CN101063187B - Preparation method of ceramic-metal composite material - Google Patents
Preparation method of ceramic-metal composite material Download PDFInfo
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- CN101063187B CN101063187B CN2007101076116A CN200710107611A CN101063187B CN 101063187 B CN101063187 B CN 101063187B CN 2007101076116 A CN2007101076116 A CN 2007101076116A CN 200710107611 A CN200710107611 A CN 200710107611A CN 101063187 B CN101063187 B CN 101063187B
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- 239000002905 metal composite material Substances 0.000 title claims description 29
- 238000002360 preparation method Methods 0.000 title claims description 28
- 239000000956 alloy Substances 0.000 claims abstract description 82
- 239000002245 particle Substances 0.000 claims abstract description 71
- 239000000843 powder Substances 0.000 claims abstract description 62
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 55
- 239000002131 composite material Substances 0.000 claims abstract description 53
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000919 ceramic Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 30
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 238000001291 vacuum drying Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000011159 matrix material Substances 0.000 claims description 104
- 238000005245 sintering Methods 0.000 claims description 82
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- 229910010038 TiAl Inorganic materials 0.000 description 2
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention discloses a preparing method of ceramic-metallic composite material, which comprises the following steps: 1) allocating basal body alloy material; choosing 2Cr33Ni48WC10MoFe8 nickel base metal as basal body alloy; 2) preparing composite ceramic phase particle; choosing Al2O3 particle coating with Ti powder as composite ceramic phase particle; 3) mixing the basal body alloy material and composite ceramic phase particle with volume ratio at 1:0. 15-0. 45; pelleting; 4) press-forming; 5) vacuum-drying; 6) vacuum-clinkering; getting the product. This invention possesses lower ceramic-metallic composite material heat transfer capacity and predominance high temperature property, which is fit for new type material of rolled steel heater block.
Description
Technical field
The present invention relates to a kind of preparation method of ceramic-metal composite material, specifically, relate to the preparation method of a kind of slide block of heater for rolling steel with ceramic-metal composite material.
Background technology
In steel rolling was produced, slab all will heat in process furnace before rolling.Support is heated the furnace gas heat etching that the slide block of slab requires to bear 1250-1400 ℃ of oxidation-vulcanized gas, can bear the high temperature sliding friction of heavy slab again.
At present, what the slide block in the heater for rolling steel used is casting 2Cr33Ni48W10Mo superalloy, but its thermal conductivity is higher, easily form " black-tape " on the steel billet top layer so that cause rolling steel plate weave construction and product performance inhomogeneous, influenced the quality of plate of moderate thickness product.
In order to address this problem, people wait in expectation, and a kind of intensity is higher, high-temperature behavior is superior, the low novel slide block material that does not significantly increase comprehensive cost simultaneously again of the capacity of heat transmission.
Because alumina-ceramic has the plurality of advantages of pottery and has characteristics such as raw material sources are wide, low price again, therefore, frequent preferred raw materials as ceramic-metal composite.But Al
2O
3Equally also having the maximum weakness of pottery, be exactly that toughness is relatively poor, and this point has seriously hindered its application on engineering, and therefore improving its fragility becomes it and enter the problem that Application Areas institute widely must solution.As everyone knows, metal and alloy thereof are ductile, the conduction, heat conductivility is good and some other premium properties, as magnetic, wave absorbtion etc., yet its relative hardness and intensity are lower, density is higher relatively.If can get up pottery and melts combine, maximize favourable factors and minimize unfavourable ones, might obtain a kind of very desirable material undoubtedly.
Al
2O
3Based composites can be used as cutting tool, is suitable for high speed cutting.Make the Al of metal bonding phase with Cr
2O
3Based composites compares Al
2O
3Ceramic machinery intensity height, and with Cr content increase in forming, anti-folding and tensile strength increase to some extent.Adopt Cr-Mo alloy better effects if, can under many hot conditionss, use.For example control pin, "T"-shaped cast gate, boiler tube, flame shield bar and thermocouple protective casing and mechanical seal ring etc. as lining, the flow of molten metal of jet flame controller, guided missile jet pipe.Al
2O
3-Fe composite hardness height, wear-resisting, corrosion-resistant, thermostability is high, is widely used as mechanical seal ring and agricultural submersible pump mechanical seal, can also use as high-temperature component under high temperature resistant, heat conduction, the conduction occasion requiring in addition.This encircles long service life, and can not make ring broken because of the interim a large amount of heat of generation that starts.
Through years of researches, there has been kinds of processes to be used for preparing Al
2O
3-metal composite.Common has: powder metallurgic method, direct oxidation method, liquid metal injection method, in-situ compositing, 3A method and wet chemistry method etc.Powder metallurgic method operation is simple relatively, but that shortcoming is that matrix mixes with second phase material is inhomogeneous, and in sintering process owing to matrix generation volumetric shrinkage, easily cause matrix material to crack.
Al
2O
3Based composites is as a kind of material system with widespread use, is exactly by rational constituent element, composition, microstructure and technological design to the main purpose of its research, makes Al
2O
3Complement each other with the performance characteristics of metal, give full play to advantage separately, overcome deficiency separately, obtain to have the Al of ideal performance
2O
3-metal composite improves reliability of material, final implementation structure function integration, thus further enlarge its range of application.
Japan Kansai Electric Power and Nagoya University, Hitachi develop the internal combustion turbine wing with high-temperature heat-resistance characteristic of the highest level in the world jointly with the nickel-based monocrystal superalloy.This alloy has been realized optimized performance based on nickel by the rational proportion of composing of alloying elements such as cobalt, chromium, tungsten, aluminium, titanium, tantalum, rhenium, hafnium.
There is research to adopt cladding process and heat pressing process to prepare Al
2O
3-Ni matrix material.Coat Al at 1450 ℃ of hot pressing Ni
2O
3Composite granule obtains the ceramic-metal composite of relative density＞98%, when temperature＞1400 ℃, along with the increase density of Ni content descends.The Ni particle is positioned at the triangle crystal boundary, and along with the increase of content, fracture mode transfers transgranular fracture to by the edge crystalline substance; At Al
2O
3Introduce the Ni particle in the matrix and can reduce grain-size, improve intensity and toughness.With single-phase Al
2O
3Mechanical property compare, the comprehensive mechanical property bending strength and the fracture toughness property of NA4 ceramic-metal composite has preferably improved 19% and 35% respectively.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art, the preparation method of a kind of slide block of heater for rolling steel with ceramic-metal composite material is provided, the service requirements that the ceramic-metal composite material capacity of heat transmission is lower, high-temperature behavior is superior, mechanical strength can reach slide block of heater for rolling steel of the present invention's preparation is a kind of type material that slide block of heater for rolling steel is used that is suitable for.New ceramics-the metal composite of the present invention's preparation also can be widely used in other high temperature resistance wear-resistant parts.
For addressing the above problem, the present invention adopts following technical scheme:
The present invention relates to a kind of preparation method of ceramic-metal composite material, described method comprises the following steps:
1), matrix alloy material proportioning: as matrix alloy, according to the composition proportion in the 2Cr33Ni48WC10MoFe8 nickel based metal (weight ratio) 2 parts in Cr powder, 33 parts in Ni powder, 48 parts in WC powder, 10 parts in Mo powder and Fe powder are mixed for 8 parts and to be prepared into the matrix alloy material with the 2Cr33Ni48WC10MoFe8 nickel based metal;
2), composite ceramics phase particulate preparation: the Al that described composite ceramics phase particle coats for the Ti powder
2O
3Particle;
3), batching and granulation: according to matrix alloy material and composite ceramics mutually the particulate volume ratio be 1: 0.15～0.45 ratio, with matrix alloy material and composite ceramics particle mixing and stirring mutually; In whipping process, drip the rubber solutions forming agent, carry out granulation; The add-on of forming agent is to add 10～15 milliliters of forming agents in per 100 gram compounds;
4), compression moulding: adopt pressing machine that the granulation material is carried out the compression moulding of base substrate, forming pressure is 100～200MPa; Dwell time is 40～100 seconds;
5), vacuum-drying: 60～90 ℃ of vacuum-dryings of the base substrate after the moulding;
6), vacuum sintering: 1250～1380 ℃ of sintering temperatures, sintering vacuum tightness are 1.0 * 10
-1～1.0 * 10
-3Pa.
Composite ceramics phase particulate preparation method of the present invention is: according to Ti powder and spherical Al
2O
3The particle weight ratio is 1: 0.01～0.05 ratio, and the Ti powder is joined Al
2O
3In the particulate material, splash into PVB (polyvinyl butyral acetal) spirituous solution binding agent, the binding agent add-on is Dropwise 5～10 milliliter in per 100 gram raw materials, mixes, make the Ti powder evenly be coated on the alumina particle surface, be prepared into particle diameter and be the Al that 0.5～1.0 millimeter, Ti powder coat
2O
3Composite ceramics phase particle.
Preferably, Ti powder of the present invention and spherical Al
2O
3The particle weight ratio is 1: 0.03.Described matrix alloy material and composite ceramics particulate volume ratio mutually are 1: 0.25.
Preferably, vacuum sintering of the present invention divided for three steps finished:
1), the degreasing pre-burning stage: sintering temperature is 0～400 ℃, and heat-up rate is 10 ℃/minute;
2), the sintering stage: the sintering stage is finished by the following step:
A, holding stage, temperature are 400 ℃, soaking time 30 minutes;
B, presintering stage, temperature is 400 ℃～1000 ℃, 10 ℃/minute of heat-up rates;
C, holding stage, temperature are 1000 ℃, soaking time 30 minutes;
D, sintering stage, temperature is 1000 a ℃～sintering temperature, 10 ℃/minute of heat-up rates;
E, sintering temperature insulation, temperature is 1250～1380 ℃, is incubated 30 minutes;
3), cooling stages: furnace cooling.
The present invention has following characteristics:
1, adopt the prepared material of method of the present invention to have lower thermal conductivity, intensity reaches service requirements.
2, coated aluminum oxide ceramic particle and Superalloy Substrate have wettability preferably, and both can combine preferably.
3, adopt the high-temperature behavior of the prepared material of method of the present invention superior.
4, adopt the composite slider material of preparation method's preparation of the present invention, good combination property, technology is simple, is suitable for suitability for industrialized production.
The service requirements that the ceramic-metal composite material capacity of heat transmission is lower, high-temperature behavior is superior, mechanical strength can reach slide block of heater for rolling steel of the present invention's preparation is a kind of type material that slide block of heater for rolling steel is used that is suitable for.New ceramics-the metal composite of the present invention's preparation also can be widely used in other high temperature resistance wear-resistant parts.
In order to obtain the ceramic-metal composite material that mechanical behavior under high temperature is superior, heat conductivility is lower, select for use the superalloy high temperature resistant, that abrasion resistance is good usually as body material.
The physical chemistry problem of ceramic-metal composite material is the key issue in the matrix material development.The selection of material component, the control of technological process play conclusive effect to the final performance of material.The dissolving of the wettability of phase interface, chemical reaction and component to phase interface in conjunction with important influence.The physics of phase interface and chemical compatibility have determined the serviceability of ceramic-metal composite material in wide temperature range.
The present invention with matching, the wettability of alternate thermal expansivity and few alternate reaction of trying one's best as the First Principles of selection, with the 2Cr33Ni48WC10MoFe8 nickel based metal as matrix alloy, the Al that coats with the Ti powder
2O
3Particle is as composite ceramics phase particle.
Physical Match in the matrix material between matrix metal and the composite ceramics phase is extremely important.So-called Physical Match is meant the consistency of two kinds of materials on physicals, mainly comprises thermal expansivity and Young's modulus.The Physical Match between the homophase will not produce very big influence to the performance of interfacial stress, load transmission and whole material.The material coefficient of thermal expansion coefficient depends on its chemical constitution and crystalline structure.After the two is determined, be difficult to change and adjustment.Thermal expansion coefficient difference is crossed conference and is caused matrix to produce stress with compound at cooling stages, reduces the intensity of matrix material, even can make the material production crackle.
Facts have proved that the difference of two-phase thermal expansivity should be not excessive in the binary ceramic matric composite, as for ceramic-metal composite, the two-phase difference of thermal expansion coefficient reaches 10 * 10 in the system
-6K
-1The time, goods can be destroyed, and difference is 5 * 10
-6K
-1The time, goods still can bear.
From reducing the intensity of unrelieved stress, raising material, should make the Young's modulus of metallic matrix less, and approaching with compound thermal expansivity mutually.High Young's modulus will make the compound bigger load of sharing mutually, also help the improvement of intensity.Therefore there is an Optimum Matching, the intensity of material and toughness are improved simultaneously.
Except the method for only a few, metal-base composites is all made under higher temperature, temperature range is lower than or the fusing point of a little higher than matrix usually slightly, so the interaction between matrix and the reinforce is inevitable, is easy to generate the compound that has a strong impact on composite property.The chemical compatibility issues of Here it is matrix and reinforce.It comprises thermodynamic compatibility and two aspects of kinetics consistency.Therefore, when selecting matrix alloy, to take into full account aspect these two, can either satisfy its temperature requirement, avoid the generation of some compounds again as far as possible.
In addition, when selecting matrix alloy, also to take into full account its wettability to compound phase.But in actual applications, wettability can not meet the demands sometimes, and this just need carry out some processing.Can take following measures to improve the wettability of metallic matrix for metal-base composites to compound phase.
1) condition of surface that changes compound phase and structure be with the increase surface tension, promptly carries out surface treatment mutually to compound, comprises machinery, physics and matting, electrochemical etching and coating.The most effective way is to carry out surface-coated to handle.
2) chemical ingredients that changes metallic matrix is to reduce interfacial tension, and the most effective way is to add alloying element in matrix.As at Ni-Al
2O
3In Ni, add Ti, Cr etc. in the system and can improve Ni Al
2O
3Wettability.
3) change temperature, elevated temperature can reduce liquid matrix and solid-state compound alternate contact angle usually, but temperature can not be too high, otherwise will promote chemical reaction between matrix and reinforce, has a strong impact on performance of composites.
4) change ambiance, as in oxidizing atmosphere, making Ni-Al
2O
3Also can reduce contact angle during matrix material and improve the performance of material.
The matrix material that processability is good should carry out optimal design according to desired material property, selects suitable material constituent element in use to bear certain function.At first select to form the material system of matrix material, promptly select bond matrix mutually with mutually compound according to the required performance of matrix material.Take all factors into consideration physics, chemical compatibility and wettability between the constituent element.Table 1 compares with several performances that can be used as bond matrix material mutually for nickel-base alloy.
The common nickel-base alloy of table 1, Ti
3Al and TiAl alloy Ti alloy property are relatively
By table 1 as seen, the creep resistance and the oxidation-resistance of nickel-base alloy are more much better than common alloy of titanium, work as with TiAl base alloy phase, but over-all properties are more superior, because it has higher hot strength, high-temperature oxidation resistance.The main application advantage of nickel-base alloy is:
(1) nickel-base alloy is than the specific rigidity high about 50% of other common structure alloys.
(2) the good resistance creep property of 800～1090 ℃ of nickel-base alloys can be used it better as high-temperature alloy part.
(3) high-yield strength of nickel-base alloy, the high anti-oxidation limit, excellent high-temperature plasticity and anti-wear all be that other materials is irreplaceable.
But the same with other metal alloy, also there is the thermal conductivity height in nickel-base alloy, and problem such as cost an arm and a leg, therefore the present invention designs the adding alumina particle and does compound phase, can utilize the low characteristics of alumina-ceramic thermal conductivity, can reduce the price of matrix material again.
Nickel, chromium are the main components of matrix alloy, and shown in nickel-chromium binary phase diagram 1: the nickel chromium triangle system has eutectoid point between nickel accounts for 27.3%～53%, and the over-all properties of nickel is better than chromium, so choose 48% and 33% respectively at the content of nickel and chromium.
Molybdenum powder is silvery white in color, density 10.22g/cm
3, fusing point is 2610 ℃.The uniform particles of molybdenum powder, mobile relatively poor.A small amount of adding of molybdenum powder mainly is in order to increase matrix alloy to the wettability of ceramic particle and the resistance to elevated temperatures of raising matrix alloy.
Selecting reduced iron powder for use is raw material, because it is economical comparatively speaking cheap, and experiment is found the influence of composite property also little.The adding of iron powder mainly is easy and other metal generation eutectic because of its, and wettability is preferably arranged.
At high temperature (1400～1800 ℃) and carbon black chemical combination form wolfram varbide by metal tungsten powder (tungstic oxide).The wolfram varbide lattice is cubes, and density is 15.5～15.7 gram per centimeters
3, have high rigidity (1700 kilograms/millimeter of microhardnesses
2) and high-melting-point (2720 ℃) and can be molten in multiple refractory carbides.Wolfram varbide is mainly used in as framework material among all kinds of hard materials such as Wimet.Wolfram varbide adds in the matrix alloy can provide the hardness and the wear resistance of material, and effectively reduces the liquid phase sintering temperature of materials with high melting point.
The experiment of the proportioning between alumina-coated that the present invention carries out and matrix alloy and the aluminum oxide sees Table 2.The compound phase material of aluminum oxide is selected aluminum oxide micro-sphere (particle diameter about 0.5～1mm) for use.
Experiment adopts the Ti powder as aluminum oxide micro-sphere surface coating.Experiment finds that the Ti powder is to Al
2O
3Wetting and the mechanical property of-Ni matrix material phase interface has better influence.
For being the alumina composite material of matrix, because the nonwetting Al of Ni with Ni base alloy
2O
3, Al
2O
3-Ni phase interface wettability is good inadequately, and interface bond strength is lower, and alumina particle is easy to extract in the material breaking-down process, and the toughening effect of matrix alloy is not fully exerted.It is additive that employing has higher chemically active Ti powder to oxygen, and its effect has following 3 points.(1) the Ti flour additive agent is owing to have high chemically reactive and at Al to oxygen
2O
3Near the enrichment-Ni phase interface has been strengthened the phase interface combination by improving the phase interface wettability, thereby has been significantly improved Al
2O
3The mechanical property of-Ni base alloy composite materials.(2) in Shi Yan the composition range, increase with the Ti powder content, the sintered density of matrix material and three-point bending strength improve; Fracture toughness property is that 3% o'clock of alumina particle quality has maximum value at the covering amount of Ti powder.(3) Al
2O
3The toughening mechanism of (coating of Ti powder)-Ni base alloy composite materials is based on bridge joint mechanism.
The proportion scheme of table 2 Composite Preparation second section experiment
At normal temperatures,, the mixing raw material powder is sent in the die cavity with the packing factor of regulation, the pressed compact that with pressure powder pressing one-tenth is had predetermined shape and size by stamping, and, be called compression molding with the process that pressure is deviate from mould with pressed compact.Usually finish by dress powder, compacting, 3 operations of the demoulding.
The employing pressing machine is pressed, forming pressure 100～200MPa, and selecting the dwell time was 40～100 seconds.
Dry: 60～90 ℃ of vacuum-dryings of the base substrate after the moulding.
The easy oxidation of metal under hot environment is so adopt vacuum sintering.Vacuum sintering has the effects such as wetting, activated sintering to solid phase of protective atmosphere, reduction, the degassing, promotion liquid phase, is applicable to avoid and keeps away the occasion that gas is made protection gas.
Vacuum sintering of the present invention divided for three steps finished:
1. degreasing: this stage is to remove the binder stage also to can be described as the pre-burning stage, will be incubated for some time in this stage in a certain temperature, its purpose: the one, and binder is fully got rid of, the 2nd, carry out self redox reaction.Pre-burning by this stage should make binder decompose, and gas is fully got rid of.
2. sintering: the temperature that the sintering stage is set promptly is the needed temperature of sintering.Because vacuum sintering has the effect of activated sintering, its sintering temperature than atmosphere sintering low 50 ℃～100 ℃.
3. cooling: furnace cooling.
During sintering, one section meadow is arranged near 400 ℃, reason be organic shaping additive of adding in the coating base substrate decomposition, volatilize, remove.
For fear of because the too quick decomposition of shaping additive component, volatilization and form bubble, slabbing, slit in base substrate, or cause other to destroy to base substrate, unsuitable too fast at the heat-up rate in this stage, experiment shows, is advisable with 10 ℃/min.For make slip additives such as PVB more fully, decompose completely, volatilize, 400 ℃ of insulations of carrying out 30min.And many metallic elements begin to carry out alloying at this temperature spot near 1000 ℃, can carry out more fully in order to make alloying, so also be incubated 30 minutes at this temperature spot, and an endotherm(ic)peak is arranged to 1370 ℃, explanation begins a large amount of appearance in this temperature spot liquid phase, therefore this experiment fixes on 1250-1340 ℃ with sintering temperature, and this temperature province is an optimal sintering temperature.Sintering temperature insulation 30 minutes.
Description of drawings
Fig. 1 is a matrix material sintering temperature synoptic diagram of the present invention.
Fig. 2 is the DTA-TG analytic curve figure of raw material.
Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d are the stereoscan photograph of the ceramic-metal composite material section of the present invention's preparation, wherein: Fig. 3 a and Fig. 3 b be profile scanning electromicroscopic photograph 40 *; Fig. 3 c be after the section polishing stereoscan photograph 40 *; Fig. 3 d be alumina particle and matrix alloy sintering rear interface in conjunction with situation 5000 *.
Embodiment
The preparation of embodiment 1 ceramic-metal composite material
1), matrix alloy material proportioning: as matrix alloy, according to the composition proportion in the 2Cr33Ni48WC10MoFe8 nickel based metal (weight ratio) 2 parts in Cr powder, 33 parts in Ni powder, 48 parts in WC powder, 10 parts in Mo powder and Fe powder are mixed for 8 parts and to be prepared into the matrix alloy material with the 2Cr33Ni48WC10MoFe8 nickel based metal;
2), composite ceramics phase particulate preparation: according to Ti powder and spherical Al
2O
3The particle weight ratio is 1: 0.03 a ratio, and the Ti powder is joined Al
2O
3In the particulate material, splash into PVB (polyvinyl butyral acetal) spirituous solution binding agent, the binding agent add-on is Dropwise 5～10 milliliter in per 100 gram raw materials, mixes, make the Ti powder evenly be coated on the alumina particle surface, be prepared into particle diameter and be the Al that 0.8 millimeter, Ti powder coat
2O
3Composite ceramics phase particle.
3), batching and granulation: according to matrix alloy material and composite ceramics mutually the particulate volume ratio be 1: 0.25 ratio, with matrix alloy material and composite ceramics particle mixing and stirring mutually; In whipping process, drip the rubber solutions forming agent, carry out granulation; The add-on of forming agent is to add 12 milliliters of forming agents in per 100 gram compounds;
4), compression moulding: adopt pressing machine that the granulation material is carried out the compression moulding of base substrate, forming pressure is 150MPa; Dwell time is 70 seconds;
5), vacuum-drying: 80 ℃ of vacuum-dryings of the base substrate after the moulding;
6), vacuum sintering: sintering vacuum tightness is 1.0 * 10
-2Pa, sintering process is:
A, degreasing pre-burning stage: sintering temperature is 0～400 ℃, and heat-up rate is 10 ℃/minute;
B, sintering stage: the sintering stage is finished by the following step:
A, holding stage, temperature are 400 ℃, soaking time 30 minutes;
B, presintering stage, temperature is 400 ℃～1000 ℃, 10 ℃/minute of heat-up rates;
C, holding stage, temperature are 1000 ℃, soaking time 30 minutes;
D, sintering stage, temperature is 1000 ℃～1300 ℃, 10 ℃/minute of heat-up rates;
E, sintering temperature insulation, temperature is 1300 ℃, is incubated 30 minutes;
C, cooling stages: furnace cooling.
The preparation of embodiment 2 ceramic-metal composite materials
1), matrix alloy material proportioning: as matrix alloy, according to the composition proportion in the 2Cr33Ni48WC10MoFe8 nickel based metal (weight ratio) 2 parts in Cr powder, 33 parts in Ni powder, 48 parts in WC powder, 10 parts in Mo powder and Fe powder are mixed for 8 parts and to be prepared into the matrix alloy material with the 2Cr33Ni48WC10MoFe8 nickel based metal;
2), composite ceramics phase particulate preparation: according to Ti powder and spherical Al
2O
3The particle weight ratio is 1: 0.01 a ratio, and the Ti powder is joined Al
2O
3In the particulate material, splash into PVB (polyvinyl butyral acetal) spirituous solution binding agent, the binding agent add-on is a Dropwise 5 milliliter in per 100 gram raw materials, mixes, and makes the Ti powder evenly be coated on the alumina particle surface, is prepared into particle diameter and is the Al that 1.0 millimeters, Ti powder coat
2O
3Composite ceramics phase particle.
3), batching and granulation: according to matrix alloy material and composite ceramics mutually the particulate volume ratio be 1: 0.15 ratio, with matrix alloy material and composite ceramics particle mixing and stirring mutually; In whipping process, drip the rubber solutions forming agent, carry out granulation; The add-on of forming agent is to add 15 milliliters of forming agents in per 100 gram compounds;
4), compression moulding: adopt pressing machine that the granulation material is carried out the compression moulding of base substrate, forming pressure is 100MPa; Dwell time is 100 seconds;
5), vacuum-drying: 60 ℃ of vacuum-dryings of the base substrate after the moulding;
6), vacuum sintering: sintering vacuum tightness is 1.0 * 10
-1Pa, sintering heats up as follows:
A, degreasing pre-burning stage: sintering temperature is 0～400 ℃, and heat-up rate is 10 ℃/minute;
B, sintering stage: the sintering stage is finished by the following step:
A, holding stage, temperature are 400 ℃, soaking time 30 minutes;
B, presintering stage, temperature is 400 ℃～1000 ℃, 10 ℃/minute of heat-up rates;
C, holding stage, temperature are 1000 ℃, soaking time 30 minutes;
D, sintering stage, temperature is 1000 ℃～1250 ℃, 10 ℃/minute of heat-up rates;
E, sintering temperature insulation, temperature is 1250, is incubated 30 minutes;
C, cooling stages: furnace cooling.
The preparation of embodiment 3 ceramic-metal composite materials
1), matrix alloy material proportioning: as matrix alloy, according to the composition proportion in the 2Cr33Ni48WC10MoFe8 nickel based metal (weight ratio) 2 parts in Cr powder, 33 parts in Ni powder, 48 parts in WC powder, 10 parts in Mo powder and Fe powder are mixed for 8 parts and to be prepared into the matrix alloy material with the 2Cr33Ni48WC10MoFe8 nickel based metal;
2), composite ceramics phase particulate preparation: according to Ti powder and spherical Al
2O
3The particle weight ratio is 1: 0.05 a ratio, and the Ti powder is joined Al
2O
3In the particulate material, splash into PVB (polyvinyl butyral acetal) spirituous solution binding agent, the binding agent add-on is to drip 10 milliliters in per 100 gram raw materials, mixes, and makes the Ti powder evenly be coated on the alumina particle surface, is prepared into particle diameter and is the Al that 0.5 millimeter, Ti powder coat
2O
3Composite ceramics phase particle.
3), batching and granulation: according to matrix alloy material and composite ceramics mutually the particulate volume ratio be 1: 0.45 ratio, with matrix alloy material and composite ceramics particle mixing and stirring mutually; In whipping process, drip the rubber solutions forming agent, carry out granulation; The add-on of forming agent is to add 10 milliliters of forming agents in per 100 gram compounds;
4), compression moulding: adopt pressing machine that the granulation material is carried out the compression moulding of base substrate, forming pressure is 200MPa; Dwell time is 40 seconds;
5), vacuum-drying: 90 ℃ of vacuum-dryings of the base substrate after the moulding;
6), vacuum sintering: sintering vacuum tightness is 1.0 * 10
-3Pa, the sintering temperature-rise period is as follows:
A, degreasing pre-burning stage: sintering temperature is 0～400 ℃, and heat-up rate is 10 ℃/minute;
B, sintering stage: the sintering stage is finished by the following step:
A, holding stage, temperature are 400 ℃, soaking time 30 minutes;
B, presintering stage, temperature is 400 ℃～1000 ℃, 10 ℃/minute of heat-up rates;
C, holding stage, temperature are 1000 ℃, soaking time 30 minutes;
D, sintering stage, temperature is 1000 ℃～1380 ℃, 10 ℃/minute of heat-up rates;
E, sintering temperature insulation, temperature is 1380 ℃, is incubated 30 minutes;
C, cooling stages: furnace cooling.
Embodiment 4 test examples
1, the test of bending strength
After sintered specimen polished polishing, again sample is cut into the regular strip that is of a size of 4mm * 20mm * 40mm, the about 0.3mm of chamfering, the room temperature bending strength of material adopts three-point bending method to measure, the about 15mm of span, bending strength experiment is carried out on the INSTRON electronic universal material testing machine, and the pressure head speed of moving down is 0.5mm/min, and the bending strength calculation formula that every group of sample surveyed 5 root timber material is as follows:
σ
f＝3PL/(2bh
2)
In the formula: σ
f-flexural strength, MPa; The span of L-fulcrum, mm; The load of P-fracture, N; The width of b-sample, mm; The thickness of h-sample, mm
According to table 4-table 6 test data, the bending strength that alumina particle adds the back matrix material has apparent in view reduction, uses in the bending strength scope that allows but can be controlled at.
The bending strength test data of table 4 material formula 1:0.25
The bending strength test data of table 5 material formula 1:0.3
The bending strength test data of table 6 matrix alloy
The bending strength of matrix material sample reduces along with the increase of alumina particle content along with the content of matrix alloy increases and increases.Isozygoty golden bending strength apparently higher than matrix material; The golden strength test data fluctuations of isozygotying is smaller, shows that size-grade distribution is more even, and the void ratio that leaves in the sintered alloy body is less.And containing the matrix material of alumina particle, the strength test data fluctuations is bigger, has illustrated that then the agglomerating material homogeneity is good not enough.The major cause that causes this situation is the wetting of matrix alloy and alumina particle and good inadequately in conjunction with situation, also exist the mechanical bond of considerable part in their interface combination, and dissolving and wetting combination and reaction bonded is not ideal enough.In the test afterwards, also need further improve wettability.Matrix material is to make through sintering by compression moulding again, but that the shortcoming of this method is that matrix material mixes with compound phase material is even inadequately, can influence the intensity of material; Thermal expansivity between nickel-base alloy and the compound phase is variant, can produce certain interfacial stress at cooling stages, thereby influences the intensity of matrix material.
2, hardness test
Table 7 is the hardness test result of matrix material.
The hardness of table 7 matrix material (HRB) test data
Annotate: adopt the 1.588mm ball indenter in the HRB test, total load is 100kg
Test data shows, change greatly with a kind of matrix material sample hardness value, this mainly be because the density unevenness of sample even due to.And the hardness value rangeability of the gold that isozygotys is smaller, illustrates that the golden density of isozygotying is more even.For containing the particulate matrix material, when pressure head was pressed on the space, hardness value was smaller; And when being pressed on the alumina particle, it is big that hardness value will become.
3, oxidation-resistance test
Oxidation resistance test is undertaken by the heated oxide weightening finish under the air atmosphere in resistance furnace, and temperature increasing schedule is: 5 ℃ of per minutes, and the highest 1250 ℃, be incubated 1 hour, furnace cooling.Table 8 is the oxidation-resistance test result of matrix material.
The rule of the high-temperature oxidation resistance of prepared matrix material is as follows: the matrix material under the same temperature, high-temperature oxidation resistance strengthens with the increase of matrix alloy degree, reduces with the increase of alumina particle content.Experimental phenomena shows that along with increasing of the compound phase of alumina particle, the batching homogeneity of matrix material is not very good, the sintered density situation is good inadequately, more spaces are arranged in the sintered compact, given oxygen and alloy substrate more contact area, cause the matrix material high temperature oxidation resistance to descend.
The oxidation-resistance test data of table 8 matrix material
4, the analysis of thermal conductivity of composite materials
The thermal conductivity of nickel-base alloy and aluminum oxide is as shown in table 9:
The thermal conductivity of table 9 nickel-base alloy and alumina-ceramic (W/m.k)
Alumina-ceramic/superalloy matrix material is as shown in table 10 1000 ℃ of thermal conductivities during with 1100 ℃ as calculated.
Table 10 alumina-ceramic/superalloy matrix material thermal conductivity (W/m.k)
By table 9 and table 10 as can be seen, along with the increase of alumina particle add-on, the thermal conductivity of alumina-ceramic/superalloy matrix material constantly reduces, and the thermal conductivity of matrix material is higher than the thermal conductivity of aluminum oxide; But be lower than the thermal conductivity of nickel-base alloy, be tangible linear change.
5, correlative factor is to the influence of composite materials property
The influence of alumina-ceramic
Test shows, the mean value of nickel-base alloy sample bending strength can reach 2065.56, and the intensity of the matrix material sample of adding alumina particle is respectively 993.55MPa and 904.36MPa.The adding of alumina particle has significantly reduced the bending strength of nickel-bass alloy material as can be seen.
The HRB mean value of nickel-base alloy sample can reach 79, and 2 mean values of the HRB of the sample of adding alumina particle are respectively 67 and 62, and the adding of alumina particle has reduced the hardness of nickel-bass alloy material as can be seen.
The adding of alumina particle to the influence of Ni-based sintered alloy material mechanical property aspect mainly contain following some:
1. the adding of alumina particle increases the blended difficulty, mixes inhomogeneous creating a great impression to the strength of materials behind moulding and the sintering;
2.Ni the coefficient of expansion (15 * 10
-6/ ℃) than Al
2O
3(8.4 * 10
-6/ ℃) big, can be during cooling at Al
2O
3/ Ni interface forms the space, reduces the mechanical property of high temperature sintering material;
3. more because of the content of Ni, Ni can pass through short-range diffusion in sintering process, causes the Ni particle agglomeration, grows up, and is unfavorable for sintering, also can reduce and Al
2O
3The particulate wettability reduces the strength of materials;
4. the alumina metals ceramic composite shrinks because inhomogeneous volume takes place base substrate in the vacuum sintering process, can cause matrix material to crack, and then influence the intensity of material;
Binding agent be added in high temperature sintering after stay pore, also can influence the intensity of material.
Though the adding of alumina particle has reduced the mechanical property of nickel-bass alloy material.But the reduction of these performances is the reductions in material uses allowed band.This research be obtain by experiment the mechanical behavior under high temperature of ceramic-metal composite and low heat conductivity can between optimal match point.
The influence of sintering temperature
Sintering temperature has important influence to composite property.When sintering temperature was lower than 1300 ℃, the metalluster of the sample after the vacuum sintering was very poor, and the matrix sintering is incomplete; And when temperature reached 1330 ℃, the major part of matrix had just begun fusing, and the sintering range of visible this aluminum oxide/nickel-base alloy matrix material is not very wide.
The influence of sintering vacuum tightness
This research is in early stage when carrying out, and sintering oven vacuum tightness is not high enough, and base substrate is oxidized easily, and the sintering quality of matrix material has been produced very big disadvantageous effect.Later experiments, the high vacuum transformation of sintering oven is finished, and the performance of institute's sintered specimen is significantly improved.
The influence of binding agent
The effect of binding agent, be to make between powdered alloy and the powdered alloy and powdered alloy and alumina particle between can firm mutually bonding together.Behind the material sintering, can burn, gasify, not stay residue, not form hole.The binding agent add-on is unsuitable too much, with the enhancing body particle that can bond, makes matrix have certain cohesiveness and dry body strength is advisable.If add-on is too much, easily on powdered alloy and alumina particle, coat the thick adhensive membrane of one deck, thus influence contact reacts each other, so that influence the quality of alloy.In addition, the gas volume that too much binding agent also can make raw material produce when compression moulding increases, thereby under the condition of high temperature, has greatly increased the volume of gas in alloy inside, and bubble can not in time be got rid of, and forms more hole, has influenced the quality of alloy.
Embodiment 5 matrix material microstructures are analyzed
Material, particularly performance of composites and its composition, weave construction have very confidential relation.Usually, the composition of material determines its weave construction, and weave construction determines its performance.Therefore, in the process of carrying out the material design, at first appropriate ingredients to be selected, just the ideal weave construction might be formed; Equally, have only moiety and weave construction are carried out appropriate design, just can make performance of composites reach design requirements.
Scanning electron microscope mainly adopts the secondary electron imaging.Secondary electron is relatively more responsive to the specimen surface feature.Can utilize scanning electron microscope bound energy spectrum analysis to observe the characteristic distributions etc. of microtexture pattern, grain size, intercrystalline bonding state, inclusion and the pore of Fracture Profile in Metallic Materials.
Fig. 3 a, Fig. 3 b, Fig. 3 c and Fig. 3 d are the stereoscan photograph of the ceramic-metal composite material section of the present invention's preparation.From Fig. 3 a, Fig. 3 b, as can be seen, still have certain wettability combination between alumina particle and the matrix alloy, but yet exist a certain amount of pore and slight crack in the matrix.Can see that from Fig. 3 c section polishing photo the associativity between the more shallow body material of alumina particle that circle, color are darker and color is better, bigger therebetween, visible slit seldom but also has tangible pore to exist on the matrix.Have wettability combination preferably between alumina particle and the matrix alloy as can be seen by 3d, both can tighterly thickly bond together.
The present invention is not limited to above-mentioned preferred forms, and other any identical with the present invention or akin products that anyone draws under enlightenment of the present invention all drop within protection scope of the present invention.
Claims (4)
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| CN114657405B (en) * | 2022-03-25 | 2023-08-29 | 湖北中烟工业有限责任公司 | Electromagnetic heating material for low-temperature cigarettes and preparation method thereof |
| CN116121577B (en) * | 2023-01-05 | 2024-06-25 | 华侨大学 | Eutectic ceramic particle reinforced titanium-based composite material, preparation method thereof and 3D laser printing method |
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