CN101067192A - Carbon fiber reinforced nickel-based composite material and producing method thereof - Google Patents
Carbon fiber reinforced nickel-based composite material and producing method thereof Download PDFInfo
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- CN101067192A CN101067192A CN 200710061689 CN200710061689A CN101067192A CN 101067192 A CN101067192 A CN 101067192A CN 200710061689 CN200710061689 CN 200710061689 CN 200710061689 A CN200710061689 A CN 200710061689A CN 101067192 A CN101067192 A CN 101067192A
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Abstract
The present invention discloses one kind of carbon fiber reinforced Ni-base composite material and its preparation process, and relates to metal-base composite material. The carbon fiber reinforced Ni-base composite material consists of carbon fiber 30-35 vol%, Cu 6-8 vol %, and Ni 57-64 vol %. The technological process of preparing the composite material includes the steps of: pre-treatment of carbon fiber, electrodepositing Cu, washing, neutralizing, electrodepositing Ni, electrodepositing Ni to form, washing, stoving, cutting, vacuum hot pressing in mold, and cooling in the furnace. The present invention prepares the composite material in a three-step electrodepositing process, and the composite material has high heat strength, high elastic modulus, low density, high smelting point and other advantages, and may be used in the vane of gas-burning turbine engine, etc.
Description
Technical field
The present invention relates to metal-base composites, particularly carbon fiber reinforced nickel-based composite material (C
f/ Ni) preparation technology.
Background technology
Metal-base composites one of the most promising application is a blade of making gas turbine engine.Therefore this class part has become an important directions of matrix material research at high temperature with near the most heavily stressed work down that existing alloy can bear.
The major part work that metal-base composites is done in recent years all is that the compound system according to aluminium and alloy matrix aluminum carries out, because this matrix manufacturing ratio is easier to, and manufacturing and use temperature are lower, can reduce matrix and fiber-reactive degree in manufacturing processed.But for requiring at high temperature to possess oxidation-resistance is arranged, the gas turbine parts of characteristic such as creep resistance, antifatigue, and aluminum matrix composite does not possess this service requirements.Must adopt more heat-stable nickel, cobalt, iron.Because manufacturing and use temperature are higher, interactional possibility has all increased between the difficulty of manufacturing matrix material and fiber and the matrix.Simultaneously, the matrix material of this class purposes is also required at high temperature to have the fortifying fibre of sufficient intensity and stability, carbon fiber is one of fortifying fibre that meets these requirements.
The metal current based composites is preparation technology mainly contain: solid state fabrication techniques, liquid manufacturing technology and other manufacturing technologies.
Solid state process is meant that matrix is in solid-state in making the metal-base composites process.Because the manufacturing temperature of solid state process is low, so the surface reaction between metallic matrix and the enhancing body is not serious.Solid state process comprises powder metallurgic method, squeeze casting method, hot isostatic pressing method, rolling, hot extrusion method and hot pull method etc.
In solid-state manufacturing process, because carbon fiber filament diameter little (6～8 μ m), the continuous carbon fibre that provides on the market all is pencil (1000/bundle or 2000/bundle), if adopt methods such as powder metallurgic method, squeeze casting method, hot isostatic pressing method, rolling, hot extrusion method and hot pull method to make C
f/ Ni matrix material can cause matrix can not wrap every fiber, therefore causes fiber and the matrix discontinuity in matrix material, so just can not give full play to the enhancement of fiber, and the therefore above solid state process that adopts is not suitable for the little fortifying fibre of diameter.
Liquid phase process is meant that metallic matrix is under the molten state manufacture method with solid-state enhancing volume recombination.Because the fusing point higher (1453 ℃) of nickel, therefore there are the following problems in manufacturing processed: the dipping temperature of (1) fortifying fibre in liquid metal nickel is wayward.(2) because the preparation temperature height, the increased activity of fiber and matrix causes the interaction between fiber and the matrix to strengthen, and is unfavorable for forming the good interface bonding state after compound, thereby influences composite property.(3) the preparation temperature height causes the complexity height of producing apparatus, can increase manufacturing cost like this.Therefore, do not adopt the liquid phase process manufacturing usually for the higher metal-base composites of preparation fusing point.
Make C with additive method (become as physical vapor deposition, chemical vapour deposition and in-situ authigenic etc.)
fThat is that all right is ripe for/Ni composite technology, and facility investment is big, can't guaranteed performance, so generally do not adopt.
Electrodip process prepares metal-base composites and does not have above problem, can make every fiber surface coat the layer of metal matrix in electrodeposition process, thereby has guaranteed even, the continuous distribution of fiber in matrix, can give full play to the enhancement of fiber." Northcentral University " once made overtesting with electrodip process to " C/Cu (Fe) matrix material " preparation technology, and processing step comprises: pre-treatment of carbon fiber, electrodeposit metals, vacuum hotpressing.Test has obtained some achievements in research aspect preparating mechanism, but the concrete technical parameter of preparation composite technology steps such as the component of relevant matrix material, proportioning, electrolyte prescription is still immature, and the technical scheme of industrial application can't be provided.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point of the prior art, a kind of carbon fiber reinforced nickel-based composite material and preparation method thereof is provided.Utilize the C of three steps electro-deposition method preparation
f/ Ni matrix material not only can satisfy the blade service requirements of gas turbine engine, and at high temperature possess oxidation-resistance is arranged, anticorrosive, creep resistance, antifatigue and the little characteristic of distortion.
Technical scheme of the present invention for achieving the above object is:
(1) material structure, component and proportioning
The structure of matrix material is the carbon fiber that copper, nickel are arranged by surface deposition, and parallel longitudinal is arranged and through the slab of pressing, the component of matrix material and proportioning:
Carbon fiber: 30～35% (volume ratios)
Copper: 6～8% (volume ratios)
Nickel: 57～64% (volume ratios)
(2) electrolyte prescription and galvanic deposit parameter
The electrolyte prescription of the first step acid copper and galvanic deposit parameter are as follows:
Solvent: distilled water
CuSO
4·5H
2O (38～43g/L)
C
6H
8O
7 (28～32g/L)
C
4H
4O
6KNa·4H
2O (20～22g/L)
NaOH transfers PH=8～10
OP-21 (emulsifying agent) (0.5～1.0g/L)
I (electric current) 0.1～0.2A
The electrolyte prescription and the galvanic deposit parameter of the second step electric deposition nickel are as follows:
Solvent: distilled water
NiSO
4·7H
2O (290～310g/L)
NiCl·6H
2O (48～52gL)
H
3BO
3 (32～36g/L)
C
12H
25SO
3Na (0.1～0.15g/L)
PH＝6~7
I (electric current) 0.5～0.7A
The electrolyte prescription of the 3rd one-step forming electric deposition nickel and galvanic deposit parameter are as follows:
Solvent: distilled water
NiSO
4·7H
2O (40～42g/L)
NiCl·6H
2O (8～12gL)
H
3BO
3 (32～35g/L)
Na
3C
6H
5O
32H
2O (Trisodium Citrate) (55～62g/L)
C
12H
25SO
3Na (sodium laurylsulfonate) (0.015～0.02g/L)
PH＝6~7
I (electric current) 0.5～0.6A
(3) processing step:
Processing step comprises: the surface preparation of carbon fiber, the first step acid copper, cleaning, neutralization, the second step electric deposition nickel, the 3rd one-step forming electric deposition nickel, taking off the composite filament blank from briquetting roller cleans, dries, cutting composite filament blank is put into mould then, carries out the hot pressing diffusion-bonded in vacuum oven, cools to room temperature with the furnace after hot pressing finishes and comes out of the stove.
C by above-mentioned prepared
fThe concrete performance of/Ni matrix material is as follows:
Matrix material C
f/ Ni (Cu)
Fiber volume fraction (V
f* 100%) 32
Tensile strength (room temperature) (σ b) 781MPa
Tensile strength (800 ℃) (σ b) 432MPa
Unit elongation (room temperature) (δ) 12%
The present invention compared with prior art owing to adopt electrodip process to prepare C
f/ Ni matrix material can make every fiber surface coat the layer of metal matrix in electrodeposition process, thereby has guaranteed even, the continuous distribution of fiber in matrix, can give full play to the enhancement of fiber.Evidence: electrodip process prepares C
f/ Ni matrix material is a kind of effective means.Its advantage is: manufacture method is simple, and cost is low; Can not cause big physical abuse to fiber in the manufacturing processed; Utilize three step electrodip processes to carry out Alloying Treatment, reach the purpose of improving the interface bonding state and improving substrate performance matrix.
The present invention is owing to adopt nickel as body material, and reinforce then strengthens with carbon fiber, and therefore, the outstanding advantage of carbon fiber reinforced nickel-based composite material is high strength, high elastic coefficient, low density, high-melting-point, good high-temperature intensity.
Description of drawings
Fig. 1 is carbon fiber reinforced nickel-based (C
f/ Ni) composite material preparation process schema;
Fig. 2 is for being carbon fiber reinforced nickel-based C
f/ Ni) matrix material electrodeposition technology setting drawing;
Fig. 3 is carbon fiber reinforced nickel-based (C
f/ Ni) the self routing setting drawing in the matrix material galvanic deposit moulding coating bath.
Below in conjunction with accompanying drawing, by preferred embodiment, the present invention is further illustrated.
Embodiment
The carbon fiber that the present invention adopts is homemade middle strong type polyacrylonitrile (PAN) carbon fiber, filament diameter (6～8) μ m, and fasciculation (1000/bundle) can be chosen by design volume proportioning 30～35%.
Its tensile strength is 2200MPa, and Young's modulus is 200GPa, and density is 1.78g/cm
3, carbon content＞95%.
Body material is an electrolytic nickel, and tensile strength is 317MPa, and alloy element copper is an industrial pure copper, and used galvanic deposit medicine is chemical pure.
Process flow sheet of the present invention as shown in Figure 1.
1, pre-treatment of carbon fiber
For avoiding being bonded together between the single fiber and interfibrous wearing and tearing, the fasciculation carbon fiber surface of being bought all scribbles cakingagent, all need before the use cakingagent is removed, at first carbon fiber is wrapped on the steel wiring round, put into then in 320 ℃ of process furnace, turn off the process furnace power supply behind the insulation 30min, be as cold as room temperature with stove and come out of the stove.
2, the first step acid copper
Because carbon fiber and nickel can interact under hot pressing temperature, produce mutual diffusion, carbon fiber surface is produced certain damage, for avoiding the big damage of carbon fiber surface, at first in carbon fiber surface galvanic deposit layer of copper (volume ratio about 6%), and belong to physical bond between copper and the carbon fiber, to not damage of carbon fiber surface, here copper has played the effect of nickel diffusion impervious layer, reaches the purpose of improving the interface bonding state.The volume content of acid copper can be controlled by adjusting the galvanic deposit current density, with the volume percent value that meets design requirement.
The electrolyte prescription of the first step acid copper and galvanic deposit parameter are as follows:
Solvent: distilled water.
First group second group the 3rd group
CuSO
4·5H
2O (38g/L) (40g/L) (43g/L)
C
6H
8O
7 (28g/L) (30g/L) (32g/L)
C
4H
4O
6KNa·4H
2O?(20g/L) (21g/L) (22g/L)
NaOH transfers PH=8 to transfer PH=9 to transfer PH=10
(0.5g/L) (0.8g/L) (1.0g/L) for OP-21 (emulsifying agent)
I (electric current) 0.1A 0.15A 0.2A
Device transmission speed: 0.5m/min
Pre-deposition copper electrolysis cells length: 1.3m
3, clean, neutralize
Because the first step galvanic deposit electrolytic solution belongs to alkaline liquid, the second step galvanic deposit electrolytic solution belongs to slant acidity liquid, just can enter the second step galvanic deposit electrolytic solution so the carbon fiber surface of the acid copper that comes out from the first step galvanic deposit electrolytic solution need be handled through rinse bath and neutralizing well, avoid the second step galvanic deposit electrolytic solution is polluted.
4, the second step electric deposition nickel
Carbon fiber surface to the first step acid copper carries out electric deposition nickel.The volume content of electric deposition nickel can be controlled by adjusting the galvanic deposit current density, with the volume percent value that meets design requirement.
The electrolyte prescription and the galvanic deposit parameter of the second step electric deposition nickel are as follows:
Solvent: distilled water
First group second group the 3rd group
NiSO
4·7H
2O (290g/L) (300g/L) (310g/L)
NiCl·6H
2O (48gL) (50gL) (52gL)
H
3BO
3 (32g/L) (34g/L) (36g/L)
C
12H
25SO
3Na (0.1g/L) (0.12g/L) (0.15g/L)
HCl transfers PH=6 to transfer PH=6 to transfer PH=7
I (electric current) 0.5A 0.6A 0.7A
Device transmission speed: 0.5m/min
Thicken electric deposition nickel slot length: 1.5m
4, the 3rd one-step forming electric deposition nickel
Carbon fiber through the second step electric deposition nickel is wrapped in the surface coats on the briquetting roller of one deck nickel foil, in the moulding coating bath, carry out electric deposition nickel, finally form the composite filament blank.The volume content of electric deposition nickel can be controlled by adjusting the galvanic deposit current density, with the volume percent value that meets design requirement.
The electrolyte prescription of the 3rd one-step forming electric deposition nickel and galvanic deposit parameter are as follows:
Solvent: distilled water
First group second group the 3rd group
NiSO
4·7H
2O (40g/L) (41g/L) (42g/L)
NiCl·6H
2O (8gL) (10gL) (12gL)
H
3BO
3 (32g/L) (33g/L) (35g/L)
Na
3C
6H
5O
32H
2(55g/L) (60g/L) (62g/L) for O (Trisodium Citrate)
C
12H
25SO
3(0.15g/L) (0.17g/L) (0.02g/L) for Na (sodium laurylsulfonate)
HCl transfers PH=6 to transfer PH=6 to transfer PH=7
I (electric current) 0.5A 0.5A 0.6A
5, clean, dry
Composite filament blank through the 3rd step electric deposition nickel is taken off from briquetting roller, wash surperficial electrolytic solution, then oven dry (in 110 ℃ of drying bakers, being incubated 2 ~ 3 hours) with clear water.
6, shear, adorn mould
The composite filament blank of oven dry is sheared, successively stacked in the graphite jig then.
7, vacuum hotpressing
The mould that the composite filament blank is housed is put into process furnace, be higher than 2 * 10
-2Be incubated after being heated to hot pressing temperature with stove under the vacuum tightness of Pa, carry out the hot pressing DIFFUSION TREATMENT behind the insulation certain hour, the hot pressing diffusion finishes the back furnace cooling comes out of the stove to room temperature, and finally the matrix material blank is hot pressed into the matrix material slab on the vacuum hotpressing unit.
The vacuum hot-pressing process parameter is as follows:
Vacuum tightness:＞2 * 10
-2Pa
Hot pressing temperature: 1080～1120 ℃
Hot pressing pressure: 30MPa
Hot pressing time: 40min
Realize process unit of the present invention as shown in Figure 2.
Carbon fiber 1 is drawn by actinobacillus wheel 6, drives by transmission rig 4.At first, clean through rinse bath 8 then, through neutralizing well 9 neutralizations, enter moulding nickel bath 11 again by connecton layout 5 again, be wrapped at last on the briquetting roller 12, form the composite filament blank through nickel bath 10 through pre-copper plating groove 7.Be connected with power supply 2 and electrolyte filtering pump 3 with each coating bath.
The self routing device of matrix material in galvanic deposit moulding coating bath as shown in Figure 3.
Composite filament 1 is passed by the nut 14 with screw mandrel 13 engagement, around to briquetting roller 16.Composite filament 1 is driven by screw mandrel 13 in the electrolytic action nickel deposited of nickel pole plate 15, and series arrangement forms carbon fiber reinforced nickel-based composite filament blank 17 on briquetting roller 16.
Claims (7)
1. carbon fiber reinforced nickel-based composite material, its characteristic is: the structure of described matrix material is: have the carbon fiber of copper, nickel, parallel longitudinal to arrange and through the slab of pressing by surface deposition; The component of matrix material and volume percent thereof are: carbon fiber: 30～35%, and copper: 6～8%, nickel: 57～64%.
2. method for preparing carbon fiber reinforced nickel-based composite material as claimed in claim 1, step comprises: pre-treatment of carbon fiber, electrodeposit metals, vacuum hotpressing is characterized in that: the processing step of described preparation carbon fiber reinforced nickel-based composite material is:
(1) pre-treatment of carbon fiber;
(2) carbon fiber surface acid copper;
(3) clean, neutralize;
(4) be coated with the carbon fiber electrically nickel deposited of copper;
(5) carbon fiber that deposits copper, nickel is wrapped on the briquetting roller moulding electric deposition nickel;
(6) taking off blank cleans, dries;
(7) shear blank, in the mould of packing into;
(8) vacuum hotpressing becomes the matrix material slab;
(9) the slab stove is chilled to room temperature.
3. according to the described method for preparing carbon fiber reinforced nickel-based composite material of claim 2, it is characterized in that: described processing step (2) carbon fiber surface acid copper, its electrolyte prescription and galvanic deposit parameter are:
Solvent: distilled water; CuSO
45H
2O:38～43g/L; C
6H
8O
7: 28～32g/L; C
3H
4O
6KNa4H2O:20～22g/L; NaOH: transfer PH=8～10; OP-21:0.5～1.0g/L; Electric current: 0.1～0.2A.
4. according to the described method for preparing carbon fiber reinforced nickel-based composite material of claim 2, it is characterized in that: described processing step (4) is coated with the carbon fiber electrically nickel deposited of copper, and its electrolyte prescription and galvanic deposit parameter are:
Solvent: distilled water; NiSO
47H
2O:290～310g/L; NiCl6H
2O:48～52gL; H
3BO
3: 32～36g/L; C
12H
25SO
3Na:0.1～0.15g/); PH=6～7; Electric current: 0.5～0.7A.
5. according to the described method for preparing carbon fiber reinforced nickel-based composite material of claim 2, it is characterized in that: the carbon fiber that described processing step (5) deposits copper, nickel is wrapped on the briquetting roller, the moulding electric deposition nickel, its electrolyte prescription and galvanic deposit parameter are:
Solvent: distilled water; NiSO
47H
2O:40～42g/L; NiCl6H
2O:8～12gL; H
3BO
3: 32～35g/L; Na
3C
6H
5O
32H
2O:55～62g/L; C
12H
25SO
3Na:0.015～0.02g/L; PH=6～7; Electric current: 0.5～0.6A.
6. according to the described method for preparing carbon fiber reinforced nickel-based composite material of claim 2, it is characterized in that: it is that the mould that the composite filament blank is housed is put into vacuum tightness 〉=2 * 10 that described processing step (8) vacuum hotpressing becomes the matrix material slab
-2In the process furnace of Pa, be heated to 1080～1120 ℃ with stove after, under 30Mpa pressure, pressurize 40min is hot-forming.
7. according to the described method for preparing carbon fiber reinforced nickel-based composite material of claim 2, it is characterized in that: described processing step (1) pre-treatment of carbon fiber, be that carbon fiber bundle is wrapped on the wiring round, put into and be chilled to room temperature with stove after 320 ℃ of process furnace are incubated 30min.
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|---|---|---|---|
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|---|---|---|---|
| CNB2007100616899A CN100507065C (en) | 2007-04-10 | 2007-04-10 | Carbon fiber reinforced nickel-based composite material and producing method thereof |
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| CN100507065C CN100507065C (en) | 2009-07-01 |
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| CN108796400A (en) * | 2018-07-11 | 2018-11-13 | 河北工业职业技术学院 | A kind of preparation method of continuous carbon fibre enhancing nickel-base composite material |
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| Publication number | Publication date |
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