CN113804004B - Method for improving reliability of oxide layer on surface of conveyor belt of sintering furnace - Google Patents
Method for improving reliability of oxide layer on surface of conveyor belt of sintering furnace Download PDFInfo
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- CN113804004B CN113804004B CN202110923667.9A CN202110923667A CN113804004B CN 113804004 B CN113804004 B CN 113804004B CN 202110923667 A CN202110923667 A CN 202110923667A CN 113804004 B CN113804004 B CN 113804004B
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- conveyor belt
- sintering furnace
- days
- oxide layer
- oxidation treatment
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- 238000005245 sintering Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000003647 oxidation Effects 0.000 claims abstract description 63
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 63
- 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 35
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims description 3
- 229910001120 nichrome Inorganic materials 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000004140 cleaning Methods 0.000 abstract description 5
- 230000014759 maintenance of location Effects 0.000 abstract description 3
- 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
- 239000000758 substrate Substances 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BIJOYKCOMBZXAE-UHFFFAOYSA-N chromium iron nickel Chemical compound [Cr].[Fe].[Ni] BIJOYKCOMBZXAE-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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: a first oxidation treatment section, wherein the temperature of the high-temperature sintering furnace is set at 990-1010 ℃, nitrogen is introduced, the conveyor belt is subjected to circulating idle operation, and the retention time in the furnace is ensured to be kept during each operation; the circulating idle running time of the conveyor belt is 1-2 days; the second oxidation treatment section is used for adjusting the temperature of the high-temperature sintering furnace to 1065-1075 ℃, introducing nitrogen, carrying out circulating idle operation on the conveyor belt treated in the step 1 again, and ensuring the residence time in the furnace during each operation; the conveyor belt is continuously idle for 4-5 days. The two-stage oxidation treatment shortens the oxidation time of the conveyor belt from about 12 to 15 days to about 5 to 7 days, reduces the oxidation treatment time and improves the production capacity and the production efficiency of the sintering furnace. Meanwhile, the cleaning frequency of the hearth is reduced, the cleaning frequency is increased 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 an oxide layer on the surface of a conveyor belt of a sintering furnace.
Background
The direct bonding copper substrate (Direct Bonding Copper, DBC) has the characteristics of high heat conduction, high electric insulation, high mechanical strength, low expansion and the like of ceramics, has high conductivity and excellent welding performance of oxygen-free copper, can etch various patterns like a PCB circuit board, and is a ceramic lining board widely applied to electronic circuit boards of semiconductor modules.
The bonding of the copper foil and the ceramic of the DBC substrate is performed in a high temperature sintering furnace, and the copper foil is directly coated on the ceramic by using oxygen-containing eutectic liquid of the copper. The conveyer belt for conveying the copper foil and the ceramic is required to be oxidized independently before being used for the first time, so that an oxide layer is formed on the surface of the conveyer belt, the conveyer belt substrate is prevented from absorbing oxygen in a hearth, the original oxygen balance in the hearth is destroyed, and the quality and the performance of the DBC substrate are affected.
The conventional conveyer belt oxidation method is that the conveyer belt enters the furnace from the outside of the furnace at room temperature, and is oxidized in a high-temperature air atmosphere at 1000 ℃ for 20min each time, so that the conveyer belt is circularly and idly operated for 12-15 days, and an oxide layer is generated on the surface. However, this treatment has the following disadvantages:
1) Because the conveyor belt is oxidized in the hot air atmosphere with the 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 and not compact, and the oxide layer is easy to fall off, and the exposed conveyor belt matrix after falling off directly absorbs oxygen in a hearth, so that the combination of copper foil and ceramic can be influenced in the production process. 2) The fallen oxide layer particles pollute the hearth and the products being sintered, so that bubbles and bad sintering are increased. 3) The conveyor belt is oxidized each time, the conveyor belt needs to be circulated and run for about 12 to 15 days, the productivity of the sintering furnace is affected, and the production efficiency is low.
Disclosure of Invention
The invention aims to solve the technical problems, aims to solve the problems that an oxide layer is loose and easy to fall off and the oxidation time is too long in the current surface oxidation treatment process of a conveyor belt, improves the oxidation process, and provides a method for improving the reliability of the oxide 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 and is easy to fall off and the oxidation time is too long are solved, the yield and performance of the product are improved, and meanwhile, the productivity and the production efficiency of the sintering furnace are improved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides 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:
(1) First oxidation treatment section
Setting the temperature of a high-temperature sintering furnace at 990-1010 ℃, introducing nitrogen, carrying out circulating idle operation on a conveyor belt, and ensuring that a high-temperature section in the furnace maintains a certain residence time during each operation; the continuous idle running time of the conveyor belt is 1-2 days;
(2) Second oxidation treatment section
The temperature of the high-temperature sintering furnace is adjusted to 1065-1075 ℃, nitrogen is also introduced, the conveyor belt treated in the step 1 is subjected to circulating idle operation again, and a certain residence time is ensured to be maintained in a high-temperature section in the furnace during each operation; the conveyor belt is continuously idle for 4-5 days.
In the invention, the conveyor belt is made of nickel-chromium-iron alloy 601 material. The first oxidation treatment section is an oxide layer generation section, when the conveyor belt enters the sintering furnace from outside the furnace, air outside the furnace is simultaneously brought into the sintering furnace, and an oxide layer is generated on the surface of the conveyor belt at the high temperature of 1000 ℃; to ensure oxide layer formation, each section of the conveyor belt is ensured to stay in the furnace for a certain time by adjusting the idle speed; when the oxygen concentration is high, the density of the oxide layer is low, and the mode of introducing nitrogen into the furnace is adopted, so that the oxygen concentration in the furnace is reduced, and the density of the oxide layer is improved.
The second oxidation treatment section is an oxidation enhancement section, and the bonding force between the oxidation layer and the conveyor belt substrate is enhanced by increasing the oxidation temperature, so that the falling degree of the oxidation layer is reduced, and meanwhile, 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 cannot be too high or too low, the concentration is too high, the air in the sintering furnace is thin, the formation of an oxide layer is not facilitated, the concentration is too low, the concentration of the oxygen is too high, and the problem of low density of the oxide layer cannot be relieved.
Preferably, in both oxidation treatment sections, the residence time of the conveyor belt in the high temperature section of the furnace is 18-22 min, preferably 20min, per run.
Preferably, in the first oxidation treatment stage, the conveyor belt is kept in idle operation for 2 days, and in the second oxidation treatment stage, the conveyor belt is kept in idle operation for 5 days.
The beneficial effects of the invention are as follows:
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 compact and high, and the appearance color is changed from black to green.
And secondly, the second oxidation treatment section is an oxidation enhancement section, the binding force between the oxidation layer and the conveyor belt substrate is enhanced by increasing the oxidation temperature to 1065-1075 ℃, the falling degree of the oxidation 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 increased.
Thirdly, 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 energy yield and the production efficiency of the sintering furnace are greatly improved.
Drawings
FIG. 1 is an appearance (blackish) of a conveyor belt after oxidation treatment using the prior art;
fig. 2 shows the appearance (greenish) of the conveyor belt after oxidation treatment by the method of the present invention.
Detailed Description
The following examples are given to illustrate the present invention in detail, but the scope of the present invention is not limited to the following examples.
The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace provided by the embodiment comprises the following steps:
(1) First oxidation treatment section
Setting the temperature of a high-temperature sintering furnace at 990-1010 ℃, introducing nitrogen with the concentration of 20L/min, carrying out circulating idle operation on a conveyor belt, and ensuring the retention time of 20min in a high-temperature section in the furnace during each operation, wherein the continuous idle operation time of the conveyor belt is 2 days;
(2) Second oxidation treatment section
The temperature of the high-temperature sintering furnace is regulated to 1065-1075 ℃, nitrogen with the concentration of 20L/min is also used, the conveyor belt treated in the step 1 is circulated and idle again, and the retention time of 20min in the high-temperature section in the furnace is ensured to be kept during each operation; the conveyor was kept idle for 5 days.
In this embodiment, the conveyor belt is made of nichrome 601 material. The first oxidation treatment section is an oxide layer generation section, when the conveyor belt enters the sintering furnace from outside the furnace, air outside the furnace is simultaneously brought into the sintering furnace, and an oxide layer is generated on the surface of the conveyor belt at the high temperature of 1000 ℃; to ensure oxide layer formation, each section of the conveyor belt is ensured to stay in the furnace for a certain time by adjusting the idle speed; when the oxygen concentration is high, the density of the oxide layer is low, and the mode of introducing nitrogen into the furnace is adopted, so that the oxygen concentration in the furnace is reduced, and the density of the oxide layer is improved.
The second oxidation treatment section is an oxidation enhancement section, and the bonding force between the oxidation layer and the conveyor belt substrate is enhanced by increasing the oxidation temperature, so that the falling degree of the oxidation layer is reduced, and meanwhile, the oxidation treatment time is reduced.
When oxidation treatment is carried out, the concentration of the introduced nitrogen cannot be too high or too low, the concentration is too high, the air in the sintering furnace is thin, the formation of an oxide layer is not facilitated, the concentration is too low, the concentration of oxygen is too high, and the problem of low density of the oxide layer cannot be relieved.
The invention divides the high-temperature oxidation in the conveyor belt furnace from one high-temperature oxidation treatment to two high-temperature oxidation treatments, and introduces a certain amount of nitrogen gas during the two high-temperature treatments, so as to reduce the oxygen concentration in the furnace, the formed oxide layer is compact and high, and the appearance color is changed from black (figure 1) to green (figure 2).
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 production capacity and the production efficiency of the sintering furnace. Meanwhile, the cleaning frequency of the hearth is reduced, the cleaning frequency is increased 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 illustrated and described, the present invention is not limited to the embodiments, and various equivalent modifications and substitutions can be made by one skilled in the art without departing from the spirit of the present invention, and these equivalent modifications and substitutions are intended to be included in the scope of the present invention as defined in the appended claims.
Claims (6)
1. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace is characterized by comprising the following steps of:
(1) First oxidation treatment section
Setting the temperature of a high-temperature sintering furnace at 990-1010 ℃, introducing nitrogen, carrying out circulating idle operation on the conveyor belt, and ensuring that a certain residence time is kept in the furnace during each operation; the continuous idle running time of the conveyor belt is 1-2 days;
(2) Second oxidation treatment section
Regulating the temperature of the high-temperature sintering furnace to 1065-1075 ℃, simultaneously introducing nitrogen, and carrying out circulating idle operation on the conveyor belt treated in the step 1 again, wherein a certain residence time is ensured to be maintained in the furnace during each operation; the continuous idle running time of the conveyor belt is 4-5 days,
wherein, in the two oxidation treatment sections, the concentration of the introduced nitrogen is 15-25L/min,
in the two oxidation treatment sections, the residence time of the conveyor belt in the high temperature section in the furnace is 18-22 min during each operation.
2. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace according to claim 1, wherein the method comprises the following steps:
wherein, the conveyer belt adopts nichrome 601 material to make.
3. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace according to claim 1, wherein the method comprises the following steps:
wherein, the concentration of the introduced nitrogen is 20L/min.
4. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace according to claim 1, wherein the method comprises the following steps:
wherein the residence time of the conveyor belt in the high temperature section of the furnace is 20min during each operation.
5. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace according to claim 1, wherein the method comprises the following steps:
wherein, in the first oxidation treatment section, the conveyor belt is continuously in idle operation for 2 days.
6. The method for improving the reliability of the oxide layer on the surface of the conveyor belt of the sintering furnace according to claim 5, wherein the method comprises the following steps:
wherein, in the second oxidation treatment section, the continuous idle running time of the conveyor belt is 5 days.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
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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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| CN113804004A CN113804004A (en) | 2021-12-17 |
| CN113804004B true CN113804004B (en) | 2024-03-19 |
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