CN108793959A - A kind of low-k ceramic material and preparation method thereof - Google Patents

A kind of low-k ceramic material and preparation method thereof Download PDF

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CN108793959A
CN108793959A CN201810855682.2A CN201810855682A CN108793959A CN 108793959 A CN108793959 A CN 108793959A CN 201810855682 A CN201810855682 A CN 201810855682A CN 108793959 A CN108793959 A CN 108793959A
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akermanite
garnet
yttrium
aluminium
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冯嘉豪
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Abstract

The invention discloses a kind of low-k ceramic materials, are made of the material of following weight：Kaolin, anorthite, akermanite, sodium carboxymethylcellulose, calcium titanate, polyvinyl alcohol, nanometer bismuth oxide, boron oxide, zinc nitrate, magnesia cordierite, fluorite, the tremolite, clinochlore, pyrophillite and yttrium-aluminium-garnet；Zinc ion in zinc nitrate can replace the magnesium position in akermanite, replace the akermanite of magnesium position to coordinate boron oxide that can reduce sintering temperature by zinc ion, and cooperation calcium titanate can adjust its temperature stability, prevent its heated fragmentation and reduce dielectric constant；Ruthenium ion in yttrium-aluminium-garnet can improve particle size distribution and lower the porosity, there is its structure and performance that the special octahedra hexatomic ring of magnesia cordierite crystal makes adjustability, yttrium-aluminium-garnet and magnesia cordierite collocation can further reduce dielectric constant and increase stability.

Description

A kind of low-k ceramic material and preparation method thereof
Technical field
Present invention relates particularly to a kind of low-k ceramic materials and preparation method thereof.
Background technology
With the rapid development of electronic information technology, the direction of advance of electronic device be smaller and smaller specification, stability and Integration degree higher, multifunction, thus people couple and the research of the relevant material of novel electron and device are very living honest and just.? Leading position is seized of in electronic information technology industry is the electronic materials such as magnetism, functional dielectrics, semiconductor and device, it Development greatly affect people economic and social life generate, thus as current research hot spot method direction.Electricity Container be it is a kind of be used for storing the device of electric energy, be one of the electronic original part generally used in electronic equipment, be widely used in every Directly, coupling, bypass, filtering, resonant tank, control circuit etc., have that use scope is wide, dosage is big, can not be substituted Feature.Inorganic ceramic dielectric material is due to superior electrical properties, mechanical property, optical property and thermal property, especially It is with high mechanical properties, high temperature resistant, high humidity, anti-good fortune is penetrated, and has wider dielectric constant, excellent dielectric property, outstanding machine The advantages that electric essence collaboration number, higher dielectric strength and larger insulation resistance and good anti-aging property, becomes in electricity Most popular material in container industry.The performance of capacitor element and material used be closely related to complement each other, mutual shadow It rings.To capacitor element, more stringent requirements are proposed for the development of electronic information technology, thus inorganic ceramic dielectric substance become work as One of the hot spot of preceding research, the performance to improving device are of great significance.But the most of dielectrics of current ceramic material are normal Number is higher, and hardness is inadequate, thermo-labile, even if being easy heated chap if heat-resisting.
Invention content
In view of this, having the object of the present invention is to provide one kind, low-k, thermal conductivity is good, hardness is high, hot firm The good ceramic material of property.
To solve the above-mentioned problems, the technical scheme is that：
A kind of low-k ceramic material, is made of the material of following weight：52-60 parts of kaolin, calcium are long 20-26 parts of stone, 17-23 parts of akermanite, 13-17 parts of sodium carboxymethylcellulose, 11-17 parts of calcium titanate, polyvinyl alcohol 11-17 Part, 9-13 parts of nanometer bismuth oxide, 9-13 parts of boron oxide, 7-11 parts of zinc nitrate, 7-9 parts of magnesia cordierite, 6-8 parts of fluorite, thoroughly 2-4 parts of 5-7 parts of amphibole, 4-6 parts of clinochlore, 4-6 parts of pyrophillite and yttrium-aluminium-garnet.
Further, the low-k ceramic material, is made of the material of following weight：Kaolin 60 Part, 20 parts of anorthite, 17 parts of akermanite, 13 parts of sodium carboxymethylcellulose, 11 parts of calcium titanate, 11 part, nanometer three of polyvinyl alcohol Aoxidize 9 parts of two bismuth, 9 parts of boron oxide, 7 parts of zinc nitrate, 7 parts of magnesia cordierite, 6 parts of fluorite, 5 parts of the tremolite, 4 parts of clinochlore, leaf 2 parts of 4 parts of cured stone and yttrium-aluminium-garnet.
Further, the low-k ceramic material, is made of the material of following weight：Kaolin 52 Part, 26 parts of anorthite, 23 parts of akermanite, 17 parts of sodium carboxymethylcellulose, 17 parts of calcium titanate, 17 part, nanometer three of polyvinyl alcohol Aoxidize 13 parts of two bismuth, 13 parts of boron oxide, 11 parts of zinc nitrate, 9 parts of magnesia cordierite, 8 parts of fluorite, 7 parts of the tremolite, 6 parts of clinochlore, 4 parts of 6 parts of pyrophillite and yttrium-aluminium-garnet.
Further, the low-k ceramic material, is made of the material of following weight：Kaolin 56 Part, 23 parts of anorthite, 20 parts of akermanite, 15 parts of sodium carboxymethylcellulose, 14 parts of calcium titanate, 14 part, nanometer three of polyvinyl alcohol Aoxidize 11 parts of two bismuth, 11 parts of boron oxide, 9 parts of zinc nitrate, 8 parts of magnesia cordierite, 7 parts of fluorite, 6 parts of the tremolite, 5 parts of clinochlore, 3 parts of 5 parts of pyrophillite and yttrium-aluminium-garnet.
Beneficial effects of the present invention:Zinc ion in zinc nitrate can replace the magnesium position in akermanite, be taken by zinc ion Sintering temperature can be reduced for the akermanite cooperation boron oxide of magnesium position, cooperation calcium titanate can adjust its temperature stability, prevent Its heated fragmentation and reduction dielectric constant；Ruthenium ion in yttrium-aluminium-garnet can improve particle size distribution and lower stomata Rate, its structure and performance that the special octahedra hexatomic ring of magnesia cordierite crystal makes have adjustability, yttrium-aluminium-garnet and magnesium Cordierite collocation can further reduce dielectric constant and increase stability.
Specific implementation method
Embodiment 1
A kind of low-k ceramic material, is made of the material of following weight：60 parts of kaolin, anorthite 20 Part, 17 parts of akermanite, 13 parts of sodium carboxymethylcellulose, 11 parts of calcium titanate, 11 parts of polyvinyl alcohol, 9 parts of nanometer bismuth oxide, 9 parts of boron oxide, 7 parts of zinc nitrate, 7 parts of magnesia cordierite, 6 parts of fluorite, 5 parts of the tremolite, 4 parts of clinochlore, 4 parts of pyrophillite and yttrium aluminium 2 parts of garnet.
A kind of preparation method of low-k ceramic material, includes the following steps:
1) 7 parts of magnesia cordierite, 6 parts of fluorite, 5 parts of the tremolite, 4 parts of clinochlore, 4 parts of pyrophillite and yttrium-aluminium-garnet 2 are taken Part, it is crushed using ball mill, drum's speed of rotation rate should be 85%, and size of powder particles 3um stirs the powder use crushed The machine of mixing is stirred mixing, and the first mixed-powder is made in mixing speed 110rpm, time 6min, spare；
2) the first mixed-powder made from step 1) is subjected to hot-pressing processing, hot-pressing processing temperature is 170 DEG C, and pressure is The first hot pressing mixture is made in 1.2MPa, time 20min, spare；
3) 17 parts of 60 parts of kaolin, 20 parts of anorthite and akermanite are taken, is crushed using ball mill, drum's speed of rotation Rate should be 90%, size of powder particles 3um, the powder crushed is stirred mixing using blender, mixing speed is The second mixed-powder is made in 50rpm, time 30min, spare；
4) the second mixed-powder made from step 3) is subjected to pre-burning, calcined temperature is 220 DEG C, time 18min, then will Temperature is reduced to 160 DEG C, time 10min, and Preburning material is made, spare；
5) the first hot pressing mixture is made in step 2) and step 4) is made Preburning material and is stirred mixing using blender, Mixing speed is 160rpm, time 12min, and third mixed-powder is made, spare；
6) third mixed-powder made from step 5) is put into container, 11 parts of polyvinyl alcohol is added and impregnates and uses water-bath Heating, soaking time 50min, bath temperature are 80 DEG C, are made and impregnate heating water bath material, spare；
7) 13 parts of sodium carboxymethylcellulose, 11 parts of calcium titanate, 9 parts of nanometer bismuth oxide, 9 parts of boron oxide and zinc nitrate are taken It 7 parts, puts that step 6) is obtained to impregnate in heating water bath material into, mixing is stirred using blender, mixing speed 80rpm, Time is 10min, and carries out blank forming, spare；
8) green body made from step 7) is sintered, sintering temperature is 200 DEG C, time 12min, then temperature is promoted It is 560 DEG C, time 30min, then temperature is promoted to 1100 DEG C, temperature is finally reduced to 800 DEG C by time 5h, and the time is 30min to get.
Embodiment 2
A kind of low-k ceramic material, is made of the material of following weight：52 parts of kaolin, anorthite 26 Part, 23 parts of akermanite, 17 parts of sodium carboxymethylcellulose, 17 parts of calcium titanate, 17 parts of polyvinyl alcohol, nanometer bismuth oxide 13 Part, 13 parts of boron oxide, 11 parts of zinc nitrate, 9 parts of magnesia cordierite, 8 parts of fluorite, 7 parts of the tremolite, 6 parts of clinochlore, 6 parts of pyrophillite With 4 parts of yttrium-aluminium-garnet.
A kind of preparation method of low-k ceramic material, includes the following steps:
1) 9 parts of magnesia cordierite, 8 parts of fluorite, 7 parts of the tremolite, 6 parts of clinochlore, 6 parts of pyrophillite and yttrium-aluminium-garnet 4 are taken Part, it is crushed using ball mill, drum's speed of rotation rate should be 75%, and size of powder particles 1um stirs the powder use crushed The machine of mixing is stirred mixing, and the first mixed-powder is made in mixing speed 90rpm, time 4min, spare；
2) the first mixed-powder made from step 1) is subjected to hot-pressing processing, hot-pressing processing temperature is 150 DEG C, and pressure is The first hot pressing mixture is made in 1.0MPa, time 16min, spare；
3) 23 parts of 52 parts of kaolin, 26 parts of anorthite and akermanite are taken, is crushed using ball mill, drum's speed of rotation Rate should be 80%, size of powder particles 1um, the powder crushed is stirred mixing using blender, mixing speed is The second mixed-powder is made in 30rpm, time 20min, spare；
4) the second mixed-powder made from step 3) is subjected to pre-burning, calcined temperature is 200 DEG C, time 14min, then will Temperature is reduced to 140 DEG C, time 8min, and Preburning material is made, spare；
5) the first hot pressing mixture is made in step 2) and step 4) is made Preburning material and is stirred mixing using blender, Mixing speed is 150rpm, time 8min, and third mixed-powder is made, spare；
6) third mixed-powder made from step 5) is put into container, 17 parts of polyvinyl alcohol is added and impregnates and uses water-bath Heating, soaking time 30min, bath temperature are 60 DEG C, are made and impregnate heating water bath material, spare；
7) 17 parts of sodium carboxymethylcellulose, 17 parts of calcium titanate, 13 parts of nanometer bismuth oxide, 13 parts of boron oxide and nitric acid are taken 11 parts of zinc is put into step 6) immersion heating water bath material obtained, is stirred mixing using blender, mixing speed is 60rpm, time 6min, and blank forming is carried out, it is spare；
8) green body made from step 7) is sintered, sintering temperature is 180 DEG C, time 8min, then temperature is promoted It is 500 DEG C, time 20min, then temperature is promoted to 1000 DEG C, temperature is finally reduced to 700 DEG C by time 3h, and the time is 20min to get.
Embodiment 3
A kind of low-k ceramic material, is made of the material of following weight：56 parts of kaolin, anorthite 23 Part, 20 parts of akermanite, 15 parts of sodium carboxymethylcellulose, 14 parts of calcium titanate, 14 parts of polyvinyl alcohol, nanometer bismuth oxide 11 Part, 11 parts of boron oxide, 9 parts of zinc nitrate, 8 parts of magnesia cordierite, 7 parts of fluorite, 6 parts of the tremolite, 5 parts of clinochlore, 5 parts of pyrophillite and 3 parts of yttrium-aluminium-garnet.
A kind of preparation method of low-k ceramic material, includes the following steps:
1) 8 parts of magnesia cordierite, 7 parts of fluorite, 6 parts of the tremolite, 5 parts of clinochlore, 5 parts of pyrophillite and yttrium-aluminium-garnet 3 are taken Part, it is crushed using ball mill, drum's speed of rotation rate should be 80%, and size of powder particles 2um stirs the powder use crushed The machine of mixing is stirred mixing, and the first mixed-powder is made in mixing speed 100rpm, time 5min, spare；
2) the first mixed-powder made from step 1) is subjected to hot-pressing processing, hot-pressing processing temperature is 160 DEG C, and pressure is The first hot pressing mixture is made in 1.1MPa, time 18min, spare；
3) 20 parts of 56 parts of kaolin, 23 parts of anorthite and akermanite are taken, is crushed using ball mill, drum's speed of rotation Rate should be 85%, size of powder particles 2um, the powder crushed is stirred mixing using blender, mixing speed is The second mixed-powder is made in 40rpm, time 25min, spare；
4) the second mixed-powder made from step 3) is subjected to pre-burning, calcined temperature is 210 DEG C, time 16min, then will Temperature is reduced to 150 DEG C, time 9min, and Preburning material is made, spare；
5) the first hot pressing mixture is made in step 2) and step 4) is made Preburning material and is stirred mixing using blender, Mixing speed is 155rpm, time 10min, and third mixed-powder is made, spare；
6) third mixed-powder made from step 5) is put into container, 14 parts of polyvinyl alcohol is added and impregnates and uses water-bath Heating, soaking time 40min, bath temperature are 70 DEG C, are made and impregnate heating water bath material, spare；
7) 15 parts of sodium carboxymethylcellulose, 14 parts of calcium titanate, 11 parts of nanometer bismuth oxide, 11 parts of boron oxide and nitric acid are taken 9 parts of zinc is put into step 6) immersion heating water bath material obtained, is stirred mixing using blender, mixing speed is 70rpm, time 8min, and blank forming is carried out, it is spare；
8) green body made from step 7) is sintered, sintering temperature is 190 DEG C, time 10min, then temperature is promoted It is 530 DEG C, time 25min, then temperature is promoted to 1050 DEG C, temperature is finally reduced to 750 DEG C by time 4h, and the time is 25min to get.
Experimental example：
The selection improved ceramic material of alundum (Al2O3) is control group, and it is normal to choose low dielectric prepared by the embodiment of the present invention three Number ceramic material is experimental group.
Low-k ceramics prepared by experimental subjects, the improved ceramic material of alundum (Al2O3) and the embodiment of the present invention three Material.
Requirement of experiment, the low-k prepared to the improved ceramic material of alundum (Al2O3) and the embodiment of the present invention three are made pottery Ceramic material is tested for the property.
Table 1 is to acquire information acquired results to experimental subjects afterwards
Table 1
In conjunction with table 1, the low dielectric of the improved ceramic material of comparison alundum (Al2O3) and the preparation of the embodiment of the present invention three is normal Number ceramic material, it can be seen that a kind of low-k ceramic material of the present invention not only has lower dielectric constant, hardness big It is strong with hot stability, also there is good heat conductivility, higher quality factor and smaller temperature coefficient of resonance frequency.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any The change or replacement expected without creative work should all be covered within the scope of the present invention.

Claims (4)

1. a kind of low-k ceramic material, it is characterised in that：It is made of the material of following weight：Kaolin 52- 60 parts, 20-26 parts of anorthite, 17-23 parts of akermanite, 13-17 parts of sodium carboxymethylcellulose, 11-17 parts of calcium titanate, polyethylene 11-17 parts of alcohol, 9-13 parts of nanometer bismuth oxide, 9-13 parts of boron oxide, 7-11 parts of zinc nitrate, 7-9 parts of magnesia cordierite, fluorite 6- 2-4 parts of 8 parts, 5-7 parts of the tremolite, 4-6 parts of clinochlore, 4-6 parts of pyrophillite and yttrium-aluminium-garnet.
2. a kind of low-k ceramic material as described in claim 1, it is characterised in that：By the material of following weight It is made：60 parts of kaolin, 20 parts of anorthite, 17 parts of akermanite, 13 parts of sodium carboxymethylcellulose, 11 parts of calcium titanate, polyethylene 11 parts of alcohol, 9 parts of nanometer bismuth oxide, 9 parts of boron oxide, 7 parts of zinc nitrate, 7 parts of magnesia cordierite, 6 parts of fluorite, 5 parts of the tremolite, tiltedly 2 parts of 4 parts of chlorite, 4 parts of pyrophillite and yttrium-aluminium-garnet.
3. a kind of low-k ceramic material as described in claim 1, it is characterised in that：By the material of following weight It is made：52 parts of kaolin, 26 parts of anorthite, 23 parts of akermanite, 17 parts of sodium carboxymethylcellulose, 17 parts of calcium titanate, polyethylene 17 parts of alcohol, 13 parts of nanometer bismuth oxide, 13 parts of boron oxide, 11 parts of zinc nitrate, 9 parts of magnesia cordierite, 8 parts of fluorite, the tremolite 7 Part, 6 parts of clinochlore, 6 parts of pyrophillite and 4 parts of yttrium-aluminium-garnet.
4. a kind of low-k ceramic material as described in claim 1, it is characterised in that：By the material of following weight It is made：56 parts of kaolin, 23 parts of anorthite, 20 parts of akermanite, 15 parts of sodium carboxymethylcellulose, 14 parts of calcium titanate, polyethylene 14 parts of alcohol, 11 parts of nanometer bismuth oxide, 11 parts of boron oxide, 9 parts of zinc nitrate, 8 parts of magnesia cordierite, 7 parts of fluorite, 6 parts of the tremolite, 3 parts of 5 parts of clinochlore, 5 parts of pyrophillite and yttrium-aluminium-garnet.
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