CN105060914A - Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion - Google Patents
Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion Download PDFInfo
- Publication number
- CN105060914A CN105060914A CN201510429864.XA CN201510429864A CN105060914A CN 105060914 A CN105060914 A CN 105060914A CN 201510429864 A CN201510429864 A CN 201510429864A CN 105060914 A CN105060914 A CN 105060914A
- Authority
- CN
- China
- Prior art keywords
- carbon
- carbon composite
- temperature
- attachment
- 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.)
- Pending
Links
Landscapes
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a carbon/carbon composite material connection method resisting high-temperature molten salt corrosion. According to the invention, nickel powder and silicon powder are mixed according to a Ni:Si molar ratio of 1:2-3:1; the mixture is alloyed with a high-energy ball milling method, such that Ni-Si compound alloy powder is obtained; the Ni-Si compound alloy powder is uniformly applied on connection surfaces of carbon/carbon composite materials; the materials with the powder are heated to a temperature of 900-1200 DEG C with a heating speed of 10-15 DEG C/min under an environment with a vacuum degree lower than 10<-2>Pa, and the temperature is maintained for 3h; and the temperature of the materials is then reduced to room temperature with a cooling speed of 50-100 DEG C/min. The invention also discloses a carbon/carbon composite material member which has carbon/carbon composite material parts connected with the above method. Compared to prior arts, with the method provided by the invention, an obtained connection layer has excellent high-temperature molten salt corrosion resistance, greatly improved overall connection strength, and more uniform connection strength distribution.
Description
Technical field
The present invention relates to a kind of carbon/carbon composite method of attachment, particularly relate to a kind of carbon/carbon composite method of attachment of high temperature resistant melt brine corrosion.
Background technology
Carbon/carbon composite has excellent a series of excellent properties such as mechanical behavior under high temperature, good thermal shock resistance, high heat conductance, low-expansion coefficient, good chemical stability, thus is widely used in the fields such as Aeronautics and Astronautics, military project, nuclear energy.Because carbon/carbon composite has good chemical stability and mechanical behavior under high temperature, can be used for preparing the interchanger in the mesophase spherule interchanger of Estimation of Nuclear Hydrogen Production and solar thermal collection system.Complex structure, the size of interchanger are larger, and structural integrity requires high, chopped carbon fiber can be adopted to strengthen or two dimension, three-dimensional or multidimensional Carbon fibe precast body, through chemical vapour deposition or resin, bituminizing-charring process repeatedly densification obtain the sheet material of desired size.After the parts such as the machined one-tenth heat exchange fin of sheet material and runner, each parts must be linked together, complete interchanger could be formed.
Realize that the method that carbon/carbon composite connects mainly contains mechanical connection, bonding connection, brazing are connected with diffusion welding at present.The mechanical connection of carbon/carbon composite mainly adopts refractory metal or carbonaceous bolt, nut carries out fastening.The jointing that machine riveting is formed forms larger stress concentration around bolt or tack hole, and the shear strength of joint and incompressible intensity are reduced.Bonding connection technique is simple, easy construction, cheap, but articulamentum can not react with carbon matrix material, causes strength of joint lower.Brazing and diffusion welding connects mainly introduces silicon, titanium, silver-colored isoreactivity metal powder in weld layer, increases the wettability of solder and carbon/carbon composite, improves welding strength.For brazing and diffusion welding, the articulamentum material of employing mainly contains Ti-Zr-Ni-Cu, Al-Ti, Ti-Cu-Be, Ag-Cu-Ti, Cu-Ti-TiB2, Ni-Ti, TiC-Si, Ni-Si, Ti-Ni-Si etc.Because the articulamentum containing the element such as Ti, Zr, Cu, Al, Ag, Si is being all corroded with during high-temperature molten salt medium contact in interchanger, thus strength of joint can be caused to reduce and impact the work-ing life of heat exchanger.
Document " Guo Lingjun etc.; the mechanical property of C/C matrix material and nickel base superalloy jointing and microtexture; Rare Metals Materials and engineering; 2011; 40(1): 111-114 " reports and adopts Ni powder and Si powder as middle layer connecting material, adopt vacuum hot-pressing process successfully to achieve the connection of C/C matrix material and nickel base superalloy, the intensity of jointing reaches 12.6MPa.But, because its method adopted is that the form directly simply mixed with Ni powder and Si powder carries out vacuum hotpressing, therefore Ni and Si free responding under high temperature and certain pressure, cause reactant in middle layer more and do not fix, the strength decentralization making final articulamentum is comparatively large and strength of joint is lower.
Summary of the invention
Technical problem to be solved by this invention is to overcome prior art deficiency, a kind of carbon/carbon composite method of attachment of high temperature resistant melt brine corrosion is provided, except there is excellent high temperature resistant molten salt corrosive property, adopt the method obtain articulamentum integrated connection intensity to be largely increased and strength of joint is more evenly distributed.
The present invention specifically solves the problems of the technologies described above by the following technical solutions:
A carbon/carbon composite method of attachment for high temperature resistant melt brine corrosion, the ratio first according to Ni:Si mol ratio being 1:2 ~ 3:1, by nickel powder and silica flour mixing, then utilizes the method for high-energy ball milling to make its alloying, obtains Ni-Si compounds bronze; The joint face of carbon/carbon composite to be connected evenly applies described Ni-Si compounds bronze, and in low vacuum in 10
-2under the environment of Pa, first with 10 ~ 15
othe temperature rise rate of C/min is warming up to 900 ~ 1200
oc is also incubated 3 hours, then with 50 ~ 100
othe rate of temperature fall of C/min is cooled to room temperature.
Preferably, the granularity of described nickel powder is 200 ~ 400 orders, and purity is 99.9%; The granularity of silica flour is 200 ~ 400 orders, and purity is 99.5%.
Preferably, the concrete technology parameter of described high-energy ball milling is as follows: ratio of grinding media to material is 20:1 ~ 40:1, and Ball-milling Time is 20 ~ 50 hours, and drum's speed of rotation is 200 ~ 500rpm.
Preferably, Ni:Si mol ratio is 1:1.
Preferably, before coating Ni-Si compounds bronze, dehydrated alcohol, acetone, washed with de-ionized water carbon/carbon composite to be connected is first used, then 120 ~ 150
oc dries 2 hours.
Following technical scheme can also be obtained according to identical invention thinking:
A kind of carbon/carbon composite component, comprises at least two interconnective carbon/carbon composite parts, and described carbon/carbon composite parts are interconnected by as above method of attachment described in arbitrary technical scheme.
Preferably, described carbon/carbon composite component is used for the interchanger in the mesophase spherule interchanger of Estimation of Nuclear Hydrogen Production or solar thermal collection system.
Compared to existing technology, the present invention has following beneficial effect:
The present invention adopts Ni-Si compounds bronze as middle layer, liguid infiltration reaction method is adopted to process, achieve liquid Ni-Si compound alloy to the infiltration in carbon/carbon composite hole on the one hand, the Ni-Si compound alloy be impregnated into after cooling in carbon/carbon composite hole plays mechanical pinning effect, enhances strength of joint; On the other hand, the Si in liquid Ni-Si compound alloy can react with the C element in matrix material and generate SiC, further enhancing strength of joint.After tested, the strength of joint between the carbon/carbon composite parts of the inventive method is adopted to reach 13.1-20.4MPa, far above the level that prior art can reach.
In the inventive method, exceeded the fusing point of Ni-Si compound alloy owing to connecting temperature, liquid Ni-Si compound alloy can infiltrate in the hole of carbon/carbon composite that, without the need to independent pressurization, therefore technique is simpler by nature under vacuo.
Embodiment
For the deficiency of the existing carbon/carbon composite interconnection technique based on nickel base superalloy, thinking of the present invention utilizes Ni-Si compound alloy as articulamentum, liguid infiltration reaction method is adopted to make liquid Ni-Si compound alloy be impregnated in the hole of carbon/carbon composite, and the Si in Ni-Si compound alloy and the C in carbon/carbon composite reacts and generates SiC, thus strengthen strength of joint.
Carbon/carbon composite method of attachment proposed by the invention is specific as follows: the ratio first according to Ni:Si mol ratio being 1:2 ~ 3:1, by nickel powder and silica flour mixing, then utilizes the method for high-energy ball milling to make its alloying, obtains Ni-Si compounds bronze; The joint face of carbon/carbon composite to be connected evenly applies described Ni-Si compounds bronze, and in low vacuum in 10
-2under the environment of Pa, first with 10 ~ 15
othe temperature rise rate of C/min is warming up to 900 ~ 1200
oc is also incubated 3 hours, then with 50 ~ 100
othe rate of temperature fall of C/min is cooled to room temperature.
Because the present invention is that the Ni-Si compound alloy that obtains using high-energy ball milling is as articulamentum, in conjunction with the liguid infiltration reaction process optimized, in connection procedure, liquid Ni-Si compound alloy is to the infiltration in carbon/carbon composite hole, the Ni-Si compound alloy be impregnated into after cooling in carbon/carbon composite hole can play mechanical pinning effect, enhances strength of joint; On the other hand, the Si in liquid Ni-Si compound alloy can react with the C element in matrix material and generate SiC, further enhancing strength of joint; In addition, under being in vacuum condition, liquid Ni-Si compound alloy can infiltrate without the need to independent pressurization in the hole of carbon/carbon composite by nature, therefore requires lower to instrument and supplies.
For the ease of public understanding, with several specific embodiment, technical solution of the present invention is further described below.
embodiment 1
1) by Ni:Si=2:1(mol ratio) take Ni powder and Si powder (nickel powder granularity 200 ~ 400 order, purity 99.9%; Silicon particle size 200 ~ 400 order, purity 99.5%);
2) high energy ball mill is adopted to carry out ball milling alloying (ratio of grinding media to material=(20 ~ 40): 1, Ball-milling Time 20 ~ 50 hours, drum's speed of rotation 200 ~ 500rpm) by after Ni powder and the mixing of Si powder;
3) with dehydrated alcohol, acetone, after washed with de-ionized water carbon/carbon composite to be connected 120 ~ 150
oc dry 2 hours for subsequent use;
4) to be connected that Ni-Si compounds bronze is evenly coated on carbon/carbon composite is placed in vacuum hotpressing stove, and makes the low vacuum of vacuum hotpressing stove in 10
-2pa;
5) with 10 ~ 15
ovacuum hotpressing stove is warming up to 900 by the temperature rise rate of C/min
oc is incubated 3 hours;
6) with 50 ~ 100
ovacuum hotpressing stove is cooled to room temperature by the rate of temperature fall of C/min.
After testing, the shearing resistance of the carbon/carbon composite articulamentum adopting aforesaid method to prepare is 13.1MPa.
embodiment 2:
1) by Ni:Si=1:2(atomic ratio) take Ni powder and Si powder (nickel powder 200 ~ 400 order, purity 99.9%; Silica flour 200 ~ 400 order, purity 99.5%);
2) high energy ball mill is adopted to carry out ball milling alloying (ratio of grinding media to material=(20 ~ 40): 1, Ball-milling Time 20 ~ 50 hours, drum's speed of rotation 200 ~ 500rpm) by after Ni powder and the mixing of Si powder;
3) with dehydrated alcohol, acetone, after washed with de-ionized water carbon/carbon composite to be connected 120 ~ 150
oc dry 2 hours for subsequent use;
4) to be connected that Ni-Si compounds bronze is evenly coated on carbon/carbon composite is placed in vacuum hotpressing stove, and makes the low vacuum of vacuum hotpressing stove in 10
-2pa;
5) with 10 ~ 15
ovacuum hotpressing stove is warming up to 1000 by the temperature rise rate of C/min
oc is incubated 3 hours;
6) with 50 ~ 100
ovacuum hotpressing stove is cooled to room temperature by the rate of temperature fall of C/min.
After testing, the shearing resistance of the carbon/carbon composite articulamentum adopting aforesaid method to prepare is 15.7MPa.
embodiment 3:
1) by Ni:Si=1:1(atomic ratio) take Ni powder and silica flour (nickel powder 200 ~ 400 order, purity 99.9%; Silica flour 200 ~ 400 order, purity 99.5%);
2) high energy ball mill is adopted to carry out ball milling alloying (ratio of grinding media to material=(20 ~ 40): 1, Ball-milling Time 20 ~ 50 hours, drum's speed of rotation 200 ~ 500rpm) by after Ni powder and the mixing of Si powder;
3) with dehydrated alcohol, acetone, after washed with de-ionized water carbon/carbon composite to be connected 120 ~ 150
oc dry 2 hours for subsequent use;
4) Ni-Si compounds bronze is evenly applied with to be connected of carbon/carbon composite on be placed in vacuum hotpressing stove, and make the low vacuum of vacuum hotpressing stove in 10
-2pa;
5) with 10 ~ 15
ovacuum hotpressing stove is warming up to 1100 by the temperature rise rate of C/min
oc is incubated 3 hours;
6) with 50 ~ 100
ovacuum hotpressing stove is cooled to room temperature by the rate of temperature fall of C/min.
After testing, the shearing resistance of the carbon/carbon composite articulamentum adopting aforesaid method to prepare is 20.4MPa.
embodiment 4:
1) by Ni:Si=3:1(atomic ratio) take Ni powder and Si powder (nickel powder 200 ~ 400 order, purity 99.9%; Silica flour 200 ~ 400 order, purity 99.5%);
2) high energy ball mill is adopted to carry out ball milling alloying (ratio of grinding media to material=(20 ~ 40): 1, Ball-milling Time 20 ~ 50 hours, drum's speed of rotation 200 ~ 500rpm) by after Ni powder and the mixing of Si powder;
3) with dehydrated alcohol, acetone, after washed with de-ionized water carbon/carbon composite to be connected 120 ~ 150
oc dry 2 hours for subsequent use;
4) to be connected that Ni-Si compounds bronze is evenly coated on carbon/carbon composite is placed in vacuum hotpressing stove, and makes the low vacuum of vacuum hotpressing stove in 10
-2pa;
5) with 10 ~ 15
ovacuum hotpressing stove is warming up to 1200 by the temperature rise rate of C/min
oc is incubated 3 hours;
6) with 50 ~ 100
ovacuum hotpressing stove is cooled to room temperature by the rate of temperature fall of C/min.
After testing, the shearing resistance of the carbon/carbon composite articulamentum adopting aforesaid method to prepare is 18.6MPa.
Known by the test result of above-described embodiment, the shearing resistance of the carbon/carbon composite articulamentum utilizing method provided by the present invention to obtain, far above the strength of joint of the existing carbon/carbon composite interconnection technique based on nickel base superalloy, is enough to meet the requirement preparing mesophase spherule interchanger.Especially, when the mol ratio of Ni and Si is 1:1, shearing resistance the highest (can 20.4MPa be reached).
The inventive method is utilized to connect carbon/carbon composite parts, can obtain that there is excellent high temperature resistant molten salt corrosive property and the carbon/carbon composite component of superelevation strength of joint, can be used for the interchanger etc. in the mesophase spherule interchanger of such as Estimation of Nuclear Hydrogen Production or solar thermal collection system.The present invention is specially adapted to require stable chemical performance, and the occasion that operating ambient temperature is high and baroque carbon/carbon composite product connect.
Claims (7)
1. the carbon/carbon composite method of attachment of a high temperature resistant melt brine corrosion, it is characterized in that, first the ratio according to Ni:Si mol ratio being 1:2 ~ 3:1, by nickel powder and silica flour mixing, then utilizes the method for high-energy ball milling to make its alloying, obtains Ni-Si compounds bronze; The joint face of carbon/carbon composite to be connected evenly applies described Ni-Si compounds bronze, and in low vacuum in 10
-2under the environment of Pa, first with 10 ~ 15
othe temperature rise rate of C/min is warming up to 900 ~ 1200
oc is also incubated 3 hours, then with 50 ~ 100
othe rate of temperature fall of C/min is cooled to room temperature.
2. carbon/carbon composite method of attachment as claimed in claim 1, is characterized in that, the granularity of described nickel powder is 200 ~ 400 orders, and purity is 99.9%; The granularity of silica flour is 200 ~ 400 orders, and purity is 99.5%.
3. carbon/carbon composite method of attachment as claimed in claim 1, is characterized in that, the concrete technology parameter of described high-energy ball milling is as follows: ratio of grinding media to material is 20:1 ~ 40:1, and Ball-milling Time is 20 ~ 50 hours, and drum's speed of rotation is 200 ~ 500rpm.
4. carbon/carbon composite method of attachment as claimed in claim 1, is characterized in that, Ni:Si mol ratio is 1:1.
5. carbon/carbon composite method of attachment as claimed in claim 1, is characterized in that, before coating Ni-Si compounds bronze, first uses dehydrated alcohol, acetone, washed with de-ionized water carbon/carbon composite to be connected, then 120 ~ 150
oc dries 2 hours.
6. a carbon/carbon composite component, comprise at least two interconnective carbon/carbon composite parts, it is characterized in that, described carbon/carbon composite parts are interconnected by method of attachment as described in any one of Claims 1 to 5.
7. carbon/carbon composite component as claimed in claim 6, is characterized in that, the interchanger in its mesophase spherule interchanger for Estimation of Nuclear Hydrogen Production or solar thermal collection system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510429864.XA CN105060914A (en) | 2015-07-21 | 2015-07-21 | Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510429864.XA CN105060914A (en) | 2015-07-21 | 2015-07-21 | Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105060914A true CN105060914A (en) | 2015-11-18 |
Family
ID=54490495
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510429864.XA Pending CN105060914A (en) | 2015-07-21 | 2015-07-21 | Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105060914A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12012827B1 (en) | 2023-09-11 | 2024-06-18 | Natura Resources LLC | Nuclear reactor integrated oil and gas production systems and methods of operation |
| US12018779B2 (en) | 2022-09-20 | 2024-06-25 | Abilene Christian University | Stabilizing face ring joint flange and assembly thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550020A (en) * | 2009-05-13 | 2009-10-07 | 西北工业大学 | Method for connecting carbon/carbon composite material with nickel-based high-temperature alloy |
| CN101709000A (en) * | 2009-11-27 | 2010-05-19 | 西安交通大学 | Method for connecting SiC ceramic by high-temperature liquid phase |
| CN103193499A (en) * | 2013-04-02 | 2013-07-10 | 江苏大学 | Connection method of carbon/carbon composite material |
| CN103232257A (en) * | 2013-04-02 | 2013-08-07 | 西安交通大学 | Fast connection method of carbon/carbon composite material |
-
2015
- 2015-07-21 CN CN201510429864.XA patent/CN105060914A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550020A (en) * | 2009-05-13 | 2009-10-07 | 西北工业大学 | Method for connecting carbon/carbon composite material with nickel-based high-temperature alloy |
| CN101709000A (en) * | 2009-11-27 | 2010-05-19 | 西安交通大学 | Method for connecting SiC ceramic by high-temperature liquid phase |
| CN103193499A (en) * | 2013-04-02 | 2013-07-10 | 江苏大学 | Connection method of carbon/carbon composite material |
| CN103232257A (en) * | 2013-04-02 | 2013-08-07 | 西安交通大学 | Fast connection method of carbon/carbon composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12018779B2 (en) | 2022-09-20 | 2024-06-25 | Abilene Christian University | Stabilizing face ring joint flange and assembly thereof |
| US12012827B1 (en) | 2023-09-11 | 2024-06-18 | Natura Resources LLC | Nuclear reactor integrated oil and gas production systems and methods of operation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101890590B (en) | Composite soldering material for soldering titanium alloy and ceramic and method for soldering by using same | |
| Wang et al. | Bonding performance and mechanism of a heat-resistant composite precursor adhesive (RT-1000∘ C) for TC4 titanium alloy | |
| CN103553637B (en) | Cubic boron nitride glomerocryst composite with surface coating structure and preparation method thereof | |
| CN110524082B (en) | Method for quickly wetting carbon fibers in ceramic matrix composite by taking Fe as active element | |
| 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 | |
| CN106588064B (en) | The solder and connection method of carbon/carbon compound material and nickel base superalloy | |
| CN102554449B (en) | Method for connecting carbon fiber-reinforced aluminum-based composite material and metal | |
| JP5295129B2 (en) | Method for refractory assembly of carbon material and copper alloy | |
| CN106884159B (en) | The method that carbon-coating coats the preparation method and its assistant brazing C/C composite material and metal of foam carbon/carbon-copper composite material | |
| CN112296472A (en) | Brazing method of graphite material | |
| CN103232257A (en) | Fast connection method of carbon/carbon composite material | |
| CN105060914A (en) | Carbon/carbon composite material connection method resisting high-temperature molten salt corrosion | |
| CN102924109B (en) | Cf/SiC ceramic matrix composite connecting method | |
| CN106216879B (en) | A kind of Cu-TiH2- Ni+B composite solders and its preparation method and application | |
| CN113149687A (en) | Method for connecting ceramic and metal | |
| CN102534300A (en) | Method for preparing in-situ growed carbon nano tube reinforcing TiNi high-temperature solders | |
| CN106736030B (en) | A kind of application method of solder in welding C/SiC composite material and metal | |
| CN104842064B (en) | Method for specially connecting Cf/Al composite material with TiAl | |
| CN112122826A (en) | Soldering paste for brazing titanium-based composite material and silicon nitride ceramic, and method and application thereof | |
| CN100496868C (en) | Novel non-corrosion fluoride solder and preparation method | |
| CN101239420A (en) | Soldering method of composite foil for carbon/silicon carbide and niobium or niobium alloy | |
| CN109467456A (en) | A method of it is modified to carbon-based material surface using metal paste | |
| CN102658368A (en) | Method for connecting carbon fiber reinforced aluminum-based composite with metal | |
| CN101402836B (en) | Organic active gelatinous material and method for welding non-metal and metallic material with glue |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20151118 |