CN110676195B - Heater preparation mold and heater preparation method - Google Patents
Heater preparation mold and heater preparation method Download PDFInfo
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- CN110676195B CN110676195B CN201910854351.1A CN201910854351A CN110676195B CN 110676195 B CN110676195 B CN 110676195B CN 201910854351 A CN201910854351 A CN 201910854351A CN 110676195 B CN110676195 B CN 110676195B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67155—Apparatus for manufacturing or treating in a plurality of work-stations
- H01L21/67207—Apparatus for manufacturing or treating in a plurality of work-stations comprising a chamber adapted to a particular process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24C—ABRASIVE OR RELATED BLASTING WITH PARTICULATE MATERIAL
- B24C1/00—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods
- B24C1/04—Methods for use of abrasive blasting for producing particular effects; Use of auxiliary equipment in connection with such methods for treating only selected parts of a surface, e.g. for carving stone or glass
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02002—Preparing wafers
- H01L21/02005—Preparing bulk and homogeneous wafers
- H01L21/02008—Multistep processes
- H01L21/0201—Specific process step
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Abstract
The invention discloses a heater preparation mould and a heater preparation method, wherein the mould comprises a first mould monomer (1) and a second mould monomer (2); the first mould single body (1) is detachably connected with the second mould single body (2); the first mould single body (1) and the second mould single body (2) enclose a closed accommodating space, and the accommodating space is used for accommodating a heater; through holes (3) are formed in the surfaces of the first die single body (1) and the second die single body (2); the through hole (3) is arranged corresponding to the conductive isolation area of the heater and used for conducting sand blasting and carving on the conductive coating exposed out of the through hole. Through designing this heater preparation mould, can realize carrying out the sandblast sculpture on the coating, can obtain comparatively accurate electrically conductive isolation region, can effectively avoid because the layering phenomenon that machining heater leads to.
Description
Technical Field
The invention relates to the technical field of material processing, in particular to a heater preparation mold and a heater preparation method.
Background
At present, some heaters are often used for heating raw materials in the aspect of industrial production, various heaters are not separated from the aspect of manufacturing solar thin film batteries, OLED flexible display panels and the production and manufacturing of some thin film materials or products, and different industries have special requirements on the heaters, for example, in the vacuum evaporation process for manufacturing the solar thin film batteries and the OLED flexible panels, the requirements on the heaters are extremely strict because the heaters are produced and manufactured in a high vacuum environment, and the heaters are required to have good temperature uniformity in order to ensure the uniform diffusion of evaporation materials and avoid the influence of overhigh local temperature on the service life of a charging container; in order to ensure the use safety of the heater and avoid production accidents caused by electric short circuit. The heater is required to have a small deformation amount at a high temperature, and an insulating part is required to be arranged between the heater and equipment; because the evaporated material often has corrosive substances, and some evaporation processes also require a certain amount of oxygen to be introduced after evaporation is finished for special treatment of the evaporated film, the material for manufacturing the heater needs to have excellent corrosion resistance and oxidation resistance in order to ensure the service life of the heater; since the evaporation process often requires a high vacuum and a high cleanliness environment, the amount of gas released and impurities released from the heater under the high vacuum are also strictly required.
At present, materials such as metal tantalum, tungsten and the like are mostly adopted in industrial production to manufacture the wire-shaped heater, but the wire-shaped heater cannot effectively avoid the problems, and finally the product yield is low.
In order to solve the above problems, in the prior art, a multilayer heater has been developed by a CVD method, wherein pyrolytic boron nitride is used as a substrate, Pyrolytic Graphite (PG) is used as a conductive ceramic coating, and a layer of pyrolytic boron nitride is covered on the conductive ceramic coating to serve as an insulating layer, and the purity of the used ceramic material can reach as high as 99.999%, and the multilayer heater has a small thermal expansion coefficient at high temperature and a small gas release amount, and is of an integrated structure, thereby avoiding the above problems. However, the multilayer heater itself has the following drawbacks:
(1) the boron nitride substrate is prepared by a CVD method, so that the size uniformity is difficult to be consistent with a drawing, and the pyrolytic graphite coated on the surface of the boron nitride substrate is 0.005-0.1mm, so that the pyrolytic graphite is required to be processed, the boron nitride substrate cannot be seriously damaged, otherwise, local overheating is caused, the temperature uniformity of a heater is affected, and the service life of the heater is prolonged, so that the high requirement on the precision of processing equipment is provided, an online measurement system is required, the processing depth is monitored and controlled in real time, and the problems of low processing efficiency and high price exist in the processing of the equipment.
(2) The pyrolytic boron nitride substrate and the pyrolytic graphite realizing the conductive function are both of a layered structure. In order to process the conductive coating, in the prior art, the conductive layer is processed in a mechanical processing manner to obtain the conductive texture, for example, a milling cutter is used to remove a part of the conductive layer in a cutting manner of a tearing layer to obtain the conductive texture, but this manner is very easy to cause a problem of breakage of a boron nitride layer structure due to an excessively fast processing speed, so that the surface layer of the boron nitride substrate and the pyrolytic graphite conductive layer fall off together. In the prior art, the milling cutter is set to be in a high spindle rotating speed and low feeding mode during machining, and the conducting layer is machined, so that the influence can be weakened to a certain extent, but the machining time is prolonged by tens of times; and adopt this kind of high rotational speed, the processing mode of low feed also can make the processing position roughness undersize and need carry out the coarsing to the processing position after accomplishing processing, otherwise can lead to the condition that the layering appears in last boron nitride coating (insulating layer) to this kind of processing mode also can make cutter wearing and tearing accelerate, need change a large amount of cutters in order to guarantee the result of working in the use. In addition, because the processing speed is too high, a certain vibration exists between the conductive layer of the heater and the substrate due to the mechanical processing mode, and the vibration exists for a long time due to long-time processing, so that the vibration is extremely unfavorable for the multilayer structure, and the multilayer structure is separated.
Disclosure of Invention
Objects of the invention
The invention aims to provide a heater preparation mold and a heater preparation method, wherein the mold is provided with a first mold monomer and a second mold monomer to form a closed accommodating space for accommodating a heater, through holes are formed in the surfaces of the first mold monomer and the second mold monomer, the through holes are arranged corresponding to a conductive isolation area of the heater, and a conductive coating exposed from the through holes can be subjected to sand blasting carving. Through designing this heater preparation mould, can realize carrying out the sandblast sculpture on the coating, can obtain comparatively accurate electrically conductive isolation region, can effectively avoid because the layering phenomenon that machining heater leads to.
(II) technical scheme
In order to solve the problems, the heater preparation mold comprises a first mold monomer and a second mold monomer; the first mould single body is detachably connected with the second mould single body; the first mould single body and the second mould single body enclose a closed accommodating space, and the accommodating space is used for accommodating the heater; through holes are formed in the surfaces of the first die single body and the second die single body; the through hole is arranged corresponding to the conductive isolation area of the heater and is used for performing sand blasting carving on the conductive coating exposed out of the through hole; the through holes are long-strip-shaped, and the number of the through holes is multiple; reinforcing ribs are arranged at intervals in the length direction of the through hole and are connected with two side walls of the through hole; the first die single body and the second die single body are respectively and oppositely provided with a positioning hole corresponding to the electrode hole on the surface of the heater so as to position the heater.
Furthermore, the outer surface of the reinforcing rib and the outer wall of the first die unit are positioned on the same surface, and the inner surface of the reinforcing rib is retracted to the inner wall of the first die unit; or the outer surface of the reinforcing rib and the outer wall of the second die unit are positioned on the same surface, and the inner surface of the reinforcing rib is retracted to the inner wall of the second die unit.
Further, the first mold monomer and the second mold monomer have the same thickness; the thickness of the reinforcing rib is 10% -50% of the thickness of the first die single body.
Furthermore, the width of the reinforcing rib is 0.5-10 mm.
Further, the reinforcing ribs are arranged at intervals of 10-100mm in the length direction of the through holes.
Further, the buffer layer comprises a flexible buffer layer; one surface of the flexible buffer layer is attached to the surface of the first die unit and the second die unit, which are provided with accommodating spaces, and the other surface of the flexible buffer layer is abutted to the heater.
Further, the thickness of the flexible buffer layer is 0.05-10 mm.
According to another aspect of the present invention, there is also provided a method of manufacturing a heater, including the steps of: depositing a conductive layer on the surface of the substrate; mounting the conductive layer in the receiving space of the mold of the first aspect; performing sand blasting treatment on the surface of the mold to form an isolation region on the surface of the conductive ceramic material layer; and depositing an insulating layer on the surface of the substrate with the conductive material layer.
Further, the step of sand blasting the surface of the mold to form the isolation region on the surface of the conductive ceramic material layer comprises: controlling the rotating speed of the die to be 0.5-50 r/min; sand grains with the Mohs hardness of 3-9 and the mesh number of 30-500 are adopted to carry out sand blasting treatment on the surface of the pyrolytic boron nitride; the pressure of sand blasting is 0.1-5MPa, and the sand blasting distance is 1-500 mm.
Further, the step of depositing a conductive layer on the surface of the substrate includes: introducing BCl into the deposition chamber3、CH4And N2Gas, depositing the conducting layer on the surface of the substrate; the conducting layer is pyrolytic graphite doped with boron carbide; wherein the BCl3、CH4And N2The volume ratio of (A) to (B) is as follows: (0.1-10): (0.1-10): 8, the mass of the boron carbide is 0.1-50% of the conductive layer.
Further, the substrate is prepared by the following method: introducing BCl into a deposition chamber containing a deposition mold3、NH3And N2The mixed gas of (3); keeping the temperature of the deposition chamber at 1200-1600 ℃, and introducing the mixed gas for 5-10 h; raising the temperature of the deposition chamber to 1700-2200 ℃ and keeping the temperature for 2-15 h; and cooling to room temperature.
Further, the step of depositing an insulating layer on the surface of the conductive layer comprises: introducing BCl into a deposition chamber containing a conductive layer3、NH3And N2Controlling the vacuum degree of the deposition chamber to be 100-500Pa and the temperature to be 1350-2000 ℃; and/or the volume ratio of BCl3 to NH3 is (0.1-10): 1.
(III) advantageous effects
The technical scheme of the invention has the following beneficial technical effects:
according to the heater preparation mold provided by the embodiment of the invention, the first mold monomer and the second mold monomer are arranged to form a closed accommodating space for accommodating the heater, in addition, through holes are arranged on the surfaces of the first mold monomer and the second mold monomer, the through holes are arranged corresponding to the conductive isolation area of the heater, and the conductive coating exposed from the through holes can be subjected to sand blasting carving. Through relating to this heater preparation mould, can realize carrying out the sandblast sculpture on the coating, can obtain comparatively accurate electrically conductive isolation region, can effectively avoid because the layering phenomenon that machining heater leads to.
Drawings
Fig. 1 is a schematic structural view of a mold according to a first embodiment of the present invention;
FIG. 2 is a front view of a first mold cell according to a first embodiment of the present invention;
FIG. 3 is an enlarged view of area A of FIG. 2;
FIG. 4 is a top view of a first mold monomer according to a first embodiment of the present invention;
FIG. 5 is a left side view of a first mold cell according to a first embodiment of the present invention;
FIG. 6 is a schematic flow chart of a method of manufacturing a heater according to a second embodiment of the present invention;
fig. 7 is a graph of the resistivity of the conductive layer versus the mass of boron carbide at different temperatures according to the third embodiment of the present invention.
Reference numerals:
1: a first mold monomer; 2: a second mold monomer; 3: a through hole; 4: reinforcing ribs; 5: electrode positioning holes; 6: a substrate to be sandblasted; 7: a flexible buffer layer; 8: a first nut; 9: a second nut; 10: a spring washer; 11: a first bolt; 12: a first arcuate shim; 13: a gasket; 14: a second bolt; 15: a second arcuate shim; 16: and (4) a flange.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
In the drawings, there is shown a schematic structural diagram according to an embodiment of the invention. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity. The shapes of various regions, layers, and relative sizes and positional relationships therebetween shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, as actually required.
In the description of the present invention, it should be noted that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Fig. 1 is a schematic structural view of a mold according to a first embodiment of the present invention. FIG. 2 is a front view of a first mold cell according to a first embodiment of the present invention; FIG. 3 is an enlarged view of area A of FIG. 2; FIG. 4 is a top view of a first mold monomer according to a first embodiment of the present invention; fig. 5 is a left side view of a first mold unit according to a first embodiment of the present invention.
As shown in fig. 1 to 5, the heater-preparing mold includes a first mold unit 1 and a second mold unit 2; the first mould single body 1 is detachably connected with the second mould single body 2; the first mould single body 1 and the second mould single body 2 enclose a closed accommodating space, and the accommodating space is used for accommodating a heater; through holes 3 are formed in the surfaces of the first mold single body 1 and the second mold single body 2; the through hole 3 is arranged corresponding to the conductive isolation area of the heater and used for conducting sand blasting and carving on the conductive coating exposed out of the through hole.
In the embodiment shown in fig. 1, the heater is cylindrical, that is, the first mold unit 1 and the second mold unit 2 are "tile" shaped, the invention is not limited thereto, and the heater may have other shapes, such as rectangular parallelepiped.
In the embodiment shown in fig. 1, the first mold unit 1 and the second mold unit 2 are identical, and of course, the arc length of the first mold unit 1 may be larger than that of the second mold unit, and other shapes may also be used as long as the two units can enclose a closed accommodating space.
In one embodiment, the through holes 3 are long and are provided in a plurality; and reinforcing ribs 4 are arranged at intervals in the length direction of the through hole 3 and are connected with two side walls of the through hole 3. When the reinforcing rib is arranged on the first die unit 1, the outer surface of the reinforcing rib 4 and the outer wall of the first die unit 1 are located on the same surface, and the inner surface of the reinforcing rib 4 is retracted to the inner wall of the first die unit 1.
When the reinforcing rib 4 is arranged on the second die unit 2, the outer surface of the reinforcing rib 4 and the outer wall of the second die unit 2 are located on the same surface, and the inner surface of the reinforcing rib 4 is retracted into the inner wall of the second die unit 1.
It should be understood that in this embodiment, the outer surface of the reinforcing rib 4 is located on the same surface of the single mold body, and one surface may be a curved surface, a flat surface, or the like.
The single body 1 shown in fig. 2 is in a tile shape, a plurality of through holes 3 are formed in the length direction of the single body, the reinforcing ribs 4 are arranged on one surfaces (the inner walls of the first single body 1 and the second single body 2) of the first single body 1 and the second single body 2, which are formed with accommodating spaces, the thickness of the reinforcing ribs 4 is smaller than that of the single body, and the outer surface of the reinforcing ribs is in a plane with the outer surface of the first single body 1, so that the reinforcing ribs and the inner wall of the first single body or the second single body have certain spaces. When the sand is blasted on the surface of the mold, the sprayed sand can enter the certain space to polish the corresponding positions of the reinforcing ribs on the inner wall of the mold. So that the polished conductive isolation regions are coherent.
It should be understood that in the example shown in fig. 1, the through hole mentioned in the present application is an elongated shape, and may be a linear elongated shape, a zigzag elongated shape, a curved elongated shape, such as a wave shape, and the like.
Fig. 3 is an enlarged view of the region a shown in fig. 2. The location of the reinforcing bars 4 is clearly shown in figure 3.
In a specific embodiment, the first mold unit 1 and the second mold unit 2 have the same thickness; the thickness of the reinforcing ribs 4 is 10% -50% of the thickness of the first die unit 1.
In a preferred embodiment the width of the ribs 4 is 0.5-10 mm. It should be noted that, the reinforcing rib is in this range, the connection strength of each position of the mould can be ensured, and the interference to the sand blasting can not be generated. If the width of strengthening rib is less than 0.5mm, then can't play the effect of strengthening the connection, if the width of strengthening rib is higher than 10mm then can produce the sandblast process and block, be unfavorable for the sculpture of pattern.
Optionally, the reinforcing ribs 4 are arranged at intervals of 10-100mm in the length direction of the through hole 3. Generally speaking, the relationship between the length and the thickness of the reinforcing ribs and the through holes designed by the invention is that the connection strength of each position of the die can be ensured and the implementation of the sand blasting carving pattern is not influenced by rotating the proper arrangement interval within the range according to the size inconsistency of the die.
In one embodiment, the first mold unit 1 and the second mold unit 2 are respectively provided with electrode positioning holes 5 corresponding to electrode holes on the surface of a heater to position the heater, thereby preventing portions not requiring sand blasting from being abraded.
In an alternative embodiment, the first mold unit 1 and the second mold unit 2 are respectively provided with positioning holes (not shown) corresponding to the mounting holes of the heater surface.
In one embodiment, a flexible buffer layer 7 is also included; one surface of the flexible buffer layer 7 is attached to the surface of the first die unit 1 and the second die unit 2, which are provided with accommodating spaces, and the other surface of the flexible buffer layer is abutted to the substrate 6 to be subjected to sand blasting. The flexible layer 7 may be made of sponge or sand-blasting tape or other flexible material with one side sticky.
In one embodiment, the first and second mold units are in the shape of "tiles", and the arc-shaped edges of the first and second mold units further extend out of a fixing portion, such as a flange 16, the fixing portion is provided with a through hole, and the bolt 14 passes through the through hole of the flange 16 to be rotatably connected with the second nut 9, so that the first and second mold units can be closed.
Optionally, in this embodiment, a first spring washer 10 may be further disposed between the second nut 9 and the flange 16 to make the closing between the first mold unit and the second mold unit tighter. The purpose of the first spring washer 10 is to avoid loosening of the bolts during use of the die, which results in an unsatisfactory engraved pattern.
Optionally, in this embodiment, a gasket 13 may be disposed between the second bolt 14 and the flange 16, so as to further close the first mold unit and the second mold unit.
Of course, in some embodiments, the first mold unit and the second mold unit may be connected by a snap or the like.
In one embodiment, the first mold unit and the second mold unit are tile-shaped. The first die unit 1 is also provided with a mounting hole 5 corresponding to an electrode hole on a substrate to be subjected to sand blasting. The one side of keeping away from second mould monomer 2 at first mould monomer 1 still is provided with first arc gasket 12, and first bolt 11 passes this mounting hole 5 and electrode hole and mould monomer 1 inside first nut 8 swivelling joint through first arc gasket 12 for the fixed substrate of treating the sandblast. A second arc gasket 15 is arranged between the nut inside the first die unit and the inner wall of the first die unit; the nut and the bolt can be tightly connected through the second arc-shaped gasket 15.
In one embodiment, the first mold unit and the second mold unit are tile-shaped. The second die unit 2 is also provided with a mounting hole 5 corresponding to an electrode hole on a substrate to be sandblasted. The inner wall and the outer wall of the second mould single body 2 are respectively provided with a first arc gasket 12 and a second arc gasket 15, and the first mould single body and the second mould single body are used for positioning the substrate to be subjected to sand blasting through the matching of the first bolt 11, the first nut 8 and the first arc gasket and the second arc gasket.
It is understood that, in the above embodiment, the first mold unit 1 and the second mold unit 2 are in the form of tiles, and when the first mold unit 1 and the second mold unit 2 are in the form of, for example, rectangular flat surfaces, the gasket may be in a flat shape, as long as the gasket is fitted to the shapes of the inner wall and the outer wall of the first mold unit.
Fig. 6 is a schematic flow chart of a heater manufacturing method according to a second embodiment of the present invention.
As shown in fig. 6, the method includes steps S101 to S104:
step S101, depositing a conductive layer on the surface of the substrate.
In one embodiment, the boron nitride substrate is suspended in a CVD apparatus for surface pyrolytic graphite deposition at a vacuum of 50-800Pa and at a temperature of 1250-4：N21:0.5-20, deposition thickness 5-200 μm; and cooling the deposition furnace to room temperature, and taking out the coated substrate. Wherein the coating is a conductive layer, i.e. a pyrolytic graphite layer. The substrate may be a PBN substrate.
In another specific embodiment, the boron nitride substrate is suspended in the CVD apparatus and the deposition chamber is vented into the BCl3、CH4And N2And gas, depositing and forming a conducting layer on the surface of the pyrolytic boron nitride substrate layer, wherein the conducting layer is pyrolytic graphite doped with boron carbide, and the mass of the boron carbide is 0.1-50% of that of the conducting layer. The mass of the boron carbide is 0.1% -50% of that of the conducting layer, so that the difference between the expansion coefficient of the conducting layer and the conducting coefficients of the insulating layer and the substrate is small, and the layering phenomenon is not easy to occur. To simplify the subsequent description, the percentage of the mass of boron carbide to the mass of the conductive layer is hereinafter referred to as the percentage of boron carbide.
Table 1 below shows the relationship between the proportion of boron carbide and the coefficient of thermal expansion of the conductive layer in the present application.
TABLE 1
As can be seen from table 1, when pyrolytic graphite is used for all of the conductive layers, 50% delamination occurs between the conductive layers and the substrate. When the percentage is 1%, the thermal expansion coefficient of the conductive layer is increased, and the delamination is improved. When the proportion of boron carbide is 30%, the conductive layer and the substrate are not layered, and when the proportion is 40%, the conductive layer and the substrate are layered by 5%. Further, when the conductive layer is pyrolytic graphite doped with boron carbide, the thermal expansion coefficient of the conductive layer can be improved, so that the conductive layer is attached to the substrate layer, and the delamination phenomenon can be reduced. The present application also finds that when the percentage of boron carbide is higher than 60%, this can result in the hardness of the conductive layer being too high, and the coating itself is prone to cracking and fails to meet applicable requirements. Therefore, the mass of boron carbide is preferably 0.1% to 40% of the conductive layer. Most preferably, the boron carbide is 30% by mass of the conductive layer.
Table 2 below shows the relationship between the proportion of boron carbide and the resistivity of the conductive layer.
TABLE 2
B4C fraction versus resistivity of conductive layer
As can be seen from table 2, as the conductive layer of the heater, not only the delamination phenomenon can be reduced but also the negative temperature characteristic of the conductive layer can be weakened and the resistivity itself can be lowered by adjusting the mass ratio of boron carbide. The application also notes that when the proportion of boron carbide is lower than 0.1%, the negative temperature characteristic of the pyrolytic graphite cannot be weakened, and when the proportion is too high, the resistivity of the pyrolytic graphite rises along with the temperature, so that the pyrolytic graphite is not suitable for manufacturing heaters. Therefore, when the ratio of boron carbide is 0.1% to 40%, the resistivity is optimal, and the method is more suitable for manufacturing heaters.
Further, BCl3、CH4And N2The volume ratio of (A) to (B) is as follows: (0.1-10): (0.1-10): 8, the mass of the boron carbide is 0.1-50% of the conductive layer.
Furthermore, the vacuum degree of the heating chamber is 10-800Pa, the temperature is 900-.
Further, the pyrolytic boron nitride substrate is prepared by the following method: introducing BCl into a heating chamber containing a deposition mold3、NH3And N2The mixed gas of (3); keeping the temperature of the heating chamber at 1200-1600 ℃, and introducing the mixed gas for 5-10 h; raising the temperature of the heating chamber to 1700-2200 ℃ and keeping the temperature for 2-15 h; and cooling to room temperature.
Further, after the temperature is reduced to the room temperature, the method also comprises the following steps: controlling the rotating speed of the pyrolytic boron nitride substrate layer to be 0.5-50 r/min; sand grains with the Mohs hardness of 3-9 and the mesh number of 30-500 are adopted to carry out sand blasting treatment on the surface of the pyrolytic boron nitride; the pressure of sand blasting is 0.1-5MPa, and the sand blasting distance is 1-500 mm. Through carrying out sand blasting treatment on the surface of the pyrolytic boron nitride substrate, the pyrolytic boron nitride substrate is more easily attached to the conducting layer, and the layering phenomenon is further avoided.
Fig. 7 is a graph of the resistivity of the conductive layer versus the mass of boron carbide at different temperatures according to the third embodiment of the present invention.
As shown in fig. 7, the resistivity at different temperatures is plotted for the line connected by the circles with a boron carbide fraction of 0%. The line connected by the triangle is a graph of the resistivity at different temperatures when the boron carbide proportion is 30%. The lines connected by the boxes are plots of resistivity at different temperatures at 60% boron carbide.
As can be seen from fig. 7, when the proportion of boron carbide is 0%, that is, the conductive layer is composed of only pyrolytic graphite, the resistivity decreases with an increase in temperature. Therefore, the heating effect of the heater is not good at this time, and temperature control operation is required.
When the percentage of boron carbide is 30%, the resistivity remains substantially constant with increasing temperature. In this case, the heater has a good heating effect and does not require excessive temperature control.
When the proportion of boron carbide is 60%, the resistivity of the conductive layer increases with the increase of temperature, which indicates that the heating effect is the best, and the temperature control operation is also needed.
Therefore, it can be seen from the comparison that the heater effect is the best when the percentage of boron carbide is 30%.
In one embodiment of the present invention, the roughness of the surface of the substrate 1 in contact with the conductive layer 2 is 1 to 8 μm, so that the substrate 1 and the conductive layer are more bonded.
In a further embodiment of this embodiment, the substrate 1 has a thickness of 0.5-5mm, preferably 1 mm; the thickness of the conductive layer 2 is 5-200 μm; the thickness of the insulating layer 3 is 0.03 to 1mm, preferably 0.1 mm.
Step S102, the substrate with the conductive layer is mounted in the accommodating space of the mold as in the first embodiment. Wherein the conductive layer is attached to the inner wall of the mold.
The conductive layer is arranged in the mold, the shape of the preset isolation region is exposed through the through hole of the mold, the preset isolation region leaked from the surface of the mold is carved and removed in a sand blasting mode, the removed part is actually a naked substrate relative to the conductive layer, the naked substrate and the conductive layer form conductive lines of a heater (the part which is not carved by sand blasting is a moving path of electrons, the part of the naked substrate is an insulating part, and the electrons cannot pass through), the naked substrate serves as the isolation region, and then the conductive layer containing the isolation region is obtained.
Optionally, the mold unit 1 and the mold unit 2 may be manufactured by injection molding or 3D printing, and the material for manufacturing the mold is selected from materials which are wear-resistant, not easy to deform and have certain micro-elasticity, such as hard rubber, PVC material, and the like. The inner wall of the accommodating space of the mold is added with 0.01-2mm of flexible filler to ensure that the inner wall of the accommodating space of the mold can be completely attached to the outer wall of the substrate, and after the mold and the substrate are positioned through electrode holes or other positioning modes, the mold unit 1 and the mold unit 2 are closed and can be fastened through bolts or buckles. Wherein, the flexible filler can be sponge or sand blasting adhesive tape or other flexible materials with single-sided stickiness.
Step S103, performing sand blasting on the conductive layer on the substrate exposed by the through hole of the mold to carve the conductive layer exposed by the through hole 3 on the surface of the mold to expose the substrate, where the exposed substrate is an isolation region.
Specifically, a mold with a built-in substrate and a shielding layer of pyrolytic graphite is fixed on a rotating table of a sand blasting machine, the equipment is started to rotate at the rotating speed of 0.5-50r/min, then sand grains with Mohs hardness of 3-9 and 30-500 meshes are adopted for surface sand blasting treatment, the sand blasting pressure is 0.1-5MPa, the sand blasting distance is 1-500mm, the sand blasting is stopped after the PBN substrate of the insulation part exposed out of the through hole 3 is completely leaked, and the substrate is taken out of the mold.
And step S104, depositing an insulating layer on the surface of the substrate with the conductive material layer.
Suspending the substrate with the pattern of the conductive isolation region engraved by sandblasting on the surface taken out from the mold into a deposition chamber of a CVD device for deposition of a surface pyrolytic boron nitride insulating layer, wherein the vacuum degree in the deposition chamber is 100-2As the carrier gas, BCl is required3：NH3(0.1-10): and 1, cooling the deposition furnace to room temperature, and taking out the coated multilayer heater.
In one embodiment, the substrate is prepared as follows:
the method comprises the steps of taking boron trichloride and ammonia as reaction gases, taking nitrogen as a carrier gas, uniformly mixing the three gases, introducing the mixture into a high-temperature deposition furnace, suspending a deposition mold processed by high-quality graphite in the deposition furnace, reacting the reaction gases at 1200-1600 ℃, generating amorphous pyrolytic boron nitride, depositing the amorphous pyrolytic boron nitride on the surface of the deposition mold, depositing for 5-10 hours, then carrying out high-temperature sintering crystallization treatment on amorphous pyrolytic Boron Nitride (BN) at a higher temperature ranging from 1700 ℃ to 2200 ℃ for 2-15 hours, cooling the deposition furnace to room temperature, and taking out the deposition mold and a boron nitride substrate PBN of a heater to be processed.
In one embodiment, after preparing the boron nitride substrate of the heater to be processed, the surface of the boron nitride substrate is further subjected to surface roughness treatment, which comprises the following steps:
fixing the boron nitride substrate on a rotating frame of sand blasting equipment, starting the equipment to rotate at the rotating speed of 0.5-50r/min, and then carrying out surface sand blasting treatment by adopting sand grains with the Mohs hardness of 3-9 and the mesh number of 30-500, wherein the sand blasting pressure is 0.1-5MPa, the sand blasting distance is 1-500mm, and the roughness of the substrate surface after sand blasting is required to be 1-8 mu m.
This example also gives a table of the relationship between the magnitude of roughness and the fit between the substrate and the conductive layer.
As can be seen from the above table, the roughness of the substrate surface can also affect the delamination of the substrate and the conductive layer of the heater, and when the roughness is 1-8 microns, the delamination phenomenon can be remarkably avoided.
The method of manufacturing the heater provided by the embodiment of the present invention will be described below by way of example.
Example 1
BCl3 and NH3 were fed into the heated deposition furnace using nitrogen as a carrier gas, and the ratio of BCl 3: NH3 ═ 2.5: 1, the temperature of a reaction cavity is 1600 ℃, the vacuum degree is 133pa, pyrolytic boron nitride with the thickness of 1.5mm is formed on the surface of a conventional graphite mold through deposition, then the temperature of the pyrolytic boron nitride matrix is raised to 1950 ℃ under vacuum, and the temperature is maintained for 3 hours, so that pyrolytic boron nitride used as a heater substrate is formed.
Fixing the pyrolytic boron nitride substrate on a rotating frame of sand blasting equipment, starting the equipment to rotate at the rotating speed of 10r/min, and then carrying out surface sand blasting treatment by using 120-mesh corundum sand, wherein the sand blasting pressure is 0.2MPa, the sand blasting distance is 250mm, and the roughness of the substrate surface after sand blasting is 3.42 mu m.
Then the processed boron nitride substrate is hung in a CVD device to carry out the deposition of surface pyrolytic graphite, and the vacuum degree is controlled to be 500pa, the temperature is controlled to be 1700 ℃, and the ratio of CH 4: n2 ═ 1:7.5, deposition thickness 85 μm; and cooling the deposition furnace to room temperature, and taking out the pyrolytic boron nitride substrate deposited with pyrolytic graphite after the coating is finished.
Fixing a mould for sand blasting on the outer surface of a substrate with a conducting layer, adding a 0.2mm flexible filler on the inner wall of the mould, ensuring that the inner wall of the mould is completely attached to the surface of the conducting layer, positioning the mould and the substrate through an electrode hole, fixing the substrate which is fastened with the mould and coated with pyrolytic graphite on a rotary table of a sand blasting machine, starting the rotation of equipment at a rotation speed of 10r/min, performing surface sand blasting treatment by adopting 120-mesh corundum sand, wherein the sand blasting pressure is 0.2MPa, the sand blasting distance is 250mm, stopping sand blasting after the PBN substrate of pyrolytic boron nitride of an insulating part is completely leaked, and taking the substrate with an insulating area out of the mould.
The substrate on which the insulating region was sandblasted and engraved was then suspended in a CVD apparatus to perform deposition of surface pyrolytic boron nitride at a vacuum degree of 133pa and a temperature of 1700 ℃, with nitrogen as a carrier gas, BCl 3: NH3 ═ 2.5: 1, after depositing pyrolytic boron nitride with the thickness of 150 mu m, cooling to room temperature, and taking out the multilayer heater with the finished coating.
Example 2
BCl3 and NH3 were fed into the heated deposition furnace using nitrogen as a carrier gas, and the ratio of BCl 3: NH3 ═ 2.5: 1, the temperature of a reaction cavity is 1600 ℃, the vacuum degree is 133pa, pyrolytic boron nitride with the thickness of 1.5mm is formed on the surface of a conventional graphite mold through deposition, then the temperature of the pyrolytic boron nitride matrix is raised to 1950 ℃ under vacuum, and the temperature is maintained for 3 hours, so that pyrolytic boron nitride used as a heater substrate is formed.
Fixing the pyrolytic boron nitride substrate on a rotating frame of sand blasting equipment, starting the equipment to rotate at the rotating speed of 10r/min, and then carrying out surface sand blasting treatment by using 120-mesh corundum sand, wherein the sand blasting pressure is 0.2MPa, the sand blasting distance is 250mm, and the roughness of the substrate surface after sand blasting is 3.42 mu m.
Then suspending the treated boron nitride substrate in CVD equipment for deposition of surface conductive layer, using nitrogen as carrier gas and BCl3And CH4Is 0.5: 4, the vacuum degree is 100Pa, the temperature is 1250 ℃, and the deposition thickness is 100 mu m; cooling the deposition furnace to room temperature, and taking out the coated substrate, wherein the coating on the surface of the substrate obtained in the step is a conductive layer doped with carbonizationPyrolytic graphite of boron. At this time, B430% of C and B4The thermal expansion coefficient of the pyrolytic graphite after C is 4.0 multiplied by 10-6At/° C, both the room-temperature resistivity and the high-temperature resistivity are 4.2 × 10-6Ω·m。
Fixing a mould for sand blasting on the outer surface of a substrate with a conducting layer, adding a 0.2mm flexible filler on the inner wall of the mould, ensuring that the inner wall of the mould is completely attached to the surface of the conducting layer, positioning the mould and the substrate through an electrode hole, fixing the substrate which is fastened with the mould and coated with pyrolytic graphite on a rotary table of a sand blasting machine, starting the rotation of equipment at a rotation speed of 10r/min, performing surface sand blasting treatment by adopting 120-mesh corundum sand, wherein the sand blasting pressure is 0.2MPa, the sand blasting distance is 250mm, stopping sand blasting after the PBN substrate of pyrolytic boron nitride of an insulating part is completely leaked, and taking the substrate with an insulating area out of the mould.
The substrate on which the insulating region was sandblasted and engraved was then suspended in a CVD apparatus to perform deposition of surface pyrolytic boron nitride at a vacuum degree of 133pa and a temperature of 1700 ℃, with nitrogen as a carrier gas, BCl 3: NH3 ═ 2.5: 1, after depositing pyrolytic boron nitride with the thickness of 150 mu m, cooling to room temperature, and taking out the multilayer heater with the finished coating.
In the heater obtained in example 1, there is no delamination between the conductive layer and the substrate, and the resistivity of the conductive layer increases with the temperature of the heater, and the fluctuation of the resistivity is less than 1%, which indicates that the heater prepared by the above method has a good effect. And the conductive layer is prepared by a sand blasting method, so that the method is easy to use and simple.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (12)
1. The heater preparation mold is characterized by comprising a first mold monomer (1) and a second mold monomer (2);
the first mould single body (1) is detachably connected with the second mould single body (2);
the first mould single body (1) and the second mould single body (2) enclose a closed accommodating space, and the accommodating space is used for accommodating a heater;
through holes (3) are formed in the surfaces of the first die single body (1) and the second die single body (2);
the through hole (3) is arranged corresponding to the conductive isolation area of the heater and is used for performing sand blasting carving on the conductive coating exposed out of the through hole;
the through holes (3) are long-strip-shaped, and the number of the through holes is set to be multiple; reinforcing ribs (4) are arranged at intervals in the length direction of the through hole (3), and the reinforcing ribs are connected with two side walls of the through hole (3);
the first die single body (1) and the second die single body (2) are respectively and oppositely provided with a positioning hole corresponding to the electrode hole on the surface of the heater so as to position the heater.
2. The mold according to claim 1,
the outer surface of the reinforcing rib (4) and the outer wall of the first die unit (1) are positioned on the same surface, and the inner surface of the reinforcing rib (4) is retracted to the inner wall of the first die unit (1); or
The outer surface of the reinforcing rib (4) and the outer wall of the second die single body (2) are located on the same surface, and the inner surface of the reinforcing rib (4) is retracted into the inner wall of the second die single body (2).
3. The mold according to claim 1 or 2,
the thicknesses of the first mould single body (1) and the second mould single body (2) are the same;
the thickness of the reinforcing rib (4) is 10% -50% of that of the first die single body (1); the width of the reinforcing rib (4) is 0.5-10 mm.
4. The mold according to claim 1 or 2,
the reinforcing ribs are arranged at intervals of 10-100mm in the length direction of the through hole (3).
5. The mold according to claim 3,
the reinforcing ribs are arranged at intervals of 10-100mm in the length direction of the through hole (3).
6. A mould according to any of claims 1, 2 or 5, further comprising a flexible buffer layer (7);
one surface of the flexible buffer layer (7) is attached to the surface of the first die unit (1) and the second die unit (2) which are provided with accommodating spaces, and the other surface of the flexible buffer layer is abutted to the heater.
7. Mould according to claim 6, characterized in that the thickness of the flexible buffer layer (7) is 0.05-10 mm.
8. A method for manufacturing a heater is characterized by comprising the following steps:
depositing a conductive layer on the surface of the substrate;
mounting the substrate with the conductive layer in the accommodating space of the mold according to any one of claims 1 to 5, the conductive layer being in abutment with the inner wall of the mold;
carrying out sand blasting treatment on the conducting layer on the substrate exposed out of the through hole of the mold so as to form an isolation region on the surface of the conducting layer;
and depositing an insulating layer on the surface of the substrate with the conducting layer.
9. The method of claim 8, wherein the step of grit blasting the mold surface to blast scribe isolation regions in the surface of the conductive layer comprises:
controlling the rotating speed of the die to be 0.5-50 r/min;
sand blasting treatment is carried out on the surface of the substrate by adopting sand grains with Mohs hardness of 3-9 and mesh number of 30-500; the pressure of sand blasting is 0.1-5MPa, and the sand blasting distance is 1-500 mm.
10. The method of claim 8, wherein the step of depositing a conductive layer on the surface of the substrate comprises:
introducing BCl into the deposition chamber3、CH4And N2Gas, depositing the conducting layer on the surface of the substrate; the conducting layer is pyrolytic graphite doped with boron carbide; wherein the BCl3、CH4And N2The volume ratio of (A) to (B) is as follows: (0.1-10): (0.1-10): 8, the mass of the boron carbide is 0.1-50% of the conductive layer.
11. The method of claim 8, wherein the substrate is prepared by:
introducing BCl into a deposition chamber containing a deposition mold3、NH3And N2The mixed gas of (3);
keeping the temperature of the deposition chamber at 1200-1600 ℃, and introducing the mixed gas for 5-10 h;
raising the temperature of the deposition chamber to 1700-2200 ℃ and keeping the temperature for 2-15 h;
and cooling to room temperature.
12. The method of claim 8, wherein depositing an insulating layer on the surface of the conductive layer comprises:
introducing BCl into a deposition chamber containing a conductive layer3、NH3And N2Controlling the vacuum degree of the deposition chamber to be 100-500Pa and the temperature to be 1350-2000 ℃; and/or the volume ratio of BCl3 to NH3 is (0.1-10): 1.
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