CN113471081B - Method for improving poor appearance of ceramic copper-clad carrier plate after high-temperature sintering - Google Patents
Method for improving poor appearance of ceramic copper-clad carrier plate after high-temperature sintering Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 48
- 238000005245 sintering Methods 0.000 title claims abstract description 47
- 239000000919 ceramic Substances 0.000 title claims abstract description 32
- 238000005406 washing Methods 0.000 claims abstract description 56
- 238000005488 sandblasting Methods 0.000 claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052802 copper Inorganic materials 0.000 claims abstract description 32
- 239000010949 copper Substances 0.000 claims abstract description 32
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005530 etching Methods 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 11
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims abstract description 8
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000007654 immersion Methods 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims abstract description 4
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- 238000011084 recovery Methods 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
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- 239000000758 substrate Substances 0.000 description 12
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- 238000005422 blasting Methods 0.000 description 8
- 206010000496 acne Diseases 0.000 description 7
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- 238000004519 manufacturing process Methods 0.000 description 3
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- 208000018999 crinkle Diseases 0.000 description 1
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- 229910001651 emery Inorganic materials 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
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Abstract
The invention relates to a method for improving poor appearance of a ceramic copper-clad carrier plate after high-temperature sintering, which comprises the following steps: A. micro-etching, namely, carrying out micro-etching on the ceramic copper-clad carrier plate by adopting a mixed solution of sulfuric acid and sodium persulfate and carrying out overflow waterWashing, wherein the concentration of sulfuric acid is 18.4-36.8 g/L, and the concentration of sodium persulfate is 20-40 g/L; B. sand blasting with Al 2 O 3 10 to 20 percent by mass of carborundum suspension is used as a sand blasting liquid, and the carborundum suspension is sprayed up and down, the sand blasting angle is 90 degrees, and the sand blasting pressure is 2kg/cm 2 The sand blasting distance is 8-12 mm, and the average thickness of the copper matrix is reduced by 0.5-0.8 mu m after sand blasting treatment; C. washing and drying, namely washing and drying by sequentially adopting recovery washing, overflow washing, pressurized washing, ultrasonic immersion washing, HF washing, swinging high-pressure washing, pressurized washing, DI washing and dry plate combination, and taking out after cooling; D. and D, sintering and recrystallizing, namely placing the product obtained after the treatment in the step C into a sintering furnace, introducing mixed gas of nitrogen and air, controlling the oxygen partial pressure in the furnace to be 8-15 ppm, and sintering at 1075-1083 ℃ to recrystallize the surface of the copper sheet.
Description
Technical Field
The invention belongs to the technical field of preparation of ceramic copper-clad carrier plates, and particularly relates to a method for improving poor appearance of a ceramic copper-clad carrier plate after high-temperature sintering in a semiconductor refrigerator, an LED and a power semiconductor.
Background
The ceramic Copper-clad carrier plate is also called a Copper-clad ceramic substrate, and is an electronic base material prepared by directly sintering Copper foil on the surface of ceramic by using a DCB (Direct Copper Bond) technology. The ceramic copper-clad carrier plate has the characteristics of excellent thermal cyclicity, stable shape, good rigidity, high thermal conductivity and high reliability, the copper-clad surface can be etched to form various patterns, and the ceramic copper-clad carrier plate is a pollution-free and nuisanceless green product, has a wide use temperature, can be used at the temperature of-55-850 ℃, has a thermal expansion coefficient close to silicon, and can be used in various industrial electronic fields such as a semiconductor refrigerator, an electronic heater, a high-power semiconductor module, a power control circuit, a power hybrid circuit, an intelligent power assembly, a high-frequency switching power supply, a solid-state relay, automotive electronics, aerospace and military electronic assemblies, a solar panel assembly, a telecommunication special exchanger, a receiving system, laser and the like.
In the high-temperature sintering process of the ceramic copper-clad carrier plate, pollution is easily brought in the process due to the limitation of environmental cleanliness, the pollution is caused by raw materials, and the bad defect of copper matrix oxidation can be amplified in the oxidation process (about 800 ℃) caused by the pollution in the process. All the defects are microscopically mainly represented by intermediate black foreign matters, and the main components of the EDX analysis are Ni, cr, C, O and the like.
The defects of the non-oxidized surface of the copper matrix can be further amplified by the sintering process at 1065-1083 ℃, and the appearance is poor such as color difference, wrinkled skin, pinholes, pimples and the like. The color difference and the wrinkle are mainly caused by uneven oxidation of a non-oxidized surface of a copper substrate, the local oxidation is too shallow, the color difference occurs, and the local oxidation is too deep, so that the wrinkle is caused on the surface of the copper; pimples and pinholes are mostly caused by foreign matters brought in the process, and in addition, the defects of surface scratch (bump) and the like caused by non-standard operation of personnel are also caused. These defects result in high product scrap rates, and how to improve these defects has always been a significant concern for those skilled in the art.
Disclosure of Invention
The invention aims to solve the technical problems, provides a method for improving poor appearance of a ceramic copper-clad carrier plate after high-temperature sintering aiming at the defects of chromatic aberration, crinkles, pimples and the like on the surface of a product, and reduces the reject ratio of a DCB product.
According to the characteristics of the sand blasting process, the invention utilizes a high-pressure mode to spray carborundum suspension on the surface of the copper substrate at a high speed, so that the appearance and the shape of the surface of the copper substrate are changed, and the surface of a product obtains certain cleanliness and uniform roughness.
In order to recover the crystal grain structure of the copper substrate surface before, the crystal grain is formed by re-burning again, the crystal grain and the roughness of the product after re-burning are the same as those of a normal product, the welding and routing performance is the same as that of the normal product, and the method can solve the problem of poor surface defects (pimples, wrinkles, pinholes, color difference, scratch (bump) injury, foreign matters and the like) after the ceramic copper-clad carrier plate is sintered and greatly improve the qualification rate of the product after multiple verification and test production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for improving poor appearance of a ceramic copper-clad carrier plate after high-temperature sintering, which comprises the following steps:
A. micro etching
Carrying out micro-etching on the ceramic copper-clad carrier plate by adopting a mixed solution of sulfuric acid and sodium persulfate, and carrying out overflow water washing, wherein the concentration of the sulfuric acid is 18.4-36.8 g/L, and the concentration of the sodium persulfate is 20-40 g/L;
B. sand blasting
By using Al 2 O 3 10 to 20 percent of carborundum suspension is used as a sand blasting liquid, and the carborundum suspension is sprayed up and down, the sand blasting angle is 90 degrees, and the sand blasting pressure is 2kg/cm 2 The sand blasting distance is 8-12 mm, and the average thickness of the copper matrix is reduced by 0.5-0.8 mu m after sand blasting treatment;
C. washing and drying
Sequentially carrying out water washing and drying by adopting the combination of recovery water washing, overflow water washing, pressurized water washing, ultrasonic immersion washing, HF water washing, swinging high-pressure water washing, pressurized water washing, DI water washing and dry plate, cooling and taking out;
D. sintering recrystallization
And C, placing the product obtained after the treatment in the step C into a sintering furnace, introducing mixed gas of nitrogen and air, controlling the oxygen partial pressure in the furnace to be 8-15 ppm, and sintering at 1075-1083 ℃ to recrystallize the surface of the copper sheet.
In the invention, firstly, removing impurities on the surface of the ceramic copper-clad carrier plate by microetching; and then, the sand blasting process is utilized to change the surface appearance of the copper body, remove impurities and endow the surface of the copper body with certain roughness, and reduce the grain boundary. After different cleaning modes are combined and cleaned, the copper substrate enters a sintering recrystallization stage, surface grains are formed after the surface of the copper substrate is sintered again, and defective products are changed into normal products. In the sintering process, the sintering temperature can not be too high or too low, crystallization is difficult to realize due to too low sintering temperature, and the crystallinity is easily increased and the particle size is increased due to too high sintering temperature, so that the surface of the product is obviously different from the surface of a peripheral product.
Preferably, in the step A, the microetching temperature is 25-30 ℃ and the time is 30-60 s. The microetching time is too short, and the impurity removal effect is poor; the treatment time is too long, and the copper body structure is easily damaged, thereby further causing defects.
Preferably, in the step a, after three times of overflow water washing, appearance inspection is also performed to check whether oxidation points and roller marks exist in the product appearance, whether the appearance color is uniform, and whether other foreign matters remain. If the above condition exists, the microetching is carried out again until the condition disappears.
Preferably, in step B, al is contained in the carborundum suspension 2 O 3 The mass percentage is 20 percent, and the sand blasting distance is 10mm.
Preferably, in step C, the pressure of the pressurized water washing is 1.5 to 2.0kg/cm 2 (ii) a In the ultrasonic immersion cleaning process, the ultrasonic frequency is 26-30 KHz; in the dry plate combination procedure, the drying temperature is 70-80 ℃.
Preferably, in step D, the sintering temperature is 1080 +/-2 ℃, and the more precise the temperature control, the better the recrystallization state.
Preferably, tap water is used for washing before the sand blasting process, and pure water is used for washing after the sand blasting process, so that the support plate is prevented from being damaged by impurities in the water.
The invention has the following beneficial effects:
the method realizes the improvement of poor appearance of the ceramic copper-clad carrier plate after high-temperature sintering through four procedures of micro-etching, sand blasting, water washing and drying and sintering and recrystallization, and firstly removes impurities on the surface of the ceramic copper-clad carrier plate through micro-etching; then, spraying carborundum suspension on the surface of the copper matrix at a high speed by using a sand blasting process, completely removing surface color difference, most pimples and wrinkled skin defects and foreign matters, and changing the surface appearance of the copper matrix; then, the impurities on the surface of the carrier are thoroughly cleaned by combining different washing modes; and finally, strictly controlling the sintering temperature to be 1075-1083 ℃, and re-sintering to form crystal grains, so that the surface of the copper substrate recovers the prior crystal grain structure, and the crystal grains and the roughness of the product are equivalent to those of a normal product.
Through multiple verification and test production, the method can solve the defects of poor surface of the ceramic copper-clad carrier plate after sintering, such as pimples, wrinkles, pinholes, color difference, scratches (bumps), foreign matters and the like, and greatly improve the qualification rate of products.
Drawings
FIG. 1 is a flow chart of the method for improving poor appearance of a ceramic copper-clad carrier after high-temperature sintering according to the invention;
FIG. 2 is a diagram of the surface of a copper sheet before grit blasting, after grit blasting, and after recrystallization, where A is after grinding and B is after recrystallization;
FIG. 3 is a surface micro-topography of a copper matrix after 500 times of crystallization magnification before and after sandblasting.
Detailed Description
The following embodiments are implemented on the premise of the technical scheme of the present invention, and give detailed implementation modes and specific operation procedures, but the protection scope of the present invention is not limited to the following embodiments.
1. Method for improving poor appearance of ceramic copper-clad carrier plate after high-temperature sintering
A. Micro-etching
The mixture of sulfuric acid and sodium persulfate is treated for 30-60 s at 25-30 deg.c and three times of overflow water washing are performed successively. In the micro-etching process, the concentration of the sulfuric acid is 18.4-36.8 g/L, namely 10-20 mL/L concentrated sulfuric acid, and the concentration of the sodium persulfate is 20-40 g/L.
When the micro-etching is carried out, the micro-etching time can be neither too long nor too short, and the removal effect of impurities is not good when the micro-etching time is too short; the treatment time is too long, which easily damages the copper structure and causes further defects.
B. Inspection of
Whether oxidation points and roller marks exist in the appearance of the product or not, whether the apparent color is uniform or not and whether other foreign matters remain or not are checked. If the above condition exists, the microetching is carried out again until the above condition disappears.
C. Sand blasting
By using Al 2 O 3 10-20 percent by mass of carborundum suspension is used as a sand blasting liquid and is sprayed up and down, the sand blasting angle is 90 degrees, and the emery suspension is sprayedThe sand pressure was 2kg/cm 2 The blasting distance is preferably 10mm, and the average thickness of the copper substrate is reduced by 0.5 to 0.8 μm after the blasting treatment.
D. Washing and drying
The method comprises the steps of sequentially carrying out recovery washing, overflow washing, pressurized washing, ultrasonic immersion washing, HF washing, swinging high-pressure washing, pressurized washing, DI washing and dry plate combination for washing and drying, and taking out after cooling.
Wherein the pressure of the pressurized water washing is 1.5-2.0 kg/cm 2 (ii) a In the ultrasonic immersion cleaning process, the ultrasonic frequency is 26-30 KHz; in the dry plate combination procedure, the drying temperature is 70-80 ℃.
Regarding the water for washing, tap water is adopted for washing before the sand blasting process, and pure water is adopted for washing after the sand blasting process, so that the support plate is prevented from being damaged by impurities in water.
E. Sintering recrystallization
And D, placing the product obtained after the treatment in the step C into a sintering furnace, introducing mixed gas of nitrogen and air, controlling the oxygen partial pressure in the furnace to be about 10ppm, and sintering under the conditions of 1075-1083 ℃ (preferably 1080 +/-2 ℃) to recrystallize the surface of the copper sheet.
2. Analysis of results
In the invention, firstly, removing impurities on the surface of the ceramic copper-clad carrier plate by microetching; and then, the sand blasting process is utilized to change the surface appearance of the copper body, remove impurities and endow the surface of the copper body with certain roughness, and reduce the grain boundary. After different cleaning modes are combined and cleaned, the copper substrate enters a sintering and recrystallization stage, surface grains are formed after the copper substrate surface is sintered again, and defective products are changed into normal products. In the sintering process, the sintering temperature can not be too high or too low, crystallization is difficult to realize due to too low sintering temperature, and the crystallinity is easily increased and the particle size is increased due to too high sintering temperature, so that the surface of the product is obviously different from the surface of a peripheral product.
The results of the change in surface roughness of the support before and after blasting are summarized in tables 1 and 2:
TABLE 1 roughness test results before grit blasting
TABLE 2 roughness test results after grit blasting
| Measuring |
1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# | 9# | 10# | max | min | AVG |
| Ra(μm) | 0.865 | 0.859 | 0.822 | 0.751 | 0.892 | 0.736 | 0.755 | 0.826 | 0.849 | 0.724 | 0.892 | 0.724 | 0.808 |
| Rz(μm) | 6.098 | 5.961 | 6.153 | 5.047 | 6.148 | 6.237 | 5.345 | 6.414 | 5.382 | 5.343 | 6.414 | 5.047 | 5.813 |
Comparing the results in tables 1 and 2, it can be seen that, before the blasting treatment: the carrier Ra of 0.725 μm, rz of 4.225 μm, ra of 0.808 μm, rz of 5.813 μm after sand blasting, surface roughness increased.
According to the graph 2, before sand blasting, the surface of the ceramic copper-clad carrier plate has obvious foreign body sensation and is integrally uneven (the graph 2A); after sand blasting treatment, the whole body is smooth and flat and is bright (figure 2B); after sintering and recrystallization, the surface of the copper sheet is not different from that of the surrounding normal copper sheet (figure 2C).
According to fig. 3, after the surface crystallization of the copper substrate is magnified by 500 times, the grain boundary of the ceramic copper-clad carrier plate is obvious before sand blasting (fig. 3A); after the sand blasting treatment, the grain boundaries were flattened and the roughness was improved (fig. 3B).
Through multiple verification and test production, the method can solve the defects of poor surface of the ceramic copper-clad carrier plate after sintering, such as pimples, wrinkles, pinholes, color difference, scratch (bump) damage, foreign matters and the like, and greatly improves the qualification rate of products.
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 (5)
1. A method for improving poor appearance of a ceramic copper-clad carrier plate after high-temperature sintering is characterized by comprising the following steps,
A. micro-etching
Carrying out micro-etching on the ceramic copper-clad carrier plate by adopting a mixed solution of sulfuric acid and sodium persulfate, and carrying out overflow water washing, wherein the concentration of the sulfuric acid is 18.4-36.8 g/L, the concentration of the sodium persulfate is 20-40 g/L, the micro-etching temperature is 25-30 ℃, and the micro-etching time is 30-60 s;
B. sand blasting
By using Al 2 O 3 10 to 20 percent of carborundum suspension is used as a sand blasting liquid, and the carborundum suspension is sprayed up and down, the sand blasting angle is 90 degrees, and the sand blasting pressure is 2kg/cm 2 The sand blasting distance is 8-12 mm, and the average thickness of the copper matrix is reduced by 0.5-0.8 mu m after sand blasting treatment;
C. washing and drying
Sequentially adopting the combination of recovery water washing, overflow water washing, pressurized water washing, ultrasonic immersion washing, HF water washing, swinging high-pressure water washing, pressurized water washing, DI water washing and dry plate for water washing and drying, cooling and taking out,
wherein the pressure of the pressurized water washing is 1.5-2.0 kg/cm 2 (ii) a In the ultrasonic immersion cleaning process, the ultrasonic frequency is 26-30 KHz; in the dry plate combination procedure, the drying temperature is 70-80 ℃;
D. sintering recrystallization
And D, placing the product obtained after the treatment in the step C into a sintering furnace, introducing mixed gas of nitrogen and air, controlling the oxygen partial pressure in the furnace to be 8-15 ppm, sintering at the temperature of 1075-1083 ℃, and recrystallizing the surface of the copper sheet.
2. The method for improving the poor appearance of the ceramic copper-clad carrier plate after high-temperature sintering according to claim 1, wherein the method comprises the following steps:
and B, in the step A, after three times of overflow water washing, performing appearance inspection to check whether oxidation points and roller marks exist in the product appearance, whether the appearance color is uniform and whether other foreign matters remain.
3. The method for improving the poor appearance of the ceramic copper-clad carrier plate after high-temperature sintering in the claim 1 is characterized by comprising the following steps:
wherein, in the step B, al is contained in the carborundum suspension 2 O 3 The mass percentage is 20 percent, and the sand blasting distance is 10mm.
4. The method for improving the appearance defect of the ceramic copper-clad carrier plate after high-temperature sintering according to claim 1, wherein the method comprises the following steps:
wherein, in the step D, the sintering temperature is 1080 +/-2 ℃.
5. The method for improving the poor appearance of the ceramic copper-clad carrier plate after high-temperature sintering according to claim 1, wherein the method comprises the following steps:
wherein, tap water is adopted for washing before the sand blasting process, and pure water is adopted for washing after the sand blasting process.
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