EP3824480A1 - Electrical insulation material comprising a mixture of micrometric inorganic fillers and manufacturing process - Google Patents
Electrical insulation material comprising a mixture of micrometric inorganic fillers and manufacturing processInfo
- Publication number
- EP3824480A1 EP3824480A1 EP19762187.3A EP19762187A EP3824480A1 EP 3824480 A1 EP3824480 A1 EP 3824480A1 EP 19762187 A EP19762187 A EP 19762187A EP 3824480 A1 EP3824480 A1 EP 3824480A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- electrical insulation
- micrometric
- charge
- composite material
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000012772 electrical insulation material Substances 0.000 title claims abstract description 31
- 239000011256 inorganic filler Substances 0.000 title claims abstract description 28
- 229910003475 inorganic filler Inorganic materials 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 title claims description 59
- 239000002131 composite material Substances 0.000 claims abstract description 72
- 239000011159 matrix material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000004593 Epoxy Substances 0.000 claims abstract description 10
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 6
- 238000010292 electrical insulation Methods 0.000 claims description 33
- 238000004132 cross linking Methods 0.000 claims description 19
- 239000003822 epoxy resin Substances 0.000 claims description 17
- 229920000647 polyepoxide Polymers 0.000 claims description 17
- 239000012190 activator Substances 0.000 claims description 13
- 239000003999 initiator Substances 0.000 claims description 13
- 239000004848 polyfunctional curative Substances 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 12
- 239000004020 conductor Substances 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000012777 electrically insulating material Substances 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 43
- 239000000463 material Substances 0.000 description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000395 magnesium oxide Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000000518 rheometry Methods 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 150000008064 anhydrides Chemical class 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 239000000615 nonconductor Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000004971 Cross linker Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 210000003934 vacuole Anatomy 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
- C08G59/245—Di-epoxy compounds carbocyclic aromatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/40—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/016—Additives defined by their aspect ratio
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Definitions
- the present invention relates to a composite material for electrical insulation, which can in particular be used as a support for electrical conductors in high-voltage electrical equipment, such as substations in a metal envelope, commonly designated by the acronym PSEM, subjected to a high voltage i alternating and / or direct current.
- PSEM high-voltage electrical equipment
- an electrical substation in a metallic envelope consists of a high voltage electrical conductor held in the center of a metallic envelope using electrical insulating supports, such as spacers or "spacers" in English.
- the outer casing is earthed and the electrical insulation of each phase from ground is provided by an insulating medium with high dielectric strength, typically SFe.
- These stations are very “impact” and can be installed inside or outside buildings.
- the material of the insulating supports In order to be used as an electrical insulator, the material of the insulating supports must have low porosity, high dielectric strength, low dielectric permittivity and low coefficient of thermal expansion. In addition, during their use, the electrical insulating supports are subjected to a permanent electrical stress which can cause the appearance of hot spikes locally. It is therefore important that the material of the insulating supports also has a high thermal conductivity, and this at the very least. long life of supports.
- the electrical insulating supports are made of a composite material, the by an assembly of at least two components; immiscible.
- the Insulating supports are composed of an organic matrix in which one or more charges are dispersed.
- the matrix is an electrical insulating material, for example formed by the crosslinking of a reticulable mixture, possibly in the presence of a hardener.
- the fillers can be of organic or inorganic type, micrometric or nanometric, and of all fbrmej. Other additives can be included in this matrix, such as diluents or plasticizers for example.
- the electrical insulating supports can be prepared in different ways, for example by extrusion, molding or injection.
- the injection process is of particular interest because it makes it possible, on the one hand, to reduce the defects which may appear during the design, such as vacuoles or deformations during removal of the material, and allows, on the other hand apart, a standardization of the parts obtained. Nevertheless, the injection step requires that the loaded crosslinkable mixture have a rheology adapted to allow gelation under automated pressure without the appearance of bubbles. Such rheology is also suitable for gravitational vacuum casting.
- Matrix-charge interfaces are an area of high electrical stress. As shown in Figure 1, when tensioning a composite electrical insulation material A, hot spots (represented by stars) can appear at the matrix a - charge b interfaces, in particular when the matrix has low thermal conductivity. This is due to the absence of a phononic network which does not allow or very badly the transfer of thermal energy through the matrix.
- nanometric charges Alone or in combination with micrometric fillers, they can allow a gain in dielectric strength and thermal conductivity.
- nanometric fillers has drawbacks: need to control the dispersion of the charges to avoid the formation of aggregates, increase in viscosity, heavy hygiene and safety constraints during their use due to the need for '' avoid their dissemination in the air, high cost ...
- Another solution for obtaining a high thermal conductivity consists in modifying the shape of the charges, and in particular in using charges having a high form factor, for example lamellar charges or charges in the form of needle. Indeed, the presence of charges with a high form factor allows a transfer of thermal energy along these charges, and over the entire network of charges, which makes it possible to increase the thermal conductivity of the material compared to a material with low form factor fillers.
- the increase in the form factor can also allow the improvement of the dielectric strength thanks to their barrier effect.
- the disadvantage of the lamellar fillers is that they cause a sharp increase in the viscosity of the crosslinkable mixture compared to the non-lamellar fillers. Consequently, the charge rates compatible with the implementation of the retlippable mixture are relatively low, which risks leading to materials whose coefficient of thermal expansion is too high, which resist resistance to surface erosion by discharges. partial and on the surface.
- the present invention therefore aims to remedy this problem by proposing a composite electrical insulation material comprising an epoxy matrix of cycloallphatic type or of diglycidyl ether type, and from 15 to 45% by volume of charges relative to the total volume of composite material d electrical insulation.
- the composite electrically insulating material according to the invention comprises a first micrometric inorganic charge having a form factor of less than 3 and a second lamellar inorganic mlcrometric charge having a form factor ranging from 3 to 100, the volume ratio between the first charge. and the second charge going from 95/05 to 40/60.
- an “epoxy matrix” designates a crosslinked epoxy polymer.
- the form factor of a particle is the ratio between the largest dimension of the particle considered and its smallest dimension.
- the largest dimension of the particle is understood as the largest dimension of the particle when it is placed between two parallel planes.
- the smallest dimension is the smallest dimension of the particle when it is between two parallel planes. The smallest dimension corresponds to the thickness of the particle when it is flat.
- micrometric load is meant loads whose largest dimension is between 2 micrometers and 100 micrometers.
- the dimensions are number average dimensions. These can be measured by the use of measurement software coupled to a microscope, such as a scanning electron microscope, SEM.
- Lamellar filler is meant a filler having a shape factor greater than or equal to 3, and often greater than 5 or even greater than 10.
- Lamellar fillers are generally in the form of stacked plates, plates, sheets or sheets. These fillers have a thickness generally between 5 and 500 nm, and a width and a length between 2 and 100 ⁇ m. These lamellar charges differ from charges in the form of a needle because of their shape. the lamellar charges are flat with a thickness at least 4 times and at most 20,000 fibers less than their width and their length, while the charges in the form of a needle are longliform and have a thickness and a width very much less than their length by at least 4 times and at most 20,000 fols.
- the composite electrical insulation material according to the invention has the advantage of being able to be prepared by an injection process or by gravitational casting while having a high dielectric strength, a low coefficient of thermal expansion, a low porosity, a thermal conductivity. relatively high, and advantageously also low dielectric permittivity. Indeed, the judicious choice of the shape and size of the fillers, and of their respective contents, made it possible to find a balance between these properties which are a priori contradictory.
- the composite electrical insulation material according to the invention may also have one or more of the following additional characteristics:
- the second micrometric inorganic filler has a form factor ranging from 10 to 50
- the second micrometric inorganic charge is chosen from BN and AI2O3, and preferably from hBN and AI2O3;
- the first micrometric inorganic charge is chosen from
- the content of fillers ranges from 20 to 40% by volume, and preferably from 25 to 35% by volume, relative to the total volume of the composite electrical insulation material;
- the volume ratio between the first micrometric inorganic charge and the second micrometric inorganic charge ranges from 70/30 to 50/50;
- the matrix is an epoxy matrix of the dlglycldylether type, and preferably an epoxy matrix of the diglycidylether type of bisphenol A (DGEBA);
- the electrical dlsolatlon composite material further comprises a third micrometric charge, distinct from the first micrometric inorganic charge and from the second micrometric inorganic charge;
- the first micrometric inorganic filler and / or the second micrometric inorganic filler and / or, when it is present, the third micrometric filler are functionalized at the surface;
- the electrical insulation composite material is in the form of an electrically insulating support capable of holding an electrical conductor in position in a station in a metallic envelope.
- the "crosslinkable mixture” is understood to mean the mixture of an epoxy resin of the cycloaliphatic type or of the glycicyl ether type, of the first and second micrometric inorganic charges, as defined in the context of the invention , a crosslinking agent, and possibly one or more additional charges el / or additive (3).
- a crosslinking agent such as a crosslinking agent, as explained below.
- epoxy resin designates an epoxy monomer or prepolymer.
- crosslinker an agent (that is to say a chemical compound) for crosslinking the epoxy resin.
- the crosslinking agent can be an activator or initiator, or a hardener in combination with an activator or with an initiator, or a combination of an activator, an initiator and a hardener.
- the method according to the invention is easy to implement, and leads to a composite material of electrical insulation having a low porosity, a high dielectric strength, a low dielectric permltivity, a low coefficient of thermal expansion, and a high thermal conductivity.
- the method according to the invention may also have one or more of the following additional characteristics:
- the crosslinkable mixture has a viscosity ranging from 6000 mPa.s to 15000 mPa.s, preferably from 10000 mPa.s to 12000 mPas, measured at 80 ° C according to ISO standard 12058;
- the crosslinking agent is an activator, or an initiator, or a hardener in combination with an activator or with an initiator, or else a combination of an activator, an initiator and a hardener;
- the introduction of the crosslinkable mixture into the mold is done by gravitational casting or by injection into the mold;
- crosslinking is carried out by application of a crosslinking means such as heating or UV;
- the crosslinkable mixture further comprises a third micrometric charge.
- crosslinking means is a physical means allowing the crosslinking of the crosslinkable mixture, such as heating or UV.
- Another object of the invention relates to a station in a metal envelope (PSEM) comprising an external envelope internally delimiting an enclosure in which is mounted a high voltage electrical conductor using electrical insulating supports made of a composite material of electrical insulation. according to llnvention, or made of an electrical material obtained by the method according to llnvention.
- PSEM metal envelope
- Figure 1 is a schematic view of a composite electrical insulation material outside the invention, composed of a matrix and of charges having a form factor of less than 3.
- the stars represent hot points appearing at the charge-matrix interface .
- Figure 2 is a schematic view of a composite insulation material according to the invention.
- the stars represent hot spots appearing at the charge-matrix interface.
- the arrows represent the heat transfer.
- Figure 3 is a sectional view of an electrical substation in a metal casing comprising an electrically insulating support in the form of a cone.
- Figure 4 is a sectional view of an electrical substation in a metal casing comprising an electrically insulating support in the form of a "post-type".
- the invention relates to a composite electrical insulation material 1 adapted to be used to form electrically insulating supports to hold in position the conductors present in the SEMCs.
- the electrical insulation composite material is composed of a matrix 2 in which a mixture of micrometric inorganic charges is dispersed.
- the matrix 2 is formed by the crosslinking of an epoxy resin of the cycloallphatic type or of an epoxy resin of the diglycidyl ether type.
- the matrix 2 is a matrix of diglycidyl ether type, and in particular diglycidyl ether of blsphenol A.
- the electrical insulation composite material 1 also comprises a mixture of at least two distinct micrometric inorganic fillers. The presence of these two charges makes it possible to increase the thermal conductivity of the composite electrical insulation material 1 as well as its electrical resistance.
- the first micrometric inorganic filler 3 has a form factor of less than 3, and preferably less than or equal to 2, or even less than or equal to 1.5.
- the first micrometric inorganic charge 3 with a form factor of less than 3 can be of any shape, and in particular spherical or almost spherical.
- any micrometric inorganic filler with a factor of less than 5, having electrical insulation and thermal conductivity, may be suitable as the first charge 3 in the context of the invention.
- the first micrometric inorganic filler 3 mention may be made of silica (SlOz), alumina (AI 2 O 3 ), aluminum hydroxide (AI (OH) 3 ), calcium oxide (CaO ), magnesium oxide (MgO), calaum carbonate (CaC0 3 ), and titanium dioxide CTIO 2 ).
- the first micrometric inorganic filler 3 is chosen from silica (S1O 2 ) or alumina (AI 2 O 3 ).
- the composite electrical insulation material 1 preferably comprises a single charge of the first micrumetric inorganic charge type 3. Nevertheless, the composite electrical insulation material 1 can comprise several charges of the first micrometric inorganic charge type 3, and in particular two.
- the second micrometric inorganic filler 4 is of the lamellar type and has a form factor ranging from 3 to 100, and preferably from 10 to 50.
- the second micrometric inorganic filler 4 is therefore neither of the spherical type nor in the form of a needle.
- any inorganic micrometric lamellar filler with a form factor ranging from 3 to 100 may be suitable in the context of the invention as a second filler 4.
- boron nitride may be mentioned (BN) in particular in hexagonal form (hBN), or alumina (AI 2 O 3 ).
- the second micrometric inorganic filler 4 and chosen from boron nitride in hexagonal form (hBN) or and alumina (AI 2 O 3 ).
- the second micrometric inorganic charge 4 lamellar is not in the form of an aggregate. Otherwise, the aggregates are preferably broken during the preparation of the electrical insulation material 1, as detailed below.
- the composite electrical insulation material 1 preferably comprises a single charge of the second inorganic micrometric lamellar charge type 4. Nevertheless, the composite electrical insulation material 1 can comprise several charges of the second micrometric inorganic charge type 4, and in particular two.
- the composite material of electrical insulation comprises from 15 to 45% by volume of charges relative to the total volume of the composite electrical insulation material 1, and preferably from 20 to 40% by volume, and better still from 25 to 35% by volume.
- This content is understood as the total content of fillers, that is to say the content of first micrometric inorganic filler 3, of second micrometric inorganic lamellar filler 4 and of additional fillers when these are present, as set out below. after.
- the first and second micrometric inorganic fillers are present in the electrical insulation composite material 1 in a volume ratio ranging from 95/05 to 40/60, and preferably ranging from 70/30 to 50/50.
- the first micrometric inorganic filler 3 is chosen from alumina (AI2O5) and silica (Si ⁇ 1 ⁇ 4)
- the second micrometric lamellar inorganic filler 4 is chosen from boron nltride in hexagonal form (hBN) and alumina (AI2O3).
- the epoxy resin is an epoxy resin of the diglyddylether type, and for example a resin of the diglyddylether type of bisphenol A, the first micrometric inorganic filler 3 is chosen from alumina (AI2O3) and silica (Si0 2 ), and the second inorganic micrometric lamellar filler 4 is chosen from boron nltride in hexagonal form (hBN) and alumina (AI2O3).
- AI2O3 alumina
- Si0 2 silica
- the second inorganic micrometric lamellar filler 4 is chosen from boron nltride in hexagonal form (hBN) and alumina (AI2O3).
- the presence of the second inorganic micrometric lamellar charge 4 makes it possible to increase the thermal conductive paths in the material, ideally by contact between the particles but also by reducing the distance between the charges within the matrix to a virtual contact, ⁇ which considerably reduces the damage to the material due to the appearance of hot spots.
- the first inorganic charge micrometric 3 having a form factor Less than 3 makes it possible to fill the empty spaces between the second inorganic micrometric lamellar fillers 4, and thus further improve the thermal conductivity of the material.
- the second inorganic micrometric lamellar charge 4 also makes it possible to improve the dielectric rigidity of the material, and in particular in comparison with the micrometrical inorganic charges in the form of needle by making a physical barrier to the propagation of electron in the material greater due to their shape.
- the composite electrical insulation material 1 also comprises one or more other charges, different from the first and from the second micrometric inorganic charges J and 4, called additional charges.
- these additional charges are micrometric and can be organic or inorganic charges, of any shape.
- additional fillers mention may be made of glass fibers.
- the additional charges do not represent more than 10% by volume, and preferably not more than 5%, relative to the total volume of the composite electrical insulation material 1.
- these charges additional allow to improve mechanical or physicochemical properties according to the applications, for example hydrophobicity, resistance to torsion, compression, flame.
- one or more charges can be functionalized on the surface. This functionalallows in particular to improve the compatibility of the charges with the matrix, and then to improve the thermal conductivity of the material and the coefficient of thermal expansion.
- the surface functionalizations of the charges are usual in the state of the art and will not be detailed here.
- the composite electrical insulation material 1 can also include additives such as plasticizers.
- the composite electrical insulation material 1 according to the invention is weakly porous, and preferably does not contain porosities. Indeed, high porosity would prevent use as an electrical insulator for high voltage.
- the composite electrical insulation material 1 according to the invention is prepared by introducing a crosslinkable mixture into a mold, followed by a crosslinking step.
- the first step is to prepare a crosslinkable mixture.
- a crosslinkable mixture for this, an epoxy resin of cycloaliphatic type or one of dlglycidylether type, and in particular an epoxy resin of dlglyddylether type of btsphenol A.
- the first and second micrometric inorganic fillers 3 and 4 as defined above, and a crosslinking agent are mixed according to any technique known to those skilled in the art. When the mixture comprises additional fillers and / or additives, these are incorporated into the crosslinkable mixture during this first step.
- an epoxy resin - fillers premix and a crosslinking agent - fillers premix can be prepared and then brought into contact in order to prepare the crosslinkable mixture.
- the second micrometric inorganic 4 lamellar filler used is not in the form of an aggregate.
- the second inorganic micrometric 4-lamellar charge used is in the form of an aggregate.
- the method then advantageously comprises a step during which the aggregates are broken, either upstream. of the preparation of the durdssable mixture, that is during its preparation. Methods for breaking the aggregates of lamellar charges are well known in the state of the art and will not be detailed here.
- the crosslinkable mixture comprises a crosslinking agent.
- the crosslinking agent may be an activator or initiator or a curing agent in combination with an activator or an initiator, or a comb i bination of an activator, an initiator and a hardener.
- the activators, hardeners and initiators which can be used for the crosslinking of the epoxy resin of cycloaliphatic type or of diglydcylether type are those usually employed in the state of the art.
- hardeners mention may be made of dlamines and anhydrides.
- the crosslinkable mixture must have a viscosity allowing manufacture by gravitational casting under vacuum or by gelling under automated pressure.
- the crosslinkable mixture obtained has a viscosity belonging to the range going from 6000 mPa.s to 15000 mPa.s, preferably going from 10000 mPa.s to 12000 mPa.s measured at 80 ° C according to the ISO 12058 standard.
- the crosslinkable mixture obtained has a viscosity belonging to the range from 15,000 mPa.s to 29,000 mPa.s, preferably from 18,000 mPa.s to 24,000 mPa.s, measured at 50 ° C according to ISO 12058 standard.
- the control of the viscosity of the crosslinkable mixture is important, because too high a viscosity would lead to a crosslinkable mixture comprising bubbles, and therefore a final material comprising defects and / or porous.
- a high viscosity would make the crosslinkable mixture difficult to introduce into the mold by injection or by gravitational casting.
- a too low viscosity would reduce the efficiency of the manufacturing process by gelation under automated pressure.
- the increase in viscosity due to these high levels of fillers is limited, which allows the gravitational casting of the crosslinkable mixture or its injection into a mold.
- crosslinkable mixtures had a rheology adapted to be implemented by gravitational casting, or even to be able to be injected into a mold, by judiciously choosing the nature and the shape of these fillers and their proportions, and lead to a material. not very porous. This is all the more surprising since the presence of lamellar fillers at these high rates is known to usually increase the viscosity of the mixture so that this implementation is difficult, if not impossible.
- the distribution of the charges in the crosslinkable mixture is homogeneous.
- the second step of the manufacturing process according to the invention consists in introducing the crosslinkable mixture, obtained in the first step, into a mold having the desired shape.
- This introduction can be carried out according to any technique known to those skilled in the art.
- this introduction into the mold is carried out either by gravitational casting or by injection according to any technique known in the state of the art.
- the third stage consists in cross-linking the crosslinkable mixture previously introduced into the mold.
- This step can be carried out according to any technique known to those skilled in the art. According to a particular embodiment, this crosslinking step can be carried out in the presence of a crosslinking means, such as heating or UV for example.
- the setting time is advantageously greater than or equal to one hour.
- the last step of the method consists in demolding the structure obtained and made of composite material of electrical insulation 1, according to any technique known in the state of the art.
- the structure made of composite material of electrical insulation 1 thus obtained is easy to prepare by injection or gravitational casting, has good thermal conductivity and electrical insulation properties, a low coefficient of thermal expansion, and a high dielectric strength.
- the structure made of composite electrical insulation material 1 thus obtained also has a low dielectric permittivity.
- the composite electrical insulation material obtained by the method according to the invention has a low porosity, and preferably is not porous. According to a particular embodiment, it is possible to further reduce the porosity of the tomposite material of electrical insulation 1, or even to eliminate it completely, by carrying out one or more degassings of the crosslinkable mixture, before its introduction into the mold. For example, degassing can be carried out under reduced pressure of ten millibars, preferably by mixing said crosslinkable mixture.
- the invention also relates to a station in a metal casing 5 comprising an external casing 6 internally delimiting an enclosure 7 dan ⁇ which is mounted a high voltage electrical conductor 8 held in position by electrically insulating supports 9 made of a composite electrical insulation material 1 according to the invention.
- the outer metal casing G has a cylindrical shape. This example is not limitative.
- a high-voltage electrical conductor 8 of any known type on the ground is mounted inside the external metal casing G.
- the high-voltage electrical conductor 8 is tubular in the embodiment shown in FIGS. 3 and 4.
- the high voltage electrical conductor 8 is held in the center of the external metal casing 6 using electrically insulating supports 9, such as spacers produced in the examples illustrated by cones ( Figure 3) or "post-types * ( Figure 4).
- electrically insulating supports 9 are made of a composite material of electrical insulation 1 according to the invention.
- the internal volume of the enclosure 7 is filled with an insulating fluid, typically an insulating gas such as SFe.
- an insulating fluid typically an insulating gas such as SFe.
- a composite material of electrical insulation A according to the intention and four materials of electrical insulation except Invention (B (without load) - C (with only a load having a form factor lower than 3), D (with only a lamellar load) and E (with a volume ratio between the form factor charge less than 3 and the lamellar charge outside the invention) were prepared (see Table 1).
- the total charge content a of the composite material D could not be increased until 37% by volume due to the too high viscosity of the crosslinkable mixture.
- the epoxy resin used is the epoxy resin of the diglycldylether type of bisphenol A (DGfcBA) supplied by Huntsman under the reference CY 5925.
- the fillers used in the various composite materials are a micrometric alumina supplied by the Imerys under the reference Alodur®WSK, and the hexagonal boron nltride hBN supplied by Momentlve under the reference PT120.
- a hardener as crosslinking agent was also used: an anhydride sold under the reference HY5925 by the company Huntsman.
- Materials A to E are prepared as follows. The charges are dried at 80 ° C under primary vacuum for 24 hours before use. An epoxy resin - fillers and hardener - fillers premix is made in order to facilitate the dispersion of the fillers. The premixes are then mixed in proportions such that the mass ratio of epoxy resin: hardener is 100; 80. All the mixes are carried out using a SpeedMixer DAC 400 planetary mixer at 2500 rpm. The crosslinkable mixture is then degassed under primary vacuum at S0 ° C for 1 hour, then is then poured by gravltional casting into a closed aluminum mold, the surface of which has been treated with a release agent. The mixture is finally crosslinked by heating according to the temperature cycle following r 4 h at 100 ° C then 8 h at 140 ° C.
- the properties of the different materials A to D were evaluated: viscosity (measured at 50 ° C according to ISO 12058 standard), dielectric strength (measured according to ISO 60243-1), thermal conductivity (measured according to ISO 8894 standard) and the coefficient of thermal expansion.
- the coefficient of thermal expansion (CTE) was determined using a TMA (Thermomechanlcal Analyzer) Q400 TA Instruments from 40 ° C to 170 ° C.
- the force applied by the quadrant expansion probe is 5 mN and the temperature ramp is 3 u C / min.
- the measurement is made under nitrogen.
- the curves used are those obtained in the 2nd temperature rise.
- the results obtained are summarized in Table 2.
- the material E was used to illustrate the importance of the ratios between charges and only the values of electrical rigidity and thermal conductivity were evaluated.
- the viscosity of crosslinkable mixtures is affected by the presence and nature of the fillers.
- the crosslinkable mixture B without filler has the lowest viscosity. This viscosity is higher in Mixed C due to the presence of polydisperse alumina.
- the viscosity when the crosslinkable mixture contains only hBN as a filler is very high, so that the total content in mixture D is 17%.
- the crosslinkable mixture A according to the invention has a high total content of fillers, and an alumina load ratio hBN of 86.5 / 13.5, while having a viscosity allowing its implementation.
- the composite material A according to the invention has a dielectric strength similar to that of the composite material C outside the invention, and substantially lower than that of the material B outside the invention.
- the addition of lamellar charge in the composite material A according to the invention does not negatively affect the dielectric strength.
- the composite material E also has a dielectric strength equivalent to the composite material C and the low charge of the lamellar type seems to have no impact on this property.
- the thermal conductivity is higher in the composite material A according to the invention compared to all the composite materials outside the invention tested (thermal conductivity increased by at least 25%).
- the thermal conductivity of the material E is very slightly higher than that of the material C and falls within the margin of error of the latter.
- the small addition of lamellar charge in the material E therefore appears to be insufficient for the latter to be in sufficient quantity allowing it to have a positive impact on this property.
- the coefficient of thermal expansion is lower for the composite material A according to the invention, compared to materials B, C and D outside the invention (reduction up to 50%).
- the composite material A according to the invention makes it possible to combine satisfactory dielectric rigidity, high thermal conductivity, and a low coefficient of thermal expansion while being easy to use thanks to a controlled viscosity. of the crosslinkable mixture.
- the composite material A has a very low porosity.
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- Organic Chemistry (AREA)
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Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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FR1856761A FR3084202B1 (en) | 2018-07-20 | 2018-07-20 | ELECTRICAL INSULATION MATERIAL INCLUDING A MIXTURE OF INORGANIC MICROMETRIC CHARGES AND METHOD OF MANUFACTURING |
PCT/FR2019/051795 WO2020016525A1 (en) | 2018-07-20 | 2019-07-17 | Electrical insulation material comprising a mixture of micrometric inorganic fillers and manufacturing process |
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EP3824480A1 true EP3824480A1 (en) | 2021-05-26 |
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EP19762187.3A Withdrawn EP3824480A1 (en) | 2018-07-20 | 2019-07-17 | Electrical insulation material comprising a mixture of micrometric inorganic fillers and manufacturing process |
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EP (1) | EP3824480A1 (en) |
JP (1) | JP2021530082A (en) |
KR (1) | KR20210064183A (en) |
CN (1) | CN112424880A (en) |
FR (1) | FR3084202B1 (en) |
WO (1) | WO2020016525A1 (en) |
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US6048919A (en) * | 1999-01-29 | 2000-04-11 | Chip Coolers, Inc. | Thermally conductive composite material |
DE602005026215D1 (en) * | 2004-07-13 | 2011-03-17 | Areva T & D Sas | METHOD FOR PRODUCING AN ISOLATOR FOR HIGH VOLTAGE APPLICATIONS |
CN101035876A (en) * | 2004-08-23 | 2007-09-12 | 莫门蒂夫性能材料股份有限公司 | Thermally conductive composition and method for preparing the same |
US20090152491A1 (en) * | 2007-11-16 | 2009-06-18 | E. I. Du Pont De Nemours And Company | Thermally conductive resin compositions |
JP4495768B2 (en) * | 2008-08-18 | 2010-07-07 | 積水化学工業株式会社 | Insulating sheet and laminated structure |
JP2011021069A (en) * | 2009-07-14 | 2011-02-03 | Sakai Chem Ind Co Ltd | Heat-radiating filler composition, resin composition, heat-radiating grease and heat-radiating coating composition |
JP5647945B2 (en) * | 2011-05-31 | 2015-01-07 | 日本発條株式会社 | Insulating resin composition for circuit board, insulating sheet for circuit board, laminated board for circuit board, and metal base circuit board |
US20140178693A1 (en) * | 2012-12-21 | 2014-06-26 | General Electric Company | High thermal conductivity composite for electric insulation, and articles thereof |
DE112014002796B4 (en) * | 2013-06-14 | 2020-07-02 | Mitsubishi Electric Corporation | Thermosetting resin composition, method of manufacturing a thermally conductive sheet and power module |
US9611414B2 (en) * | 2014-07-11 | 2017-04-04 | Henkel IP & Holding GmbH | Thermal interface material with mixed aspect ratio particle dispersions |
JP6547277B2 (en) * | 2014-10-31 | 2019-07-24 | 住友ベークライト株式会社 | Molding materials and articles |
TWI710595B (en) * | 2014-12-08 | 2020-11-21 | 日商昭和電工材料股份有限公司 | Epoxy resin composition, resin sheet, prepreg, metal foil with resin, metal substrate and power semiconductor device |
TW201704413A (en) * | 2015-06-08 | 2017-02-01 | 漢高股份有限及兩合公司 | High thermally conductive low pressure moldable hotmelt |
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2018
- 2018-07-20 FR FR1856761A patent/FR3084202B1/en active Active
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2019
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- 2019-07-17 JP JP2020572816A patent/JP2021530082A/en active Pending
- 2019-07-17 WO PCT/FR2019/051795 patent/WO2020016525A1/en unknown
- 2019-07-17 KR KR1020217001898A patent/KR20210064183A/en unknown
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JP2021530082A (en) | 2021-11-04 |
CN112424880A (en) | 2021-02-26 |
FR3084202B1 (en) | 2020-10-23 |
WO2020016525A1 (en) | 2020-01-23 |
KR20210064183A (en) | 2021-06-02 |
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