CN103589365A - Inorganic filler for copper-cladded plate and preparation method thereof - Google Patents

Inorganic filler for copper-cladded plate and preparation method thereof Download PDF

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Publication number
CN103589365A
CN103589365A CN201310540237.4A CN201310540237A CN103589365A CN 103589365 A CN103589365 A CN 103589365A CN 201310540237 A CN201310540237 A CN 201310540237A CN 103589365 A CN103589365 A CN 103589365A
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Prior art keywords
copper
clad plate
mineral filler
less
raw material
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CN201310540237.4A
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Chinese (zh)
Inventor
李宝智
夏古俊
贾波
刘建明
黄勇峰
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Jin Yi silicon materials development corporation, Ltd. of Chongqing City
Suzhou Branch, Chongqing Jinyi Silicon Material Development Co., Ltd.
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SUZHOU BRANCH CHONGQING JINYI SILICON MATERIAL DEVELOPMENT Co Ltd
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Priority to CN201310540237.4A priority Critical patent/CN103589365A/en
Publication of CN103589365A publication Critical patent/CN103589365A/en
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Abstract

The invention discloses an inorganic filler for a copper-cladded plate and a preparation method thereof, wherein the method comprises the following steps: carrying out insulation dehydration of a kaolin raw material at the temperature of 600 DEG C-920 DEG C to form anhydrous aluminum silicate having an amorphous layered gap structure; and breaking apart anhydrous aluminum silicate having the amorphous layered gap structure, grading, and carrying out surface modification to obtain the inorganic filler for the copper-cladded plate. The inorganic filler for the copper-cladded plate has relatively low dielectric constant, relatively low hardness and other excellent characteristics, can meet needs of copper-cladded basal plates for high-frequency signal transmission, and has excellent machining performance.

Description

Mineral filler and preparation method thereof for copper-clad plate
Technical field
The invention belongs to copper-clad plate raw material production processing technique field, be specifically related to the preparation method of mineral filler and this material for a kind of copper-clad plate.
Background technology
As everyone knows, in copper-clad plate, with adding the common practice that inorganic powder is copper-clad plate industry in resin glue, add inorganic powder to improve mechanical property, dimensional performance and the electric property of the rear material of resin assimilation.As United States Patent (USP) 5264056 is pointed out, mineral filler add the dimensional stability that can improve the copper-clad base plate after Resin adhesive water cure, dimensional stability is a very important index in copper-clad base plate Hou road complete processing.Meanwhile, Japanese Patent points out for No. 222950, No. 97633, inorganic powder add the mobility that weakens resin glue, improve punching performance.In addition, in resin glue, add the good aluminum oxide inorganic powder of heat conductivility, also can improve the thermal conductivity of copper-clad plate.
Along with the development of advanced communication equipment and technology, be widely used in the demand of various high-frequency electronic equipment of communication field also in growth at full speed.For meeting the transmission of high-frequency signal, the demand of high transmission speed and high-frequency low-consumption, the copper-clad plate base material of various low-ks (Dk) is also in constantly developing, simultaneously, because copper-clad base plate needs to carry out the processing such as a large amount of cuttings, boring in process for processing, and the conventional silica powder adding can cause the increase of copper-clad plate hardness, increased the tooling cost in later stage, and difficulty of processing is larger in copper-clad plate.
In view of this, a kind of novel inorganic powder material need to be provided, the demand of low-k and soft two aspects can be met.
Summary of the invention
One of object of the present invention is to provide the preparation method of a kind of copper-clad plate with mineral filler, and it can meet the process requirements of copper-clad plate.
The present invention also aims to provide a kind of copper-clad plate mineral filler.
One of for achieving the above object, the invention provides the preparation method of mineral filler for a kind of copper-clad plate, the method comprises the following steps:
Kaolin raw material is incubated in the temperature range of 600 ℃ ~ 920 ℃ to dehydration and forms the anhydrous aluminium silicate that amorphous stratiform is free gap structure;
By described amorphous stratiform be that the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
As a further improvement on the present invention, SiO in described kaolin raw material 2and Al 2o 3be by weight percentage:
SiO 2:?38%~63%;
Al 2O 3:?23%~45%。
As a further improvement on the present invention, in described kaolin raw material, also comprise the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
As a further improvement on the present invention, the time range of described " kaolin raw material is incubated in the temperature range of 600 ℃ ~ 920 ℃ " is 1 ~ 5 hour.
As a further improvement on the present invention, the copper-clad plate obtaining described in is less than 10um by the mean particle size of mineral filler.
As a further improvement on the present invention, the copper-clad plate obtaining described in is not more than 25um by the maximum particle size of mineral filler.
As a further improvement on the present invention, the copper-clad plate obtaining described in the dielectric constant range of mineral filler be 2.5 ~ 5.5, durometer level is 3.5 ~ 5.5.
As a further improvement on the present invention, described in the copper-clad plate that obtains with the conductivity range of mineral filler, be that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, whiteness scope is 80.00% ~ 93.00%.
For realizing above-mentioned another goal of the invention, the invention provides a kind of copper-clad plate mineral filler, described copper-clad plate comprises by weight percentage with mineral filler: 45% ~ 60% SiO 2, 35% ~ 50% Al 2o 3.
As a further improvement on the present invention, described copper-clad plate also comprises the Fe that is less than by weight percentage 0.35% with mineral filler 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO2.
Compared with prior art, copper-clad plate provided by the invention forms by kaolin raw material being incubated in the temperature range of 600 ℃ ~ 920 ℃ to dehydration the anhydrous aluminium silicate that amorphous stratiform is free gap structure by the preparation method of mineral filler, and further the amorphous stratiform obtaining is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler, it has the lower good characteristic that waits of the lower and hardness of specific inductivity, can meet the needs of copper-clad base plate for high-frequency signal transmission, and processing characteristics is excellent.
Accompanying drawing explanation
Fig. 1 is the preparation method's of mineral filler schema for copper-clad plate of the present invention.
Embodiment
Below with reference to specific embodiment describe the present invention (with reference to Fig. 1).
Embodiment mono-
1) take kaolin raw material, control SiO in kaolin raw material 2and Al 2o 3be SiO by weight percentage 2: 38%, Al 2o 3: 44%, in kaolin raw material, also comprise the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
2) the kaolin raw material in step (1) is incubated to 3.5 hours at the temperature of 600 ℃, makes the dehydration of kaolin raw material form the anhydrous aluminium silicate that amorphous stratiform is free gap structure.
3) the amorphous stratiform obtaining in step (2) is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
Wherein, breaing up in step (3), classification guarantee to control the copper-clad plate that obtains with the mean particle size of mineral filler be less than 10um, maximum particle size is not more than 25um.
The copper-clad plate finally obtaining with the dielectric constant range of mineral filler be 2.5 ~ 5.5, conductivity range is that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, durometer level is 3.5 ~ 5.5, whiteness scope is 80.00% ~ 93.00%.
Embodiment bis-
1) take kaolin raw material, control SiO in kaolin raw material 2and Al 2o 3be SiO by weight percentage 2: 63%, Al 2o 3: 25%, in kaolin raw material, also comprise the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
2) the kaolin raw material in step (1) is incubated to 1 hour at the temperature of 650 ℃, makes the dehydration of kaolin raw material form the anhydrous aluminium silicate that amorphous stratiform is free gap structure.
3) the amorphous stratiform obtaining in step (2) is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
Wherein, breaing up in step (3), classification guarantee to control the copper-clad plate that obtains with the mean particle size of mineral filler be less than 10um, maximum particle size is not more than 25um.
The copper-clad plate finally obtaining with the dielectric constant range of mineral filler be 2.5 ~ 5.5, conductivity range is that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, durometer level is 3.5 ~ 5.5, whiteness scope is 80.00% ~ 93.00%.
Embodiment tri-
1) take kaolin raw material, control SiO in kaolin raw material 2and Al 2o 3be SiO by weight percentage 2: 55%, Al 2o 3: 34%, in kaolin raw material, also comprise the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
2) the kaolin raw material in step (1) is incubated to 4.5 hours at the temperature of 770 ℃, makes the dehydration of kaolin raw material form the anhydrous aluminium silicate that amorphous stratiform is free gap structure.
3) the amorphous stratiform obtaining in step (2) is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
Wherein, breaing up in step (3), classification guarantee to control the copper-clad plate that obtains with the mean particle size of mineral filler be less than 10um, maximum particle size is not more than 25um.
The copper-clad plate finally obtaining with the dielectric constant range of mineral filler be 2.5 ~ 5.5, conductivity range is that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, durometer level is 3.5 ~ 5.5, whiteness scope is 80.00% ~ 93.00%.
Embodiment tetra-
1) take kaolin raw material, control SiO in kaolin raw material 2and Al 2o 3be SiO by weight percentage 2: 60%, Al 2o 3: 23%, in kaolin raw material, also comprise the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
2) the kaolin raw material in step (1) is incubated to 4.5 hours at the temperature of 920 ℃, makes the dehydration of kaolin raw material form the anhydrous aluminium silicate that amorphous stratiform is free gap structure.
3) the amorphous stratiform obtaining in step (2) is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
Wherein, breaing up in step (3), classification guarantee to control the copper-clad plate that obtains with the mean particle size of mineral filler be less than 10um, maximum particle size is not more than 25um.
The copper-clad plate finally obtaining with the dielectric constant range of mineral filler be 2.5 ~ 5.5, conductivity range is that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, durometer level is 3.5 ~ 5.5, whiteness scope is 80.00% ~ 93.00%.
Embodiment five
1) take kaolin raw material, control SiO in kaolin raw material 2and Al 2o 3be SiO by weight percentage 2: 43%, Al 2o 3: 45%, in kaolin raw material, also comprise the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
2) the kaolin raw material in step (1) is incubated to 5 hours at the temperature of 800 ℃, makes the dehydration of kaolin raw material form the anhydrous aluminium silicate that amorphous stratiform is free gap structure.
3) the amorphous stratiform obtaining in step (2) is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
Wherein, breaing up in step (3), classification guarantee to control the copper-clad plate that obtains with the mean particle size of mineral filler be less than 10um, maximum particle size is not more than 25um.
By the above embodiments, available copper-clad plate of the present invention comprises by weight percentage with mineral filler: 45% ~ 60% SiO 2; 35% ~ 50% Al 2o 3; Be less than 0.35% Fe 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO2.
Wherein, the copper-clad plate obtaining with the dielectric constant range of mineral filler be 2.5 ~ 5.5, conductivity range is that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, durometer level is 3.5 ~ 5.5, whiteness scope is 80.00% ~ 93.00%.
Copper-clad plate provided by the invention is higher by mineral filler whiteness, and has preferably particle diameter, can improve thermotolerance and wet fastness, and through the material of surface modification, can improve the cohesiveness of Copper Foil and resin insulating barrier in following process.
The present invention has following beneficial effect by above-described embodiment: copper-clad plate provided by the invention forms by kaolin raw material being incubated in the temperature range of 600 ℃ ~ 920 ℃ to dehydration the anhydrous aluminium silicate that amorphous stratiform is free gap structure by the preparation method of mineral filler, and further the amorphous stratiform obtaining is to the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler, it has the lower good characteristic that waits of the lower and hardness of specific inductivity, can meet the needs of copper-clad base plate for high-frequency signal transmission, and processing characteristics is excellent.
Be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Listed a series of detailed description is above only illustrating for feasibility embodiment of the present invention; they are not in order to limit the scope of the invention, all disengaging within equivalent embodiment that skill spirit of the present invention does or change all should be included in protection scope of the present invention.

Claims (10)

1. a preparation method for mineral filler for copper-clad plate, is characterized in that, the method comprises the following steps:
Kaolin raw material is incubated in the temperature range of 600 ℃ ~ 920 ℃ to dehydration and forms the anhydrous aluminium silicate that amorphous stratiform is free gap structure;
By described amorphous stratiform be that the anhydrous aluminium silicate of free gap structure is broken up, classification surface modification obtain copper-clad plate mineral filler.
2. method according to claim 1, is characterized in that, SiO in described kaolin raw material 2and Al 2o 3be by weight percentage:
SiO 2:?38%~63%;
Al 2O 3:?23%~45%。
3. method according to claim 2, is characterized in that, in described kaolin raw material, also comprises the Fe that is less than by weight percentage 0.35% 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO 2.
4. method according to claim 1, is characterized in that, the time range of described " kaolin raw material is incubated in the temperature range of 600 ℃ ~ 920 ℃ " is 1 ~ 5 hour.
5. method according to claim 1, is characterized in that, described in the copper-clad plate that obtains by the mean particle size of mineral filler, be less than 10um.
6. method according to claim 1, is characterized in that, described in the copper-clad plate that obtains by the maximum particle size of mineral filler, be not more than 25um.
7. method according to claim 1, is characterized in that, described in the copper-clad plate that obtains with the dielectric constant range of mineral filler be 2.5 ~ 5.5, durometer level is 3.5 ~ 5.5.
8. method according to claim 1, is characterized in that, described in the copper-clad plate that obtains with the conductivity range of mineral filler, be that 3.0us/cm ~ 50.0us/cm, oil number scope are 50g/100g ~ 65g/100g, whiteness scope is 80.00% ~ 93.00%.
9. a copper-clad plate mineral filler, is characterized in that, described copper-clad plate comprises by weight percentage with mineral filler: 45% ~ 60% SiO 2, 35% ~ 50% Al 2o 3.
10. copper-clad plate mineral filler according to claim 9, is characterized in that, described copper-clad plate also comprises the Fe that is less than by weight percentage 0.35% with mineral filler 2o 3, be less than 0.25% CaO, be less than 0.1% MgO, be less than 1.2% TiO2.
CN201310540237.4A 2013-11-05 2013-11-05 Inorganic filler for copper-cladded plate and preparation method thereof Withdrawn CN103589365A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1528829A (en) * 2003-09-29 2004-09-15 华东师范大学 Method for preparing modified calcined superfine kaoline filler
CN1654549A (en) * 2005-01-26 2005-08-17 宜昌地质矿产研究所 Process for preparing butyl rubber bottle stopper reinforced filling by using coals kaolin
CN102036815A (en) * 2008-05-19 2011-04-27 松下电工株式会社 Laminate, metal-foil-clad laminate, circuit board, and circuit board for LED mounting
CN102123966A (en) * 2008-08-19 2011-07-13 巴斯夫公司 A novel blended hydrous kaolin clay product
CN102264539A (en) * 2008-12-26 2011-11-30 三菱瓦斯化学株式会社 Copper foil with resin
CN102924089A (en) * 2012-12-03 2013-02-13 桂林理工大学 Method for preparing beta-sialon ceramic powders through using coal ash and kaolin
CN103057213A (en) * 2012-12-31 2013-04-24 金安国纪科技股份有限公司 Environment-friendly copper clad laminate for LED monochrome display, glue solution and preparation method

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1528829A (en) * 2003-09-29 2004-09-15 华东师范大学 Method for preparing modified calcined superfine kaoline filler
CN1654549A (en) * 2005-01-26 2005-08-17 宜昌地质矿产研究所 Process for preparing butyl rubber bottle stopper reinforced filling by using coals kaolin
CN102036815A (en) * 2008-05-19 2011-04-27 松下电工株式会社 Laminate, metal-foil-clad laminate, circuit board, and circuit board for LED mounting
CN102123966A (en) * 2008-08-19 2011-07-13 巴斯夫公司 A novel blended hydrous kaolin clay product
CN102264539A (en) * 2008-12-26 2011-11-30 三菱瓦斯化学株式会社 Copper foil with resin
CN102924089A (en) * 2012-12-03 2013-02-13 桂林理工大学 Method for preparing beta-sialon ceramic powders through using coal ash and kaolin
CN103057213A (en) * 2012-12-31 2013-04-24 金安国纪科技股份有限公司 Environment-friendly copper clad laminate for LED monochrome display, glue solution and preparation method

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Title
沈上越等: "宜昌地区煤系高岭土矿石特征及应用前景分析", 《非金属矿》 *
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Application publication date: 20140219