A DCB production method for preparing aluminum nitride copper-clad ceramic substrate

Abstract

The invention relates to the technical field of DCB production methods, and specifically discloses a DCB production method for preparing an aluminum nitride copper-clad ceramic carrier plate. The method comprises the following steps: S1: cleaning the aluminum nitride ceramic sheet and activating the copper ions to obtain a prefabricated DCB plate; S2: performing oxidation treatment and double-sided sintering on the prefabricated DCB plate in sequence to obtain an aluminum nitride copper-clad ceramic carrier plate.

Description

Technical Field

[0001] The invention relates to the technical field of DCB production methods, in particular to a DCB production method for preparing an aluminum nitride copper-clad ceramic carrier board. Background Art

[0002] Because aluminum nitride itself does not react with copper, and the wetting effect of copper-oxygen eutectic liquid on aluminum nitride ceramics is poor, the direct copper coating method for preparing aluminum nitride copper-clad ceramic substrates requires pre-oxidation of the aluminum nitride ceramics. First, a dense and stable aluminum oxide layer is generated on the surface of the aluminum nitride ceramic, and then the aluminum oxide layer and the copper sheet continue to react. In order to generate a dense aluminum oxide layer on the surface of the aluminum nitride ceramic, the aluminum nitride ceramic must be activated first. The existing activation process is complicated and the activation effect is poor. When preparing aluminum nitride copper-clad ceramic substrates, a large number of bubbles will be generated at the interface between copper and aluminum nitride, resulting in a significant decrease in the peeling strength and thermal conductivity of the substrate, and a low yield rate.

[0003] In summary, it is of great significance to invent a DCB production method for preparing aluminum nitride copper-clad ceramic substrates. Summary of the invention

[0004] The object of the present invention is to provide a method for manufacturing a selectively gold-plated double-sided heat dissipating copper-based carrier board to solve the problems raised in the above-mentioned background technology.

[0005] A DCB production method for preparing an aluminum nitride copper-clad ceramic substrate comprises the following steps:

[0006] S1: After cleaning the aluminum nitride ceramic sheet, copper ion activation is performed to obtain a prefabricated DCB board;

[0007] S2: The prefabricated DCB board is subjected to oxidation treatment and double-sided sintering in sequence to obtain an aluminum nitride copper-clad ceramic substrate.

[0008] More optimally, the copper ion activation includes the following 6 steps: discharging, spray cleaning, water stop washing, overflow water washing, drying, and collecting.

[0009] More optimally, liquid medicine is used in the spray cleaning; the raw materials of the liquid medicine include sodium chlorate, cupric chloride and hydrochloric acid.

[0010] More optimally, the H of the potion + The concentration is 1.5-2.5 mol / L, the copper ion concentration is 2-3 mol / L, and the specific density is 1.0-1.5 kg / L.

[0011] More optimally, the conductivity of the sodium chlorate in the medicine is 500-600.

[0012] The optimal process parameters of the spray cleaning are: the spray pressure is 1.5-3.0 kg / cm 2 , the line speed is 0.5~1.5m / min.

[0013] The more optimized process parameters of the double-sided sintering are: temperature of 1070-1080° C., oxygen partial pressure of 50-100 ppm, and belt speed of 30-90 mm / min.

[0014] The more optimized process parameters of the oxidation treatment are: oxidation temperature of 1050-1100° C., and oxidation time of 5-6.5 hours.

[0015] Compared with the prior art, the present invention has the following beneficial effects: (1) the present invention develops a new economical and efficient activation method for aluminum nitride ceramic sheets, so that the aluminum nitride ceramic sheets have a better oxidation effect and bubbles are not easily generated on the surface after sintering. (2) a double-sided sintering process is used, and both sides are sintered at the same time, so that the production efficiency is doubled. (3) a copper-clad ceramic substrate with less warping can be obtained. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0017] Figures 1-2 This is an appearance diagram of the aluminum nitride copper-clad ceramic carrier board of Example 1;

[0018] Figures 3-4 This is an appearance diagram of the aluminum nitride copper-clad ceramic carrier board of Example 2;

[0019] Figures 5-6 This is an appearance diagram of the aluminum nitride copper-clad ceramic carrier board of Example 3;

[0020] Figures 7-8 This is the appearance of the aluminum nitride copper-clad ceramic substrate of Comparative Example 1;

[0021] Fig. 9 This is a graph showing the result of the aluminum nitride copper-clad ceramic substrate in Example 1 after 0 hot and cold cycles;

[0022] Fig.10 This is a graph showing the results of 30 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate in Example 1;

[0023] Fig.11 This is a graph showing the results of 40 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate in Example 1;

[0024] Fig.12 This is a graph showing the results of 50 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate in Example 1;

[0025] Fig.13 This is a graph showing the result of the aluminum nitride copper-clad ceramic substrate of Example 2 undergoing 0 hot and cold cycles;

[0026] Fig.14 This is a graph showing the results of 30 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of Example 2;

[0027] Fig.15 This is a graph showing the results of 40 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of Example 2;

[0028] Fig.16 This is a graph showing the results of 50 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of Example 2;

[0029] Fig.17 This is a graph showing the result of the aluminum nitride copper-clad ceramic substrate of Example 3 undergoing 0 hot and cold cycles;

[0030] Fig.18 This is a graph showing the results of 30 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of Example 3;

[0031] Fig.19 This is a graph showing the results of 40 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of Example 3;

[0032] Fig. 20 This is a graph showing the results of 50 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of Example 3;

[0033] Fig.21 This is a graph showing the results of the aluminum nitride copper-clad ceramic substrate of comparative example 1 after 0 hot and cold cycles;

[0034] Fig. 22 This is a graph showing the results of 30 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate in comparative example 1;

[0035] Fig.23 This is a graph showing the results of 40 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate of comparative example 1;

[0036] Fig.24 This is a graph showing the results of 50 hot and cold cycles of the aluminum nitride copper-clad ceramic substrate in Example 1. DETAILED DESCRIPTION

[0037] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0038] The specific embodiments of the present invention are as follows:

[0039] Example 1: A DCB production method for preparing an aluminum nitride copper-clad ceramic substrate, comprising the following steps:

[0040] S1: After vertically cleaning the aluminum nitride ceramic sheet, 6 stages of copper ion activation treatment were sequentially performed at a line speed of 0.5 m / min to obtain a prefabricated DCB board;

[0041] Among them, the potion used for the spray cleaning of copper ion activation treatment is added with sodium chlorate, copper chloride, and hydrochloric acid; H + The concentration range is 1.5mol / L, the conductivity of sodium chlorate is 500, and the copper ion concentration is 2mol / L; the specific density of the solution is 1.0kg / L, and the spray pressure is 1.5kg / cm 2 ;

[0042] S2: The prefabricated DCB board is oxidized at 1050°C for 2 hours, heated to 1100°C for 0.5 hours, cooled for about 3 hours, and when the temperature drops below 100°C, it is taken out and placed in a turnover box, and then double-sided sintering is performed to obtain an aluminum nitride copper-clad ceramic substrate;

[0043] The process parameters of double-sided sintering are: temperature of 1070°C, oxygen partial pressure of 50ppm, and belt speed of 30mm / min.

[0044] Example 2: A DCB production method for preparing an aluminum nitride copper-clad ceramic substrate, comprising the following steps:

[0045] S1: After vertically cleaning the aluminum nitride ceramic sheet, 6 stages of copper ion activation treatment were sequentially performed at a line speed of 1.0 m / min to obtain a prefabricated DCB board;

[0046] Among them, the potion used in the spray cleaning for copper ion activation treatment is added with sodium chlorate, copper chloride, and hydrochloric acid; H + The concentration is 2.0mol / L, the conductivity of sodium chlorate is 550, the concentration of copper ions is 2.5mol / L; the specific density of the solution is 1.5kg / L, and the spraying pressure of the solution is 2.0kg / cm 2 ;

[0047] S2: The prefabricated DCB board is oxidized at 1050°C for 2 hours, heated to 1100°C for 0.5 hours, cooled for about 3 hours, and when the temperature drops below 100°C, it is taken out and placed in a turnover box, and then double-sided sintering is performed to obtain an aluminum nitride copper-clad ceramic substrate;

[0048] The process parameters of double-sided sintering are: temperature of 1075°C, oxygen partial pressure of 75ppm, and belt speed of 40mm / min.

[0049] Example 3: A DCB production method for preparing an aluminum nitride copper-clad ceramic substrate, comprising the following steps:

[0050] S1: After vertically cleaning the aluminum nitride ceramic sheet, 6 stages of copper ion activation treatment were sequentially performed at a line speed of 1.5 m / min to obtain a prefabricated DCB board;

[0051] Among them, the potion used in the spray cleaning for copper ion activation treatment is added with sodium chlorate, copper chloride, and hydrochloric acid; H + The concentration is 2.5mol / L, the conductivity of the solution is 600, the concentration of copper ions is 3.0mol / L; the specific density of the solution is 2.0kg / L, and the spray pressure is 2.5kg / cm 2 ;

[0052] S2: The prefabricated DCB board is oxidized at 1050°C for 2 hours, heated to 1100°C for 0.5 hours, cooled for about 3 hours, and when the temperature drops below 100°C, it is taken out and placed in a turnover box, and then double-sided sintering is performed to obtain an aluminum nitride copper-clad ceramic substrate;

[0053] The process parameters of double-sided sintering are: temperature of 1080°C, oxygen partial pressure of 100ppm, and belt speed of 50mm / min.

[0054] Comparative Example 1: The aluminum nitride ceramic sheet was not activated:

[0055] A DCB production method for preparing an aluminum nitride copper-clad ceramic substrate comprises the following steps:

[0056] The aluminum nitride ceramic sheet and the copper sheet are cleaned and oxidized respectively. After the oxidized aluminum nitride ceramic sheet is covered with oxidized copper sheets on both sides, double-sided sintering is performed at a belt speed of 40 mm / min, an oxygen partial pressure of 75 ppm and 1075°C to obtain an aluminum nitride copper-clad ceramic substrate.

[0057] Test 1: Take photos to record the appearance of the aluminum nitride copper-clad ceramic substrates of Examples 1 to 3 and Comparative Example 1, as shown in Table 1;

[0058] Remark Example 1 Figures 1-2 Example 2 Figures 3-4 Example 3 Figures 5-6 Comparative Example 1 Figures 7-8

[0059] Table 1

[0060] Conclusion: Compared with comparative example 1, the aluminum nitride copper-clad ceramic substrates of Examples 1 to 3 have better sintering effects, and the sintering bubble rate of the activated aluminum nitride ceramic sheet after oxidation is significantly lower than that of the unactivated aluminum nitride ceramic sheet.

[0061] Test 2: Examples 1 to 3 and Comparative Example 1 were placed in a temperature range of -55°C to 150°C and subjected to 50 cycles of hot and cold shock to test the reliability of Examples 1 to 3 and Comparative Example 1, as shown in Table 2;

[0062] Hot and cold cycles Example 1 Example 2 Example 3 Comparative Example 1 0 times Fig. 9 Fig.13 Fig.17 Fig.21 30 times Fig.10 Fig.14 Fig.18 Fig. 22 40 times Fig.11 Fig.15 Fig.19 Fig.23 50 times Fig.12 Fig.16 Fig. 20 Fig.24

[0063] Table 2

[0064] Conclusion: Compared with the comparative example 1 subjected to hot and cold cycle shock between -55°C and 150°C, the embodiments 1 to 3 have better reliability performance. After 50 cycles, the edge of the comparative example 1 has begun to copper-shed, while the embodiments 1 to 3 have not yet had obvious copper-shedding.

[0065] Test 3: The peel strength (N / m) of the circular surface and the non-circular surface of Examples 1 to 3 and Comparative Example 1 was tested, as shown in Table 3;

[0066]

[0067] Table 3

[0068] Conclusion: It can be seen from Table 3 that compared with Comparative Example 1, the aluminum nitride ceramic sheets of Examples 1 to 3 are activated, then oxidized, and double-sided sintered to obtain aluminum nitride copper-clad ceramic substrates with stronger copper-ceramic bonding, and all meet the standards; however, the bonding strength of Comparative Example 1 is not only at the lower limit but also lower than the standard at some points.

[0069] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0070] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A DCB production method for preparing an aluminum nitride copper-clad ceramic substrate, characterized in that: The steps include: S1: After cleaning the aluminum nitride ceramic sheet, the copper ion activation treatment is carried out in six stages in sequence: discharging, spray cleaning, water stop cleaning, overflow water cleaning, drying, and collecting to obtain a prefabricated DCB board; S2: performing oxidation treatment and double-sided sintering on the prefabricated DCB board in sequence to obtain an aluminum nitride copper-clad ceramic substrate; The raw materials of the medicine used in the spray cleaning include sodium chlorate, copper chloride and hydrochloric acid; The H of the potion + The concentration is 1.5-2.5 mol / L, the copper ion concentration is 2-3 mol / L, and the specific density is 1.0-1.5 kg / L; the conductivity of the sodium chlorate in the medicine is 500-600.

2. The DCB production method for preparing an aluminum nitride copper-clad ceramic substrate according to claim 1, characterized in that: The process parameters of the spray cleaning are: the spray pressure is 1.5-3.0 kg / cm 2 , the line speed is 0.5~1.5m / min.

3. The DCB production method for preparing an aluminum nitride copper-clad ceramic substrate according to claim 1, characterized in that: The process parameters of the double-sided sintering are: temperature of 1070-1080° C., oxygen partial pressure of 50-100 ppm, and belt speed of 30-90 mm / min.

4. The DCB production method for preparing an aluminum nitride copper-clad ceramic substrate according to claim 1, characterized in that: The process parameters of the oxidation treatment are: oxidation temperature is 1050-1100° C., and oxidation time is 5-6.5 hours.

5. The aluminum nitride copper clad ceramic substrate is obtained according to the DCB production method for preparing an aluminum nitride copper clad ceramic substrate according to any one of claims 1 to 4.

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