CN106851874B - Ceramic electrothermal element core and preparation method thereof and ceramic electrothermal element fire-bar and heater - Google Patents
Ceramic electrothermal element core and preparation method thereof and ceramic electrothermal element fire-bar and heater Download PDFInfo
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- CN106851874B CN106851874B CN201710060329.0A CN201710060329A CN106851874B CN 106851874 B CN106851874 B CN 106851874B CN 201710060329 A CN201710060329 A CN 201710060329A CN 106851874 B CN106851874 B CN 106851874B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 293
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 196
- 239000010949 copper Substances 0.000 claims abstract description 196
- 229910052802 copper Inorganic materials 0.000 claims abstract description 196
- 239000000758 substrate Substances 0.000 claims abstract description 161
- 239000012790 adhesive layer Substances 0.000 claims abstract description 15
- 239000000853 adhesive Substances 0.000 claims abstract description 5
- 230000001070 adhesive effect Effects 0.000 claims abstract description 5
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 33
- 239000005751 Copper oxide Substances 0.000 claims description 33
- 229910000431 copper oxide Inorganic materials 0.000 claims description 33
- 239000001301 oxygen Substances 0.000 claims description 26
- 229910052760 oxygen Inorganic materials 0.000 claims description 26
- 239000004411 aluminium Substances 0.000 claims description 24
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 24
- 229910052782 aluminium Inorganic materials 0.000 claims description 24
- 238000010030 laminating Methods 0.000 claims description 22
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 230000003647 oxidation Effects 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 17
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 14
- 230000007797 corrosion Effects 0.000 claims description 10
- 238000005260 corrosion Methods 0.000 claims description 10
- 239000012298 atmosphere Substances 0.000 claims description 8
- 239000010410 layer Substances 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- 230000009477 glass transition Effects 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 5
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 230000017525 heat dissipation Effects 0.000 claims 1
- 238000012546 transfer Methods 0.000 abstract description 21
- 239000013464 silicone adhesive Substances 0.000 abstract description 10
- 238000012360 testing method Methods 0.000 description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 15
- 239000000741 silica gel Substances 0.000 description 15
- 229910002027 silica gel Inorganic materials 0.000 description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000013527 degreasing agent Substances 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229920001646 UPILEX Polymers 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 229910017083 AlN Inorganic materials 0.000 description 1
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
- H05B3/26—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base
- H05B3/265—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base the insulating base being an inorganic material, e.g. ceramic
-
- 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
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Resistance Heating (AREA)
- Surface Heating Bodies (AREA)
Abstract
The present invention relates to ceramic electrothermal element fields, disclose ceramic electrothermal element core and preparation method thereof and ceramic electrothermal element fire-bar and heater.Ceramic electrothermal element core includes：Ceramic electrothermal element plate covers copper ceramic substrate and adhesive layer；Wherein, the copper ceramic substrate that covers includes ceramic insulating substrate and the copper electrode piece on the part surface of the ceramic insulating substrate, does not have adhesive between the copper electrode piece and the ceramic insulating substrate；The adhesive layer is arranged between the ceramic electrothermal element plate and the copper electrode piece, is bonded for will cover copper ceramic substrate described at least two with the ceramic electrothermal element plate.It realizes and covers copper ceramic substrate and can be molded when without using silicone adhesive, have good adhesion strength, the high heater of heat transfer efficiency can be made.
Description
Technical field
The present invention relates to ceramic electrothermal element heater contexts, and in particular, to ceramic electrothermal element core prepares the pottery
The method of porcelain heating element core and ceramic electrothermal element fire-bar comprising the ceramic electrothermal element core and include the pottery
The heater of porcelain heating element core.
Background technology
Heater using ceramic electrothermal element (PTC) has the characteristics that quick heating.At present by PTC processing for heater
When middle, usually first pass through silica gel and paste copper electrode and ceramic insulating substrate, through hot setting, make copper electrode and insulating ceramics base
Plate is strong bonded；Then it is again that the substrate and PTC is bonding, it forms PTC cores and is used to prepare heater.In ceramic substrate, copper
It is separated between electrode and ceramic insulating substrate, there be one layer of layer of silica gel in centre.Due to the relatively low (1W/ (mK) of silica gel thermal conductivity factor
Left and right), the heat transfer efficiency of PTC is influenced, and silica gel high temperature ageing is obvious, caking property is deteriorated after aging, and heat conduction declines, and influences
The heat transmission of PTC can reduce heater power after long-time service.
The content of the invention
It is existing to cover copper the purpose of the invention is to overcome in ceramic electrothermal element core prepared by ceramic electrothermal element
Ceramic substrate influences the defects of ceramic electrothermal element heat transfer, provides ceramic electrothermal element core and preparation method thereof and ceramics
Heating element fire-bar and heater.
To achieve these goals, the present invention provides ceramic electrothermal element core, which includes：Ceramic electrothermal element
Plate covers copper ceramic substrate and adhesive layer；Wherein, the copper ceramic substrate that covers includes ceramic insulating substrate and in the insulating ceramics
Copper electrode piece on the part surface of substrate does not have adhesive between the copper electrode piece and the ceramic insulating substrate；It is described
Adhesive layer is arranged between the ceramic electrothermal element plate and the copper electrode piece, for will cover copper ceramic base described at least two
Plate is bonded with the ceramic electrothermal element plate.
The present invention also provides prepare the present invention ceramic electrothermal element core method, including：
(1) at least one side of copper electrode piece is subjected to oxidation and forms copper oxide, obtain the copper electrode with copper oxide
Piece；Then it is bonded the copper electrode piece with copper oxide respectively in the both sides of ceramic insulating substrate；Wherein described oxidation
Layers of copper is between the ceramic insulating substrate and the copper electrode piece；
(2) product made from step (1) is sintered and cooled down, obtain the laminating copper electrode piece at least two sides
Substrate；
(3) substrate is subjected to copper corrosion, obtains only one side and cover copper ceramic substrate with the copper electrode piece；
(4) will cover that copper ceramic substrate is bonded in ceramic electrothermal element plate described at least two using binding agent at least two
On face；Wherein, the copper electrode piece be located at the ceramic electrothermal element plate and it is described cover copper ceramic substrate between, be made ceramic electrical
Thermal element core.
The present invention also provides ceramic electrothermal element fire-bar, including：Aluminium side leads to, and internal heating is led to positioned at the aluminium side
Core and the aluminium side lead to the insulating film between the heats；The heats is ceramics provided by the invention
Heating element core.
The present invention also provides ceramic electrothermal element heater, including：It multigroup fire-bar and is connected with the fire-bar
Multigroup radiating fin；Wherein, the fire-bar is ceramic electrothermal element fire-bar provided by the invention.
Through the above technical solutions, the pottery of ceramic electrothermal element heater to be preferably used for the present invention provides heat transfer efficiency
Porcelain heating element core, the copper ceramic substrate therein that covers first pass through high temperature sintering in the fitting of the both sides of ceramic insulating substrate with oxygen
Change the copper electrode piece of layers of copper, then only retain the copper electrode piece of ceramic insulating substrate one side through copper corrosion again and be made.The present invention
What is provided covers the defects of copper ceramic substrate can be easily bent to avoid copper electrode piece and ceramic insulating substrate compound tense, realizes and covers
Copper ceramic substrate can be molded when without using silicone adhesive, so as to provide heat transfer efficiency high heater.
The other feature and technique effect of the present invention will be described in detail in subsequent specific embodiment part.
Description of the drawings
Attached drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool
Body embodiment is together for explaining the present invention, but be not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is each several part decomposition diagram of the ceramic electrothermal element core of the present invention；
Fig. 2 a are in the schematic diagram of the laminating copper electrode piece in the two sides of ceramic insulating substrate in method provided by the invention；
Fig. 2 b are in the top view of the laminating copper electrode piece in the two sides of ceramic insulating substrate in method provided by the invention；
Fig. 2 c are the schematic diagrames for covering copper ceramic substrate of the present invention, and the copper electrode piece of one side is corroded；
Fig. 2 d are the top views for covering copper ceramic substrate of the present invention；
Fig. 3 is the decomposition diagram of ceramic electrothermal element core of the copper electrode piece with ceramic insulating substrate after laminating；
Fig. 4 is the structure diagram of ceramic electrothermal element fire-bar；
Fig. 5 is the structure diagram of ceramic electrothermal element heater.
Reference sign
1st, ceramic insulating substrate 2, copper electrode piece 3, ceramic electrothermal element plate
4th, aluminium side leads to 5, insulating film 6, ceramic electrothermal element fire-bar
7th, radiating fin
Specific embodiment
The specific embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The endpoint of disclosed scope and any value are not limited to the accurate scope or value herein, these scopes or
Value should be understood to comprising the value close to these scopes or value.For numberical range, between the endpoint value of each scope, respectively
It between the endpoint value of a scope and individual point value and can be individually combined with each other between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The first object of the present invention provides ceramic electrothermal element core, which includes：Ceramic electrothermal element plate covers copper
Ceramic substrate and adhesive layer；Wherein, the copper ceramic substrate that covers includes ceramic insulating substrate and in the ceramic insulating substrate
Copper electrode piece on part surface does not have adhesive between the copper electrode piece and the ceramic insulating substrate；The adhesive layer
It is arranged between the ceramic electrothermal element plate and the copper electrode piece, for copper ceramic substrate and institute will to be covered described at least two
Ceramic electrothermal element plate is stated to be bonded.
Ceramic electrothermal element core provided by the invention, including ceramic electrothermal element plate be by ceramic electrothermal element
(PTC) plate that straight forming obtains.The ceramic electrothermal element core is eventually for preparing ceramic electrothermal element heater, institute
Strip plate can be processed as needed by stating ceramic electrothermal element plate, as shown in fig. 1.Can be commercially available.It is shown
Ceramic electrothermal element can be barium titanate base class ceramic material.General ceramic electrothermal element thickness is 2~4cm.
In ceramic electrothermal element core provided by the invention, the preferably described copper ceramic substrate that covers coats the ceramic electric heating member
Part.There can be the copper ceramic substrate that covers to coat respectively in the both sides of the ceramic electrothermal element as shown in Figure 3.It is described to cover copper pottery
Porcelain substrate includes the copper electrode piece and the ceramic insulating substrate, between the copper electrode piece and the ceramic insulating substrate not
It is bonded by adhesive, i.e., without using silica gel, but the ceramic insulating substrate is passed through into first two sides and is sintered laminating institute
Copper electrode piece is stated, then erodes the method preparation of one side copper electrode piece, it can the copper electrode piece and the ceramic insulating substrate
It is directly laminating, it eliminates caused by the prior art exists due to silica gel and covers the defects of copper ceramic substrate heat transfer efficiency is poor.The copper
Electrode slice can be material commonly used in the art, for powering on, heating ceramic heating element.The insulating ceramics base
Plate can be baseplate material commonly used in the art, can be aluminium oxide ceramics or aluminium nitride ceramics.The insulating ceramics base
The thickness of plate can be 0.3~1.5mm, and the thickness of the copper electrode piece can be 0.1~0.5mm.The one of the copper electrode piece
Side has the terminal stretched out on the outside of the ceramic insulating substrate, and for connecting power supply, the terminal stretches out the insulating ceramics base
Length about more than 15mm on the outside of plate.And other each sides of the copper electrode piece are without departing from the model of the ceramic insulating substrate
It encloses, in order to avoid electric leakage.The appearance and size of the general copper electrode piece is smaller 1~3mm than the appearance and size of the ceramic insulating substrate.Such as
Shown in Fig. 2 d and Fig. 3.
In ceramic electrothermal element core provided by the invention, as shown in figure 4, the appearance and size of the ceramic electrothermal element is not
Beyond the appearance and size of the ceramic insulating substrate, not with the device contacts covered beyond copper ceramic substrate.
It is described to cover between copper ceramic substrate and the ceramic electrothermal element in ceramic electrothermal element core provided by the invention
It is bonded as one by the adhesive layer.The adhesive layer can be layer of silica gel.The adhesive layer thickness can be 0.1~
0.3mm。
The second object of the present invention provides the method for preparing the ceramic electrothermal element core of the present invention, including：
(1) at least one side of copper electrode piece is subjected to oxidation and forms copper oxide, obtain the copper electrode with copper oxide
Piece；Then it is bonded the copper electrode piece with copper oxide respectively in the both sides of ceramic insulating substrate；Wherein described oxidation
Layers of copper is between the ceramic insulating substrate and the copper electrode piece；
(2) product made from step (1) is sintered and cooled down, obtain the laminating copper electrode piece at least two sides
Substrate；
(3) substrate is subjected to copper corrosion, obtains only one side and cover copper ceramic substrate with the copper electrode piece；
(4) will cover that copper ceramic substrate is bonded in ceramic electrothermal element plate described at least two using binding agent at least two
On face；Wherein, the copper electrode piece be located at the ceramic electrothermal element plate and it is described cover copper ceramic substrate between, be made ceramic electrical
Thermal element core.
In the method provided by the invention for preparing ceramic electrothermal element core, the copper electrode piece and the insulating ceramics base
Plate it is laminating, preferably take first the two sides of ceramic insulating substrate simultaneously the laminating copper electrode piece, using the side of high temperature sintering
Method carries out laminating；Then copper electrode piece is corroded again, obtains covering copper ceramic substrate only in one side with copper electrode piece.First
Two-sided laminating copper electrode piece can be overcome when progress high temperature sintering is laminating by copper electrode piece and ceramic insulating substrate, copper electrode
Piece is easily bent deformation with ceramic insulating substrate or even ceramic insulating substrate fractures, it is impossible to which obtain qualification covers copper ceramic substrate
The defects of.
In the present invention, step (1) on the surface of the copper electrode piece for first forming copper oxide, to facilitate further
The copper electrode piece and the ceramic insulating substrate are sintered to form one.Specifically, the oxidation can be in micro- oxygen
It is carried out under atmosphere, such as the mixed gas using oxygen and nitrogen, wherein oxygen content is 100~500ppm (volume).Oxidation
Temperature is 600~900 DEG C, and oxidization time is 10~30min.A kind of preferred embodiment, oxygen content in micro- oxygen atmosphere
For 300~400ppm (volume)；Oxidizing temperature is 650~750 DEG C.The oxidation is carried out under the conditions of above-mentioned micro- oxygen atmosphere to obtain
Copper oxide can have suitable structure, further by sintering by the copper electrode piece and the ceramic insulating substrate phase
When bonding, contribute in the effect of sintering to provide better adhesion strength, and the ceramic electrothermal element heating finally obtained is provided
Utensil has high heat transfer efficiency.The thickness of the copper oxide of acquisition can be with there is no particular limitation, about 5~25 μm, preferably
10~20 μm.After the completion of sintering, the oxidation can be not present between the copper electrode piece and the ceramic insulating substrate
Layers of copper.The copper electrode piece is directly joined together with the ceramic insulating substrate.It preferably, can be only by the copper electrode piece
Carry out on one side oxidation form copper oxide.Further, which carries out laminating with the ceramic insulating substrate, realizes
The final copper electrode piece is laminating with the ceramic insulating substrate.In the sintering process, the copper oxide with it is described absolutely
Bonding can be more readily formed between edge ceramic substrate, realize more preferable between the copper electrode piece and the ceramic insulating substrate
Bonding.Such as can be by being covered described in stretching test measurement in copper ceramic substrate, the copper electrode piece and the insulating ceramics
Adhesion strength between substrate reaches more than 500N, is preferably 860N~870N.Caking property is better than the effect using silica gel.
In the present invention, step (2) is used in the two-sided by being sintered the laminating copper electrode piece of the ceramic insulating substrate.
Two opposite faces on the two-sided generally ceramic insulating substrate.As shown in figures 2 a and 2b.Under preferable case, sintering temperature is
1050~1080 DEG C.Sintering can be from room temperature to the sintering temperature, Ran Houbao with the heating rate of 5~10 DEG C/min
10~30min of temperature is completed.Cooling can be Slow cooling, in order to avoid influence between the copper electrode piece and the ceramic insulating substrate
Bond effect, such as can be cooled to less than 50 DEG C with 5~10 DEG C/min of rate of temperature fall.
In the present invention, step (3) only retains one side on the ceramic insulating substrate for part copper electrode slice to be eroded
There is copper electrode piece, become and cover copper ceramic substrate, available for subsequently preparing ceramic electrothermal element core.The corrosion can be by step
Suddenly after the substrate that (2) obtain protects face copper electrode piece therein, it is put into and extra copper electrode piece is removed in etching solution, until dew
Go out ceramic insulating substrate.As illustrated in figures 2 c and 2d.
In above-mentioned preparation method provided by the invention, it may further include the copper electrode piece and carry out before oxidation clearly
It washes.The similary ceramic insulating substrate is cleaned before progress is laminating.The cleaning can use cleaning solution, such as weak acid and
Degreaser.
It is flat it is possible to further be polishing to the obtained copper electrode piece surface for covering copper ceramic substrate in the present invention
It is whole, so as to bonding subsequently with ceramic electrothermal element plate.
In the present invention, step (4) is used to cover copper ceramic substrate and the ceramic electrothermal element plate is bonding by described.It is preferred that
Ground, in step (4), by the binding agent film it is described cover copper ceramic substrate in the copper electrode on piece, then with institute
It states the bonding of ceramic electrothermal element plate and cures 20~30min at 200~300 DEG C.The binding agent can be silica gel.The silicon
Glue is binding material commonly used in the art, is repeated no more.The thickness for the adhesive layer that the silica gel is formed can be 0.1~
0.3mm.Ensure to obtain the adhesion strength needed.
The third object of the present invention provides ceramic electrothermal element fire-bar, including：Aluminium side leads to, and leads to positioned at the aluminium side interior
The heats in portion and the aluminium side lead to the insulating film between the heats；The heats carries for the present invention
The ceramic electrothermal element core of confession.
In the present invention, the aluminium side leads to the device that can be this field conventionally used for loading ceramic electrothermal element core.Such as
Shown in Fig. 4, it can be that section is rectangular tubing that the aluminium side, which leads to,.The heats is loaded after being coated by the insulating film
The inside led into the aluminium side.Lead to it is preferred that can the aluminium side be squeezed by press again, lead to the aluminium side, insulating film and add
It is adjacent between hot core, wherein the aluminium side, which leads to, can play the role of fixed, heat conduction, is conducive to what ceramic electrothermal element was sent
Heat outwards transmits.
In the present invention, the insulating film can be Kapton.Can be polypyromelliticimide film or biphenyl
Type Kapton.The relative density of the Kapton can be 1.39~1.45.It can be with 280 DEG C or more
Glass transition temperature, preferably can be using glass transition temperature as 280~600 DEG C.The insulating film can be commercially available, such as Dupont
The polypyromelliticimide film of the trade name Kapton of company or the trade name Upilex's of company of Ube Industries Ltd.
Biphenyl polyimide film.
The fourth object of the present invention provides ceramic electrothermal element heater, including：Multigroup fire-bar and with it is described plus
Multigroup radiating fin of hot item connection；Wherein, the fire-bar is ceramic electrothermal element fire-bar provided by the invention.
Ceramic electrothermal element heater provided by the invention, as shown in figure 5, can be that multigroup fire-bar is arranged side by side, it is more
Group radiating fin bonds multigroup fire-bar.The heat that the radiating fin can send the ceramic electrothermal element in the fire-bar
Amount distributes.
The present invention will be described in detail by way of examples below.
In following embodiment and comparative example, the adhesion strength for covering copper ceramic substrate is measured by stretching test method.
Ceramic electrothermal element heater heat transfer efficiency can be drawn by testing heater power；
The raw material used is commercially available product.
Embodiment 1
(1) by two copper electrode pieces, (a length of 20cm (not including terminal), width 1.5cm, thickness 0.3mm have the end of 15mm
Son) and ceramic insulating substrate (a length of 21cm, width 2cm, thickness 1.2mm) using acetic acid and degreaser (model LB-116) progress
Cleaning；
By the copper electrode piece after cleaning micro- oxygen atmosphere (oxygen and nitrogen mixture, oxygen content are 300ppm (volume))
Under, 700 DEG C of oxidation 25min obtain the copper electrode piece with copper oxide, about 15 μm of copper oxide thickness；
(2) copper oxide of two copper electrode pieces is bonded to two sides of ceramic insulating substrate after cleaning respectively
On, it is then sintered, 1050 DEG C of sintering temperature is warming up to the heating rate of 10 DEG C/min, and keeps the temperature 20min；Then with 5
DEG C/rate of temperature fall of min carries out being cooled to 40 DEG C, obtain the substrate of the laminating copper electrode piece in two sides；
(3) substrate for obtaining step (3), carries out overlay film protection on one side, and another side uses etching solution (corrosive liquid model
QK-005 corrosion) is carried out until exposing ceramic insulating substrate；The copper electrode piece of reservation is polished flat, obtains covering copper ceramics
Substrate；Copper ceramic substrate will be covered and carry out adhesion strength test, result (is glued between copper electrode piece and ceramic insulating substrate at this time for 860N
Knot is destroyed)；
(4) silica gel (Toshiba XE14-0425) is applied to two and covers copper ceramic substrate by what step (1)-(3) obtained
Copper electrode on piece, then the both sides of ceramic electrothermal element plate (thickness 2cm) are respectively adhered on, then cured at 200 DEG C,
Adhesive layer thickness is 0.2mm, obtains ceramic electrothermal element core.
(5) by ceramic electrothermal element core coat upper Kapton (Upilex R, 280 DEG C of glass transition temperature, relatively
Density 1.41) after, the inside that aluminium side leads to is loaded into, then through press extruding aluminium side is made to lead to and Kapton, ceramic electric heating member
It is adjacent between part core, obtains ceramic electrothermal element fire-bar；
(6) the multiple ceramic electrothermal element fire-bars that will be obtained through step (5) are by silicone adhesive radiating fin, and arrange
It is assembled into ceramic electrothermal element heater.
Ceramic electrothermal element heater is subjected to heat transfer efficiency test, Energy Efficiency Ratio result is 98.7%.
Embodiment 2
(1) by two copper electrodes, (a length of 20cm of piece (not including terminal), width 1.5cm, thickness 0.3mm have the end of 15mm
Son) and ceramic insulating substrate (a length of 21cm, width 2cm, thickness 1.2mm) using acetic acid and degreaser (model SJ612A) progress
Cleaning；
By the copper electrode piece after cleaning micro- oxygen atmosphere (oxygen and nitrogen mixture, oxygen content are 400ppm (volume))
Under, 750 DEG C of oxidation 10min obtain the copper electrode piece with copper oxide, about 10 μm of copper oxide thickness；
(2) copper oxide of two copper electrode pieces is bonded to two sides of ceramic insulating substrate after cleaning respectively
On, it is then sintered, 1080 DEG C of sintering temperature is warming up to the heating rate of 8 DEG C/min, and keeps the temperature 30min；Then with 10
DEG C/rate of temperature fall of min carries out being cooled to 45 DEG C, obtain the substrate of the laminating copper electrode piece in two sides；
(3) substrate for obtaining step (3), carries out overlay film protection on one side, and another side uses etching solution (corrosive liquid model
Corrosion 89-21254) is carried out until exposing ceramic insulating substrate；The copper electrode piece of reservation is polished flat, obtains covering copper pottery
Porcelain substrate；Copper ceramic substrate will be covered and carry out adhesion strength test, result 870N；
(4) silica gel (Toshiba XE14-0425) is applied to two and covers copper ceramic substrate by what step (1)-(3) obtained
Then copper electrode on piece is respectively adhered on the both sides of ceramic electrothermal element plate (thickness 3cm), then is cured at 300 DEG C,
Adhesive layer thickness is 0.1mm, obtains ceramic electrothermal element core.
(5) by ceramic electrothermal element core coat upper Kapton (Upilex S, 500 DEG C of glass transition temperature, relatively
Density 1.45) after, the inside that aluminium side leads to is loaded into, then through press extruding aluminium side is made to lead to and Kapton, ceramic electric heating member
It is adjacent between part core, obtains ceramic electrothermal element fire-bar；
(6) the multiple ceramic electrothermal element fire-bars that will be obtained through step (5) are by silicone adhesive radiating fin, and arrange
It is assembled into ceramic electrothermal element heater.
Ceramic electrothermal element heater is subjected to heat transfer efficiency test, Energy Efficiency Ratio result is 98.6%.
Embodiment 3
(1) by two copper electrodes, (a length of 20cm of piece (not including terminal), width 1.5cm, thickness 0.3mm have the end of 15mm
Son) and ceramic insulating substrate (a length of 21cm, width 2cm, thickness 1.2mm) using acetic acid and degreaser (model LB-116) progress
Cleaning；
By the copper electrode piece after cleaning micro- oxygen atmosphere (oxygen and nitrogen mixture, oxygen content are 350ppm (volume))
Under, 650 DEG C of oxidation 30min obtain the copper electrode piece with copper oxide, about 20 μm of copper oxide thickness；
(2) copper oxide of two copper electrode pieces is bonded to two sides of ceramic insulating substrate after cleaning respectively
On, it is then sintered, 1070 DEG C of sintering temperature is warming up to the heating rate of 5 DEG C/min, and keeps the temperature 30min；Then with 8
DEG C/rate of temperature fall of min carries out being cooled to 30 DEG C, obtain the substrate of the laminating copper electrode piece in two sides；
(3) substrate for obtaining step (3), carries out overlay film protection on one side, and another side uses etching solution (corrosive liquid model
QK-005 corrosion) is carried out until exposing ceramic insulating substrate；The copper electrode piece of reservation is polished flat, obtains covering copper ceramics
Substrate；Copper ceramic substrate will be covered and carry out adhesion strength test, result 870N；
(4) silica gel (Toshiba XE14-0425) is applied to two and covers copper ceramic substrate by what step (1)-(3) obtained
Then copper electrode on piece is respectively adhered on the both sides of ceramic electrothermal element plate (thickness 4cm), then is cured at 250 DEG C,
Adhesive layer thickness is 0.3mm, obtains ceramic electrothermal element core.
(5) by the upper Kapton of ceramic electrothermal element core cladding, (Kapton, 385 DEG C of glass transition temperature are relatively close
After spending 1.39), the inside that aluminium side leads to is loaded into, then through press extruding aluminium side is made to lead to and Kapton, ceramic electrothermal element
It is adjacent between core, obtains ceramic electrothermal element fire-bar；
(6) the multiple ceramic electrothermal element fire-bars that will be obtained through step (5) are by silicone adhesive radiating fin, and arrange
It is assembled into ceramic electrothermal element heater.
Ceramic electrothermal element heater is subjected to heat transfer efficiency test, Energy Efficiency Ratio result is 98.7%.
Embodiment 4
According to the method for embodiment 1, the difference is that, in step (1), with " oxygen content is 100ppm (volume)) ", it replaces
" oxygen content is 300ppm (volume)) ", about 8 μm of copper oxide thickness.
The copper ceramic substrate that covers prepared carries out adhesion strength test, result 760N.
It prepares ceramic electrothermal element heater and carries out heat transfer efficiency test, Energy Efficiency Ratio result is 96.7%.
Embodiment 5
According to the method for embodiment 1, the difference is that, in step (1), with " 600 DEG C of oxidation 25min ", replace " 700 DEG C of oxygen
Change 25min ", about 24 μm of copper oxide thickness.
The copper ceramic substrate that covers prepared carries out adhesion strength test, result 780N.
It prepares ceramic electrothermal element heater and carries out heat transfer efficiency test, Energy Efficiency Ratio result is 95.7%.
Embodiment 6
According to the method for embodiment 1, the difference is that, in step (1), with " oxygen content is 500ppm (volume)) ", it replaces
" oxygen content is 300ppm (volume)) ", about 25 μm of copper oxide thickness.
The copper ceramic substrate that covers prepared carries out adhesion strength test, result 730N.
It prepares ceramic electrothermal element heater and carries out heat transfer efficiency test, Energy Efficiency Ratio result is 91.0%.
Embodiment 7
According to the method for embodiment 1, the difference is that, in step (1), with " 900 DEG C of oxidation 25min ", replace " 700 DEG C of oxygen
Change 25min ", about 8 μm of copper oxide thickness.
The copper ceramic substrate that covers prepared carries out adhesion strength test, result 750N.
It prepares ceramic electrothermal element heater and carries out heat transfer efficiency test, Energy Efficiency Ratio result is 93.5%.
Comparative example 1
(1) by copper electrode piece (a length of 20cm (not including terminal), width 1.5cm, thickness 0.3mm have the terminal of 15mm) and
Ceramic insulating substrate (a length of 21cm, width 2cm, thickness 1.2mm) is cleaned using acetic acid and degreaser (model LB-116)；
(2) silica gel (Toshiba XE14-0425) is applied to copper electrode on piece, then be pasted onto on ceramic insulating substrate, then
Cured at 200 DEG C, obtain covering copper ceramic substrate.
Copper ceramic substrate will be covered and carry out adhesion strength test, result 24N.
(3) silica gel (Toshiba XE14-0425) is applied to two and covers copper ceramic substrate by what step (1)-(2) obtained
Copper electrode on piece, then the both sides of ceramic electrothermal element plate are respectively adhered on, then cured at 200 DEG C, obtain ceramic electrical
Thermal element core.
(4) after ceramic electrothermal element core being coated upper Kapton, the inside that aluminium side leads to is loaded into, then through press
Extruding makes aluminium side lead between Kapton, ceramic electrothermal element core to be adjacent to, obtain ceramic electrothermal element fire-bar；
(5) the multiple ceramic electrothermal element fire-bars that will be obtained through step (4) are by silicone adhesive radiating fin, and arrange
It is assembled into ceramic electrothermal element heater.
Ceramic electrothermal element heater is subjected to heat transfer efficiency test, Energy Efficiency Ratio result is 85%.
Embodiment 8
The energization that the ceramic electrothermal element heater that embodiment 1,4,5 and comparative example 1 are each obtained carries out 1000h adds
Heat operation, then carries out heat transfer efficiency test respectively again：
The Energy Efficiency Ratio for the ceramic electrothermal element heater that embodiment 1 obtains is 95.7%；
The Energy Efficiency Ratio for the ceramic electrothermal element heater that embodiment 4 obtains is 90.2%；
The Energy Efficiency Ratio for the ceramic electrothermal element heater that embodiment 5 obtains is 89.8%；
The Energy Efficiency Ratio for the ceramic electrothermal element heater that comparative example 1 obtains is 80%.
As can be seen from the above Examples and Comparative Examples, copper ceramic substrate is covered the present invention provides no silicone adhesive,
The substrate can have a good adhesion strength, and further ceramic electrothermal element heater obtained compared to using silicone adhesive
When, there is better heat transfer efficiency.By long-term operation, the ceramic electrothermal element provided by the invention for covering copper ceramic substrate is used
Heater still can keep high Energy Efficiency Ratio, and use the ceramic electrical for covering copper ceramic substrate of the prior art (with silicone adhesive)
The Energy Efficiency Ratio of thermal element heater then declines.
Under the micro- oxygen oxidizing condition used in embodiment, copper oxide obtained can provide copper electrode piece and insulating ceramics
Better adhesion strength is obtained when substrate is sintered, and then ensures the heat transfer efficiency of ceramic electrothermal element heater.Wherein, it is real
The better adhesion strength of copper ceramic substrate acquisition, ceramic electrothermal element heating utensil can be covered compared to embodiment 4-7 by applying a 1-3
There is better heat transfer efficiency.
The preparation provided in the present invention is covered in the method for copper ceramic substrate, using first two-sided laminating copper electrode piece, Ran Houzai
Corrosion only retains a face copper electrode piece, it is ensured that obtain it is indeformable, do not fracture cover copper ceramic substrate, realize copper electrode piece with
Silicone adhesive is not required between ceramic insulating substrate, you can obtain covering copper ceramic substrate.It can ensure to cover copper ceramic substrate using this
Ceramic electrothermal element heater heat transfer efficiency.
Claims (10)
1. a kind of ceramic electrothermal element core, the core include：Ceramic electrothermal element plate covers copper ceramic substrate and adhesive layer；Its
In, the copper ceramic substrate that covers includes ceramic insulating substrate and the copper electrode on the part surface of the ceramic insulating substrate
Piece does not have adhesive between the copper electrode piece and the ceramic insulating substrate；The adhesive layer is arranged on the ceramic electric heating
Between element board and the copper electrode piece, for will be covered described at least two copper ceramic substrate and the ceramic electrothermal element plate into
Row bonds；
The preparation method of the core includes：At least one side of copper electrode piece is subjected to oxidation and forms copper oxide, is had
The copper electrode piece of copper oxide；Then it is bonded the copper electrode with copper oxide respectively in the both sides of ceramic insulating substrate
Piece；Wherein described copper oxide is between the ceramic insulating substrate and the copper electrode piece；By the copper electrode piece with it is described
Ceramic insulating substrate is sintered and cools down, and obtains the laminating substrate of the copper electrode piece in two sides；The substrate is subjected to copper
Corrosion obtains only one side and covers copper ceramic substrate with the copper electrode piece；The copper electrode piece and the ceramic insulating substrate
It is directly joined together, forms bonding.
2. ceramic electrothermal element core according to claim 1, wherein, the thickness of the ceramic electrothermal element plate for 2~
4cm, the thickness of the copper electrode piece is 0.1~0.5mm, and the thickness of the ceramic insulating substrate is 0.3~1.5mm, described viscous
The thickness for tying layer is 0.1~0.3mm.
3. ceramic electrothermal element core according to claim 1 or 2, wherein, the one side of the copper electrode piece, which has, to be stretched out
Terminal on the outside of the ceramic insulating substrate, for connecting power supply, the terminal stretches out the length on the outside of the ceramic insulating substrate
Spend about more than 15mm；The appearance and size of the copper electrode piece is smaller 1~3mm than the appearance and size of the ceramic insulating substrate.
4. a kind of method for preparing the ceramic electrothermal element core in claim 1-3 described in any one, including：
(1) at least one side of copper electrode piece is subjected to oxidation and forms copper oxide, obtain the copper electrode piece with copper oxide；So
It is bonded the copper electrode piece with copper oxide respectively in the both sides of ceramic insulating substrate afterwards；Wherein described copper oxide exists
Between the ceramic insulating substrate and the copper electrode piece；
(2) product made from step (1) is sintered and cooled down, obtain the laminating substrate of the copper electrode piece in two sides；
(3) substrate is subjected to copper corrosion, obtains only one side and cover copper ceramic substrate with the copper electrode piece；
(4) at least two faces of ceramic electrothermal element plate copper ceramic substrate will be covered described at least two are bonded in using binding agent
On；Wherein, ceramic electric heating is made between the ceramic electrothermal element plate and the ceramic insulating substrate in the copper electrode piece
Element core.
5. according to the method described in claim 4, wherein, in step (1), the oxidation carries out under micro- oxygen atmosphere, described
Oxygen content is 100~500ppm (volume) in micro- oxygen atmosphere；Oxidizing temperature is 600~900 DEG C, oxidization time for 10~
30min。
6. according to the method described in claim 4, wherein, in step (2), sintering temperature is 1050~1080 DEG C.
7. according to the method described in claim 4, wherein, in step (4), the binding agent is applied to and described covers copper ceramics
The copper electrode on piece in substrate, then with the ceramic electrothermal element plate bond and at 200~300 DEG C cure 20~
30min。
8. a kind of ceramic electrothermal element fire-bar, including：Aluminium side leads to, and internal heats, Yi Jisuo are led to positioned at the aluminium side
It states aluminium side and leads to insulating film between the heats；The heats is described in any one in claim 1-3
Ceramic electrothermal element core.
9. ceramic electrothermal element fire-bar according to claim 8, wherein, the insulating film is Kapton；Institute
The relative density of Kapton is stated as 1.39~1.45, the phase glass transition temperature of the Kapton for 280 DEG C with
On.
10. a kind of ceramic electrothermal element heater, including：Multigroup fire-bar and the multigroup heat dissipation being connected with the fire-bar
Fin；Wherein, the fire-bar is the ceramic electrothermal element fire-bar described in claim 8 or 9.
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| CN108601103A (en) * | 2018-05-16 | 2018-09-28 | 浙江欧兰顿电器科技有限公司 | A kind of processing method of age inhibiting PTC heat generating components |
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