parts of silicon powder, 3 parts of Fluorspar Powder, 30 parts of boric acid, 2 parts of barium carbonate, lubricant 2
It is part, 0.2 part of guar gum, 0.1 part of polyethylene glycol, 10 parts of acrylic acid, 2 parts of polyvinylpyrrolidone, 2 parts of phlogopite crystallite, water-soluble
4 parts of polyacrylamide of property, 28 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, is ground 22h at rotating speed 170rpm using planetary ball mill, wherein ratio of grinding media to material
It is 25:1；
(2) guar gum, polyethylene glycol and 50 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
15h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
60min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 130 DEG C, and outlet temperature is 75 DEG C, pressure
Power is 0.08MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 250MPa
Press 1min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 50 parts of deionized waters are mixed, is put into ball in ball grinder
Grind 5h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3h in ball grinder, cross 40 mesh sieve, wherein mixed powder
Material, water, ball mass ratio be 1:1:5；
(9) beeswax, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Embodiment 2
A kind of package substrate composite material is prepared by following component with parts by weight：55 parts of silica, carbon nanohorn 20
Part, 1.5 parts of giantreed charcoal, 12 parts of spodumene, 12 parts of silicon powder, 4 parts of Fluorspar Powder, 35 parts of boric acid, 2.5 parts of barium carbonate, lubrication
2.5 parts of agent, 0.3 part of guar gum, 0.2 part of polyethylene glycol, 15 parts of acrylic acid, 2.5 parts of polyvinylpyrrolidone, phlogopite crystallite 3
Part, 5 parts of water-soluble polyacrylamide, 31 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, is ground 23h at rotating speed 175rpm using planetary ball mill, wherein ratio of grinding media to material
It is 25:1；
(2) guar gum, polyethylene glycol and 60 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
16h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 60 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
65min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 135 DEG C, and outlet temperature is 80 DEG C, pressure
Power is 0.09MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 260MPa
Press 1min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 60 parts of deionized waters are mixed, is put into ball in ball grinder
Grind 5.5h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3.5h in ball grinder, cross 40 mesh sieve, wherein mixing
Powder, water, ball mass ratio be 1:1:5；
(9) castor oil, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3.5h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Embodiment 3
A kind of package substrate composite material is prepared by following component with parts by weight：60 parts of silica, carbon nanohorn 22
Part, 1.5 parts of giantreed charcoal, 13 parts of spodumene, 13 parts of silicon powder, 4 parts of Fluorspar Powder, 35 parts of boric acid, 2.5 parts of barium carbonate, lubrication
2.5 parts of agent, 0.3 part of guar gum, 0.2 part of polyethylene glycol, 15 parts of acrylic acid, 3 parts of polyvinylpyrrolidone, 3 parts of phlogopite crystallite,
6 parts of water-soluble polyacrylamide, 34 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, is ground 23h at rotating speed 175rpm using planetary ball mill, wherein ratio of grinding media to material
It is 25:1；
(2) guar gum, polyethylene glycol and 60 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
17h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 60 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
70min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 140 DEG C, and outlet temperature is 85 DEG C, pressure
Power is 0.09MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 260MPa
Press 2min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 60 parts of deionized waters are mixed, is put into ball in ball grinder
Grind 6h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3.5h in ball grinder, cross 40 mesh sieve, wherein mixing
Powder, water, ball mass ratio be 1:1:5；
(9) calcium sulfonate complex grease, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 4h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Embodiment 4
A kind of package substrate composite material is prepared by following component with parts by weight：70 parts of silica, carbon nanohorn 25
Part, 2 parts of giantreed charcoal, 15 parts of spodumene, 15 parts of silicon powder, 5 parts of Fluorspar Powder, 40 parts of boric acid, 3 parts of barium carbonate, lubricant 3
Part, 0.5 part of guar gum, 0.1-0.3 parts of polyethylene glycol, 20 parts of acrylic acid, 4 parts of polyvinylpyrrolidone, 4 parts of phlogopite crystallite,
8 parts of water-soluble polyacrylamide, 40 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, is ground for 24 hours at rotating speed 180rpm using planetary ball mill, wherein ratio of grinding media to material
It is 25:1；
(2) guar gum, polyethylene glycol and 70 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
18h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50-70 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
80min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 150 DEG C, and outlet temperature is 90 DEG C, pressure
Power is 0.1MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 270MPa
Press 2min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 70 parts of deionized waters are mixed, is put into ball in ball grinder
Grind 6h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 4h in ball grinder, cross 40 mesh sieve, wherein mixed powder
Material, water, ball mass ratio be 1:1:5；
(9) glyceryl tristearate, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 4h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Comparative example 1
Difference lies in without containing giantreed charcoal with embodiment 1 for the present embodiment.Specifically：
A kind of package substrate composite material is prepared by following component with parts by weight：50 parts of silica, carbon nanohorn 18
Part, 10 parts of spodumene, 10 parts of silicon powder, 3 parts of Fluorspar Powder, 30 parts of boric acid, 2 parts of barium carbonate, 2 parts of lubricant, 0.2 part of guar gum,
0.1 part of polyethylene glycol, 10 parts of acrylic acid, 2 parts of polyvinylpyrrolidone, 2 parts of phlogopite crystallite, 4 parts of water-soluble polyacrylamide,
28 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon gas protection after vacuumizing, with not
The steel ball that becomes rusty is that mill is situated between, and is ground 22h at rotating speed 170rpm using planetary ball mill, wherein ratio of grinding media to material 25:1；
(2) guar gum, polyethylene glycol and 50 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
15h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
60min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 130 DEG C, and outlet temperature is 75 DEG C, pressure
Power is 0.08MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 250MPa
Press 1min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 50 parts of deionized waters are mixed, is put into ball in ball grinder
Grind 5h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3h in ball grinder, cross 40 mesh sieve, wherein mixed powder
Material, water, ball mass ratio be 1:1:5；
(9) beeswax, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Comparative example 2
Difference lies in without containing Fluorspar Powder with embodiment 1 for the present embodiment.Specifically：
A kind of package substrate composite material is prepared by following component with parts by weight：50 parts of silica, carbon nanohorn 18
Part, 1 part of giantreed charcoal, 10 parts of spodumene, 10 parts of silicon powder, 30 parts of boric acid, 2 parts of barium carbonate, 2 parts of lubricant, guar gum 0.2
Part, 0.1 part of polyethylene glycol, 10 parts of acrylic acid, 2 parts of polyvinylpyrrolidone, 2 parts of phlogopite crystallite, water-soluble polyacrylamide 4
Part, 28 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, is ground 22h at rotating speed 170rpm using planetary ball mill, wherein ratio of grinding media to material
It is 25:1；
(2) guar gum, polyethylene glycol and 50 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
15h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
60min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 130 DEG C, and outlet temperature is 75 DEG C, pressure
Power is 0.08MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 250MPa
Press 1min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, boric acid, barium carbonate and 50 parts of deionized waters are mixed, is put into ball milling 5h in ball grinder；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3h in ball grinder, cross 40 mesh sieve, wherein mixed powder
Material, water, ball mass ratio be 1:1:5；
(9) beeswax, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Comparative example 3
Difference lies in without containing barium carbonate with embodiment 1 for the present embodiment.Specifically：
A kind of package substrate composite material is prepared by following component with parts by weight：50 parts of silica, carbon nanohorn 18
Part, 1 part of giantreed charcoal, 10 parts of spodumene, 10 parts of silicon powder, 3 parts of Fluorspar Powder, 30 parts of boric acid, 2 parts of lubricant, guar gum 0.2
Part, 0.1 part of polyethylene glycol, 10 parts of acrylic acid, 2 parts of polyvinylpyrrolidone, 2 parts of phlogopite crystallite, water-soluble polyacrylamide 4
Part, 28 parts of absolute ethyl alcohol.
The preparation method of above-mentioned package substrate composite material is：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, is ground 22h at rotating speed 170rpm using planetary ball mill, wherein ratio of grinding media to material
It is 25:1；
(2) guar gum, polyethylene glycol and 50 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
15h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide is added, the wet ball grinding in three-dimensional material mixer
60min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 130 DEG C, and outlet temperature is 75 DEG C, pressure
Power is 0.08MPa；
(4) it is encapsulated with plastic film after dry-pressing formed, is placed in the oil cylinder of cold isostatic compaction machine, is protected under the pressure of 250MPa
Press 1min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid and 50 parts of deionized waters are mixed, is put into ball milling 5h in ball grinder；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3h in ball grinder, cross 40 mesh sieve, wherein mixed powder
Material, water, ball mass ratio be 1:1:5；
(9) beeswax, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
Dielectric constant and bending strength are all made of national standard.
The partial properties index of 1 package substrate composite material of table
| Name of product | Dielectric constant | Dielectric loss value | Bending strength (MPa) |
| Embodiment 1 | 6.16 | 4.72×10-3 | 169.41 |
| Embodiment 2 | 6.19 | 4.69×10-3 | 169.43 |
| Embodiment 3 | 6.26 | 4.65×10-3 | 169.49 |
| Embodiment 4 | 6.23 | 4.68×10-3 | 169.46 |
| Comparative example 1 | 6.12 | 4.89×10-3 | 160.50 |
| Comparative example 2 | 6.14 | 5.06×10-3 | 164.41 |
| Comparative example 3 | 5.12 | 5.35×10-3 | 142.76 |
The partial properties index of package substrate composite material of the present invention is seen the above table, it will be seen that material of the present invention have compared with
High dielectric constant is 6.26, very low dielectric loss value, only 4.65 × 10-3, while there is good anti-bending strength, most
High reachable 169.49MPa.
Claims (5)
1. a kind of package substrate composite material, it is characterised in that：It is prepared with parts by weight by following component：Silica 50-
70 parts, 18-25 parts of carbon nanohorn, 1-2 parts of giantreed charcoal, 10-15 parts of spodumene, 10-15 parts of silicon powder, 3-5 parts of Fluorspar Powder,
30-40 parts of boric acid, 2-3 parts of barium carbonate, 2-3 parts of lubricant, 0.2-0.5 parts of guar gum, 0.1-0.3 parts of polyethylene glycol, acrylic acid
10-20 parts, 2-4 parts of polyvinylpyrrolidone, 2-4 parts of phlogopite crystallite, 4-8 parts of water-soluble polyacrylamide, absolute ethyl alcohol 28-
40 parts.
2. a kind of package substrate composite material according to claim 1, it is characterised in that：By following component with parts by weight system
It is standby to form：60 parts of silica, 22 parts of carbon nanohorn, 1.5 parts of giantreed charcoal, 13 parts of spodumene, 13 parts of silicon powder, Fluorspar Powder
4 parts, it is 35 parts of boric acid, 2.5 parts of barium carbonate, 2.5 parts of lubricant, 0.3 part of guar gum, 0.2 part of polyethylene glycol, 15 parts of acrylic acid, poly-
3 parts of vinylpyrrolidone, 3 parts of phlogopite crystallite, 6 parts of water-soluble polyacrylamide, 34 parts of absolute ethyl alcohol.
3. a kind of package substrate composite material according to claim 1, it is characterised in that：The lubricant be castor oil,
One or more of calcium sulfonate complex grease, glyceryl tristearate or beeswax.
4. a kind of preparation method of package substrate composite material of claim 1 to 2 any one of them, it is characterised in that：Including
Following steps：
(1) carbon nanohorn, giantreed charcoal and silicon powder are mixed, is placed in sealing in stainless-steel vacuum tank and is passed through argon after vacuumizing
Gas shielded is that mill is situated between with stainless steel ball, 22-24h is ground at rotating speed 170-180rpm using planetary ball mill,
In, ratio of grinding media to material 25:1；
(2) guar gum, polyethylene glycol and 50-70 parts of deionized waters are added, is put into stirring and is sanded in dispersion machine agitator tank, in rotating speed
15-18h is stirred under 900rpm, is placed in oven and dried after taking-up for 24 hours, is crossed 80 mesh sieve, is discarded bulky grain；
(3) 50-70 deionized waters, absolute ethyl alcohol and water-soluble polyacrylamide, the wet ball grinding 60- in three-dimensional material mixer is added
80min forms composite spheroidal particle by spray drying, and spray drying inlet temperature is 130-150 DEG C, outlet temperature 75-
90 DEG C, pressure 0.08-0.1MPa；
(4) it is encapsulated, is placed in the oil cylinder of cold isostatic compaction machine, in the pressure of 250-270MPa with plastic film after dry-pressing formed
Lower pressurize 1-2min；
(5) be placed in graphite crucible, be put into vacuum sintering furnace, be sintered under argon atmosphere powder A, sintering process are：
1000 DEG C of heat preservation 25min are warming up to, 1250 DEG C of heat preservation 30min are continuously heating to, 1850 DEG C of heat preservation 30min is warming up to, is warming up to
2100 DEG C of heat preservation 30min, Temperature fall cooling, wherein all heating rates are 10 DEG C/min；
(6) silica, spodumene, Fluorspar Powder, boric acid, barium carbonate and 50-70 parts of deionized waters are mixed, is put into ball grinder
Ball milling 5-6h；
(7) 40 mesh sieve is crossed after drying, is put into crucible, is placed in pre-burning at 600 DEG C in temperature automatically controlled sintering furnace, and heat preservation 3h obtains glass powder
Material；
(8) powder A, glass powder and deionized water are mixed, is put into ball milling 3-4h in ball grinder, cross 40 mesh sieve, wherein mixing
Powder, water, ball mass ratio be 1:1:5；
(9) lubricant, acrylic acid, polyvinylpyrrolidone and phlogopite crystallite is added, continues to grind 3-4h；
(10) compression moulding, briquetting pressure 20MPa；
(11) it is put into vacuum sintering furnace, is sintered under argon atmosphere, to obtain the final product, sintering process is natural cooling：It is warming up to 450
DEG C, 2h is kept the temperature, is warming up to 850 DEG C, keeps the temperature 60min.
5. a kind of preparation method of package substrate composite material according to claim 1, it is characterised in that：The giantreed life
The preparation method of object charcoal is：
The first step：It is dried after giantreed is cleaned, is crushed to 40 mesh, be put into air dry oven in 105 DEG C of dry 5-8h；
Second step：10 parts of giantreed powder, 25 parts of pyrophosphoric acids and 30 parts of deionized waters are mixed, stirs evenly, impregnates 4- at room temperature
5h；
Third walks：Filtering, is transferred in Muffle furnace, the carbonization-activation 1h at 350-600 DEG C；
4th step：It is cooled to room temperature, is washed with distilled water to neutrality, be put into baking oven the drying at 100 DEG C, be ground to grain size ＜
20 μm to obtain the final product.
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| CN113087502A (en) * | 2021-03-29 | 2021-07-09 | 电子科技大学 | High-strength high-modulus magnesium-aluminum silicon substrate material and preparation method thereof |
| CN113087502B (en) * | 2021-03-29 | 2022-01-25 | 电子科技大学 | High-strength high-modulus magnesium-aluminum silicon substrate material and preparation method thereof |
| CN116102355A (en) * | 2023-02-23 | 2023-05-12 | 宝兴易达光伏刃料有限公司 | Carbon crucible with small thermal expansion coefficient and preparation method thereof |
| CN116102355B (en) * | 2023-02-23 | 2023-12-01 | 宝兴易达光伏刃料有限公司 | Carbon crucible with small thermal expansion coefficient and preparation method thereof |
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