CN114315402B - 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
- Publication number
- CN114315402B CN114315402B CN202210024460.2A CN202210024460A CN114315402B CN 114315402 B CN114315402 B CN 114315402B CN 202210024460 A CN202210024460 A CN 202210024460A CN 114315402 B CN114315402 B CN 114315402B
- Authority
- CN
- China
- Prior art keywords
- silicon carbide
- carbide ceramic
- welding
- flux
- powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Ceramic Products (AREA)
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: (1) pretreatment: 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; (2) preparing flux into paste; (3) pasting, namely brushing the welding flux prepared into the paste on the welding surfaces of the two silicon carbide ceramics; (4) and (3) welding, namely putting 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 existing soldering flux for soldering is poor in the connection performance of ceramic-ceramic or ceramic-metal, and the parts to be connected before connection are lack of effective treatment.
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:
(1) pretreatment: 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;
(2) preparing the flux into paste, namely mixing the flux and an organic solvent to prepare the paste;
(3) pasting, namely brushing the welding flux prepared into the paste on the welding surfaces of the two silicon carbide ceramics, wherein the thickness of the welding flux is 100 mu m;
(4) and (3) welding, namely placing the two silicon carbide ceramics into a clamping tool, brazing in a heat treatment furnace at 1400 ℃/15 minutes under the argon atmosphere, wherein the heating rate and the cooling rate are less than or equal to 5 ℃/min.
In one or more specific embodiments of the present application, in the (1), 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, in the (2), the organic solvent is a PVA solution, and the mass ratio of the flux to the PVA solution =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 ℃/2h.
The invention also provides a connector of the silicon carbide ceramic.
The connecting head of the silicon carbide ceramic is formed by the connecting 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 ultrasonic cleaning for 20min in an acetone solution;
FIG. 2 is an enlarged photograph of a braze joint.
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 Si powder, 2.5kg Ti powder, 2.5kg Zr powder, 12.5kg B powder, 1.5kg Fe powder, 8.5kg Cu powder and 1.5kg Hf powder are mixed in an agate mortar and ground uniformly, then the mixture is placed in a graphite crucible for sintering under the sintering condition of 1400 ℃/2h, and after sintering is finished, the mixture is placed in a planetary ball mill for fine grinding and screening to obtain the 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 at the sintering condition of 1400 ℃/2h, placing in a planetary ball mill for fine grinding and screening after sintering, and obtaining the welding 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:
(1) pretreatment, namely polishing a ceramic-10X 3mm shearing sample piece and a 20X 10X 3mm stretching sample piece by a palm brush (sequentially polishing the ceramic shearing sample piece by water-based sand paper with the roughness of 300-2000 meshes step by step, polishing each piece by the sand paper with the roughness for 30 min) → a silicon carbide coating (namely coating the silicon carbide coating on the surface of the ceramic shearing sample piece, wherein the silicon carbide coating 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 and the adhesion force with staggered welding flux during welding on the other hand) → 30 minutes ultrasonic cleaning by an acetone solution → 20 minutes natural drying → 20 minutes ultrasonic cleaning by alcohol → 20 minutes natural drying → 30 minutes cleaning by deionized water → 40 minutes drying by an air drier at 120 ℃. Through sanding, secondary ultrasonic cleaning and primary deionized water cleaning, on one hand, 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 on the other hand, 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) And (3) preparing a flux paste, namely mixing the flux and PVA solution =4:1 (mass ratio) to prepare the paste.
(3) And (3) pasting, namely brushing the welding flux prepared into the paste on the welding surface of the ceramic sample by a manual screen printing table to form the thickness of 100 mu m.
(4) And (3) welding, namely putting the ceramic sample piece into a clamping tool after finishing paste coating, and brazing in an argon atmosphere through a heat treatment furnace at 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 | √ | √ | √ |
| Percentage 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 (7)
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:
(1) pretreatment: polishing the parts to be welded of the two silicon carbide ceramics, and then respectively carrying out ultrasonic cleaning by an acetone solution, ultrasonic cleaning by alcohol and cleaning by deionized water;
(2) preparing the flux into paste, namely mixing the flux and an organic solvent to prepare the paste; the welding flux is formed by grinding and sintering 30-40 parts by weight of Si powder, 1-3 parts by weight of Ti powder, 1-4 parts by weight of Zr powder, 10-15 parts by weight of B powder, 1-2 parts by weight of Fe powder, 5-10 parts by weight of Cu powder and 1-5 parts by weight of Hf powder;
(3) pasting, namely brushing the welding flux prepared into the paste on the welding surfaces of the two silicon carbide ceramics, wherein the thickness of the welding flux is 100 mu m;
(4) and (3) welding, namely placing the two silicon carbide ceramics into a clamping tool, brazing in a heat treatment furnace at 1400 ℃/15 minutes under the argon atmosphere, wherein the heating rate and the cooling rate are less than or equal to 5 ℃/min.
2. The method for joining silicon carbide ceramics according to claim 1, wherein in the step (1), 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 bonding silicon carbide ceramics according to claim 1, wherein in the step (1), before the ultrasonic cleaning with the acetone solution, the portions to be welded of the two silicon carbide ceramics are further coated with a silicon carbide coating.
4. The method for bonding silicon carbide ceramics according to any one of claims 1 to 3, wherein in the step (2), 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 preparing the flux for silicon carbide ceramic bonding according to claim 1, wherein the sintering parameter is 1400 ℃/2h.
6. A joint of silicon carbide ceramics, which is formed by the joining method of silicon carbide ceramics according to any one of claims 1 to 5.
7. A silicon carbide ceramic comprising at least two or more silicon carbide ceramic elements, wherein adjacent two of the silicon carbide ceramic elements are joined together by the joint of the silicon carbide ceramic according to claim 6.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210024460.2A CN114315402B (en) | 2022-01-11 | 2022-01-11 | Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210024460.2A CN114315402B (en) | 2022-01-11 | 2022-01-11 | Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114315402A CN114315402A (en) | 2022-04-12 |
| CN114315402B true CN114315402B (en) | 2023-03-14 |
Family
ID=81026068
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210024460.2A Active CN114315402B (en) | 2022-01-11 | 2022-01-11 | Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114315402B (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5447683A (en) * | 1993-11-08 | 1995-09-05 | General Atomics | Braze for silicon carbide bodies |
| CN101628364B (en) * | 2009-07-08 | 2012-06-06 | 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 |
| CN106112309B (en) * | 2016-07-27 | 2018-02-23 | 江苏科技大学 | A kind of brazing material for SiC ceramic soldering and the technique using material progress soldering |
| CN107457499B (en) * | 2017-08-09 | 2020-01-17 | 合肥工业大学 | High-temperature solder preparation and brazing process for silicon carbide ceramic and composite material thereof |
| CN109877413B (en) * | 2019-02-01 | 2022-04-29 | 北方民族大学 | Brazing material for SiC ceramic brazing and brazing method |
-
2022
- 2022-01-11 CN CN202210024460.2A patent/CN114315402B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN114315402A (en) | 2022-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110330356B (en) | Silicon carbide ceramic brazing connection method | |
| CN107649758B (en) | A method of porous silicon nitride ceramic and invar alloy are brazed using composite soldering | |
| CN105522244B (en) | A kind of low temperature glass method for welding of ultrasonic assistant | |
| CN105643038B (en) | Brazed porous Si3N4The method of ceramics and Invar alloys | |
| CN110369820B (en) | Method for brazing Hastelloy N alloy by adopting Ni-Cr-W-B-Si-Fe brazing filler metal | |
| CN105149717A (en) | Silicon-based ceramic surface metallization method | |
| CN105418131A (en) | Alumina ceramic low temperature brazing connection method | |
| CN109047963B (en) | CfComposite brazing connection method of/C composite material and nickel-based high-temperature alloy | |
| CN101733497A (en) | Hard soldering method of high volume fraction SiC particle-reinforced Al matrix composite and kovar alloy dissimilar material | |
| CN100584801C (en) | Braze welding method of composite powder used for carbon/silicon carbide and niobium or niobium alloy | |
| CN102430829A (en) | Brazing method for ZrB2-based material | |
| CN108838504A (en) | It is a kind of for spread connection silicon carbide ceramics composite interlayer and its Joining Technology | |
| CN104496511B (en) | A kind of online reaction forming method of ceramic form | |
| CN114315402B (en) | Connection method of silicon carbide ceramic, silicon carbide ceramic connector and silicon carbide ceramic | |
| CN111843165B (en) | Diffusion connection method for diamond micro-channel | |
| CN114346523B (en) | Welding flux for silicon carbide ceramic connection and preparation method thereof | |
| CN108555476B (en) | Composite brazing filler metal for brazing quartz fiber reinforced composite ceramic and Invar alloy and preparation method and brazing method thereof | |
| CN112122826A (en) | Soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and method and application thereof | |
| CN106242606B (en) | A method of utilizing Zr-Ni base solder brazing ZrB2-SiC composite ceramics | |
| CN114513869B (en) | Binding post for aluminum nitride ceramic device and fixing process thereof | |
| CN114133264B (en) | Method for connecting silicon carbide ceramic composite material and nickel-based high-temperature alloy and joint | |
| CN113182631B (en) | Method for preparing high-strength C/C composite material and TC4 alloy joint | |
| CN110026634B (en) | Method for brazing carbon fiber reinforced carbon-based composite material by using Si-Zr high-temperature brazing filler metal | |
| CN114749743A (en) | High-temperature connection method for brazing C/C composite material and Ni-based alloy by adopting pure Cu | |
| CN114315401A (en) | Transient liquid phase connection method of alumina ceramics |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |