Device and method for preparing black aluminum oxide ceramic substrate with high mechanical and breakdown strength

Abstract

The invention discloses a device and a method for preparing a black aluminum oxide ceramic substrate with high mechanical and breakdown strength, and relates to the technical field of ceramic substrate preparation, the device comprises an outer cylinder and a bracket for mounting the outer cylinder, a driving part for driving the outer cylinder to rotate is mounted on the bracket, and grinding balls with different sizes are arranged in the outer cylinder. A plurality of partition seats are annularly arrayed on the inner wall of the outer barrel around the axis of the outer barrel, and a return groove for accommodating a partition arc plate is formed in each partition seat, so that adjustable grinding ball distribution control is realized, the uniformity and grinding efficiency of black aluminum oxide ceramic slurry are remarkably improved, the core problems of low efficiency, high pollution and poor uniformity in traditional ball milling are solved, and the service life of the ball milling machine is prolonged. The sintered substrate is uniform in color, grinding balls of different sizes can be blanked according to the spheroidal graphite requirement, the spheroidal graphite effect is improved, the components of the black aluminum oxide ceramic substrate are uniform, the problems of agglomeration, pollution and the like can be effectively avoided, and it is ensured that the substrate meets the requirements for high mechanical strength and high insulativity at the same time.

Description

Technical Field

[0001] The invention relates to the technical field of ceramic substrate preparation, and in particular to a device and method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength. Background Art

[0002] In the preparation process of black alumina ceramic substrates with high mechanical properties and high breakdown strength, ball milling is a key step that affects powder uniformity, sintering activity and final performance.

[0003] Black colorants (such as CoFe 2 O 4 Cr 2 O 3 etc.) due to density differences (such as Al 2 O 3 Density 3.95g / cm 3 , CoFe 2 O 4 Density 5.3g / cm 3 ) is easy to settle, resulting in local enrichment. During the ball milling process, when grinding balls of different sizes are used together, the particle size after ball milling will be uneven, resulting in low efficiency, high pollution, and poor uniformity in ball milling, making the color of the substrate uneven after sintering. Summary of the invention

[0004] The purpose of the present invention is to provide a device and method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength, which has adjustable grinding ball distribution control, significantly improves the uniformity and grinding efficiency of the black alumina ceramic slurry, solves the core problems of low efficiency, high pollution and poor uniformity in traditional ball milling, and has the advantage of uniform color of the substrate after sintering.

[0005] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength, comprising an outer cylinder and a bracket for mounting the outer cylinder, a driving member for driving the outer cylinder to rotate is mounted on the bracket, grinding balls of different sizes are arranged inside the outer cylinder, a plurality of partition seats are arranged in a ring around the axis of the inner wall of the outer cylinder, and a return groove for accommodating a partition arc plate is opened in each partition seat;

[0006] When the outer cylinder is in a stationary state, the grinding balls are respectively arranged between the partition seats, and the partition arc plate can rotate around the axis of the outer cylinder in the return groove to adjust the opening spacing between two adjacent partition seats.

[0007] Furthermore, both ends of the outer cylinder are axially connected to the bracket, a feed port is provided on the outer surface of the outer cylinder, and a closed door is provided on the feed port.

[0008] Furthermore, one end of the separation arc plate is connected to a linkage ring, an external gear is arranged on the linkage ring, and one end of the outer cylinder is provided with a driving assembly, which is butt-jointed with the external gear.

[0009] Furthermore, an extension plate is provided on the separation seat, a linkage gear is axially connected to the extension plate, and an arc-shaped tooth groove meshing with the linkage gear is provided on the surface of the separation arc plate.

[0010] Furthermore, one end of the separation arc plate is a U-shaped end, and the U-shaped end is butted with the return groove through a spring.

[0011] Furthermore, a center plate is installed at one end of the outer cylinder through a bearing, a retractable shaft is arranged on the center plate, and two sections of arc-shaped teeth are installed on the shaft.

[0012] Furthermore, the two sections of arc-shaped teeth are movably meshed with the linkage gear, and a driver capable of driving the center plate to rotate is arranged on the bracket.

[0013] The present invention also provides a method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength, comprising the following steps:

[0014] S1: Mix α-alumina powder with a purity of ≥99.5%, black colorant, sintering aid and dispersant, wherein the black colorant is spinel CoFe 2 O 4 or MnFe 2 O 4 At least one of the following, the addition amount is 2-5wt%, and the sintering aid is MgO-SiO 2 -CaO system, the addition amount is 0.5-2wt%;

[0015] S2: ball-milling the mixed powder, organic solvent, binder and plasticizer into a uniform slurry, with the ball-milling time being ≥ 12 hours;

[0016] S3: The green body is prepared by tape casting or dry pressing, the thickness of the tape casting green body is 0.1-1 mm, and the dry pressing pressure is 100-200 MPa;

[0017] S4: Raise the temperature to 600°C at 1-2°C / min and keep it at this temperature for 2 hours to remove organic matter;

[0018] S5: Pre-sinter at 1200-1400℃ for 2 hours, then sinter at 1500-1650℃ in hydrogen or vacuum environment for 1-3 hours;

[0019] S6: The sintered body is subjected to hot isostatic pressing at 1600° C. and 100-200 MPa Ar atmosphere for 1 hour.

[0020] Furthermore, the black colorant is Cr2 O 3 With MnO 2 According to the 1:1 mass ratio of composite doping, the total addition amount is 3-6wt%, MgO, SiO in the sintering aid 2 The mass ratio of CaO is 1:1:0.5.

[0021] Furthermore, during the sintering process, the grain size is controlled to be less than 5 μm, and the porosity of the final ceramic substrate is less than 0.5%. After the static pressure treatment, the substrate surface needs to be polished, and the surface roughness of the substrate is controlled to be Ra less than 0.1 μm using diamond polishing liquid.

[0022] Technical effects and advantages of the present invention:

[0023] 1. The dividing arc plate of the present invention can rotate around the axis of the outer cylinder in the return groove, and is used to adjust the opening spacing between two adjacent dividing seats. The adjustable grinding ball distribution control significantly improves the uniformity and grinding efficiency of the black alumina ceramic slurry. The grinding balls are divided into zones according to size through the dividing seats to avoid the problem of uneven grinding efficiency caused by the mixing of large and small grinding balls in traditional ball mills. The dividing arc plate can be rotated to adjust the opening size between adjacent dividing seats, and the movement range of the grinding balls can be flexibly controlled. The pressure sensor and temperature probe are embedded in the inner wall of the outer cylinder to provide real-time feedback on the slurry viscosity and temperature, and automatically adjust the speed and cooling rate of the driving part. The device solves the core problems of low efficiency, high pollution and poor uniformity in traditional ball mills through dynamic zone grinding and intelligent regulation, so that the color of the substrate is uniform after sintering, providing reliable equipment support for the industrial production of high-performance ceramic substrates.

[0024] 2. The driving assembly of the present invention can drive the separation arc plate to rotate in the return groove, so as to adjust the opening spacing between two adjacent separation seats, and control the rotation spacing of the separation arc plate as needed. Grinding balls of different sizes can be fed according to the needs of spheroidal graphite, thereby improving the spheroidal graphite effect, making the composition of the black alumina ceramic substrate uniform, and effectively avoiding problems such as agglomeration and pollution, ensuring that the substrate meets the requirements of high mechanical strength and high insulation at the same time.

[0025] 3. The present invention provides arc-shaped tooth grooves on each dividing arc plate. When the dividing arc plate moves to the material discharge position, it is driven by the arc-shaped teeth to open. When the dividing arc plate rotates to leave the material discharge position, the dividing arc plate automatically resets to close the opening between two adjacent dividing seats, so that the outer cylinder is in a closed state, and the material and the grinding balls can be in uniform contact, thereby realizing ball milling and solving the problem of poor material discharge, thereby improving grinding efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0027] Figure 2It is a half-section view of the outer cylinder structure of the present invention;

[0028] Figure 3 A side half-section view of the outer cylinder of the present invention;

[0029] Figure 4 It is a schematic diagram of the separation structure of the separation seat and the separation arc plate of the present invention;

[0030] Figure 5 This is a schematic diagram of the overall structure of Embodiment 2 of the present invention;

[0031] Figure 6 This is a schematic diagram of the internal structure of the outer cylinder of the second embodiment of the present invention;

[0032] Figure 7 For the present invention Figure 6 A magnified image of point A;

[0033] Figure 8 It is a plan view of the docking of the partition seat and the partition arc plate of the present invention.

[0034] In the figure:

[0035] 1. Outer cylinder; 11. Bracket; 12. Driving member; 13. Grinding ball; 14. Feed inlet; 141. Closing door; 2. Partition seat; 21. Partition arc plate; 211. Arc tooth groove; 22. Return groove; 23. Linkage ring; 231. External gear; 24. Driving assembly; 25. Extension plate; 251. Linkage gear; 3. Center plate; 31. Shaft; 32. Arc tooth. DETAILED DESCRIPTION

[0036] 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.

[0037] Example 1: Reference Figure 1 - Figure 4, which is the first embodiment of the present invention, provides a black alumina ceramic substrate preparation device with high mechanical strength and breakdown strength, including an outer cylinder 1 and a bracket 11 for mounting the outer cylinder 1, a driving member 12 for driving the outer cylinder 1 to rotate is installed on the bracket 11, grinding balls 13 of different sizes are arranged inside the outer cylinder 1, a plurality of partition seats 2 are arranged in a ring around the axis of the outer cylinder 1 on the inner wall of the outer cylinder 1, each partition seat 2 is provided with a return groove 22 for accommodating a partition arc plate 21, when the outer cylinder 1 is stationary, the grinding balls 13 are respectively arranged between the partition seats 2, and the partition arc plate 21 can rotate in the return groove 22 around the axis of the outer cylinder 1, and is used to adjust the opening spacing between two adjacent partition seats 2, and the adjustable grinding The distribution control of the balls 13 significantly improves the uniformity and grinding efficiency of the black alumina ceramic slurry. The grinding balls 13 are divided into zones by size through the separator seats 2 to avoid the problem of uneven grinding efficiency caused by the mixing of large and small grinding balls 13 in traditional ball mills. The separator arc plate 21 can rotate to adjust the opening size between adjacent separator seats 2, flexibly control the movement range of the grinding balls 13, and embed pressure sensors and temperature probes on the inner wall of the outer cylinder 1 to provide real-time feedback on the slurry viscosity and temperature, and automatically adjust the speed and cooling rate of the drive member 12. The device solves the core problems of low efficiency, high pollution and poor uniformity in traditional ball mills through dynamic zone grinding and intelligent regulation, and provides reliable equipment support for the industrial production of high-performance ceramic substrates.

[0038] Both ends of the outer cylinder 1 are axially connected to the bracket 11. A feed port 14 is provided on the outer surface of the outer cylinder 1. A closed door 141 is provided on the feed port 14, which can be opened and closed by the closed door 141 to realize material feeding and discharging.

[0039] A linkage ring 23 is connected to one end of the separation arc plate 21, and an external gear 231 is arranged on the linkage ring 23. A driving assembly 24 is arranged at one end of the outer cylinder 1, and the driving assembly 24 is connected to the external gear 231. The driving assembly 24 includes a motor and a gear combination. The driving assembly 24 can drive the separation arc plate 21 to rotate in the return groove 22, so as to adjust the opening spacing between two adjacent separation seats 2, and control the separation arc plate 21 to rotate out of the spacing as needed. Grinding balls 13 of different sizes can be fed according to the needs of spheroidal graphite, thereby improving the spheroidal graphite effect, making the composition of the black alumina ceramic substrate uniform, and effectively avoiding problems such as agglomeration and pollution, ensuring that the substrate meets the requirements of high mechanical strength and high insulation at the same time.

[0040] Specifically, when small-sized grinding balls 13 are needed for spheroidal graphite treatment, the motor drives the outer gear 231 and the linkage ring 23 to rotate through the gear, and the partition arc plate 21 is screwed out of the return groove 22, and a part of the opening between the two adjacent partition seats 2 is closed, so that the opening between the two adjacent partition seats 2 is only for the small-sized grinding balls 13 to go out, and the small-sized grinding balls 13 fall from the opening to the material in the outer cylinder 1 for fine spheroidal graphite treatment. When large-sized grinding balls 13 are needed for spheroidal graphite treatment, the partition arc plate 21 is rotated into the return groove 22, and the opening between the two adjacent partition seats 2 is opened, so that the opening can accommodate the large-sized grinding balls 13 to fall, thereby realizing spheroidal graphite treatment according to size.

[0041] Example 2: Reference Figure 5 - Figure 8 , which is the second embodiment of the present invention. This embodiment is different from the first embodiment. During the implementation of the first embodiment, it was found that when the separation arc plate 21 partially closes the opening between two adjacent separation seats 2, the material is easy to enter between the separation seats 2, resulting in difficulty in discharging the material.

[0042] In order to solve the above problems, this embodiment provides arc-shaped tooth grooves 211 on each dividing arc plate 21. When the dividing arc plate 21 moves to the unloading position, it is driven by the arc-shaped teeth 32 to open. When the dividing arc plate 21 rotates to leave the unloading position, the dividing arc plate 21 automatically resets to close the opening between two adjacent dividing seats 2, so that the outer cylinder 1 is in a closed state, and the material and the grinding balls 13 can be in uniform contact, thereby realizing ball milling and solving the problem of poor material discharge, thereby improving grinding efficiency.

[0043] An extension plate 25 is provided on the partition seat 2, and a linkage gear 251 is axially connected to the extension plate 25. An arc-shaped tooth groove 211 meshing with the linkage gear 251 is provided on the surface of the partition arc plate 21. One end of the partition arc plate 21 is a U-shaped end, and the U-shaped end is connected to the return groove 22 through a spring. A center plate 3 is installed at one end of the outer cylinder 1 through a bearing, and a retractable shaft rod 31 is provided on the center plate 3. Two sections of arc-shaped teeth 32 are installed on the shaft rod 31, and the two sections of arc-shaped teeth 32 are movably meshed with the linkage gear 251. A driver that can drive the center plate 3 to rotate is provided on the bracket 11. The partition arc plate 21 can be automatically popped out by a spring. In the initial state, the partition arc plate 21 extends to completely close the opening between two adjacent partition seats 2 to prevent materials from entering between the partition seats 2 and avoid grinding dead corners. In addition, by providing two sections of arc-shaped teeth 32, the material can be cut off at the unloading position. The retraction degree of the partition arc plate 21 is adjusted according to the length of the arc teeth 32, and the size of the falling grinding balls 13 is adjusted according to the needs of the ball mill. It should be noted that the arc teeth 32 can be set in multiple sections according to needs. By setting arc teeth 32 of different lengths, the opening size between adjacent partition seats 2 can be adjusted. When the ball mill completes material discharge, the center plate 3 is driven to rotate by the driver, and then the arc teeth 32 are driven to rotate to the bottom of the outer cylinder 1. When the partition arc plate 21 rotates to the bottom of the outer cylinder 1, the linkage gear 251 engages with the arc teeth 32, and then drives the partition arc plate 21 to retract into the return groove 22 at the bottom of the outer cylinder 1. At this time, the grinding balls 13 in the outer cylinder 1 fall into the opening between the partition seats 2 to complete the pre-storage of the grinding balls 13. When the arc teeth 32 need to be adjusted, the cylinder drives the shaft 31 to move, thereby adjusting the alignment of the arc teeth 32 of different lengths with the linkage gear 251.

[0044] Embodiment 3: This is the third embodiment of the present invention, which provides a method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength, comprising the following steps:

[0045] S1: Mix α-alumina powder with a purity of ≥99.5%, black colorant, sintering aid and dispersant, wherein the black colorant is spinel CoFe 2 O 4 or MnFe 2 O 4 At least one of the following, the addition amount is 2-5wt%, and the sintering aid is MgO-SiO 2 -CaO system, the addition amount is 0.5-2wt%;

[0046] S2: ball-milling the mixed powder, organic solvent, binder and plasticizer into a uniform slurry, with the ball-milling time being ≥ 12 hours;

[0047] S3: The green body is prepared by tape casting or dry pressing, the thickness of the tape casting green body is 0.1-1 mm, and the dry pressing pressure is 100-200 MPa;

[0048] S4: Raise the temperature to 600°C at 1-2°C / min and keep it at this temperature for 2 hours to remove organic matter;

[0049] S5: Pre-sinter at 1200-1400℃ for 2 hours, then sinter at 1500-1650℃ in hydrogen or vacuum environment for 1-3 hours;

[0050] S6: The sintered body is subjected to hot isostatic pressing at 1600° C. and 100-200 MPa Ar atmosphere for 1 hour.

[0051] Black colorant is Cr 2 O 3 With MnO 2 According to the 1:1 mass ratio of composite doping, the total addition amount is 3-6wt%, MgO, SiO in the sintering aid 2 The mass ratio of CaO is 1:1:0.5.

[0052] During the sintering process, the grain size is controlled to be less than 5 μm, and the porosity of the final ceramic substrate is less than 0.5%. After the static pressure treatment, the substrate surface needs to be polished, and the surface roughness of the substrate is controlled to Ra less than 0.1 μm using diamond grinding liquid.

[0053] Finally, it should be noted that the above 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, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength, comprising an outer cylinder (1) and a bracket (11) for mounting the outer cylinder (1), wherein a driving member (12) for driving the outer cylinder (1) to rotate is mounted on the bracket (11), characterized in that: Grinding balls (13) of different sizes are arranged inside the outer cylinder (1), and a plurality of partition seats (2) are arranged in a circular pattern around the axis of the inner wall of the outer cylinder (1), and each partition seat (2) is provided with a return groove (22) for accommodating a partition arc plate (21); When the outer cylinder (1) is in a stationary state, the grinding balls (13) are respectively arranged between the separation seats (2), and the separation arc plate (21) can rotate around the axis of the outer cylinder (1) in the return groove (22) to adjust the opening spacing between two adjacent separation seats (2).

2. The device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 1, characterized in that: The two ends of the outer cylinder (1) are axially connected to the bracket (11), and a feed port (14) is provided on the outer surface of the outer cylinder (1), and a closed door (141) is provided on the feed port (14).

3. The device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 2, characterized in that: One end of the separation arc plate (21) is connected to a linkage ring (23), an external gear (231) is provided on the linkage ring (23), and one end of the outer cylinder (1) is provided with a driving assembly (24), which is butt-jointed with the external gear (231).

4. The device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 3 is characterized in that: The partition seat (2) is provided with an extension plate (25), a linkage gear (251) is axially connected to the extension plate (25), and an arc-shaped tooth groove (211) meshing with the linkage gear (251) is provided on the surface of the partition arc plate (21).

5. The device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 4, characterized in that: One end of the separation arc plate (21) is a U-shaped end, and the U-shaped end is butted with the return groove (22) via a spring.

6. The device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 5, characterized in that: A center plate (3) is installed at one end of the outer cylinder (1) via a bearing, a retractable shaft (31) is provided on the center plate (3), and two sections of arc-shaped teeth (32) are installed on the shaft (31).

7. The device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 6, characterized in that: The two sections of arc-shaped teeth (32) are movably meshed with the linkage gear (251), and a driver capable of driving the center plate (3) to rotate is arranged on the bracket (11).

8. A method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength, which is applied to the device for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength as described in claim 1, characterized in that: The steps include: S1: Mix α-alumina powder with a purity of ≥99.5%, a black colorant, a sintering aid and a dispersant, wherein the black colorant is at least one of spinel CoFe2O4 or MnFe2O4, and the addition amount is 2-5wt%, and the sintering aid is a MgO-SiO2-CaO system, and the addition amount is 0.5-2wt%; S2: ball-milling the mixed powder, organic solvent, binder and plasticizer into a uniform slurry for ≥12 hours; S3: preparing a green body by tape casting or dry pressing, the thickness of the tape casting green body is 0.1-1 mm, and the dry pressing pressure is 100-200 MPa; S4: Raise the temperature to 600°C at 1-2°C / min and keep it at this temperature for 2 hours to remove organic matter; S5: Pre-sinter at 1200-1400℃ for 2 hours, then sinter at 1500-1650℃ in hydrogen or vacuum environment for 1-3 hours; S6: The sintered body is subjected to hot isostatic pressing at 1600° C. and 100-200 MPa Ar atmosphere for 1 hour.

9. The method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 8, characterized in that: The black colorant is Cr2O3 and MnO2 compositely doped in a mass ratio of 1:1, with a total addition amount of 3-6wt%. The mass ratio of MgO, SiO2 and CaO in the sintering aid is 1:1:0.

5.

10. The method for preparing a black alumina ceramic substrate with high mechanical strength and breakdown strength according to claim 9, characterized in that: During the sintering process, the grain size is controlled to be less than 5 μm, and the porosity of the final ceramic substrate is less than 0.5%. After the static pressure treatment, the substrate surface needs to be polished, and the surface roughness of the substrate is controlled to Ra less than 0.1 μm using diamond grinding liquid.

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