CN115107324A - Method for increasing DCB copper thickness - Google Patents
Method for increasing DCB copper thickness Download PDFInfo
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- CN115107324A CN115107324A CN202210845532.XA CN202210845532A CN115107324A CN 115107324 A CN115107324 A CN 115107324A CN 202210845532 A CN202210845532 A CN 202210845532A CN 115107324 A CN115107324 A CN 115107324A
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- 239000010949 copper Substances 0.000 title claims abstract description 177
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 176
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000000919 ceramic Substances 0.000 claims abstract description 80
- 239000000758 substrate Substances 0.000 claims abstract description 56
- 230000003647 oxidation Effects 0.000 claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 21
- 238000005245 sintering Methods 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 116
- 229910052757 nitrogen Inorganic materials 0.000 claims description 51
- 238000000137 annealing Methods 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 abstract description 8
- 230000001590 oxidative effect Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract 1
- 230000003245 working effect Effects 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 6
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000010587 phase diagram Methods 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/10—Interconnection of layers at least one layer having inter-reactive properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/041—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B37/00—Joining burned ceramic articles with other burned ceramic articles or other articles by heating
- C04B37/02—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles
- C04B37/021—Joining burned ceramic articles with other burned ceramic articles or other articles by heating with metallic articles in a direct manner, e.g. direct copper bonding [DCB]
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/10—Oxidising
Abstract
The invention provides a method for increasing the thickness of DCB copper, which designs a plurality of thickness combination modes according to the thickness of DCB copper sheets required by a copper-clad ceramic substrate, preparing copper sheets with corresponding thickness according to a thickness combination mode, carrying out dry thermal oxidation pretreatment on the copper sheets, oxidizing the bottom of the copper sheet to form a copper sheet with a single-side oxidized, stacking and sintering the copper sheet with the single-side oxidized and the ceramic sheet to obtain a thickened copper sheet with the thickness of 0.4mm, 0.45mm, 0.5mm, 0.55mm, 0.6mm and the like, through calculating the technological process that decomposes, copper sheet preoxidation, copper sheet ceramic chip pile up the sintering with required bodiness copper sheet, the bodiness DCB product precision that obtains is high, and the working property is unanimous with the thick copper clad ceramic substrate of customization copper, has avoided producing the condition that specific thick copper product cost is too high and leads to the loss, has simply effectively solved the supply of material demand problem of unconventional thick copper product simultaneously.
Description
Technical Field
The invention relates to the technical field of copper-clad ceramic substrate preparation, in particular to a method for increasing the copper thickness of DCB.
Background
The copper-clad ceramic substrate is mainly used as a lining board of a semiconductor chip, when the copper-clad ceramic substrate is prepared, a copper sheet and a ceramic sheet need to be connected with each other through welding flux sintering, in the actual production process, a copper coil with a specified thickness is directly purchased by a conventional process to be cut, oxidized and sintered, but the copper sheet with certain thickness is often insufficient due to low demand of the copper-clad ceramic substrate with specific copper thickness or the difficulty of the process of a supplier.
Meanwhile, in the conventional copper-clad ceramic substrate sintered and connected by using the solder, the final thickness accuracy of the copper-clad ceramic substrate is not high due to the fact that the solder cannot be used accurately, so that the requirement of a customer cannot be met, if the copper-clad ceramic substrate with specific copper thickness is produced in a large scale, resources are surplus, and if the copper-clad ceramic substrate is produced in a small scale, the cost is too high, so that a method for increasing the DCB copper thickness, which is low in cost, easy to operate and easy to obtain, is urgently needed.
Disclosure of Invention
The present invention is directed to a method for increasing the copper thickness of DCB, so as to solve the above-mentioned problems in the background art.
In order to solve the technical problems, the invention provides the following technical scheme:
a method for increasing the copper thickness of DCB is characterized in that: the method comprises the following steps:
s1) designing a plurality of thickness combination modes according to the thickness of the DCB copper sheet required by the copper-clad ceramic substrate, and preparing copper sheets with corresponding thicknesses according to the thickness combination modes;
s2) taking the copper sheets prepared in the step S1), and respectively carrying out bottom surface thermal oxidation pretreatment to obtain single-surface oxidized copper sheets;
s3) taking the copper sheets processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet is in contact with the unoxidized surface of the lower copper sheet during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic sheet for stacking, and the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic sheet and then sintering to obtain the product copper-clad ceramic substrate.
Further, when the thickness of the DCB copper sheet is 0.4mm, the thickness combination mode is that two 0.2mm copper sheets are stacked and compounded;
when the thickness of the DCB copper sheet is 0.45mm, the thickness combination mode is that the 0.2mm copper sheet and the 0.25mm copper sheet are stacked and compounded;
when the thickness of the DCB copper sheet is 0.5mm, the thickness combination mode is that the 0.2mm copper sheet and the 0.3mm copper sheet are combined in a stacking mode or two 0.25mm copper sheets are combined in a stacking mode;
when the thickness of the DCB copper sheet is 0.55mm, the thickness combination mode is that the 0.25mm copper sheet and the 0.25mm copper sheet are stacked and compounded;
when the thickness of the DCB copper sheet is 0.6mm, the thickness combination mode is that two 0.3mm copper sheets are stacked and compounded.
Further, 11 temperature zones are arranged in the annealing furnace, wherein the temperature of the temperature zone 1 is 510 ℃, the temperature of the temperature zone 2 is 690 ℃, the temperature of the temperature zone 3 is 790 ℃, the temperature of the temperature zone 4 is 800 ℃, the temperature of the temperature zone 5 is 800 ℃, the temperature of the temperature zone 6 is 800 ℃, the temperature of the temperature zone 7 is 800 ℃, the temperature of the temperature zone 8 is 800 ℃, the temperature of the temperature zone 9 is 720 ℃, the temperature of the temperature zone 10 is 660 ℃, and the temperature of the temperature zone 11 is 640 ℃.
Further, in the step (2), during bottom surface thermal oxidation pretreatment, the nitrogen flow rate of the inlet area is 55-65L/min, the nitrogen flow rate above the temperature area 1 is 8-12L/min, the nitrogen flow rate above the temperature area 2 is 8-12L/min, the nitrogen flow rate above the temperature area 3 is 3-7L/min, the nitrogen flow rate of the temperature area 4, the temperature area 5, the temperature area 6, the temperature area 7, the temperature area 8, the temperature area 9, the temperature area 10, the temperature area 11 is 60-100L/min, the nitrogen flow rate of the cooling area is 25-45L/min, and the nitrogen flow rate of the outlet area is 50-60L/min.
Further, in the step (2), the copper sheet is moved into an annealing furnace for bottom surface thermal oxidation pretreatment, and the bottom surface is oxidized in a mixed atmosphere of nitrogen and oxygen, wherein the oxidation temperature is 500-800 ℃.
Further, during thermal oxidation of the bottom surface, the oxygen concentration is 1200-1300 ppm, wherein the nitrogen flow rate below the temperature zone 1 is 33-37L/min, the nitrogen flow rate below the temperature zone 2 is 33-37L/min, and the nitrogen flow rate below the temperature zone 3 is 28-32L/min.
Further, the air exhaust flow of the annealing furnace is 4-6L/min.
Further, in the step (3), the sintering temperature is 1065-1083 ℃, and the sintering time is 9-13 min.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, a plurality of thickness combination modes are designed according to the thickness of a DCB copper sheet required by a copper-clad ceramic substrate, copper sheets with corresponding thicknesses are prepared according to the thickness combination modes, then the copper sheets are subjected to preoxidation treatment, then the copper-clad ceramic substrate and a ceramic chip which are subjected to preoxidation are stacked and sintered, a copper-oxygen eutectic liquid phase can be generated on a copper surface oxidation layer under the mixed atmosphere environment of 1065-1083 ℃ and nitrogen and oxygen, a liquid phase is formed between copper and copper to sinter two layers of copper together, meanwhile, the copper-oxygen eutectic liquid phase at the bottom of the copper sheets is gradually infiltrated, the surface of the ceramic chip is integrated and reacts with the surface of the ceramic chip to form a dielectric layer, the copper sheets and the ceramic chip are firmly bonded along with the subsequent temperature which is gradually reduced, wherein the chemical reaction process generated in the stacking and sintering process is as follows:
Cu 2 O+Al 2 O 3 →2CuAlO 2
according to the invention, dry thermal oxidation sintering is adopted, the bottom surface of the copper sheet is subjected to oxidation sintering, the copper sheet with a single surface oxidized is obtained, the weight of an oxidation layer of the copper sheet is 8-12 mg, the thickness of the oxidation layer is only 1-1.5 mu m, the obtained thickened copper-clad ceramic substrate has high precision, and the peeling strength and the cold and hot circulation effect have no obvious difference with those of a customized copper-clad ceramic substrate.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of a copper sheet and a ceramic sheet stacking manner during a stacking and sintering process;
FIG. 2 is a copper-oxygen eutectic phase diagram during the stack sintering process;
FIG. 3 is a ultrasonic scanning chart of a copper-clad ceramic substrate of a comparative example before a cooling-heating cycle;
FIG. 4 is a diagram showing the ultrasonic scan of the copper-clad ceramic substrate of example 1 before the cooling and heating cycles;
FIG. 5 is a ultrasonogram obtained after 30 cycles of cooling and heating for a comparative example copper-clad ceramic substrate;
FIG. 6 is a ultrasonographic chart after 30 cycles of a cooling-heating cycle of the copper-clad ceramic substrate according to example 1;
FIG. 7 is a ultrasonic scan of a copper-clad ceramic substrate of a comparative example after 40 cycles of cooling and heating;
FIG. 8 is a diagram showing the ultrasonic scan of the copper-clad ceramic substrate of example 1 after 40 cycles of cooling and heating;
in fig. 1, copper sheet; 2. a tile.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
Comparative example (0.4mm positive) in the detailed descriptionCopper clad ceramic substrates of normal copper thickness) are derived from copper clad ceramic substrates produced by Ferrotec; examples 0.2mm, 0.25mm, 0.3mm pieces of DCB copper were purchased from Aurubis at 99.99% oxygen free copper; the tiles were 96% Al from Ceramtec 2 O 3 。
Example 1: preparing a 0.4 thickened DCB copper-clad ceramic substrate;
s1) selecting two 0.2mm copper sheets for later use according to the 0.4mm DCB copper sheet required by the copper-clad ceramic substrate;
s2) taking the copper sheet prepared in the step S1), transferring the copper sheet into an annealing furnace, respectively carrying out bottom surface thermal oxidation pretreatment, and oxidizing in a nitrogen and oxygen mixed atmosphere to obtain a single-surface oxidized copper sheet, wherein the oxygen concentration is 1200ppm, the temperature of a temperature zone 1 in the annealing furnace is 510 ℃, the flow rate of nitrogen at the upper part is 8L/min, and the flow rate of nitrogen at the lower part is 33L/min; the temperature of the temperature zone 2 is 690 ℃, the flow rate of nitrogen gas at the upper part is 8L/min, and the flow rate of nitrogen gas at the lower part is 33L/min; the temperature of the temperature zone 3 is 790 ℃, the flow rate of nitrogen at the upper part is 3L/min, and the flow rate of nitrogen at the lower part is 28L/min;
s3) taking the copper sheets 1 processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet 1 is in contact with the unoxidized surface of the lower copper sheet 1 during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip 2 for stacking, the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip 2, and sintering at 1065 ℃ for 9min to obtain the copper-clad ceramic substrate.
Example 2: preparing a 0.45 thickened DCB copper-clad ceramic substrate;
s1) selecting a 0.2mm copper sheet and a 0.25mm copper sheet for standby according to the DCB copper sheet with the thickness of 0.45mm required by the copper-clad ceramic substrate;
s2) taking the copper sheet prepared in the step S1), transferring the copper sheet into an annealing furnace, respectively carrying out bottom surface thermal oxidation pretreatment, and oxidizing in a nitrogen and oxygen mixed atmosphere to obtain a single-surface oxidized copper sheet, wherein the oxygen concentration is 1200ppm, the temperature of a temperature zone 1 in the annealing furnace is 510 ℃, the flow rate of nitrogen at the upper part is 8L/min, and the flow rate of nitrogen at the lower part is 33L/min; the temperature of the temperature zone 2 is 690 ℃, the flow rate of nitrogen gas at the upper part is 8L/min, and the flow rate of nitrogen gas at the lower part is 33L/min; the temperature of the temperature zone 3 is 790 ℃, the flow rate of nitrogen at the upper part is 3L/min, and the flow rate of nitrogen at the lower part is 28L/min;
s3) taking the copper sheets 1 processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet 1 is in contact with the unoxidized surface of the lower copper sheet 1 during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip 2 for stacking, the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip 2, and sintering at 1068 ℃ for 10min to obtain the copper-clad ceramic substrate.
Example 3: preparing a 0.5 thickened DCB copper-clad ceramic substrate (0.2mm +0.3 mm);
s1) selecting one 0.2mm copper sheet and one 0.3mm copper sheet for later use according to the DCB copper sheet with the thickness of 0.5mm required by the copper-clad ceramic substrate;
s2) taking the copper sheet prepared in the step S1), transferring the copper sheet into an annealing furnace, respectively carrying out bottom surface thermal oxidation pretreatment, and oxidizing in a nitrogen and oxygen mixed atmosphere to obtain a single-surface oxidized copper sheet, wherein the oxygen concentration is 1250ppm, the temperature of a temperature zone 1 in the annealing furnace is 510 ℃, the flow of nitrogen above is 10L/min, and the flow of nitrogen below is 35L/min; the temperature of the temperature zone 2 is 690 ℃, the flow rate of nitrogen gas at the upper part is 10L/min, and the flow rate of nitrogen gas at the lower part is 35L/min; the temperature of the temperature zone 3 is 790 ℃, the flow rate of nitrogen gas at the upper part is 5L/min, and the flow rate of nitrogen gas at the lower part is 30L/min;
s3) taking the copper sheets 1 processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet 1 is in contact with the unoxidized surface of the lower copper sheet 1 during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip 2 for stacking, the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip 2, and sintering at 1065 ℃ for 10min to obtain the copper-clad ceramic substrate.
Example 4: preparing a 0.5 thickened DCB copper clad ceramic substrate (0.25mm +0.25 mm);
s1) selecting two 0.25mm copper sheets for later use according to the 0.5mm DCB copper sheet required by the copper-clad ceramic substrate;
s2) taking the copper sheet prepared in the step S1), transferring the copper sheet into an annealing furnace, respectively carrying out bottom surface thermal oxidation pretreatment, and oxidizing in a nitrogen and oxygen mixed atmosphere to obtain a single-surface oxidized copper sheet, wherein the oxygen concentration is 1250ppm, the temperature of a temperature zone 1 in the annealing furnace is 510 ℃, the flow of nitrogen above is 10L/min, and the flow of nitrogen below is 35L/min; the temperature of the temperature zone 2 is 690 ℃, the flow rate of nitrogen gas at the upper part is 10L/min, and the flow rate of nitrogen gas at the lower part is 35L/min; the temperature of the temperature zone 3 is 790 ℃, the flow rate of nitrogen gas at the upper part is 5L/min, and the flow rate of nitrogen gas at the lower part is 30L/min;
s3) taking the copper sheet 1 processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet 1 is in contact with the unoxidized surface of the lower copper sheet 1 during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip 2 for stacking, the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip 2, and sintering at 1070 ℃ for 11min to obtain the copper-clad ceramic substrate.
Example 5: preparing a DCB copper-clad ceramic substrate with the thickness of 0.55;
s1) selecting one copper sheet with the thickness of 0.25mm and one copper sheet with the thickness of 0.3mm for standby according to the DCB copper sheets with the thickness of 0.55mm required by the copper-clad ceramic substrate;
s2) taking the copper sheet prepared in the step S1), transferring the copper sheet into an annealing furnace, respectively carrying out bottom surface thermal oxidation pretreatment, and oxidizing in a nitrogen and oxygen mixed atmosphere to obtain a single-surface oxidized copper sheet, wherein the oxygen concentration is 1300ppm, the temperature of a temperature zone 1 in the annealing furnace is 510 ℃, the flow rate of nitrogen at the upper part is 12L/min, and the flow rate of nitrogen at the lower part is 37L/min; the temperature of the temperature zone 2 is 690 ℃, the flow rate of nitrogen at the upper part is 12L/min, and the flow rate of nitrogen at the lower part is 37L/min; the temperature of the temperature zone 3 is 790 ℃, the flow rate of nitrogen gas above is 7L/min, and the flow rate of nitrogen gas below is 32L/min;
s3) taking the copper sheets 1 processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet 1 is in contact with the unoxidized surface of the lower copper sheet 1 during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip 2 for stacking, the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip 2, and sintering at 1080 ℃ for 11min to obtain the copper-clad ceramic substrate.
Example 6: preparing a DCB copper-clad ceramic substrate with the thickness of 0.55;
s1) selecting two 0.3mm copper sheets for later use according to the 0.6mm DCB copper sheet required by the copper-clad ceramic substrate;
s2) taking the copper sheet prepared in the step S1), transferring the copper sheet into an annealing furnace, respectively carrying out bottom surface thermal oxidation pretreatment, and oxidizing in a nitrogen and oxygen mixed atmosphere to obtain a single-surface oxidized copper sheet, wherein the oxygen concentration is 1300ppm, the temperature of a temperature zone 1 in the annealing furnace is 510 ℃, the flow rate of nitrogen at the upper part is 12L/min, and the flow rate of nitrogen at the lower part is 37L/min; the temperature of the temperature zone 2 is 690 ℃, the flow rate of nitrogen at the upper part is 12L/min, and the flow rate of nitrogen at the lower part is 37L/min; the temperature of the temperature zone 3 is 790 ℃, the flow rate of nitrogen at the upper part is 7L/min, and the flow rate of nitrogen at the lower part is 32L/min;
s3) taking the copper sheet 1 processed in the step S2), stacking, wherein the oxidized surface of the upper copper sheet 1 is in contact with the unoxidized surface of the lower copper sheet 1 during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip 2 for stacking, the oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip 2, and sintering at 1083 ℃ for 13min to obtain the copper-clad ceramic substrate.
Comparative example: a DCB copper clad ceramic substrate of 0.4mm normal copper thickness was purchased as a comparative example.
Experiment of
(1) Taking the copper-clad ceramic substrate of the comparative example and the copper-clad ceramic substrate in the example 1, testing the peel strength, wherein the experimental values are shown in the following table 1:
table 1: peel strength test data
As shown in table 1, it can be seen that the peel strength of the thickened copper-clad ceramic substrate prepared by the thickening method of the present invention is not much different from that of the custom copper-thick copper-clad ceramic substrate purchased directly;
(2) two sheets of the comparative copper-clad ceramic substrate and two sheets of the thickened copper-clad ceramic substrate in the example 1 are taken for a cold-hot circulation test, and the test conditions are as follows: the high temperature and the low temperature stay for 30 minutes respectively to form a cycle, the switching time is less than 30 seconds, the cold-hot cycle is carried out for 40 times at the temperature of minus 55 ℃ to 150 ℃, and ultrasonic scanning charts are shown in figures 3 to 8, so that the peeling strength of the thickened copper-clad ceramic substrate prepared by the thickening method is not greatly different from the cold-hot cycle performance of a directly purchased customized copper-thick copper-clad ceramic substrate;
and (4) conclusion: according to the preparation method, the obtained thickened copper-clad ceramic substrate is high in accuracy, the peeling strength and the cold and hot circulation effect are not obviously different from those of a customized copper-thick copper-clad ceramic substrate which is directly purchased, obviously, the method for increasing the DCB copper thickness is simpler and more effective than the method for customizing a copper-thick product, and through the method for increasing the DCB copper thickness, the thickness accuracy of the copper-clad ceramic substrate is improved, and the production efficiency of the product is improved.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for increasing the copper thickness of DCB is characterized in that: the method specifically comprises the following steps:
s1) designing a plurality of thickness combination modes according to the thickness of the DCB copper sheet required by the copper-clad ceramic substrate, and preparing copper sheets with corresponding thicknesses according to the thickness combination modes;
s2) taking the copper sheet prepared in the step S1), and respectively carrying out bottom surface thermal oxidation pretreatment to obtain a copper sheet (1) with one surface oxidized;
s3) taking the copper sheet (1) processed in the step S2), stacking, wherein an oxidized surface of the upper copper sheet (1) is in contact with an unoxidized surface of the lower copper sheet (1) during stacking to form a DCB copper sheet, then placing the DCB copper sheet above the ceramic chip (2) for stacking, and an oxidized surface of the DCB copper sheet is in contact with the upper surface of the ceramic chip (2), and then sintering to obtain the product copper-clad ceramic substrate.
2. The method of claim 1, wherein the copper thickness of the DCB is increased by: when the thickness of the DCB copper sheet is 0.4mm, the thickness combination mode is that two 0.2mm copper sheets are stacked and compounded;
when the thickness of the DCB copper sheet is 0.45mm, the thickness combination mode is that the 0.2mm copper sheet and the 0.25mm copper sheet are stacked and compounded;
when the thickness of the DCB copper sheet is 0.5mm, the thickness combination mode is that the 0.2mm copper sheet and the 0.3mm copper sheet are combined in a stacking mode or two 0.25mm copper sheets are combined in a stacking mode;
when the thickness of the DCB copper sheet is 0.55mm, the thickness combination mode is that the 0.25mm copper sheet and the 0.25mm copper sheet are stacked and compounded;
when the thickness of the DCB copper sheet is 0.6mm, the thickness combination mode is that two 0.3mm copper sheets are stacked and compounded.
3. The method of claim 1, wherein the copper thickness of the DCB is increased by: the annealing furnace is provided with 11 temperature zones, wherein the temperature of a temperature zone 1 is 510 ℃, the temperature of a temperature zone 2 is 690 ℃, the temperature of a temperature zone 3 is 790 ℃, the temperature of a temperature zone 4 is 800 ℃, the temperature of a temperature zone 5 is 800 ℃, the temperature of a temperature zone 6 is 800 ℃, the temperature of a temperature zone 7 is 800 ℃, the temperature of a temperature zone 8 is 800 ℃, the temperature of a temperature zone 9 is 720 ℃, the temperature of a temperature zone 10 is 660 ℃, and the temperature of a temperature zone 11 is 640 ℃.
4. The method of claim 1, wherein the copper thickness of the DCB is increased by: in the step (2), during thermal oxidation pretreatment of the bottom surface, the nitrogen flow rate of an inlet area is 55-65L/min, the nitrogen flow rate above a temperature area 1 is 8-12L/min, the nitrogen flow rate above a temperature area 2 is 8-12L/min, the nitrogen flow rate above a temperature area 3 is 3-7L/min, the nitrogen flow rate of a temperature area 4, a temperature area 5, a temperature area 6, a temperature area 7, a temperature area 8, a temperature area 9, a temperature area 10 and a temperature area 11 is 60-100L/min, the nitrogen flow rate of a cooling area is 25-45L/min, and the nitrogen flow rate of an outlet area is 50-60L/min.
5. The method of claim 1, wherein the copper layer comprises: in the step (2), the copper sheet is moved into an annealing furnace for bottom surface thermal oxidation pretreatment, and the bottom surface is oxidized in a mixed atmosphere of nitrogen and oxygen, wherein the oxidation temperature is 500-800 ℃.
6. The method of claim 1, wherein the copper thickness of the DCB is increased by: during thermal oxidation of the bottom surface, the oxygen concentration is 1200-1300 ppm, wherein the nitrogen flow below the temperature zone 1 is 33-37L/min, the nitrogen flow below the temperature zone 2 is 33-37L/min, and the nitrogen flow below the temperature zone 3 is 28-32L/min.
7. The method of claim 1, wherein the copper thickness of the DCB is increased by: the air exhaust flow of the annealing furnace is 4-6L/min.
8. The method of claim 1, wherein the copper thickness of the DCB is increased by: in the step (3), the sintering temperature is 1065-1083 ℃, and the sintering time is 9-13 min.
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| CN116001387A (en) * | 2022-12-31 | 2023-04-25 | 江苏富乐华半导体科技股份有限公司 | Method for increasing copper thickness by DCB |
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