CN116420927A - Ceramic heating sheet and preparation method thereof - Google Patents
Ceramic heating sheet and preparation method thereof Download PDFInfo
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- CN116420927A CN116420927A CN202310377126.XA CN202310377126A CN116420927A CN 116420927 A CN116420927 A CN 116420927A CN 202310377126 A CN202310377126 A CN 202310377126A CN 116420927 A CN116420927 A CN 116420927A
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 107
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910052751 metal Inorganic materials 0.000 claims abstract description 53
- 239000002184 metal Substances 0.000 claims abstract description 53
- 239000011521 glass Substances 0.000 claims abstract description 14
- 238000001465 metallisation Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 16
- 238000004544 sputter deposition Methods 0.000 claims description 15
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- 238000004519 manufacturing process Methods 0.000 claims description 9
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- 229910052709 silver Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 abstract description 22
- 238000001755 magnetron sputter deposition Methods 0.000 abstract description 11
- 238000007650 screen-printing Methods 0.000 abstract description 5
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Images
Classifications
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
- A24F40/46—Shape or structure of electric heating means
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/70—Manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/04—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers
- B28B11/044—Apparatus or processes for treating or working the shaped or preshaped articles for coating or applying engobing layers with glaze or engobe or enamel or varnish
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B11/00—Apparatus or processes for treating or working the shaped or preshaped articles
- B28B11/14—Apparatus or processes for treating or working the shaped or preshaped articles for dividing shaped articles by cutting
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
Abstract
The invention discloses a ceramic heating plate and a preparation method thereof, relates to the field of ceramic heating plates, and aims to solve the problems of low heat conductivity and uneven heat conduction of the conventional heating plate, and the technical scheme is as follows: a ceramic heating plate comprises a ceramic plate and a metallized layer which is sputtered on the surface of the ceramic plate by magnetron sputtering, wherein a glass phase metal heating body is printed on the surface of the metallized layer in a screen printing mode, and a cleaning glaze is coated on the surface of the metal heating body. The ceramic heating plate and the preparation method thereof can prepare the ceramic heating plate with uniform heat conduction and high heat conductivity.
Description
Technical Field
The invention relates to the field of ceramic heating, in particular to a ceramic heating sheet and a preparation method thereof.
Background
The heating non-burning type electronic cigarette has the characteristics of no tar, no ash, no open fire, no harm of second hand smoke and the like by inserting the special cigarette bullet into the heating appliance, penetrating the cigarette bullet by utilizing the ceramic heating sheet in the appliance and baking at the low temperature of about 300 ℃ to release the nicotine and the smoke in the cigarette bullet.
The prior ceramic heating sheet is made of ZrO 2 Or Al 2 O 3 The ceramic material is used as a base material, heating slurry and a plurality of glaze layers are printed on the surface of the base material by adopting a screen printing process, and then the ceramic material is sintered by an air tunnel furnace co-firing process. The heating slurry is formed by uniformly mixing a noble metal heating phase, a binding phase and an organic carrier. Wherein the binding phase is glass powder material, and the glass powder wets the surface of the substrate at high temperature, thereby generating combination. In order to improve the bonding strength and relieve the thermal expansion stress, a glaze layer is also burnt on the surface of the ceramic as a transition layer. However, the thermal conductivity of glass is only about 1W/(mK), and ZrO 2 Or Al 2 O 3 The heat conductivity of the ceramic is also lower, so that heat generated by the heating element is difficult to be quickly conducted to the ceramic plate, the overall temperature of the ceramic plate is difficult to reach balance in a short time, the temperature of the heating plate is uneven, and the design difficulty of a heating pattern circuit is increased.
There is therefore a need to propose a new solution to this problem.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a ceramic heating sheet, metal atoms are sputtered on the ceramic sheet to form a metallization layer by utilizing a magnetron sputtering technology, then a metal heating body without a glass phase is screen-printed, and after the metal heating body is sintered by a muffle furnace, a clean glaze layer is screen-printed on the surface, so that the glaze is combined on the ceramic and the heating film to form protection. Finally, the electroless plating or electroplating technology is used at the specific position, and metal with excellent welding performance and conductivity is precisely plated at the bonding pad position, so that the integral ceramic heating sheet is finally formed.
The technical aim of the invention is realized by the following technical scheme: a ceramic heat generating sheet, characterized in that: comprises a ceramic plate and a metallized layer which is sputtered on the surface of the ceramic plate by magnetron, wherein the surface of the metallized layer is screen-printed with a metal heating element with or without a glass phase, and the surface of the metal heating element is covered with clean glaze.
The invention is further provided with: the ceramic sheet is Si 3 N 4 Or AlN material, the thickness of the ceramic plate is 0.15-0.8mm, and the thermal conductivity is more than 80W/(m.K).
The invention is further provided with: the metallized layer is Ti, zr or Cr, and the thickness is 0.1-2 mu m.
The invention is further provided with: the glass-phase-free metal heating element is Ag and contains metal oxide for adjusting conductivity, the thickness of the glass-phase-free metal heating element is 8-20 mu m, and the sheet resistance is 10-80mΩ/≡.
The invention is further provided with: the metal oxide includes TiO 2 、ZrO 2 。
The invention is further provided with: the electrode and the bonding pad are made of Ag or Au, and the thickness of the electrode and the bonding pad is 1-10 mu m.
8. The invention also provides a preparation method of the ceramic heating sheet, which comprises the following steps:
s1) preparation of a ceramic surface metallization layer: using magnetron sputtering equipment, taking Ti or Zr or Cr metal target as cathode heating sputtering, and performing Si 3 N 4 Or sputtering a metallized layer film on the AlN ceramic plate;
s2) preparing a metal heating element: ag powder, metal oxide and organic carrier in 80-90 weight portions: 0.5-5:5-20, grinding the slurry by using a three-roller grinder, dispersing and mixing, printing on a metallized ceramic sheet by using a screen printer, sintering a heating body on the metallized ceramic sheet by air sintering at 800-900 ℃ to form a heating pattern, and spontaneously oxidizing a metallized layer in a non-pattern area to convert a conductor into an insulator;
s3) clean glaze preparation: the surface of the metal heating body prepared in the step S2 is screen-printed with clean glaze, and the surface of the metal heating body is stuck and covered after being sintered by air;
s4) pad, electrode fabrication: electroplating or electroless plating is carried out on the bonding pad and the electrode, so that the solderable thickness is increased;
s5) laser dicing: and (3) cutting the whole ceramic heating sheet into a single product by utilizing a laser cutting process.
The invention is further provided with: in step S1, sputtering parameters: the working temperature is 200-350 ℃, the current is 15-25A, and the working vacuum degree is 1-3X 10 -1 Pa。
In summary, the invention has the following beneficial effects:
1. the magnetron sputtering process is adopted, a metallization layer is pretreated on the surface of the ceramic sheet, and the sintering temperature of the glass-phase-free metal heating body is reduced by utilizing the transitional connection effect of the metallization layer;
2. the heating element does not contain glass phase with poor heat conduction capability, and the ceramic, the metallization layer and the metal heating element all have high heat conduction capability, so that the whole heat of the heating sheet is diffused very rapidly, the temperature uniformity is high, and a new design thought is provided for improving the temperature uniformity of the ceramic heating sheet;
3. the metallized layer of the non-heating pattern area can generate oxidation insulation during air sintering, thereby avoiding the short circuit of the heating element.
Drawings
FIG. 1 is an exploded view of a ceramic heat-generating plate of the present invention;
FIG. 2 is a flow chart of a process for preparing the ceramic heat-generating plate of the invention;
FIG. 3 is a cross-sectional SEM image of the heat-generating region of a ceramic heat-generating sheet in example 1;
wherein, 1, a ceramic plate; 2. a metallization layer; 3. a metal heating element; 4. cleaning glaze; 5. and a bonding pad.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Aiming at the problems existing in the prior art, the invention provides the ceramic heating sheet with the pretreated ceramic surface and the preparation method thereof, the metal heating body does not contain glass phase, the metal heating body is connected with the ceramic sheet with high heat conductivity through innovative material and process collocation, the high heat conductivity of metal is utilized, the problems of slow heat conduction of the heating body and poor heat conduction of the ceramic are fundamentally solved, and the overall temperature uniformity of the ceramic heating sheet is improved.
The invention is based on the following principle: firstly, the metal can be deformed and agglomerated due to the surface tension of the liquid phase at high temperature, so that the glass-phase-free metal heating element needs to avoid generating a large amount of liquid phase, is only suitable for medium-low temperature sintering, and is difficult to directly infiltrate with the ceramic surface during medium-low temperature sintering, and has extremely poor binding force. At this time, if the surface of the ceramic is subjected to the pretreatment of metallization, the effective connection between the ceramic and the metal heating element can be realized by utilizing the transitional connection effect of the metallization layer. The magnetron sputtering is used as a common means of PVD, the bonding strength can be ensured, a metal layer with specified thickness is deposited on the surface of the ceramic, a proper metal target is selected, and the sputtering of a metallization layer with certain thickness on the surface of the ceramic can be realized by adjusting parameters such as working temperature, working pressure, sputtering current and the like, so that the bonding strength between a heating element without glass phase and a ceramic sheet is improved; in addition, the redundant metallization layer can be spontaneously oxidized in the sintering process, so that the heating pattern is prevented from being short-circuited.
The method comprises the steps of preprocessing the ceramic surface by utilizing a magnetron sputtering process, forming a metallization layer on the ceramic surface, wherein the metallization layer is tightly combined with the ceramic, and realizing the combination of a glass-phase-free metal heating element and a ceramic plate at medium and low temperature by utilizing the transitional connection effect of the metallization layer, so that the metal layer is directly connected between the ceramic plate and the heating element, the heat conductivity is greatly improved, and the temperature of the ceramic heating element is promoted to be more uniform; the method breaks through the conventional development process and provides a new design idea for improving the temperature uniformity of the ceramic heating sheet.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
in a first aspect of the present invention, there is provided a ceramic heat-generating sheet with a pretreated ceramic surface, as shown in fig. 1, comprising a ceramic sheet 1 and a metallized layer 2 pretreated on the surface of the ceramic sheet 1 by magnetron sputtering, wherein a metallic heat-generating body 3 with or without a glass phase is screen-printed on the metallized ceramic sheet 1, and a cleaning glaze 4 is coated on the surface of the metallic heat-generating body 3.
And sputtering metal atoms on the ceramic sheet 1 by utilizing a magnetron sputtering technology to form a metallization layer 2, then screen printing a metal heating body 3 without a glass phase, sintering by a muffle furnace, then screen printing a cleaning glaze 4 on the surface to ensure that the glaze is combined on the ceramic and the heating film to form protection, finally precisely plating metal with excellent welding performance and conductivity on the position of the bonding pad 5 by utilizing a chemical plating or electroplating technology at a specific position, and finally forming the integral ceramic heating sheet.
In the ceramic heating sheet provided by the invention, the ceramic sheet 1 is Si 3 N 4 Or AlN material, the thickness of the ceramic plate 1 is 0.15-0.8mm, and the thermal conductivity is more than 80W/(m.K);
the sputtered metallized layer 2 is active metal such as Ti, zr, cr and the like, and the thickness of the metallized layer is 0.1-2 mu m;
the metal heating element 3 without glass phase is Ag metal as main component and contains other TiO for regulating conductivity 2 、ZrO 2 The thickness of the metal oxide-free glass phase metal heating body 3 is 8-20 mu m, and the sheet resistance is 10-80mΩ/≡;
the bonding pad 5 is made of Ag or Au and has a thickness of 1-10 μm.
Meanwhile, the preparation method of the ceramic heating sheet, as shown in fig. 2, comprises the following steps:
s1) preparation of a ceramic surface metallization layer: using magnetron sputtering equipment, using Ti, zr, cr and other metal targets as cathode, heating and sputtering at normal temperature or 200-350 deg.C, and forming Si 3 N 4 Or a metal layer film with specific composition and thickness is sputtered on the AlN ceramic. Sputtering parameters: the working temperature is 200-350 ℃, the current is 15-25A, and the working vacuum degree is 1-3X 10 -1 Pa;
S2) preparing a metal heating element: ag powder and TiO 2 、ZrO 2 80-90 percent of metal oxide and organic carrier:0.5-5: mixing 5-20 mass percent, grinding the slurry by using a three-roller grinder, and dispersing and mixing; printing on the metallized ceramic sheet by using a screen printer, and sintering the heating element on the metallized ceramic sheet by air sintering at 800-900 ℃ to form a heating pattern; meanwhile, the metallization layer of the non-pattern area is spontaneously oxidized in the process and is converted into an insulator from a conductor, so that the short-circuit heating layer is avoided; the thickness, the resistance value and the uniformity of heat distribution of the heating element are adjusted by changing the mesh number, the oxide content, the solid content of the sizing agent and the heating circuit pattern of the wire;
s3) preparing a cleaning glaze layer: after the heating body in the step S2 is manufactured, screen printing a cleaning glaze with a certain thickness on the surface of the heating body, wherein the smooth cleaning glaze has the characteristics of water repellency and oil repellency, and is adhered to the surface of the whole heating sheet after being sintered by air, so that the subsequent cleaning and maintenance are facilitated;
s4) manufacturing a bonding pad: electroplating or electroless plating is carried out on the positions of the welding pads, so that the weldability of the welding pads is improved, the weldability thickness is increased, the welding strength and the welding reliability are improved, and meanwhile, the heating of the welding pad areas is avoided;
s5) laser dicing: and (3) cutting the whole ceramic heating sheet into a single product by utilizing a laser cutting process.
Example 1:
s1) preparation of a ceramic surface metallization layer: si with thickness of 0.4mm 3 N 4 The ceramic wafer 1 uses a metal Ti target as a cathode, and uses a magnetron sputtering device to produce Si 3 N 4 Deposition of 400nm thick metallic Ti film on ceramic, i.e. metallization layer 2, sputtering parameters: operating temperature 200 ℃, current 15A and vacuum degree 2X 10 -1 Pa;
S2) preparing a metal heating element: ag powder and TiO 2 Organic carrier at 85:2:13 mass ratio, grinding the slurry by a three-roller grinder, uniformly mixing, printing on an S1 metallized ceramic sheet 1 by a screen printer, selecting a 250 steel wire composite screen as a screen frame, sintering by a muffle furnace through 850 ℃ air, forming a 15 mu m heating body 3 on a metallized layer 2, oxidizing metal Ti in a non-pattern area, and converting the electric conductor into an insulator TiO 2 Thereby (a)The short-circuit heating layer is avoided;
s3) preparing a cleaning glaze layer: after the heating element 3 of the S2 is manufactured, the whole surface is printed with the cleaning glaze 4 by using a 100-mesh screen, and then the cleaning glaze 4 with the thickness of 30 mu m is formed by sintering the whole surface for 30min at the temperature of 700 ℃ by using a muffle furnace, and the smooth cleaning glaze 4 has the characteristics of water repellency and oleophobic property, so that the cleaning maintenance is convenient;
s4) manufacturing a bonding pad: and electroplating the pad position with electroplating current of 0.6A, and thickening the pad region of the Ag heating element with pure Ag to form a thickened Ag layer with thickness of 10 μm.
S5) laser dicing: and (3) cutting the whole ceramic heating sheet into a single product by utilizing a laser cutting process.
As shown in the SEM result of the cross section of fig. 3, an effective bond is formed between the cleaning glaze 4, the Ag heat-generating body and the ceramic sheet 1.
Example 2:
s1) preparation of a ceramic surface metallization layer: taking an AlN ceramic plate 1 with the thickness of 0.3mm, taking a metal Zr target as a cathode, and depositing a metal Ti film with the thickness of 200nm, namely a metallization layer 2, on the AlN ceramic plate 1 by utilizing magnetron sputtering equipment, wherein the sputtering parameters are as follows: operating temperature 300 ℃, current 18A, vacuum degree 3×10 -1 Pa;
S2) preparing a metal heating element: ag powder, zrO 2 Organic carrier 88:1:11 mass ratio, grinding and uniformly mixing the slurry by using a three-roller grinder; printing on the S1 metallized ceramic sheet 1 with screen printer, selecting 280 steel wire composite net as screen frame, sintering with 850 deg.C air in muffle furnace to form 10 μm heater 3 on the metallized layer 2, oxidizing Zr in non-pattern area, and converting from conductor to insulator ZrO 2 Thereby avoiding short-circuiting the heating layer;
s3) preparing a cleaning glaze layer: after the heating body of the S2 is manufactured, printing a cleaning glaze on the whole surface by using an 80-mesh screen, and then sintering the cleaning glaze for 50min at 720 ℃ by using a muffle furnace to form a cleaning glaze 4 with the thickness of 35 mu m;
s4) manufacturing a bonding pad: and (3) carrying out an electroless plating process on the position of the bonding pad 5, and thickening pure Au on the bonding pad area of the Ag heating element to form a thickened Au layer with the thickness of 5 mu m.
S5) laser dicing: and (3) cutting the whole ceramic heating sheet into a single product by utilizing a laser cutting process.
Comparative example 1:
comparative example 1 the control group was example 1, with the modification that no ceramic pretreatment process was used.
S1) preparation of a metal heating element: ag powder and TiO 2 Organic carrier at 85:2:13 mass ratio, grinding the slurry by a three-roll grinder, uniformly mixing, and then using a screen printer to obtain Si with a thickness of 0.4mm 3 N 4 Printing on the ceramic sheet 1, selecting a 250 steel wire composite net as a net frame, and sintering the ceramic sheet 1 by using a muffle furnace through air at 850 ℃ to form a 15-mu m heating body 3;
s2) preparing a cleaning glaze layer: after the heating body 3 of the S1 is manufactured, printing a cleaning glaze on the whole surface by using a 100-mesh screen, and then sintering the cleaning glaze for 30 minutes at 700 ℃ by using a muffle furnace to form a cleaning glaze 4 with the thickness of 30 mu m;
s3) manufacturing a bonding pad: electroplating the pad position with electroplating current of 0.6A, and thickening pure Ag in the pad 5 area of the Ag heating element 3 to form a thickened Ag layer with thickness of 10 μm;
s4) laser dicing: and (3) cutting the whole ceramic heating sheet into a single product by utilizing a laser cutting process.
The ceramic heat-generating sheets of examples 1, 2 and comparative example 1 were taken, and the bonding strength of the heat-generating body and the ceramic was tested under the same test conditions, and the temperature uniformity at 300 ℃ was compared, and the test results are shown in the following table:
the above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (7)
1. A ceramic heat generating sheet, characterized in that: comprises a ceramic plate and a metallized layer which is sputtered on the surface of the ceramic plate by magnetron, wherein the surface of the metallized layer is screen-printed with a metal heating element with or without a glass phase, and the surface of the metal heating element is covered with clean glaze.
2. A ceramic heat generating sheet as defined in claim 1, wherein: the ceramic sheet is Si 3 N 4 Or AlN material, the thickness of the ceramic plate is 0.15-0.8mm, and the thermal conductivity is more than 80W/(m.K).
3. A ceramic heat generating sheet as defined in claim 1, wherein: the metallized layer is Ti, zr or Cr, and the thickness is 0.1-2 mu m.
4. A ceramic heat generating sheet as defined in claim 1, wherein: the glass-phase-free metal heating element is Ag and contains metal oxide for adjusting conductivity, the thickness of the glass-phase-free metal heating element is 8-20 mu m, and the sheet resistance is 10-80mΩ/≡.
5. A ceramic heat generating sheet as defined in claim 4, wherein: the metal oxide includes TiO 2 、ZrO 2 。
6. A ceramic heat generating sheet as defined in claim 1, wherein: the bonding pad is made of Ag or Au, and the thickness of the bonding pad is 1-10 mu m.
7. A method for producing the ceramic heat generating sheet according to any one of claims 1 to 6, comprising the steps of:
s1) preparation of a ceramic surface metallization layer: by means ofMagnetron sputtering equipment, which uses Ti or Zr or Cr metal target as cathode heating sputtering, and uses Si as cathode heating sputtering material 3 N 4 Or sputtering a metallized layer film on the AlN ceramic plate;
s2) preparing a metal heating element: ag powder, metal oxide and organic carrier in 80-90 weight portions: 0.5-5:5-20, grinding the slurry by using a three-roller grinder, dispersing and mixing, printing on a metallized ceramic sheet by using a screen printer, sintering a heating body on the metallized ceramic sheet by air sintering at 800-900 ℃ to form a heating pattern, and spontaneously oxidizing a metallized layer in a non-pattern area to convert a conductor into an insulator;
s3) clean glaze preparation: the surface of the metal heating body prepared in the step S2 is screen-printed with clean glaze, and the surface of the metal heating body is stuck and covered after being sintered by air;
s4) manufacturing a bonding pad: electroplating or electroless plating is carried out on the position of the welding disc, so that the thickness of the welding disc is increased;
s5) laser dicing: and (3) cutting the whole ceramic heating sheet into a single product by utilizing a laser cutting process.
The method of manufacturing according to claim 7, wherein: in step S1, sputtering parameters: the working temperature is 200-350 ℃, the current is 15-25A, and the working vacuum degree is 1-3X 10 -1 Pa。
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5009357A (en) * | 1988-07-28 | 1991-04-23 | Lilliwyte Societe Anonyme | Joining of ceramic components to metal components |
CN214509370U (en) * | 2020-12-11 | 2021-10-29 | 常州市派腾电子技术服务有限公司 | Atomizing core, atomizer and aerosol generating device |
CN214675729U (en) * | 2021-02-09 | 2021-11-09 | 厦门海赛米克新材料科技有限公司 | Ceramic heater structure with stronger bonding force and heating plate structure thereof |
CN113826962A (en) * | 2021-09-22 | 2021-12-24 | 东莞市维万特智能科技有限公司 | Atomizing core, atomizer, aerosol generating device and atomizing core preparation method |
CN115153112A (en) * | 2022-08-04 | 2022-10-11 | 江苏富乐华功率半导体研究院有限公司 | High-efficiency electronic cigarette double-sided heating sheet and preparation method thereof |
CN115381143A (en) * | 2022-08-17 | 2022-11-25 | 江苏富乐华功率半导体研究院有限公司 | Electronic cigarette ceramic heating sheet based on magnetron sputtering process and preparation method thereof |
-
2023
- 2023-04-11 CN CN202310377126.XA patent/CN116420927B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5009357A (en) * | 1988-07-28 | 1991-04-23 | Lilliwyte Societe Anonyme | Joining of ceramic components to metal components |
CN214509370U (en) * | 2020-12-11 | 2021-10-29 | 常州市派腾电子技术服务有限公司 | Atomizing core, atomizer and aerosol generating device |
CN214675729U (en) * | 2021-02-09 | 2021-11-09 | 厦门海赛米克新材料科技有限公司 | Ceramic heater structure with stronger bonding force and heating plate structure thereof |
CN113826962A (en) * | 2021-09-22 | 2021-12-24 | 东莞市维万特智能科技有限公司 | Atomizing core, atomizer, aerosol generating device and atomizing core preparation method |
CN115153112A (en) * | 2022-08-04 | 2022-10-11 | 江苏富乐华功率半导体研究院有限公司 | High-efficiency electronic cigarette double-sided heating sheet and preparation method thereof |
CN115381143A (en) * | 2022-08-17 | 2022-11-25 | 江苏富乐华功率半导体研究院有限公司 | Electronic cigarette ceramic heating sheet based on magnetron sputtering process and preparation method thereof |
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