CN114315402A - Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic - Google Patents
Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic Download PDFInfo
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- CN114315402A CN114315402A CN202210024460.2A CN202210024460A CN114315402A CN 114315402 A CN114315402 A CN 114315402A CN 202210024460 A CN202210024460 A CN 202210024460A CN 114315402 A CN114315402 A CN 114315402A
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Abstract
The invention discloses a silicon carbide ceramic connecting method, a silicon carbide ceramic connector and silicon carbide ceramic, wherein a welding flux is welded on a welding surface of one silicon carbide ceramic unit and a welding surface of the other silicon carbide ceramic unit, and the method comprises the following steps: preprocessing: polishing the parts to be welded of the two silicon carbide ceramics, and then respectively carrying out ultrasonic cleaning by using an acetone solution, ultrasonic cleaning by using alcohol and cleaning by using deionized water; preparing paste by using the welding flux; thirdly, pasting, namely brushing the welding flux prepared into the paste on the welding surfaces of the two silicon carbide ceramics; welding, namely placing the two silicon carbide ceramics into a clamping tool and brazing the two silicon carbide ceramics in a heat treatment furnace, wherein the heating rate and the cooling rate are less than or equal to 5 ℃/min. The invention realizes the good connection of SiC ceramics, and the maximum value of the shearing strength of the SiC/welding flux/SiC joint is 150MPa under the conditions of 1400 ℃, the heat preservation time is 10min and the thickness of the brazing filler metal is 2 layers.
Description
Technical Field
The invention relates to the field of aviation materials, in particular to a connection method of silicon carbide ceramics, a connector of the silicon carbide ceramics and the silicon carbide ceramics.
Background
Silicon carbide ceramics have been a material with great development prospect in the field of structural materials due to the advantages of low density, high strength, high elastic modulus, high thermal conductivity and the like, but the preparation processes of the silicon carbide materials at present, including normal pressure sintering, reaction sintering and hot pressing sintering processes with higher requirements on equipment, are difficult to prepare devices with large sizes and complex shapes, so that the further application of the silicon carbide ceramics is limited. At present, the connection process of the silicon carbide ceramics mainly comprises brazing, diffusion welding, a glass solder method, a reaction connection method, a cementing method and the like, compared with other processes, the brazing has more advantages in process practicability and connection performance, and is widely applied to industrial production. The brazing of ceramics needs to solve the problem of wettability of the solder to the ceramics and the problem of thermal stress generated by different thermal expansion coefficients of different materials at a connecting interface.
However, the prior brazing flux joint ceramic-ceramic or ceramic-metal joint has poor performance and lacks effective treatment for the parts to be joined before joining.
Disclosure of Invention
Based on the problems, the invention provides a connection method of silicon carbide ceramics, which realizes good connection of SiC ceramics, and the maximum value of the shearing strength of a SiC/welding flux/SiC joint is 150MPa under the conditions of 1400 ℃, the heat preservation time is 10min and the thickness of a brazing filler metal is 2 layers.
A method of joining a silicon carbide ceramic element to a joining surface of another silicon carbide ceramic element by welding flux to the joining surface of one silicon carbide ceramic element, comprising the steps of:
preprocessing: polishing the parts to be welded of the two silicon carbide ceramics, and then respectively carrying out ultrasonic cleaning by using an acetone solution, ultrasonic cleaning by using alcohol and cleaning by using deionized water;
preparing the flux into paste, namely mixing the flux and an organic solvent to prepare the paste;
thirdly, pasting the welding flux which is prepared into the paste to the welding surfaces of the two silicon carbide ceramics, wherein the thickness of the welding flux is 100 mu m;
welding, namely placing the two silicon carbide ceramics into a clamping tool, and brazing in an argon atmosphere at the temperature rise rate and the temperature reduction rate of less than or equal to 5 ℃/min in a heat treatment furnace at the temperature of 1400 ℃/15 minutes.
In one or more specific embodiments of the present application, in the (r), the acetone solution is ultrasonically cleaned for 30 minutes, the alcohol is ultrasonically cleaned for 20 minutes, and the deionized water is cleaned for 30 minutes.
In one or more specific embodiments of the present application, the organic solvent is a PVA solution, and a mass ratio of the flux to the PVA solution is 4: 1.
In one or more specific embodiments of the present application, the flux is prepared by grinding and sintering 30 to 40 parts by weight of Si powder, 1 to 3 parts by weight of Ti powder, 1 to 4 parts by weight of Zr powder, 10 to 15 parts by weight of B powder, 1 to 2 parts by weight of Fe powder, 5 to 10 parts by weight of Cu powder, and 1 to 5 parts by weight of Hf powder.
In one or more specific embodiments of the present application, the sintering parameter is 1400 ℃/2 h.
The invention also provides a connector of the silicon carbide ceramic.
A silicon carbide ceramic connector is formed by the connection method of the silicon carbide ceramic.
The invention also provides the silicon carbide ceramic.
The silicon carbide ceramic is formed by at least more than two silicon carbide ceramic units, and the adjacent two silicon carbide ceramic units are connected into a whole by the connector of the silicon carbide ceramic.
The principle and the beneficial effects of the invention are as follows:
according to the invention, Ti, Si, Zr, Hf and B are effectively added into Fe and Cu, so that the formed welding flux can effectively realize the wetting of oxide, carbide and nitride ceramics on one hand, and influence the organization structure, strength and fracture morphology of a welding seam on the other hand, the SiC ceramics can be well connected under the conditions of the brazing temperature of 1250-1450 ℃, the heat preservation time of 5-30 min and the brazing filler metal thickness of 50-200 mu m (1-2 layers of brush are arranged on a screen printing table tool), and the maximum value of the shearing strength of the SiC/welding flux/SiC joint is 150MPa under the conditions of 1400 ℃, the heat preservation time of 10min and 2 layers of the brazing filler metal thickness.
Drawings
FIG. 1 is an effect diagram of a brazing sample piece in an acetone solution for ultrasonic cleaning for 20 min;
FIG. 2 is an enlarged photograph of a braze weld.
Detailed Description
The invention will be further explained with reference to the drawings.
Example 1
Mixing 32.55kg of Si powder, 2.45kg of Ti powder, 2kg of Zr powder, 12.3kg of B powder, 1.1kg of Fe powder, 6.5kg of Cu powder and 2.5kg of Hf powder in an agate mortar, uniformly grinding, then placing in a graphite crucible for sintering under the sintering condition of 1400 ℃/2h, and after sintering, placing in a planetary ball mill for fine grinding and screening to obtain the flux product.
Example 2
36.55kg of Si powder, 2.5kg of Ti powder, 2.5kg of Zr powder, 12.5kg of B powder, 1.5kg of Fe powder, 8.5kg of Cu powder and 1.5kg of Hf powder are mixed in an agate mortar and uniformly ground, then the mixture is placed in a graphite crucible for sintering, the sintering condition is 1400 ℃/2h, and after the sintering is finished, the mixture is placed in a planetary ball mill for fine grinding and screening to obtain the welding flux product.
Example 3
Mixing 40kg of Si powder, 2.7kg of Ti powder, 3.5kg of Zr powder, 14.2kg of B powder, 1.5kg of Fe powder, 9.5kg of Cu powder and 1.7kg of Hf powder in an agate mortar, uniformly grinding, then placing in a graphite crucible for sintering under the sintering condition of 1400 ℃/2h, and after sintering, placing in a planetary ball mill for fine grinding and screening to obtain the flux product.
The fluxes prepared in examples 1 to 3 were used for the welding of ceramics to each other by brazing, respectively, and the welding method included the following steps:
preprocessing, namely, polishing a ceramic-10-3 mm shearing sample piece and a 20-10-3 mm stretching sample piece by a brown brush (sequentially polishing the sample pieces by water-based sand paper with the roughness of 300-2000 meshes step by step and polishing the sample pieces by the sand paper with each roughness for 30min), → a silicon carbide coating (namely coating the surface of the ceramic shearing sample piece with a silicon carbide coating which enhances the oxidation resistance of the ceramic sample piece on one hand and enables the surface of the ceramic sample piece to have certain roughness on the other hand so that a welding flux has staggered adhesion force during welding), ultrasonic cleaning by an acetone solution for 30min, natural drying for 20min, ultrasonic cleaning by alcohol for 20min, natural drying for 20min, cleaning by deionized water for 30min, and drying by a blast dryer at 120 ℃ for 40 min. Through sanding with sand paper, secondary ultrasonic cleaning and primary deionized water cleaning, the adhesive force of the welding flux on the surface of an object during brazing is improved, the wettability of the welding flux is improved, and the oxidation of the welding flux is reduced.
FIG. 1 is a graph showing the effect of ultrasonic cleaning of a brazing sample in an acetone solution for 20 min.
② preparing soldering flux paste, namely mixing the soldering flux and PVA solution in a mass ratio of 4:1 to prepare the soldering flux paste.
Thirdly, coating paste, wherein the welding flux prepared into the paste is brushed on the welding surface of the ceramic sample piece through a manual screen printing table, and the thickness is 100 mu m.
Welding, namely placing the ceramic sample piece into a clamping tool after finishing paste coating, and brazing in an argon atmosphere through a heat treatment furnace at the temperature of 1400 ℃/15 minutes, wherein the heating rate and the cooling rate are less than or equal to 5 ℃/min.
And (3) detecting the connecting effect of the ceramic sample after brazing, wherein the process performance of the joint is shown in the following table 1, and the mechanical property is shown in the following table 2.
TABLE 1
| Example 1 | Example 2 | Example 3 | |
| Appearance of weld bead | √ | √ | √ |
| Shape of weld bead | √ | √ | √ |
| Rate of penetration | √ | ○ | △ |
| Detachability of slag | ○ | △ | √ |
Remarking: in Table 1, √ excellent,. smallcircle-,. DELTA. -normal,. times. -defective.
TABLE 2
The welded seam after brazing of the invention is shown in figure 2, and figure 2 is an enlarged photograph of the brazed seam.
According to the invention, Ti, Si, Zr, Hf and B are effectively added into Fe and Cu, so that the formed welding flux can effectively realize the wetting of oxide, carbide and nitride ceramics on one hand, and influence the organization structure, strength and fracture morphology of a welding seam on the other hand, the SiC ceramics can be well connected under the conditions of the brazing temperature of 1250-1450 ℃, the heat preservation time of 5-30 min and the brazing filler metal thickness of 50-200 mu m (1-2 layers of brush are arranged on a screen printing table tool), and the maximum value of the shearing strength of the SiC/welding flux/SiC joint is 150MPa under the conditions of 1400 ℃, the heat preservation time of 10min and 2 layers of the brazing filler metal thickness.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method of joining a silicon carbide ceramic element to a joining surface of another silicon carbide ceramic element by welding flux to the joining surface of one silicon carbide ceramic element, comprising the steps of:
preprocessing: polishing the parts to be welded of the two silicon carbide ceramics, and then respectively carrying out ultrasonic cleaning by using an acetone solution, ultrasonic cleaning by using alcohol and cleaning by using deionized water;
preparing the flux into paste, namely mixing the flux and an organic solvent to prepare the paste;
thirdly, pasting the welding flux which is prepared into the paste to the welding surfaces of the two silicon carbide ceramics, wherein the thickness of the welding flux is 100 mu m;
welding, namely placing the two silicon carbide ceramics into a clamping tool, and brazing in an argon atmosphere at the temperature rise rate and the temperature reduction rate of less than or equal to 5 ℃/min in a heat treatment furnace at the temperature of 1400 ℃/15 minutes.
2. The method for connecting silicon carbide ceramics according to claim 1, wherein in the formula (i), the acetone solution is ultrasonically cleaned for 30 minutes, the alcohol is ultrasonically cleaned for 20 minutes, and the deionized water is cleaned for 30 minutes.
3. The method for connecting silicon carbide ceramics according to claim 1, wherein in the above formula (i), before ultrasonic cleaning with an acetone solution, the portions to be welded of the two silicon carbide ceramics are further coated with a silicon carbide coating.
4. The method of joining silicon carbide ceramics according to any one of claims 1 to 3, wherein the organic solvent is a PVA solution, and the mass ratio of the flux to the PVA solution is 4: 1.
5. The method for bonding silicon carbide ceramics according to any one of claims 1 to 4, wherein the flux is prepared by grinding and sintering 30 to 40 parts by weight of Si powder, 1 to 3 parts by weight of Ti powder, 1 to 4 parts by weight of Zr powder, 10 to 15 parts by weight of B powder, 1 to 2 parts by weight of Fe powder, 5 to 10 parts by weight of Cu powder, and 1 to 5 parts by weight of Hf powder.
6. The method of claim 5, wherein the sintering parameter is 1400 ℃/2 h.
7. A joint of silicon carbide ceramics, which is formed by the method of joining silicon carbide ceramics according to any one of claims 1 to 6.
8. A silicon carbide ceramic comprising at least two or more silicon carbide ceramic units, wherein two adjacent silicon carbide ceramic units are connected to each other by the connecting head of the silicon carbide ceramic according to claim 7.
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| CN202210024460.2A CN114315402B (en) | 2022-01-11 | 2022-01-11 | Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic |
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| CN202210024460.2A CN114315402B (en) | 2022-01-11 | 2022-01-11 | Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic |
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Citations (5)
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|---|---|---|---|---|
| US5447683A (en) * | 1993-11-08 | 1995-09-05 | General Atomics | Braze for silicon carbide bodies |
| CN101628364A (en) * | 2009-07-08 | 2010-01-20 | 哈尔滨工业大学 | In-situ reinforced solid welding wire for welding a welding seam by melting SiC particle reinforced aluminum-based composite material |
| CN106112309A (en) * | 2016-07-27 | 2016-11-16 | 江苏科技大学 | A kind of brazing material for SiC ceramic soldering and use the technique that this material carries out soldering |
| CN107457499A (en) * | 2017-08-09 | 2017-12-12 | 合肥工业大学 | A kind of high-temp solder preparation method and soldering processes for silicon carbide ceramics and its composite |
| CN109877413A (en) * | 2019-02-01 | 2019-06-14 | 北方民族大学 | A kind of brazing material and method for welding for SiC ceramic soldering |
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- 2022-01-11 CN CN202210024460.2A patent/CN114315402B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5447683A (en) * | 1993-11-08 | 1995-09-05 | General Atomics | Braze for silicon carbide bodies |
| CN101628364A (en) * | 2009-07-08 | 2010-01-20 | 哈尔滨工业大学 | In-situ reinforced solid welding wire for welding a welding seam by melting SiC particle reinforced aluminum-based composite material |
| CN106112309A (en) * | 2016-07-27 | 2016-11-16 | 江苏科技大学 | A kind of brazing material for SiC ceramic soldering and use the technique that this material carries out soldering |
| CN107457499A (en) * | 2017-08-09 | 2017-12-12 | 合肥工业大学 | A kind of high-temp solder preparation method and soldering processes for silicon carbide ceramics and its composite |
| CN109877413A (en) * | 2019-02-01 | 2019-06-14 | 北方民族大学 | A kind of brazing material and method for welding for SiC ceramic soldering |
Non-Patent Citations (1)
| Title |
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| 张建军等: ""用铁粉坯连接碳化硅陶瓷界面的微观结构"", 《机械工程材料》 * |
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