CN117645493B - Oscillation pressure auxiliary ceramic connection method - Google Patents
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- CN117645493B CN117645493B CN202311629913.5A CN202311629913A CN117645493B CN 117645493 B CN117645493 B CN 117645493B CN 202311629913 A CN202311629913 A CN 202311629913A CN 117645493 B CN117645493 B CN 117645493B
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- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000010355 oscillation Effects 0.000 title claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000005498 polishing Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000013461 design Methods 0.000 claims abstract description 4
- 238000003825 pressing Methods 0.000 claims abstract description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 30
- 238000005304 joining Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 abstract description 18
- 230000007547 defect Effects 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000011534 incubation Methods 0.000 description 12
- 238000005520 cutting process Methods 0.000 description 11
- 238000005245 sintering Methods 0.000 description 11
- 229910003460 diamond Inorganic materials 0.000 description 10
- 239000010432 diamond Substances 0.000 description 10
- 229910052727 yttrium Inorganic materials 0.000 description 10
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 10
- 229910000679 solder Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007545 Vickers hardness test Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007656 fracture toughness test Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000013500 performance material Substances 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C04B37/001—Joining burned ceramic articles with other burned ceramic articles or other articles by heating directly with other burned ceramic articles
-
- 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
- C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
- C04B2237/50—Processing aspects relating to ceramic laminates or to the joining of ceramic articles with other articles by heating
- C04B2237/52—Pre-treatment of the joining surfaces, e.g. cleaning, machining
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses an oscillation pressure auxiliary ceramic connection method, which comprises the following steps: step 1: polishing the ceramic samples, stacking the samples to be connected, and fully contacting the samples; step 2: heating the sample to a target temperature, preserving heat, and applying pressure to the design value up and down on the sample; step 3: applying periodically-changing oscillating pressure, stopping applying the pressure after connection is completed, and cooling to obtain connected ceramic; the invention can obviously improve the defects of the material by oscillating pressure, obviously reduce the agglomeration pores, microcracks and the like in the material and has more uniform microstructure; the mechanical property of the ceramic can be effectively improved; the mechanical property of the ceramic after connection is obviously higher than the strength of the base material.
Description
Technical Field
The invention relates to the technical field of ceramic preparation, in particular to an oscillation pressure auxiliary ceramic connection method.
Background
The existing ceramic sintering can only prepare samples with regular shapes, and in order to meet the requirements of special-shaped or large-sized samples in practical application, the ceramic materials are generally connected together by adopting a connecting technology. The connections are divided into two categories depending on the presence or absence of solder: 1) Solder-free joining, typically by diffusion or plastic deformation, of materials; but this method requires a higher temperature and a longer time. As disclosed in Transparent YAG ceramic/sapphire composite fabricated by pressureless direct thermal diffusion bonding,, YAG ceramics and alumina single crystals were joined together by incubating at a high temperature of 1650℃for 10 hours. In addition, the grain size of the connected sample can also grow obviously, and the performance of the material is reduced. 2) The connection with solder generally produces a liquid phase at low temperature by the solder, promoting diffusion between materials, and further reducing the temperature and time of connection. However, the connection of the materials after the addition of the solder is limited by the solder, and the high temperature resistance and the corrosion resistance are obviously lower than those of the base material, so that the performance requirements are difficult to meet. If 2021110715049, a method for connecting zirconia ceramics by glass solder penetration is adopted, the highest room temperature strength of the method is 851MPa, which is obviously lower than the strength of the common zirconia parent metal of 1200MPa.
Disclosure of Invention
The invention provides an oscillation pressure auxiliary ceramic connecting method aiming at the problems existing in the prior art.
The technical scheme adopted by the invention is as follows: an oscillation pressure assisted ceramic joining method comprising the steps of:
step 1: polishing the ceramic samples, stacking the samples to be connected, and fully contacting the samples;
Step 2: heating the sample to a target temperature, preserving heat, and applying pressure to the design value up and down on the sample;
step 3: and (3) applying periodically-changed oscillation pressure, stopping applying the pressure after the connection is completed, and cooling to obtain the connected ceramic.
Further, the roughness of the contact surface of the sample in the step 1 is less than or equal to 1 mu m.
Further, the median value of the oscillation pressure in the step 3 is 10-200 MPa.
Further, the oscillation pressure periodically changed in the step 3 has an amplitude of 1-100 MPa and a frequency of 0.1-50 Hz.
Further, the ceramic is zirconia ceramic.
Further, the target temperature in the step 2 is 1000-1800 ℃.
Further, the time for applying the oscillating pressure in the step 3 is 1-120 min.
Further, the stacked samples in step 1 are applied with a set pressure value so as to be in sufficient contact.
The beneficial effects of the invention are as follows:
(1) According to the invention, the ceramic material is connected through the oscillation pressure, so that the mechanical property of the ceramic can be effectively improved; the mechanical property of the ceramic after connection is obviously higher than the strength of the base material;
(2) The invention can obviously improve the defects of the material by oscillating pressure, obviously reduce the agglomeration pores, microcracks and the like in the material and has more uniform microstructure.
Drawings
FIG. 1 is a schematic diagram of the method of the present invention.
FIG. 2 shows the results of the strength measurement before and after the connection of the sample obtained in example 1 of the present invention.
FIG. 3 shows the results of fracture toughness test before and after joining the test pieces obtained in example 1 of the present invention.
Fig. 4 is an SEM image of the front and rear surfaces of the sample connection obtained in example 1 of the present invention, a being the original sample, and b being the sample obtained in example 1.
Fig. 5 is an SEM image of the fracture before and after the connection of the sample obtained in example 1 of the present invention, a is an original sample, and b is a sample obtained in example 1.
Detailed Description
The invention will be further described with reference to the drawings and specific examples.
As shown in fig. 1, an oscillation pressure-assisted ceramic joining method includes the steps of:
step 1: polishing the ceramic samples, stacking the samples to be connected, and fully contacting the samples;
firstly, cutting the sample into a required shape and size, and polishing to obtain the sample with the connection end surface roughness less than or equal to 1 mu m. A small pressure (pressure less than 10 MPa) is applied to both ends of the test specimen as long as good contact of the test specimen is ensured.
Step 2: heating the sample to a target temperature, preserving heat, and applying pressure to the design value up and down on the sample;
And heating to the target temperature, and preserving heat for a set time, wherein the time is determined according to actual conditions, and the temperature of the sample is ensured to be consistent with the furnace temperature. The connection temperature is 1000-1800 ℃ and the vacuum degree is more than 10Pa.
Step 3: and (3) applying periodically-changed oscillation pressure, stopping applying the pressure after the connection is completed, and cooling to obtain the connected ceramic. The pressure is first raised to the median pressure value and the oscillating pressure is started to be applied. The oscillation pressure parameters are: the median pressure is 10-200 MPa, the amplitude is 1-100 MPa, and the frequency is 0.1-50 Hz; and (3) performing heat preservation from the step (2) to the step (3) and finishing connection, wherein the heat preservation time is 1-120 min. The heat preservation time in the step 2 is very short, and the temperature of the sample is guaranteed to be consistent with the furnace temperature, so that specific limitation is not made; the incubation time in step 3 is the incubation time under the applied pressure.
Example 1
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 10 mm, height: 25 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples as shown in FIG. 1, and heating the samples to 1450 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 75MPa, the amplitude is 35MPa, and the frequency is 2Hz; the incubation time was 60min.
The joint samples obtained in example 1 were tested for breaking strength and evaluated by a three-point bending method, the dimensions of the test samples being 3×4×20 and the span being 15. As a result, FIG. 2 shows that OS is the original sample, and it can be seen from the graph that when the connection pressure is 75.+ -.35 MPa, the bending strength of the corresponding sample DJ 75.+ -. 35/2 is 1552.+ -. 225MPa. Compared with the original sample, the strength of the sample connected by the oscillation pressure auxiliary is not reduced, the performance is obviously improved, the strength of the connected sample is improved by more than one time, and the defect of reduced performance of the traditional connecting material is overcome.
The fracture toughness of the test pieces before and after joining of example 1 was tested using the vickers indentation method, and the results are shown in fig. 3. As can be seen from the figure, the fracture toughness of the samples after connection was not reduced but slightly improved. The vibration pressure auxiliary connection improves the strength of the material, and meanwhile, the toughness of the material is not lost, so that the problem that the strength and the toughness are contradictory is solved.
Example 1 SEM images of the front and rear surfaces of the joint and the fracture are shown in fig. 4 and 5, and it can be seen from the figures that there are significant pores and micro cracks in the sample before the joint, which are the main reasons for the lower strength of the original sample. By adopting the oscillation pressure auxiliary connection, obvious air holes and micro cracks are hardly observed in the connected samples, the microstructure of the material is obviously optimized, and the microstructure is a main reason for obviously improving the strength of the material. As can be seen from fig. 5, the ratio of the crystal-through fracture of the sample after joining is significantly increased compared with the original sample, meaning that the grain boundary strength is significantly increased, which is also one reason why the strength of the material after joining is improved.
Example 2
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 5mm, height: 15 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1800 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 200MPa, the amplitude is 100MPa, and the frequency is 50Hz; the incubation time was 1min.
Example 3
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 50mm, height: 120 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1800 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 50MPa, the amplitude is 25MPa, and the frequency is 10Hz; the incubation time was 60min.
Example 4
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 500 mm, height: 1200 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1800 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 10MPa, the amplitude is 1MPa, and the frequency is 0.1Hz; the incubation time was 120min.
Example 5
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 5mm, height: 15 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1400 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 200MPa, the amplitude is 100MPa, and the frequency is 0.1Hz; the incubation time was 1min.
Example 6
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 50mm, height: 120 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1400 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 50MPa, the amplitude is 25MPa, and the frequency is 10Hz; the incubation time was 60min.
Example 7
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 500 mm, height: 1200 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1400 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 10MPa, the amplitude is 1MPa, and the frequency is 50Hz; the incubation time was 120min.
Example 8
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 5mm, height: 15 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1000 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 200MPa, the amplitude is 100MPa, and the frequency is 0.1Hz; the incubation time was 1min.
Example 9
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 50mm, height: 120 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1000 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 50MPa, the amplitude is 25MPa, and the frequency is 10Hz; the incubation time was 60min.
Example 10
Step 1: the yttrium stable zirconia ceramics with the average grain diameter of 400nm are processed into a cylinder shape by wire cutting, and the size is that: diameter 500 mm, height: 1200 mm. The ceramic was mechanically polished in such a manner that the grain sizes of the diamond polishing papers were 9 μm, 6 μm, 3 μm, and 1 μm in this order, and finally a polished sample having a roughness of the joint end face of 1 μm was obtained.
Step 2: connecting the polished samples according to the method shown in FIG. 1, and heating the samples to 1000 ℃; wherein the vacuum degree in the sintering process is more than 10Pa.
Step 3: applying periodically-changing oscillation pressure, wherein the median pressure is 10MPa, the amplitude is 1MPa, and the frequency is 50Hz; the incubation time was 120min.
The application adopts an oscillation auxiliary mode to connect ceramics, wherein zirconia ceramics are connected, and other ceramics can also be connected by adopting the mode. On one hand, the method accelerates mass transfer by oscillating pressure, and effectively eliminates air holes; on the other hand, the oscillation pressure improves the plastic deformation capability of the material, effectively bridges microcracks under shear strain, and introduces defects such as dislocation, twin crystal, stacking fault and the like near the grain boundary to strengthen the grain boundary. The strength of the ceramic is not reduced after connection, but the strength of the ceramic can be obviously improved, and the requirement of industrial development on higher-performance materials is met.
Claims (4)
1. An oscillation pressure assisted ceramic joining method comprising the steps of:
step 1: polishing the ceramic samples, stacking the samples to be connected, and fully contacting the samples;
step 2: heating the sample to 1000-1800 ℃, and applying pressure to the design value from top to bottom;
step 3: applying periodically-changing oscillating pressure, stopping applying the pressure after connection is completed, and cooling to obtain connected ceramic;
firstly, increasing the pressure to a pressure median value, and starting to apply oscillation pressure;
The oscillation pressure parameters are: the median pressure is 10-200 MPa; the amplitude is 1-100 MPa, the frequency is 0.1-50 Hz, and the time for applying the oscillating pressure is 1-120 min.
2. The method for joining ceramics with assistance of oscillating pressure according to claim 1, wherein the roughness of the contact surface of the sample in the step 1 is not more than 1 μm.
3. The method of claim 1, wherein the ceramic is a zirconia ceramic.
4. The method of claim 1, wherein the stacked samples of step 1 are subjected to a predetermined pressure to be in sufficient contact.
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| Densification and grain growth in oscillatory pressure sintering of alumina toughened zirconia ceramic composites;Fan, Jianye等;JOURNAL OF ALLOYS AND COMPOUNDS;20201231;全文 * |
| Transparent YAG ceramic/sapphire composite fabricated by pressureless direct thermal diffusion bonding;Feng, Zhe等;JOURNAL OF THE EUROPEAN CERAMIC SOCIETY;20211231;全文 * |
| 振荡压力烧结技术制备高性能碳化硅陶瓷;徐广平等;中国陶瓷;20220305;全文 * |
| 振荡压力烧结氮化硅陶瓷微观形貌及其力学性能;秦笑威;盛利文;李双;谢志鹏;;硅酸盐学报;20201231(第06期);全文 * |
| 模拟核芯FCM燃料的振荡烧结行为研究;何宗倍等;无机材料学报;20240122;全文 * |
| 高熵合金/陶瓷复合点阵结构成形及性能研究;平子龙;万方数据;20231130;全文 * |
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