CN116705591A - Ceramic chip cleaning process and cleaning fluid for copper-clad ceramic substrate production - Google Patents
Ceramic chip cleaning process and cleaning fluid for copper-clad ceramic substrate production Download PDFInfo
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- CN116705591A CN116705591A CN202310682687.0A CN202310682687A CN116705591A CN 116705591 A CN116705591 A CN 116705591A CN 202310682687 A CN202310682687 A CN 202310682687A CN 116705591 A CN116705591 A CN 116705591A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 149
- 238000004140 cleaning Methods 0.000 title claims abstract description 59
- 239000000758 substrate Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000012530 fluid Substances 0.000 title abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000007788 roughening Methods 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000005406 washing Methods 0.000 claims description 26
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- 239000012298 atmosphere Substances 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 7
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 7
- 238000005238 degreasing Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 23
- 239000011889 copper foil Substances 0.000 abstract description 12
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 12
- 239000010949 copper Substances 0.000 description 11
- 229910052802 copper Inorganic materials 0.000 description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 10
- 239000007864 aqueous solution Substances 0.000 description 9
- 238000005452 bending Methods 0.000 description 8
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 7
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 7
- 229940112669 cuprous oxide Drugs 0.000 description 7
- 230000007704 transition Effects 0.000 description 7
- 230000035882 stress Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910002480 Cu-O Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The application discloses a ceramic chip cleaning process and cleaning fluid for copper-clad ceramic substrate production, and relates to the technical field of copper-clad ceramic substrate processing. The cleaning process comprises the following steps: s1: removing oil from the ceramic chip and cleaning; s2: the deoiling ceramic chip is placed in a roughening solution for pretreatment; s3: pre-treating ceramic chips for high-temperature oxidation; s4: the ceramic tile is washed by cleaning liquid, water, alkali liquor and water in turn, and the ceramic tile is obtained by circulating 10-30 times in turn. The ceramic chip cleaned by the method is applied to the production of the copper-clad ceramic substrate, and the obtained copper-clad ceramic substrate has the advantages of high bonding strength between copper foil and ceramic chip, high temperature cycle reliability and strong thermal fatigue resistance under 300 ℃ high temperature environment.
Description
Technical Field
The application relates to the technical field of copper-clad ceramic substrate processing, in particular to a ceramic chip cleaning process and cleaning liquid for copper-clad ceramic substrate production.
Background
With the increasing operating voltage and current of power devices and the continuous shrinking of chip size, the power density of chips has increased dramatically, which creates a higher challenge for the reliability of heat dissipating packages for chips. Conventional flexible substrates or metal substrates have failed to meet the requirements of high power and high heat dissipation of semiconductor modules, and ceramic substrates have the advantages of excellent thermal conductivity, heat resistance, insulation and low thermal expansion coefficient. The copper-clad ceramic substrate prepared by directly sintering the copper foil on the ceramic surface has the characteristics of excellent thermal cycling performance, stable shape, good rigidity, high thermal conductivity and high reliability, and the copper-clad surface can be etched with various patterns, and is a pollution-free and pollution-free green product with quite wide use temperature.
Copper-clad ceramic substrates directly apply copper to the ceramic surface using an oxygen-containing eutectic solution of copper, with a transition layer between the copper and the ceramic, but since aluminum nitride ceramics have little wettability to copper, pretreatment of the ceramic surface is required. In the prior art, the interface of the substrate is bonded by virtue of the eutectic layer, so that the interface layer is hollow, when the interface hole bears a large current, larger thermal stress appears around the interface hole, and ceramics comprise aluminum oxide, aluminum nitride, silicon nitride and the like. At present, a layer of alumina is formed on the surface of an aluminum nitride substrate by an oxidation method in air, and is combined with metal copper through the transition layer, however, the difference of thermal expansion coefficients of the alumina thin layer and the aluminum nitride quality test is large, internal stress is easy to generate in the oxidation and the bonding process, so that the strength is reduced, and in addition, the physical and chemical properties of the surface of the substrate, such as grain size and grain boundary phase, can influence the bonding strength.
Disclosure of Invention
The application aims to provide a ceramic chip cleaning process and cleaning fluid for copper-clad ceramic substrate production, which solve the following technical problems:
when the existing copper-clad ceramic substrate bears a large current, the interface between the ceramic and the metal is cracked and failed due to large thermal expansion difference.
The aim of the application can be achieved by the following technical scheme:
the ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: the ceramic chip is degreased and cleaned to obtain degreased ceramic chip;
s2: soaking, washing and drying the deoiling ceramic chip in coarsening liquid to obtain a pretreated ceramic chip;
s3: oxidizing the pretreated ceramic chip for 2-4 hours at 1000-1100 ℃ in a mixed atmosphere of nitrogen and oxygen to obtain an oxidized ceramic chip;
s4: placing the oxidized ceramic chip in a cleaning solution for standing and washing, placing the oxidized ceramic chip in an alkali solution for standing and washing to obtain a reprocessed ceramic chip;
s5: and (5) circulating the step in the step S4 for 10-30 times to obtain the ceramic tile.
As a further aspect of the application: the nitrogen and oxygen mixed atmosphere is obtained by mixing nitrogen and oxygen in a volume ratio of 1:4-9.
As a further aspect of the application: the ceramic chip is an aluminum nitride ceramic chip.
As a further aspect of the application: the specific steps of degreasing and cleaning are as follows: placing the ceramic tile in absolute ethyl alcohol, ultrasonically cleaning for 10-30min, taking out, washing with water, and drying.
As a further aspect of the application: the specific steps of soaking in the coarsening liquid in S2 are as follows: heating to 60-80deg.C, and soaking for 10-30min.
As a further aspect of the application: the roughening solution is 30-60wt% sodium hydroxide water solution.
As a further aspect of the application: s4, placing the oxidized ceramic chip in a cleaning solution for standing specifically: heating to 60-70deg.C, and standing for 0.5-2min.
As a further aspect of the application: s4, placing the reprocessed porcelain piece in alkali liquor for standing specifically: heating to 60-70deg.C, and standing for 0.1-1min.
As a further aspect of the application: the alkali liquor in S4 is 1-2mol/L sodium hydroxide aqueous solution.
A cleaning solution for use in any one of the cleaning processes described above.
As a further aspect of the application: the cleaning liquid is prepared by mixing copper sulfate, distilled water and sodium thiosulfate.
As a further aspect of the application: the copper sulfate: distilled water: the mass ratio of the sodium thiosulfate is 1-5:100-200:5-20.
The application has the beneficial effects that:
(1) According to the application, absolute ethyl alcohol is used for degreasing and cleaning, then sodium hydroxide solution is used for roughening the surface of the aluminum nitride ceramic chip, a glass phase at the grain boundary of the aluminum nitride is corroded, the corrosion is expanded to the inside of crystal grains, a plurality of incomplete crystal grain structures are generated after the corrosion, an obvious surface roughening effect is obtained, and the binding force of a plating layer is improved, so that the pretreated ceramic chip is obtained; and then placing the pretreated ceramic chip in a mixed atmosphere of nitrogen and oxygen for high-temperature oxidation to obtain an oxidized ceramic chip, heating and oxidizing the aluminum nitride ceramic in the air to generate a dense aluminum oxide layer with a certain thickness on the surface of the oxidized ceramic chip, and effectively combining the aluminum oxide layer with the surface of the aluminum nitride ceramic substrate to form a dense aluminum oxide transition layer. The method comprises the steps of cleaning the oxidized ceramic chip by using a cleaning liquid, and depositing a cuprous oxide film on the surface of aluminum oxide to obtain the ceramic chip.
The surface of the cleaned ceramic chip is coated with a layer of cuprous oxide film, then the pure copper foil is closely contacted with the surface of the ceramic chip, and is subjected to bonding in a nitrogen atmosphere at 1070 ℃, the cuprous oxide on the transition layer is uniformly distributed and closely distributed, and the pure copper foil is convenient to be used in nitrogenWetting the surface of the aluminum-melting ceramic chip; gao Wenfu in-process cuprous oxide and aluminum oxide to CuAlO 2 And copper and cuprous oxide are generated by the Cu-O eutectic liquid, the bonding strength between the pure copper foil and the ceramic chip is enhanced, the cuprous oxide on the surface of the pure copper foil is similar to the cuprous oxide on the surface of aluminum nitride, the wetting is convenient, the pure copper foil is conveniently coated on aluminum oxide, and the pure copper foil and the ceramic chip are further metallized at high temperature, when the temperature is reduced, the copper liquid phase starts to be solidified from the copper side due to higher heat conductivity of the copper, the solidification front is continuously pushed to the oxidation layer side, an interface reaction product is formed, and a firm bonding surface is formed along with the further reduction of the temperature.
(2) According to the application, the aluminum nitride ceramic chip and the aluminum oxide form tensile stress between the oxide layer and the aluminum nitride because of unmatched thermal expansion coefficients, the thermal expansion coefficient of the pure copper foil is higher than that of the aluminum oxide transition layer, after the aluminum oxide transition layer is bonded with copper, the compressive stress is caused in the aluminum oxide transition layer, and the compressive stress and the tensile stress compensate and offset each other, so that the strength of the ceramic chip and the oxide layer is enhanced, positive effects are played on bonding strength, and adverse effects of the tensile stress are correspondingly weakened.
Drawings
The application is further described below with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of the test of the bond strength of the detection interface of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
The preparation method of the cleaning liquid comprises the following steps:
10g of copper sulfate, 1000mL of distilled water and 50g of sodium thiosulfate were mixed.
Example 2
The preparation method of the cleaning liquid comprises the following steps:
30g of copper sulfate, 1000mL of distilled water, and 100g of sodium thiosulfate were mixed to prepare a mixture.
Example 3
The preparation method of the cleaning liquid comprises the following steps:
50g of copper sulfate, 1000mL of distilled water, and 200g of sodium thiosulfate were mixed to prepare a mixture.
Example 4
The ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: aluminum nitride ceramics are selected: thermal conductivity 190W/mK, bending strength 450MPa;
s2: placing the aluminum nitride ceramic chip in absolute ethyl alcohol, ultrasonically cleaning for 20min, taking out, and then washing and drying to obtain an oil-removed ceramic chip;
s3: placing the deoiled ceramic tile in a 50wt% sodium hydroxide aqueous solution, heating to 70 ℃, soaking for 20min, washing with water, and drying to obtain a pretreated ceramic tile;
s4: oxidizing the pretreated ceramic chip for 3 hours at 1100 ℃ in a mixed atmosphere of nitrogen and oxygen with the volume ratio of 1:4 to obtain oxidized ceramic chip;
s5: placing the oxidized ceramic chip in the cleaning solution prepared in the embodiment 1, heating to 70 ℃, standing for 0.5min, washing, placing in 1mol/L sodium hydroxide aqueous solution, heating to 70 ℃, standing for 0.5min, washing, and obtaining the reprocessed ceramic chip;
s6: and (5) circulating the step in the step S5 for 30 times to obtain the ceramic tile.
Example 5
The ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: aluminum nitride ceramics are selected: thermal conductivity 190W/mK, bending strength 450MPa;
s2: placing the aluminum nitride ceramic chip in absolute ethyl alcohol, ultrasonically cleaning for 20min, taking out, and then washing and drying to obtain an oil-removed ceramic chip;
s3: placing the deoiled ceramic tile in a 50wt% sodium hydroxide aqueous solution, heating to 70 ℃, soaking for 20min, washing with water, and drying to obtain a pretreated ceramic tile;
s4: oxidizing the pretreated ceramic chip for 3 hours at 1100 ℃ in a mixed atmosphere of nitrogen and oxygen with the volume ratio of 1:4 to obtain oxidized ceramic chip;
s5: placing the oxidized ceramic chip in the cleaning solution prepared in the embodiment 2, heating to 70 ℃, standing for 0.5min, washing, placing in 1mol/L sodium hydroxide aqueous solution, heating to 70 ℃, standing for 0.5min, washing, and obtaining the reprocessed ceramic chip;
s6: and (5) circulating the step in the step S5 for 30 times to obtain the ceramic tile.
Example 6
The ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: aluminum nitride ceramics are selected: thermal conductivity 190W/mK, bending strength 450MPa;
s2: placing the aluminum nitride ceramic chip in absolute ethyl alcohol, ultrasonically cleaning for 20min, taking out, and then washing and drying to obtain an oil-removed ceramic chip;
s3: placing the deoiled ceramic tile in a 50wt% sodium hydroxide aqueous solution, heating to 70 ℃, soaking for 20min, washing with water, and drying to obtain a pretreated ceramic tile;
s4: oxidizing the pretreated ceramic chip for 3 hours at 1100 ℃ in a mixed atmosphere of nitrogen and oxygen with the volume ratio of 1:4 to obtain oxidized ceramic chip;
s5: placing the oxidized ceramic chip in the cleaning solution prepared in the embodiment 3, heating to 70 ℃, standing for 0.5min, washing, placing in 1mol/L sodium hydroxide aqueous solution, heating to 70 ℃, standing for 0.5min, washing, and obtaining the reprocessed ceramic chip;
s6: and (5) circulating the step in the step S5 for 30 times to obtain the ceramic tile.
Example 7
The preparation method of the copper-clad ceramic substrate comprises the following steps:
(1) Pure copper foil is selected: copper content 99.9%, oxygen content less than 0.03%;
(2) And (3) bonding pure copper foil with the surface of the ceramic chip prepared in the embodiment 4, and heating to 1070 ℃ in an oxidizing atmosphere to obtain the copper-clad ceramic substrate through bonding.
Example 8
In this example, compared with example 7, only the tile prepared in example 4 was replaced with the tile prepared in example 5, and the remaining steps were identical to those of example 7.
Example 9
In this example, compared with example 7, only the tile prepared in example 4 was replaced with the tile prepared in example 6, and the remaining steps were identical to those of example 7.
Comparative example 1
The ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: aluminum nitride ceramics are selected: thermal conductivity 190W/mK, bending strength 450MPa;
s2: placing the aluminum nitride ceramic chip in absolute ethyl alcohol, ultrasonically cleaning for 20min, taking out, and then washing and drying to obtain an oil-removed ceramic chip;
s3: placing the deoiled ceramic tile in a 50wt% sodium hydroxide aqueous solution, heating to 70 ℃, soaking for 20min, washing with water, and drying to obtain a pretreated ceramic tile;
s4: oxidizing the pretreated ceramic tile for 3 hours at 1100 ℃ in a mixed atmosphere of nitrogen and oxygen with the volume ratio of 1:4 to obtain the ceramic tile.
Comparative example 2
The ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: aluminum nitride ceramics are selected: thermal conductivity 190W/mK, bending strength 450MPa;
s2: placing the aluminum nitride ceramic chip in absolute ethyl alcohol, ultrasonically cleaning for 20min, taking out, and then washing and drying to obtain an oil-removed ceramic chip;
s3: oxidizing the deoiled ceramic tile for 3 hours at 1100 ℃ in a mixed atmosphere of nitrogen and oxygen with the volume ratio of 1:4 to obtain oxidized ceramic tile;
s4: placing the oxidized ceramic chip in the cleaning solution prepared in the embodiment 1, heating to 70 ℃, standing for 0.5min, washing, placing in 1mol/L sodium hydroxide aqueous solution, heating to 70 ℃, standing for 0.5min, washing, and obtaining the reprocessed ceramic chip;
s5: and (3) circulating the step in the step S4 for 30 times to obtain the ceramic tile.
Comparative example 3
The ceramic chip cleaning process for producing the copper-clad ceramic substrate comprises the following steps:
s1: aluminum nitride ceramics are selected: thermal conductivity 190W/mK, bending strength 450MPa;
s2: placing the aluminum nitride ceramic chip in absolute ethyl alcohol, ultrasonically cleaning for 20min, taking out, and then washing and drying to obtain an oil-removed ceramic chip;
s3: and oxidizing the deoiled ceramic tile for 3 hours at 1100 ℃ in a mixed atmosphere of nitrogen and oxygen with the volume ratio of 1:4 to obtain the ceramic tile.
Comparative example 4
In this example, compared with example 7, the tile prepared in example 4 was merely replaced with the tile prepared in comparative example 1, and the remaining steps were identical to those of example 7.
Comparative example 5
In this example, compared with example 7, the tile prepared in example 4 was merely replaced with the tile prepared in comparative example 2, and the remaining steps were identical to those of example 7.
Comparative example 6
In this example, compared with example 7, the tile prepared in example 4 was merely replaced with the tile prepared in comparative example 3, and the remaining steps were identical to those of example 7.
Performance detection
(1) Thermal shock resistance
Placing the substrates prepared in examples 7-9 and comparative examples 4-6 in an oven, heating to 300 ℃ and preserving heat for 3min, taking out the substrates after being heated uniformly, immediately putting the substrates into water, circulating in the way, and testing the circulation times when cracks appear on the substrates according to the condition that the cracks appear on the substrates, wherein the detection results are shown in table 1;
(2) Interfacial bond strength:
the substrates prepared in examples 7-9 and comparative examples 4-6 were subjected to bending strength test by using a high-low temperature double-column electronic tester, and the bonding strength was indirectly reflected by the bending strength comparison; the experiment adopts a point bending method, the span is L=80 mm, and the test speed is V=0.5 mm/min. 5 samples were tested for each sample under the same conditions and then averaged. The test schematic diagram is shown in fig. 1, and the detection results are shown in table 1.
Table 1: statistical table of performance test data for examples 7-9 and comparative examples 4-6
As can be seen from Table 1, the substrate materials prepared in examples 7 to 9 of the present application have high bonding strength between copper foil and ceramic chip, high reliability in temperature cycle, and high resistance to thermal fatigue at 300 ℃.
The foregoing describes one embodiment of the present application in detail, but the description is only a preferred embodiment of the present application and should not be construed as limiting the scope of the application. All equivalent changes and modifications within the scope of the present application are intended to be covered by the present application.
Claims (10)
1. The ceramic chip cleaning process for the production of the copper-clad ceramic substrate is characterized by comprising the following steps of:
s1: the ceramic chip is degreased and cleaned to obtain degreased ceramic chip;
s2: soaking, washing and drying the deoiling ceramic chip in coarsening liquid to obtain a pretreated ceramic chip;
s3: oxidizing the pretreated ceramic chip for 2-4 hours at 1000-1100 ℃ in a mixed atmosphere of nitrogen and oxygen to obtain an oxidized ceramic chip;
s4: placing the oxidized ceramic chip in a cleaning solution for standing and washing, placing the oxidized ceramic chip in an alkali solution for standing and washing to obtain a reprocessed ceramic chip;
s5: and (5) circulating the step in the step S4 for 10-30 times to obtain the ceramic tile.
2. The tile cleaning process for copper-clad ceramic substrate production of claim 1, wherein the tiles are aluminum nitride tiles.
3. The tile cleaning process for copper-clad ceramic substrate production according to claim 1, wherein the specific steps of degreasing and cleaning are: placing the ceramic tile in absolute ethyl alcohol, ultrasonically cleaning for 10-30min, taking out, washing with water, and drying.
4. The tile cleaning process for copper-clad ceramic substrate production according to claim 1, wherein the specific steps of soaking in the roughening solution in S2 are as follows: heating to 60-80deg.C, and soaking for 10-30min.
5. The tile cleaning process for copper-clad ceramic substrate production according to claim 4, wherein the roughening solution is 30-60wt% aqueous sodium hydroxide solution.
6. The tile cleaning process for copper-clad ceramic substrate production according to claim 4, wherein the placing of the oxidized tile in the cleaning solution in S4 is specifically: heating to 60-70deg.C, and standing for 0.5-2min.
7. The tile cleaning process for copper-clad ceramic substrate production according to claim 4, wherein the placing in an alkaline solution in S4 is specifically: heating to 60-70deg.C, and standing for 0.1-1min.
8. A cleaning solution characterized in that it is applied to the cleaning process according to any one of claims 1 to 9.
9. A cleaning solution according to claim 8, wherein the cleaning solution is prepared by mixing copper sulfate, distilled water, and sodium thiosulfate.
10. A cleaning solution according to claim 9, wherein the copper sulfate: distilled water: the mass ratio of the sodium thiosulfate is 1-5:100-200:5-20.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310682687.0A CN116705591A (en) | 2023-06-09 | 2023-06-09 | Ceramic chip cleaning process and cleaning fluid for copper-clad ceramic substrate production |
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| CN202310682687.0A CN116705591A (en) | 2023-06-09 | 2023-06-09 | Ceramic chip cleaning process and cleaning fluid for copper-clad ceramic substrate production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117457504A (en) * | 2023-12-22 | 2024-01-26 | 成都万士达瓷业有限公司 | Production method for copper-clad ceramic packaging surface |
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- 2023-06-09 CN CN202310682687.0A patent/CN116705591A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117457504A (en) * | 2023-12-22 | 2024-01-26 | 成都万士达瓷业有限公司 | Production method for copper-clad ceramic packaging surface |
| CN117457504B (en) * | 2023-12-22 | 2024-03-08 | 成都万士达瓷业有限公司 | Production method for copper-clad ceramic packaging surface |
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