CN113804004A - Method for improving reliability of surface oxide layer of sintering furnace conveyor belt - Google Patents
Method for improving reliability of surface oxide layer of sintering furnace conveyor belt Download PDFInfo
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- CN113804004A CN113804004A CN202110923667.9A CN202110923667A CN113804004A CN 113804004 A CN113804004 A CN 113804004A CN 202110923667 A CN202110923667 A CN 202110923667A CN 113804004 A CN113804004 A CN 113804004A
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- conveyor belt
- sintering furnace
- oxide layer
- furnace
- temperature
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- 238000005245 sintering Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000003647 oxidation Effects 0.000 claims abstract description 70
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 70
- 238000011282 treatment Methods 0.000 claims abstract description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 230000014759 maintenance of location Effects 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 229910001120 nichrome Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 14
- 239000001301 oxygen Substances 0.000 description 14
- 229910052760 oxygen Inorganic materials 0.000 description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 239000000758 substrate Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 239000011889 copper foil Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 229910000640 Fe alloy Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- BIJOYKCOMBZXAE-UHFFFAOYSA-N chromium iron nickel Chemical compound [Cr].[Fe].[Ni] BIJOYKCOMBZXAE-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/02—Supplying steam, vapour, gases, or liquids
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B9/00—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity
- F27B9/14—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment
- F27B9/20—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace
- F27B9/24—Furnaces through which the charge is moved mechanically, e.g. of tunnel type; Similar furnaces in which the charge moves by gravity characterised by the path of the charge during treatment; characterised by the means by which the charge is moved during treatment the charge moving in a substantially straight path tunnel furnace being carried by a conveyor
- F27B9/243—Endless-strand conveyor
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
- F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/12—Mountings, e.g. non-detachable insulating substrates
- H01L23/14—Mountings, e.g. non-detachable insulating substrates characterised by the material or its electrical properties
- H01L23/142—Metallic substrates having insulating layers
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Tunnel Furnaces (AREA)
Abstract
The invention relates to a method for improving the reliability of an oxide layer on the surface of a conveyor belt of a sintering furnace, which comprises the following steps: in the first oxidation treatment stage, the temperature of the high-temperature sintering furnace is set to 990-1010 ℃, nitrogen is introduced, the conveyor belt is circularly operated in an empty mode, and the retention time in the furnace is ensured during each operation; the circulating idle running time of the conveyor belt is 1-2 days; in the second oxidation treatment stage, the temperature of the high-temperature sintering furnace is adjusted to 1065-1075 ℃, nitrogen is introduced, the conveying belt treated in the step 1 is subjected to circulating idle operation again, and the retention time in the furnace is ensured during each operation; the time for the conveyor belt to continuously carry out idle running is 4-5 days. By the two-stage oxidation treatment, the oxidation time of the conveyor belt is shortened from about 12-15 days to about 5-7 days, the oxidation treatment time is shortened, and the productivity and the production efficiency of the sintering furnace are improved. Meanwhile, the cleaning frequency of the hearth is reduced, the cleaning frequency is improved to more than 180 days from the original 60 days, and the sintering yield of the product is improved.
Description
Technical Field
The invention belongs to the technical field of DBC substrate sintering, and particularly relates to a method for improving the reliability of a surface oxide layer of a conveyor belt of a sintering furnace.
Background
The Direct Bonding Copper substrate (DBC) has the characteristics of high thermal conductivity, high electrical insulation, high mechanical strength, low expansion and the like of ceramics, has the high conductivity and excellent welding performance of oxygen-free Copper, can etch various patterns like a PCB (printed circuit board), and is a ceramic lining plate widely applied to electronic circuit boards of semiconductor modules.
The combination of the copper foil of the DBC substrate and the ceramic is carried out in a high-temperature sintering furnace, and the copper foil is directly connected with the ceramic in a covering mode by utilizing oxygen-containing eutectic liquid of copper. And the conveyor belt for conveying the copper foil and the ceramic needs to be independently oxidized before being used for the first time, so that an oxide layer is formed on the surface, and the condition that the conveyor belt matrix absorbs oxygen in a hearth and destroys the original oxygen balance in a furnace is prevented, thereby influencing the quality and the performance of the DBC substrate.
The current common conveyor belt oxidation method is that a conveyor belt enters a furnace from the outside of the furnace at room temperature, and oxidation is carried out in a high-temperature hot air atmosphere of 1000 ℃ for 20min each time, so that circulation idle running is carried out for 12-15 days, and an oxide layer is generated on the surface. However, this treatment method has the following disadvantages:
1) because the conveyor belt is oxidized in the hot air atmosphere with the high temperature of 1000 ℃, the oxygen concentration in the furnace is higher, the appearance color of an oxide layer formed on the surface is blacker, loose, not dense and easy to fall off, and the exposed conveyor belt matrix directly absorbs oxygen in a hearth after falling off, so that the combination of the copper foil and the ceramic is influenced in the production process. 2) The particles of the oxide layer after the shedding pollute the hearth and the products being sintered, so that the air bubbles and poor sintering are increased. 3) The conveyor belt oxidation needs to be circulated for about 12-15 days every time, the productivity of the sintering furnace is influenced, and the production efficiency is low.
Disclosure of Invention
The invention aims to solve the technical problems, improves the oxidation process aiming at the problems that the oxidation layer is loose and easy to fall off and the oxidation time is overlong in the current oxidation treatment process of the surface of the conveyor belt, and provides a method for improving the reliability of the oxidation layer on the surface of the conveyor belt of a sintering furnace.
According to the invention, the high-temperature oxidation in the conveyor belt furnace is divided into two high-temperature oxidation treatments from one high-temperature oxidation treatment, namely a high-temperature oxidation section and an oxidation enhancement section, and a certain amount of nitrogen is introduced during the two high-temperature treatments, so that the oxygen concentration in the furnace is reduced, the problems that the conventional conveyor belt oxidation layer is loose and not compact, is easy to fall off and has overlong oxidation time are solved, the yield and performance of products are improved, and the productivity and production efficiency of a sintering furnace are improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for improving the reliability of a surface oxide layer of a sintering furnace conveyor belt, which comprises the following steps:
(1) first oxidation treatment stage
Setting the temperature of the high-temperature sintering furnace at 990-1010 ℃, introducing nitrogen gas, performing circulating idle operation on the conveyor belt, and ensuring that a certain retention time is kept in a high-temperature section in the furnace during each operation; the time for the conveyor belt to continuously carry out idle running is 1-2 days;
(2) second oxidation treatment stage
Adjusting the temperature of the high-temperature sintering furnace to 1065-1075 ℃, introducing nitrogen at the same time, performing circulating idle operation on the conveyor belt treated in the step 1 again, and ensuring that a certain retention time is kept in a high-temperature section in the furnace during each operation; the time for the conveyor belt to continuously carry out idle running is 4-5 days.
In the invention, the conveyor belt is made of a nickel-chromium-iron alloy 601 material. The first oxidation treatment section is an oxidation layer generation section, when the conveyor belt enters the furnace from the outside of the furnace, air outside the furnace is simultaneously brought into the sintering furnace, and an oxidation layer is generated on the surface of the conveyor belt at the high temperature of 1000 ℃; in order to ensure the generation of an oxidation layer, each section of the conveyor belt is ensured to stay in the furnace for a certain time by adjusting the air running speed; when the oxygen concentration is high, the density of the oxide layer is low, and the oxygen concentration in the furnace is reduced and the density of the oxide layer is improved by adopting a mode of introducing nitrogen into the furnace.
The second oxidation treatment section is an oxidation enhancement section, the bonding force between the oxide layer and the conveyor belt substrate is enhanced by increasing the oxidation temperature, the falling degree of the oxide layer is reduced, and the oxidation treatment time is reduced.
Preferably, the concentration of the introduced nitrogen in the two oxidation treatment sections is 15-25L/min, preferably 20L/min. The concentration of the introduced nitrogen can not be too high or too low, the air in the sintering furnace is easy to be thin due to the too high concentration, the formation of an oxidation layer is not facilitated, the concentration is too low, the oxygen concentration is higher, and the problem of low density of the oxidation layer can not be relieved.
Preferably, the residence time of the conveyor belt in the high-temperature section in the furnace in each operation of the two oxidation treatment sections is 18-22 min, and preferably 20 min.
Preferably, the time period during which the conveyor belt continues to perform the idling operation in the first oxidation treatment stage is 2 days, and the time period during which the conveyor belt continues to perform the idling operation in the second oxidation treatment stage is 5 days.
The invention has the following beneficial effects:
firstly, the high-temperature oxidation in the conveyor belt furnace is divided into two high-temperature oxidation treatments from one high-temperature oxidation treatment, a certain amount of nitrogen is introduced during the two high-temperature treatments, the oxygen concentration in the furnace is reduced, the formed oxide layer is high in compactness, and the appearance color is changed from black to green.
And secondly, the second oxidation treatment section is an oxidation enhancement section, the bonding force between the oxide layer and the conveyor belt substrate is enhanced by increasing the oxidation temperature to 1065-1075 ℃, the falling degree of the oxide layer is reduced, the pollution to a hearth and products is reduced, the cleaning frequency of the hearth is increased to more than 180 days from the original 60 days, and the sintering yield of the products is improved.
Thirdly, the two-stage oxidation treatment reduces the oxidation treatment time, shortens the oxidation time of the conveyor belt from about 12 to 15 days to about 5 to 7 days, and greatly improves the productivity and the production efficiency of the sintering furnace.
Drawings
FIG. 1 is a graph of the appearance of a conveyor belt after oxidation treatment using the prior art (blackish);
FIG. 2 shows the appearance of the conveyor belt after oxidation treatment by the method of the present invention (greenish).
Detailed Description
The following examples are given to illustrate the practice of the present invention, and the following examples are given on the premise of the technical solution of the present invention, and give detailed embodiments and specific procedures, but the scope of the present invention is not limited to the following examples.
The method for improving the reliability of the surface oxide layer of the sintering furnace conveyor belt comprises the following steps:
(1) first oxidation treatment stage
Setting the temperature of the high-temperature sintering furnace at 990-1010 ℃, introducing nitrogen with the concentration of 20L/min, performing circulating idle operation on the conveyor belt, and ensuring that the conveyor belt keeps the retention time of 20min in the high-temperature section of the furnace during each operation, wherein the idle operation time of the conveyor belt is 2 days;
(2) second oxidation treatment stage
Adjusting the temperature of the high-temperature sintering furnace to 1065-1075 ℃, simultaneously carrying out circulating idle operation on the conveyor belt treated in the step 1 by using nitrogen with the concentration of 20L/min, and ensuring that the retention time of 20min is also kept in the high-temperature section in the furnace during each operation; the conveyor belt continued to run empty for 5 days.
In this embodiment, the conveyor belt is made of a nickel-chromium-iron alloy 601 material. The first oxidation treatment section is an oxidation layer generation section, when the conveyor belt enters the furnace from the outside of the furnace, air outside the furnace is simultaneously brought into the sintering furnace, and an oxidation layer is generated on the surface of the conveyor belt at the high temperature of 1000 ℃; in order to ensure the generation of an oxidation layer, each section of the conveyor belt is ensured to stay in the furnace for a certain time by adjusting the air running speed; when the oxygen concentration is high, the density of the oxide layer is low, and the oxygen concentration in the furnace is reduced and the density of the oxide layer is improved by adopting a mode of introducing nitrogen into the furnace.
The second oxidation treatment section is an oxidation enhancement section, the bonding force between the oxide layer and the conveyor belt substrate is enhanced by increasing the oxidation temperature, the falling degree of the oxide layer is reduced, and the oxidation treatment time is reduced.
When the oxidation treatment is carried out, the concentration of the introduced nitrogen can not be too high or too low, the air in the sintering furnace is easy to thin due to the too high concentration, the formation of an oxide layer is not facilitated, and the problem of low density of the oxide layer cannot be solved due to the too low concentration and the too high oxygen concentration.
The invention divides the high-temperature oxidation in the conveyor belt furnace into two high-temperature oxidation treatments from one high-temperature oxidation treatment, and a certain amount of nitrogen is introduced during the two high-temperature treatments, so that the oxygen concentration in the furnace is reduced, the formed oxide layer is high in compactness, and the appearance color is changed from the previous partial black (figure 1) to partial green (figure 2).
Through the two-stage oxidation treatment, the oxidation treatment time is reduced, the oxidation time of the conveyor belt is shortened from about 12-15 days to about 5-7 days, and the capacity and the production efficiency of the sintering furnace are greatly improved. Meanwhile, the cleaning frequency of the hearth is reduced, the cleaning frequency is improved to more than 180 days from the original 60 days, and the sintering yield of the product is improved.
While the preferred embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the invention is not limited thereto, and that various changes and modifications may be made without departing from the spirit of the invention, and the scope of the appended claims is to be accorded the full scope of the invention.
Claims (8)
1. A method for improving the reliability of a surface oxide layer of a sintering furnace conveyor belt is characterized by comprising the following steps:
(1) first oxidation treatment stage
Setting the temperature of the high-temperature sintering furnace at 990-1010 ℃, introducing nitrogen gas, performing circulating idle operation on the conveyor belt, and ensuring that a certain retention time is kept in the furnace during each operation; the time for the conveyor belt to continuously carry out idle running is 1-2 days;
(2) second oxidation treatment stage
Adjusting the temperature of the high-temperature sintering furnace to 1065-1075 ℃, introducing nitrogen at the same time, performing circulating idle operation on the conveyor belt treated in the step 1 again, and ensuring that a certain retention time is kept in the furnace during each operation; the time for the conveyor belt to continuously perform idle running is 4-5 days.
2. The method for improving the reliability of the surface oxide layer of the conveyor belt of the sintering furnace according to claim 1, characterized in that:
wherein, the conveyer belt adopts nichrome 601 material to make.
3. The method for improving the reliability of the surface oxide layer of the conveyor belt of the sintering furnace according to claim 1, characterized in that:
wherein, the concentration of the introduced nitrogen in the two oxidation treatment sections is 15-25L/min.
4. The method for improving the reliability of the surface oxide layer of the sintering furnace conveyor belt according to claim 3, characterized in that:
wherein the concentration of the introduced nitrogen is 20L/min.
5. The method for improving the reliability of the surface oxide layer of the conveyor belt of the sintering furnace according to claim 1, characterized in that:
in the two oxidation treatment sections, the retention time of the conveyor belt in the high-temperature section in the furnace is 18-22 min during each operation.
6. The method for improving the reliability of the surface oxide layer of the sintering furnace conveyor belt according to claim 5, characterized in that:
wherein the retention time of the conveyor belt in the high-temperature section in the furnace is 20min during each operation.
7. The method for improving the reliability of the surface oxide layer of the conveyor belt of the sintering furnace according to claim 1, characterized in that:
wherein, in the first oxidation treatment section, the time for the conveyor belt to continuously carry out the idle running is 2 days.
8. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace according to claim 7, wherein:
wherein, in the second oxidation treatment section, the time for the conveyor belt to continuously carry out idle running is 5 days.
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| CN202110923667.9A CN113804004B (en) | 2021-08-12 | 2021-08-12 | Method for improving reliability of oxide layer on surface of conveyor belt of sintering furnace |
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| CN202110923667.9A CN113804004B (en) | 2021-08-12 | 2021-08-12 | Method for improving reliability of oxide layer on surface of conveyor belt of sintering furnace |
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