CN116178000B - Quartz fiber reinforced silica low dielectric composite material - Google Patents
Quartz fiber reinforced silica low dielectric composite material Download PDFInfo
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- CN116178000B CN116178000B CN202310109493.1A CN202310109493A CN116178000B CN 116178000 B CN116178000 B CN 116178000B CN 202310109493 A CN202310109493 A CN 202310109493A CN 116178000 B CN116178000 B CN 116178000B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 239000000835 fiber Substances 0.000 title claims abstract description 40
- 239000010453 quartz Substances 0.000 title claims abstract description 32
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 45
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 33
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 20
- 229920000742 Cotton Polymers 0.000 claims abstract description 15
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000004891 communication Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- 239000011363 dried mixture Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000011810 insulating material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000008054 signal transmission Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B11/00—Communication cables or conductors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/02—Disposition of insulation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/522—Oxidic
- C04B2235/5232—Silica or silicates other than aluminosilicates, e.g. quartz
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Insulating Materials (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a quartz fiber reinforced silicon dioxide low dielectric composite material, which is characterized in that the preparation raw materials comprise: 75% by weight of fumed silica, 25% by weight of nano silica, 20% by weight of quartz fiber cotton based on the total mass of fumed silica and nano silica, and 0-5% by weight of calcium carbonate based on the total mass of fumed silica and nano silica. The invention has good dielectric property, insensitivity to temperature and good thermal stability.
Description
Technical Field
The invention belongs to the field of low-dielectric composite materials, and particularly relates to a low-dielectric composite material of quartz fiber reinforced silicon dioxide.
Background
Fumed silica is a high-purity nanoscale white powder, has good porosity, high temperature resistance, low dielectric property, mechanical property and the like, and the nanoparticle characteristic and high purity of the fumed silica lead the fumed silica to play a leading role in the application of the fumed silica in the electronic and optical fiber industries. But the pure fumed silica insulating material is easy to peel off and fall off in the use process of the cable, and certain quartz fiber is added into the fumed silica matrix to enhance the continuity of the fumed silica material in the cable and improve the mechanical property of the cable and the stability of signal transmission. In the high-temperature-resistant communication cable, the fumed silica has the advantages of improving the dielectric property and the mechanical property of the fumed silica as an insulating material, so that the cable can stably and continuously transmit signals in extreme environments, and can be widely applied to aerospace, nuclear power and military projects.
The low dielectric cable insulating material which is currently mainstream is a silicon dioxide-based organic composite material, and can fail under the ultra-high temperature use environment to cause cable breakdown, and the high temperature resistance and the dielectric property are required to be further improved.
For example, the high temperature resistant cable insulation composite material with the application number of CN201910164806.7 contains organic matters such as resin, fluoroplastic and the like, and the high temperature resistance of the composite material is required to be improved. The dielectric property of the mesoporous silica nano composite nuclear power cable insulating material with the application number of CN201510168701.0 is to be improved.
The foregoing is provided merely for the purpose of facilitating understanding of the technical solutions of the present invention and is not intended to represent an admission that the foregoing is prior art.
Disclosure of Invention
The invention aims to solve the problems and provide a quartz fiber reinforced silicon dioxide low dielectric composite material.
In order to achieve the above object, the technical scheme of the present invention is as follows:
a quartz fiber reinforced silicon dioxide low dielectric composite material is prepared from the following raw materials: 75% by weight of fumed silica, 25% by weight of nano silica, 20% by weight of quartz fiber cotton based on the total mass of fumed silica and nano silica, and 0-5% by weight of calcium carbonate based on the total mass of fumed silica and nano silica.
Specifically, the quartz fiber reinforced silica low dielectric composite material is prepared from the following raw materials: 75% by weight of fumed silica, 25% by weight of nano silica, 20% by weight of quartz fiber cotton based on the total mass of fumed silica and nano silica, and 3% by weight or 5% by weight of calcium carbonate based on the total mass of fumed silica and nano silica.
Further, the preparation method comprises the following steps: s6, pressing and forming the powder prepared from all the raw materials on a powder tablet press;
s7, carrying out heat treatment and heat preservation on the formed powder for 1-6h in the environment of 400-800 ℃.
Further, the powder is prepared by the following steps: s1, cutting quartz fiber cotton, and grinding into chopped fibers;
s2, uniformly mixing fumed silica, nano silica and ground quartz fiber cotton in absolute ethyl alcohol, and dispersing by using ultrasonic waves;
s3, adding calcium carbonate, and uniformly mixing;
s4, adding silica sol for impregnation;
s5, drying, and grinding the dried mixture into powder.
In addition, the invention also provides a high-temperature-resistant communication cable which comprises a silicon dioxide insulating layer, wherein the silicon dioxide insulating layer is made of the quartz fiber reinforced silicon dioxide low-dielectric composite material.
By adopting the technical scheme, the invention has the following advantages:
1. the invention adopts quartz fiber cotton to replace common high silica fiber reinforced silicon dioxide powder, and can improve the structural stability and low dielectric property of the composite material.
2. The addition of calcium carbonate can effectively reduce the dielectric constant of the material.
3. The invention carries out heat treatment on the composite material to remove structural water and residual organic matters in the powder, thereby greatly reducing dielectric loss of the composite material.
4. According to the invention, silica sol is added for impregnation, so that the adhesiveness of silica powder on quartz fibers is improved, the impact resistance of the silica low-dielectric composite material is enhanced, and the problem that the signal transmission is unstable due to the fact that a cable insulating layer is provided with gaps when the cable is impacted in the use process is avoided.
5. The quartz fiber reinforced silicon dioxide low-dielectric composite material prepared by the invention has good dielectric property, the lowest dielectric constant can reach 1.76 at 10MHz, and the lowest dielectric loss is 3 multiplied by 10 -3 Is insensitive to temperature and has good thermal stabilityThe dielectric constant is increased by about 5% at an ultra-high temperature (1000 ℃), and the dielectric loss is further reduced by 56% or more. When the silica high-temperature-resistant communication cable is applied to the cable, the 18GHz maximum attenuation of the silica high-temperature-resistant communication cable is less than 2, and the rate is more than 86%.
Drawings
Fig. 1 is a schematic structural view of a silica high temperature resistant communication cable.
FIG. 2 is a graph of the dielectric constants of the composite materials of groups 1, 2, and 3 of the present invention.
FIG. 3 is a graph of dielectric loss for the composites of groups 1, 2, and 3 of the present invention.
FIG. 4 is a graph of the dielectric constants of the composite materials of groups 4, 5, and 6 of the present invention.
FIG. 5 is a transmission electron micrograph (1000000 times) of a composite of group 3 of the present invention.
FIG. 6 is a scanning electron micrograph (15000 Xmagnification) of a composite of group 3 of the present invention.
FIG. 7 is a scanning electron micrograph (15000 Xmagnification) of a composite of group 3 of the present invention.
Detailed Description
It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1: a quartz fiber reinforced silicon dioxide low dielectric composite material is prepared from the following raw materials: 75% by weight of fumed silica, 25% by weight of nano silica, 20% by weight of quartz fiber cotton based on the total mass of fumed silica and nano silica, and 0-5% by weight of calcium carbonate based on the total mass of fumed silica and nano silica.
The preparation method comprises the following steps: s1, cutting quartz fiber cotton, grinding the cut fiber cotton into chopped fibers so as to fully mix silicon dioxide and the quartz fiber, wherein the combination between the fiber and powder can be enhanced to improve the bending resistance of the silicon dioxide composite material;
s2, uniformly mixing fumed silica, nano silica and quartz fiber cotton in absolute ethyl alcohol, and dispersing for 1h by using an ultrasonic dispersing machine until the quartz fiber cotton is completely dispersed in silica particles;
s3, adding calcium carbonate, and uniformly mixing;
s4, adding silica sol for impregnation, wherein the addition standard of the silica sol is 5-12 wt% based on the total mass of the fumed silica and the nano silica, and continuing to use ultrasonic dispersion for 30 min until the silica sol is completely impregnated;
s5.80 ℃ drying until absolute ethyl alcohol is completely volatilized, and then grinding the dried mixture into powder;
s6, pressing and forming the powder on a powder tablet press; the press and heat treatment is carried out firstly, so that certain porosity can be obtained under the condition of ensuring compactness.
The preparation method of the invention also comprises a step S7, which is divided into the following three types:
s71, carrying out heat treatment and heat preservation on the formed powder in a resistance furnace at 400 ℃ for 1-6h.
S72, carrying out heat treatment and heat preservation on the formed powder in a resistance furnace at 600 ℃ for 1-6h.
S73, carrying out heat treatment and heat preservation on the formed powder in a resistance furnace at 800 ℃ for 1-6h.
The invention provides 6 groups of components and a heat treatment environment, and the following heat treatment is kept for 4 hours. As shown in table 1:
TABLE 1
The prepared quartz fiber reinforced silica low dielectric composite material was subjected to a dielectric property test, and a broadband dielectric impedance spectrometer (instrument model 40) was used to test the dielectric constant and dielectric loss tangent of the sample at an air humidity of 30%. And observing the surface microscopic morphology of the silicon dioxide composite material by using a field emission scanning electron microscope (instrument model: JSM-7500F). The surface microscopic morphology of the silica particles was observed using a field emission transmission electron microscope (instrument model: JEM-2100F).
The composite material of the present invention can be applied to a silica insulation layer portion of a high temperature resistant communication cable, as shown in fig. 1.
Fig. 2 and 3 are graphs of dielectric constants and dielectric losses for the composites of groups 1, 2, and 3, from which it can be seen that high temperature heat treatment helps to reduce the dielectric loss tangent of the silica composite, but increases the dielectric constant.
To test the variation of dielectric properties of the silica composite at ultra-high temperature, it was sintered at 1000℃for 30 min, and after the test, the dielectric constant, dielectric loss tangent, weight loss ratio, etc. were respectively tested. The weight loss rate of the group 1 product after 30 min of ultra-high temperature treatment at 1000 ℃ is 2.07 percent, and the dielectric constant and dielectric loss before ultra-high temperature treatment are respectively 2.65 and 5.11 x 10 -3 The dielectric constant rises by 5.95% and the dielectric loss falls by 59.87% after the treatment; the weight loss rate of the group 2 product after 30 min of 1000 ℃ ultrahigh temperature treatment is 1.74 percent, and the dielectric constant and dielectric loss before ultrahigh temperature treatment are respectively 2.68 and 4.03 x 10 -3 The dielectric constant after treatment rises by 4.62 percent in the same ratio, the dielectric loss is reduced by 56.75 percent, the reason that the dielectric loss is reduced is that the high temperature is favorable for removing carbon residue and moisture, the rise of the dielectric constant is also within 10 percent, and the high-temperature resistance is good and the high-temperature resistance is also excellent.
FIG. 4 is a graph of the dielectric constants of the composites of groups 4, 5, and 6, and it can be seen from the graph that the dielectric constant of the silica composite is significantly reduced by 23.2% for the 5 th group of products compared with the 4 th group, and by 20.1% for the 6 th group compared with the 4 th group.
Fig. 5 is a TEM image of 1000000 times of the 3 rd composite material, which shows that nano silica particles with different diameters are connected together, and smaller nano silica particles are filled with large silica particles, so that a close-packed structure is formed, and the overall density is improved.
Fig. 6 is a SEM image of group 3 composite material at 15000 x, and it is clear that fumed silica powder is firmly attached to chopped quartz fibers, which can enhance toughness of the silica composite material, and the phenomenon of breakdown caused by notch generation does not occur when the cable is bent or collided.
Fig. 7 is a SEM image of group 3 composites at 15000 x, showing that fumed silica is uniformly adhered to the surface of the silica fibers.
The foregoing description of the preferred embodiments of the present invention should not be taken as limiting the scope of the invention, but rather should be understood to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the following description and drawings.
Claims (3)
1. The quartz fiber reinforced silica low dielectric composite material is characterized in that the preparation raw materials comprise: 75wt% of fumed silica, 25wt% of nano silica, 20wt% of quartz fiber cotton based on the total mass of the fumed silica and the nano silica, and 3-5wt% of calcium carbonate based on the total mass of the fumed silica and the nano silica;
the preparation method of the quartz fiber reinforced silicon dioxide low-dielectric composite material comprises the following steps: s1, cutting quartz fiber cotton, and grinding into chopped fibers; s2, uniformly mixing fumed silica, nano silica and ground quartz fiber cotton in absolute ethyl alcohol, and dispersing by using ultrasonic waves; s3, adding calcium carbonate, and uniformly mixing; s4, adding silica sol for impregnation; s5, drying, and grinding the dried mixture into powder; s6, pressing the prepared powder on a powder tablet press to form; s7, carrying out heat treatment and heat preservation on the formed powder for 1-6h in the environment of 400-800 ℃.
2. The silica fiber reinforced silica low dielectric composite of claim 1, wherein the raw materials for preparation comprise: 75% by weight of fumed silica, 25% by weight of nano silica, 20% by weight of quartz fiber cotton based on the total mass of fumed silica and nano silica, and 3% by weight or 5% by weight of calcium carbonate based on the total mass of fumed silica and nano silica.
3. High temperature resistant communication cable comprising a silica insulation layer, characterized in that the silica insulation layer is made of a silica low dielectric composite material reinforced with quartz fibers according to any of claims 1-2.
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| CN202310109493.1A CN116178000B (en) | 2023-02-13 | 2023-02-13 | Quartz fiber reinforced silica low dielectric composite material |
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| CN111892339A (en) * | 2020-07-31 | 2020-11-06 | 航天特种材料及工艺技术研究所 | Nano heat insulation sheet and preparation method thereof |
| CN114437488A (en) * | 2022-01-26 | 2022-05-06 | 金发科技股份有限公司 | Low-dielectric, high-impact-resistance and high-heat-resistance cycloolefin composition as well as preparation method and application thereof |
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| KR20070066729A (en) * | 2005-12-22 | 2007-06-27 | 재단법인 포항산업과학연구원 | Fabrication method of high density & high fracture toughness silica radome |
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