CN102357653A - Preparation process for nanoparticle reinforced die steel - Google Patents
Preparation process for nanoparticle reinforced die steel Download PDFInfo
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- CN102357653A CN102357653A CN2011103587682A CN201110358768A CN102357653A CN 102357653 A CN102357653 A CN 102357653A CN 2011103587682 A CN2011103587682 A CN 2011103587682A CN 201110358768 A CN201110358768 A CN 201110358768A CN 102357653 A CN102357653 A CN 102357653A
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Abstract
The invention discloses a preparation process for nanoparticle reinforced die steel. The process comprises the following steps of: performing pre-dispersion mixing on in-situ synthesized TiNC/Si3N4 nano mixed powder and pre-dispersion iron powder, preparing a dispersed precast block, adding the precast block into a steel ladle, synthesizing the precast block into TiNC/Si3N4/Al2O3 mixed nanoparticles in molten steel in situ by using the high-temperature molten steel, uniformly dispersing the TiNC/Si3N4/Al2O3 nanoparticle mixed powder in a die steel matrix by using an electromagnetic agitator and forming the die steel by adopting a casting method. By the preparation process, the in-situ synthesized nanoparticles are adopted, so the wettability of the nanoparticles and the matrix is improved; and the die steel with uniformly distributed nanoparticles is obtained by secondary dispersion and electromagnetic agitating processes, so the die steel is modified and reinforced. The volume fraction of the nanoparticles is regulated by regulating the addition of the nanoparticles, so the requirements of different working conditions can be met. The nano modified die steel with high abrasive resistance has high mechanical properties, and is simple in preparation and low in preparation cost.
Description
Technical field
The invention belongs to the mould steel technical field, relate to a kind of nano-powder reinforced die steels preparation method, particularly a kind of nano particle strengthens the mould steel and is equipped with technology.
Background technology
Development along with modern machinery and equipment and manufacturing technology; Performance and quality to part have proposed increasingly high and more and more harsher performance demands; The conventional molds steel is through in smelting molten steel, adding the alloying element of some, making its primary carbide that in process of setting, forms some, and make it separate out the proeutectoid carbide of some again through heat treatment; Thereby make material on the basis that keeps certain toughness, reach wear resistance.But owing to receive the restriction of manufacturing process; The total amount of its carbide is generally less than 20%; Because the content of carbide is less relatively; Thereby the anti-wear performance of material can't satisfy the requirement of modern industry to the material abrasion resistance, and the material that promptly requires that more can't satisfy under abominable industrial and mineral service condition has high-wearing feature, possesses the harsh requirement of multinomial performances such as high strength, high tenacity utmost point corrosion resistance again.Therefore research and develop high-performance, high life mould steel not only has good economic benefit, but also has important science and social effect.
A particulate reinforced metal-based nano composite material is exactly that nano particle is fused in metallic matrix, and nano particle and metallic matrix are combined closely, and makes it to have long-term stability.And after compound, also can demonstrate bigger advantage at aspects such as optics, mechanical performances.Carry out nano material and metallic matrix organically compound, the effect of utilizing the interaction of nano material and matrix to produce can also realize both mutual supplement with each other's advantages, the new functional material of exploitation excellent performance.Experiment shows: in steel, add nonmetal nano powder, can roll up heterogeneous core external in the molten steel, make the field trash disperseization in the steel, reduce or eliminate the illeffects of field trash, so just can reduce the requirement to the steel degree of purity.Add the also matrix of possible refinement steel of nonmetal nano powder in the steel, the existence of a large amount of heterogeneous particles can play dispersion-strengtherning in steel.Therefore, in steel, add the performance that nonmetal nano powder can improve steel greatly, improve the quality of steel.Have that mechanical property is good, shear strength is high, operating temperature is higher, wear-resistant, conductive and heat-conductive good, non-hygroscopic, not air-breathing, dimensionally stable, advantage such as aging, so with its excellent performance applications in automation, space flight, aviation and high-tech sectors such as auto industry, advanced manufacturing industry.
Because above-mentioned each item premium properties that metal-base nanometer composite material had and the extensive market prospects that is had, R and D are energetically all being carried out to it in countries in the world, and have developed various preparation technologies.At present; The method of being developed both at home and abroad for preparing metal-base nanometer composite material mainly contains mechanical alloying method (Mechanical alloying; MA), melt spinning (Meltspun; MS) method, powder metallurgic method (Powder metallurgy; PM), machinery bring out self propagating high temperature synthetic (Self-propagatinghigh-temperature synthesis, SHS) reaction method, vacuum evaporation inert gases agglomeration and vacuum add in-place platen press (Inert gas con-densation method combined with vacuum co-evaporation andin-situ compaction, ICVCSC) etc.; They differ from one another above-mentioned various preparation technology; The scope of application is not quite similar, and the prepared various metal-base nanometer composite materials that go out are compared all with traditional material on performance and are greatly improved, and are playing huge impetus aspect development conventional composite materials and the development of new composite.But all there is self limitation in these technologies of preparing, and wherein great majority are because apparatus expensive, complex process and be difficult to control and still concentrate on the laboratory research stage.
For realizing the manufacturing of nano particle reinforced composite, all carried out a large amount of research and developments both at home and abroad, constantly worked out new preparation technology; Making on the non-ferrous metal nano particle reinforced composite technology, Chinese invention patent ZL200510011568.4 discloses a kind of nano particle and has strengthened high-toughness casting magnesium alloy and preparation moulding process thereof, and the magnesium alloy substrate component of this technology manufacturing and weight percent content are 5.0～10.0%Al; 0.1～1.0%Zn, 0.05～0.5%Mn, constraint element Si≤0.05%; Fe≤0.005%; Cu≤0.01%, Ni≤0.002%, all the other are magnesium.The particle that uses is the SiC nano particle, and particle diameter is less than 100nm, and addition is 0.1～3.0% of an alloy volume content.The SiC nano particle will carry out preliminary treatment before adding, and its pretreating process is:
1, in container, import an amount of straight alcohol of analyzing, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, the ratio of SiC nano particle and ethanol is 1g/10ml～1g/3ml;
The poly-vinyl alcohol solution that 2, will account for said mixture volume 1/50～1/10 joins in the mixture of SiC nano particle and ethanol, fully stirs, and mixes;
The said mixture that 3, will contain the SiC nano particle places baking oven dry, and baking temperature is 80～95 ℃.
The preparation moulding process that nano particle strengthens cast magnesium alloy is:
1, magnesium alloy materials is joined in the dry crucible of brushing coating,, use solvent or high-purity argon gas to protect, dissolve the back solution temperature and remain on 680～720 ℃ for preventing magnesium alloy from oxidative combustion in the fusion process;
2, control magnesium alloy solution temperature to 650～700 ℃ (being higher than 60～80 ℃ of liquid magnesium alloy phase lines) or 5850～610 ℃ (being lower than 50～30 ℃ of liquid magnesium alloy phase lines); Remove surface scum; The SiC nano particle that passes through liquor treating process that accounts for magnesium alloy volume 0.1～3.0 is added in the alloy liquid; Be pressed under the liquid level and stir mixing time 3～10 minutes, 10000～2000 rev/mins of agitator speeds;
3, after the refining degasification, the control pouring temperature is 650～700 ℃ and removes out surface scum, obtains the high-toughness casting Mg alloy castings that nano particle strengthens through gravity mold casting or die casting.This technology through adding the nano reinforcement particle, improves the obdurability of cast magnesium alloy on the basis of traditional cast magnesium alloy; Through nano particle is carried out preliminary treatment, increase the wetability of particle and magnesium alloy; Through controlling suitable liquid magnesium alloy temperature and mechanical agitation technology, nano particle is evenly distributed in liquid magnesium alloy.But because the employed SiC nano particle of this technology just can decompose at 800 ℃, and along with the rising of temperature, decomposition becomes more violent; And the SiC nano particle directly adds in the alloy; Can't solve the reunion of nano particle, the enhanced granule amount is few, uses mechanical agitation; Therefore this technology is only applicable to non-ferrous metal, and inapplicable and high-temperature metal.Chinese invention patent ZL200510127307.9 discloses a kind of composite material with nano silicon carbide granulate strengthening aluminium base and preparation method, and this method is to adopt nano silicon carbide granulate and aluminium powder to process as raw material; Wherein the volume of nano silicon carbide granulate accounts for 0.5～20% of raw material volume, and the volume of aluminium powder accounts for 80～99.5% of raw material volume.Its preparation method is: 1, raw material mix is dropped into to vacuumize behind the sealing ball grinder and charge into argon gas again and carry out repeatedly 2～10 times; 2, high-energy ball milling; 3, hot pressed sintering; 4, hot extrusion promptly obtains composite material with nano silicon carbide granulate strengthening aluminium base.Preparation technology of the present invention is simple, and cost is low, and nano silicon carbide granulate is evenly distributed in aluminum substrate, and the powder process rate is high, and the mechanical property of composite is significantly increased.It has solved, and the nanoscale enhanced granule can not be uniformly distributed in the aluminum substrate in the method for traditional preparation process particle enhanced aluminum-based composite material, and preparation technology is numerous and diverse, the problem that cost is high.But because this process using aluminium powder is made raw material, and hot extrusion again behind the employing powder metallurgical technique hot pressed sintering, because complex process, cost is high, and equipment investment is big, and technical difficulty is big, is only applicable to low-temperature metal equally.
For realizing the production of nano alloyed steel, make it on mold materials and high-abrasive material field, realize using, in recent years, carried out a large amount of research both at home and abroad, developed some novel preparation process.Chinese invention patent ZL200610046063.6 discloses a kind of high-strength abrasion-proof thermostable nano alloyed steel material and preparation method thereof, and this invention is for to produce nano alloyed steel according to smelting process.The chemical composition of this material (by weight percentage) is: tungsten (W) 0.06～6.0%, manganese (Mn) 0.6～3.0%, vanadium (V) 0.06～6.0%; Niobium (Nb) 0.22～4.0%, molybdenum (Mo) 0.0～7.0, carbon (C) 0.5～4.0; Chromium (Cr) 1.0～8.0, other elements 0.1～3.0, all the other are iron (Fe).Used main equipment is a vaccum sensitive stove.Technological process mainly comprises the raw material preparation, goes into three process such as stove smelting, casting.Raw material adopts the pig iron or straight carbon steel, and alloy adopts the ferroalloy of above-mentioned institute formulated component element.Production technology is for to carry out vacuum metling with above-mentioned various raw materials in vaccum sensitive stove, when temperature reaches 1620～1750 ℃, feed stock for blast furnace all melt and composition evenly after, smelt tapping, the ingot casting moulding.The steel ingot of being produced is through checking 80% grain size less than 50nm.It is simple that this technology has production technology, low cost and other advantages.But this technology only is to utilize at present the microalloy crystal grain thinning of institute's extensive use both at home and abroad; Suppress through alloying element that the grain growth principle of steel prepares; That utilizes especially that niobium (Nb) had in the metallic crystal process can suppress crystallization again; The performance of the recrystallization temperature of raising material is made, and the steel ingot of manufacturing still belongs to the fine-grained steel scope, can not be called nano alloyed steel.And this technology is the mode that combines through high cleanliness molten metal and microalloying, at the certain forming core particle of the inner formation of steel, because these particles are almost separated out in the subsolidus austenite; So the forming core to austenite itself does not have the forming core central role, promptly, can only play the pinning inhibition to the grain growth in the later stage hot procedure to the not effect of refinement as cast condition crystal grain; Thereby existing degree of purity to require height to molten steel, the quality stability of the steel alloy of being produced is poor, lacks the pinning of the second phase particle to crystal grain; Difficult quality guarantee; Defectives such as process controllability is poor, and production process control is had relatively high expectations, and the control difficulty is big.
Because the particle diameter of nano powder is little, the surface can be high, thereby have the trend of spontaneous reunion, is difficult to its ground in medium is spread out.So how improving the dispersiveness of nano-powder in medium is the key problem in technology during nano-powder material is used.Metal nano powder is applied to powder metallurgical technique, to reduce sintering temperature and to improve the performance of metallurgical product, what at first need consider is how to make metal nano powder homodisperse problem in micron powder commonly used.In addition, the nano metal based composites the preparation process in, tend to run into the consistency problem that strengthens between body and the metallic matrix, promptly strengthen the wetability requirement of body and metallic matrix.Simultaneously, no matter be solid phase method or liquid phase method, strengthen between body and the metallic matrix all having interfacial reaction, it has influence on metal-base composites performance and stability during with the high temperature application when high temperature prepares.Can from metallic matrix, direct (being original position) generate if strengthen body (particle, nano particle, whisker etc.), then above-mentioned consistency problem can be solved preferably.Generated in-situ enhancing body combines well with the metallic matrix interface, and the thermodynamic stability of production phase is good, does not have the problems such as wetting and interfacial reaction that strengthen between body and the metallic matrix, and this preparation method is exactly an in-situ compositing.
The synthetic notion of original position originates from in-situ crystallization and in-situ polymerization in the process of setting, receives the generally attention of Chinese scholars as a kind of breakthrough new complex technique.Several method at present commonly used have original position solidify from think of a way, reaction in-situ pressure sintering, internal oxidation process method, reaction mechanical alloying technology etc.The original position synthetic technology can overcome matrix with second mutually or with strengthen body and soak into bad; Interfacial reaction produces brittle layer; Problems such as second phase or wild phase skewness; Thereby have great potential in development of new metal-base nanometer composite material side, but present research work is focusing more on the aluminum matrix composite, and relevant original position synthesis iron base composite study is just receiving increasing attention.Because the mould steel fusion temperature is high; After adding in the steel, nano particle exists many key factors such as even dispersion technology difficulty in steel is big; Seriously restricting the Application and Development of metal-base nanometer composite material; Cause the preparation technology of present domestic and international some metal-base nanometer composite materials of developing still to rest on the experimental stage, make present research still belong to vacancy, at least also do not form product for Metal Substrate one nano composite material.
Therefore; To have preparation technology simple in research and development, and the nano powder modified and reinforced die steels preparation method that production cost is low is to improving mould steel service life; Reduce the mould manufacturing cost and use cost; Enhance productivity, practice thrift valuable alloy and energy resource consumption, have great scientific meaning and economic implications.
Summary of the invention
The objective of the invention is to solve deficiency of the prior art; Provide a kind of nano particle to strengthen mould steel Preparation Method; Nano particle is added in the mould steel matrix, receive meter particle is evenly distributed in the mould steel parent metal, realize the effectively compound of nano particle and die steel material; Thereby the nano powder modified high abrasion mould steel of the novel high-performance of preparing excellent performance; It is simple that acquisition has preparation technology, and production cost is low, the nano modification high abrasion mould steel preparation method of good product performance.
Content of the present invention comprises: original position synthesis of nano particle technology, the wear-resisting mould steel technology of preparation nano reinforcement.
It is at present domestic and international applied various hot die steels, cold work die steel, plastic die steel, high-speed steel, heat-resistance stainless steel, high temperature alloy, tool steel that nano-powder of the present invention is strengthened the reinforced die steels basic material, and its chemical component weight percentage is standard type component and weight percent content or the modified component and the weight percent content of above-mentioned various mould steel, high-speed steel, heat-resistance stainless steel, high temperature alloy, tool steel; The synthetic nano particle of institute's original position is the complex that any two kinds and the two or more amalgams among various carbide, nitride, carbonitride, oxide or carbide, nitride, boride, the oxide formed; The nano particle diameter is less than 100nm, and addition is 0.1%～6% of a mould steel percentage by weight.
Preparation technology of the present invention is:
1, original position synthesis of nano particle prefabricated section preparation technology:
(1) original position synthesis of nano particle strengthens prefabricated section preparation technology:
More than or equal to 99%, granularity is less than the industrial Ti powder of 800 μ m with purity, and purity is more than or equal to 99%, and granularity is less than industrial Al powder, silicon nitride powder and the graphite powder of 400 μ m, and configuration proportion is Si
3N
4: the mol ratio of Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain size less than the synthetic TiNC/Si of the original position of 100nm
3N
4/ Al
2O
3The nanometer mixed powder; With the synthetic TiNC/Si of the made original position of getting ready
3N
4/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of percentage by weight; After putting into agitating ball mill and mixing; The polyvinyl alcohol weak solution that accounts for said mixture volume 1/30～1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the mixed powder that contains prediffusion original position synthesis of nano particle after mixing through 70 ℃～100 ℃ temperature baking;
(2) nano particle strengthens dispersion prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: sodium carbonate: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder percentage by weight: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the original position synthesis of nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
(3) the preparation molding process of nano particle enhancing tool steel is:
A, employing casting production process; After said original position synthesis of nano powder compound prefabricated section taken by weighing by 0.1%～6% addition of mould steel molten steel weight; Place it in the bottom of steel ladle; With the mould steel of required composition according to smelting process require to smelt with refining after pour the steel ladle of putting into nano-powder compound prefabricated section into, the nano-powder compound prefabricated section at the bottom of high-temperature molten steel and the steel ladle reacts, prefabricated section original position in molten steel is synthesized TiNC/Si
3N
4/ Al
2O
3The nanometer hybrid particles; Steel ladle called in carried out electromagnetic agitation in the magnetic stirrer about 5～15 minutes; Through adjustment and control electromagnetic agitation intensity, make original position synthesis of nano powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, be evenly distributed in the mould steel molten steel;
B: moulding by casting
To spread has original position to synthesize TiNC/Si
3N
4/ Al
2O
3The mould molten steel of nanometer hybrid particles carries out permanent mold casting, sand casting, vacuum full mold casting, centrifugal casting, vacuum pressing and casting moulding according to conventional mould steel cast shaping process; Promptly obtain nano modification mould steel casting ingot, will contain TiNC/Si according to conventional processing technology
3N
4/ Al
2O
3The mould steel casting ingot of nanometer mixed powder modification carries out electroslag smelting casting or forging molding, and the nano particle that manufactures required geometry and size strengthens mould steel.
Beneficial effect
Compared with present technology, the present invention produces effect and is embodied in:
1, the present invention adds an amount of iron powder with original position synthesis of nano particle to carry out pre-dispersed; Add an amount of binding agent and flux then and process the dispersion prefabricated section; Add in the steel ladle; Adopt the block dispersion method that nano particle is diffused in the mould steel matrix, through magnetic stirrer it is formed evenly in the mould steel matrix and disperse, adopt the casting moulding.This process using original position synthesis of nano particle process improving the wettability of nano particle and mould steel matrix, it is pollution-free to strengthen the surface, and compatibility is good between matrix, interface bond strength is high; Saved that the enhancing body is synthetic separately, operations such as processing and adding, therefore, its technology is simple, cost is relatively low.
2, owing to add Al
2O
3The nanometer wild phase has promoted the nanometerization of powder, shortens the time of nanometerization, improves grinding efficiency, plays the effect of rapid nanoization.Simultaneously, can stop TiNC/Si effectively
3N
4The grain growth of nano particle in high-temperature molten steel.
3, solved the difficult problem of nanoparticle agglomerates through prediffused technique; And increased the decentralization of nano particle in matrix; Through evenly the distributed mould steel of nano particle of secondary diffusion technique and electromagnetic agitation technology, make mould steel obtain modification and reinforcement.Its volume fraction of addition scalable through the adjustment nano particle; Under the prerequisite that guarantees material impact toughness; The nano particle volume fraction is big more, and material wear ability is high more, in addition because the adding of nano particle can obtain heterogeneous forming core; Refinement carbide grain, the also corresponding wearability that improves material.
4, on the basis of traditional moulds steel and metal wear resistant material casting,, improve die steel material intensity, obdurability and anti-wear performance through adding the nano reinforcement particle.
5, on diffusion technique,, make distribution and the strengthening effect of nano particle in the die steel material molten metal more effective through control proper metal liquid temp and electromagnetic agitation technology.
6, nano powder modified mould steel of the present invention has good mechanical property; Can satisfy the instructions for use under the various operating modes, greatly reduce the preparation cost of nano particle enhancing modified mould steel, production technology is simple; Need not special installation, conventional cast factory can produce.
The specific embodiment
Embodiment 1
At Cr
12Add nano particle in the MoV cold work die steel and carry out modification.Cr
12The chemical composition of MoV cold work die steel is C1.45～1.70, Cr4.75～5.5, and Mo0.40～0.60, Si＜0.40, V0.15～0.30, Mn＜0.40, weight is 1000kg.TiB
2/ Al
2O
3Nanoparticle size is 100nm, and the addition percentage by weight is 1.5%.Preparation technology is:
1) original position synthesis of nano particle prefabricated section preparation technology:
More than or equal to 99%, granularity is less than the industrial Ti powder of 800 μ m with purity, and purity is more than or equal to 99%, and granularity is less than industrial Al powder, silicon nitride powder and the graphite powder of 400 μ m, and configuration proportion is Si
3N
4: the mol ratio of Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometerization of powder, shorten the time of nanometerization, improve grinding efficiency, play the effect of rapid nanoization.To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain size less than the synthetic TiNC/Si of the original position of 100nm
3N
4/ Al
2O
3The nanometer mixed powder; With the synthetic TiNC/Si of the made original position of getting ready
3N
4/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of percentage by weight; After putting into agitating ball mill and mixing; The polyvinyl alcohol weak solution that accounts for said mixture volume 1/30～1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the mixed powder that contains prediffusion original position synthesis of nano particle after mixing through 70 ℃～100 ℃ temperature baking;
2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: sodium carbonate: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder percentage by weight: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
3) the preparation molding process of nano particle enhancing mould steel is:
A, employing permanent mold casting production technology are pressed Cr with said nano-powder compound prefabricated section
12After 1.6% addition of MoV cold work die steel molten steel weight takes by weighing, place it in the bottom of steel ladle, according to Cr
12MoV cold-work die composition of steel requires and smelting process requires to smelt with molten steel after refining to pour the steel ladle of putting into original position synthesis of nano powder compound prefabricated section into; Original position synthesis of nano powder compound prefabricated section at the bottom of high-temperature molten steel and the steel ladle reacts, the synthetic TiNC/Si of prefabricated section original position in molten steel
3N
4/ Al
2O
3The nanometer hybrid particles is called in steel ladle and was carried out electromagnetic agitation in the magnetic stirrer about 6 minutes, makes nano-powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, is evenly distributed on Cr
12In the MoV cold work die steel molten steel;
With spreading the Cr that nano particle is arranged
12MoV cold work die steel molten steel pours into casting in the metal mold, promptly obtains the Cr that nano particle strengthens
12MoV cold work die steel casting ingot; Nano particle after the moulding is strengthened Cr
12MoV cold work die steel casting ingot carries out electroslag smelting casting and forging molding processing according to conventional processing technology, manufactures the nano powder modified high abrasion Cr of required geometry and size
12The MoV cold work die steel.
Embodiment 2
In the H13 hot die steel, add nano particle and carry out modification.The chemical composition of H13 hot die steel is C 0.31～0.45, Cr4.75～5.5, and Mo1.10～1.75, Si0.81～1.20, V0.80～1.20, Mn＜0.40, weight is 1000kg.TiB
2/ Al
2O
3Nanoparticle size is 50nm, and the addition percentage by weight is 2.5%.Preparation technology is:
1) original position synthesis of nano particle prefabricated section preparation technology:
More than or equal to 99%, granularity is less than the industrial Ti powder of 800 μ m with purity, and purity is more than or equal to 99%, and granularity is less than industrial Al powder, silicon nitride powder and the graphite powder of 400 μ m, and configuration proportion is Si
3N
4: the mol ratio of Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometerization of powder, shorten the time of nanometerization, improve grinding efficiency, play the effect of rapid nanoization.To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain size less than the synthetic TiNC/Si of the original position of 100nm
3N
4/ Al
2O
3The nanometer mixed powder; With the synthetic TiNC/Si of the made original position of getting ready
3N
4/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of percentage by weight; After putting into agitating ball mill and mixing; The polyvinyl alcohol weak solution that accounts for said mixture volume 1/30～1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the mixed powder that contains prediffusion original position synthesis of nano particle after mixing through 70 ℃～100 ℃ temperature baking;
2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: sodium carbonate: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder percentage by weight: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
3) the preparation molding process of nano particle enhancing mould steel is:
A, employing permanent mold casting production technology; After said nano-powder compound prefabricated section taken by weighing by 1.6% addition of H13 hot die steel molten steel weight; Place it in the bottom of steel ladle; Require to smelt to pour the steel ladle of putting into original position synthesis of nano powder compound prefabricated section into according to requirement of H13 hot-work die composition of steel and smelting process with molten steel after refining; Original position synthesis of nano powder compound prefabricated section at the bottom of high-temperature molten steel and the steel ladle reacts, the synthetic TiNC/Si of prefabricated section original position in molten steel
3N
4/ Al
2O
3The nanometer hybrid particles is called in steel ladle and is carried out electromagnetic agitation in the magnetic stirrer, makes nano-powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, is evenly distributed in the H13 hot die steel molten steel.
Be that with the difference of embodiment the time of carrying out electromagnetic agitation is about 8 minutes.Other technical process and embodiment 1 omit together.
Embodiment 3
At W
6Mo
5Cr
4V
2Adding nano particle in the high-speed steel carries out modified and reinforced.W
6Mo
5Cr
4V
2The chemical composition of high-speed steel is C0.80～0.90, Cr3.80～4.40, and W4.50～5.50, Mo5.50～6.75, Si＜0.40, Mn＜0.40, V1.75～2.25, weight is 1000kg.TiB
2/ Al
2O
3Nanoparticle size is 70nm, and the addition percentage by weight is 0.7%.
1) original position synthesis of nano particle prefabricated section preparation technology:
More than or equal to 99%, granularity is less than the industrial Ti powder of 800 μ m with purity, and purity is more than or equal to 99%, and granularity is less than industrial Al powder, silicon nitride powder and the graphite powder of 400 μ m, and configuration proportion is Si
3N
4: the mol ratio of Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometerization of powder, shorten the time of nanometerization, improve grinding efficiency, play the effect of rapid nanoization.To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain size less than the synthetic TiNC/Si of the original position of 100nm
3N
4/ Al
2O
3The nanometer mixed powder; With the synthetic TiNC/Si of the made original position of getting ready
3N
4/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of percentage by weight; After putting into agitating ball mill and mixing; The polyvinyl alcohol weak solution that accounts for said mixture volume 1/30～1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the mixed powder that contains prediffusion original position synthesis of nano particle after mixing through 70 ℃～100 ℃ temperature baking;
2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: sodium carbonate: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder percentage by weight: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
3) the preparation molding process of nano particle enhancing mould steel is:
A, employing permanent mold casting production technology are pressed W with said nano-powder compound prefabricated section
6Mo
5Cr
4V
2After 1.6% addition of high-speed steel molten steel weight takes by weighing, place it in the bottom of steel ladle, according to W
6Mo
5Cr
4V
2The high-speed steel composition requires and smelting process requires to smelt with molten steel after refining to pour the steel ladle of putting into original position synthesis of nano powder compound prefabricated section into; Original position synthesis of nano powder compound prefabricated section at the bottom of high-temperature molten steel and the steel ladle reacts, the synthetic TiNC/Si of prefabricated section original position in molten steel
3N
4/ Al
2O
3The nanometer hybrid particles is called in steel ladle and is carried out electromagnetic agitation in the magnetic stirrer, makes nano-powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, is evenly distributed on W
6Mo
5Cr
4V
2In the high-speed steel molten steel.
Be that with the difference of embodiment the time of carrying out electromagnetic agitation is about 12 minutes.
Other technical process and embodiment 1,2 omit together.
Claims (2)
1. a nano particle enhancing mould steel is equipped with technology, and its preparation technology and step are following:
(1) original position synthesis of nano particle strengthens prefabricated section preparation technology:
More than or equal to 99%, granularity is less than the industrial Ti powder of 800 μ m with purity, and purity is more than or equal to 99%, and granularity is less than industrial Al powder, silicon nitride powder and the graphite powder of 400 μ m, and configuration proportion is Si
3N
4: the mol ratio of Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain size less than the synthetic TiNC/Si of the original position of 100nm
3N
4/ Al
2O
3The nanometer mixed powder; With the synthetic TiNC/Si of the made original position of getting ready
3N
4/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of percentage by weight; After putting into agitating ball mill and mixing; The polyvinyl alcohol weak solution that accounts for said mixture volume 1/30～l/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the mixed powder that contains prediffusion original position synthesis of nano particle after mixing through 70 ℃～100 ℃ temperature baking;
(2) nano particle strengthens dispersion prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: sodium carbonate: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder percentage by weight: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the original position synthesis of nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
(3) the preparation molding process of nano particle enhancing tool steel is:
A, employing casting production process; After said original position synthesis of nano powder compound prefabricated section taken by weighing by 0.1%～6% addition of mould steel molten steel weight; Place it in the bottom of steel ladle; With the mould steel of required composition according to smelting process require to smelt with refining after pour the steel ladle of putting into nano-powder compound prefabricated section into, the nano-powder compound prefabricated section at the bottom of high-temperature molten steel and the steel ladle reacts, prefabricated section original position in molten steel is synthesized TiNC/Si
3N
4/ Al
2O
3The nanometer hybrid particles; Steel ladle called in carried out electromagnetic agitation in the magnetic stirrer about 5～15 minutes; Through adjustment and control electromagnetic agitation intensity, make original position synthesis of nano powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, be evenly distributed in the mould steel molten steel;
B: moulding by casting
To spread has original position to synthesize TiNC/Si
3N
4/ Al
2O
3The mould steel molten steel of nanometer hybrid particles carries out permanent mold casting, sand casting, vacuum full mold casting, centrifugal casting, vacuum pressing and casting moulding according to conventional mould steel cast shaping process; Promptly obtain nano modification mould steel casting ingot, will contain TiNC/Si according to conventional processing technology
3N
4/ Al
2O
3The mould steel casting ingot of nanometer mixed powder modification carries out electroslag smelting casting or forging molding, and the nano particle that manufactures required geometry and size strengthens mould steel.
2. nano particle according to claim 1 strengthens mould steel; It is characterized in that: it is various hot die steels, cold work die steel, plastic die steel, high-speed steel, heat-resistance stainless steel, high temperature alloy, tool steel that nano particle strengthens mould steel matrix material, and its chemical component weight percentage is standard type component and weight percent content or the modified component and the weight percent content of above-mentioned various mould steel, high-speed steel, heat-resistance stainless steel, high temperature alloy, tool steel material.
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| CN103212718A (en) * | 2013-04-18 | 2013-07-24 | 辽宁科技大学 | Preparation method of over-spreading pre-dispersion molten iron attached nanometer oxide powder |
| CN103243194A (en) * | 2013-05-31 | 2013-08-14 | 安徽工业大学 | Method for optimizing steel structure by adding nano particles into steel liquid |
| CN104726639A (en) * | 2015-03-13 | 2015-06-24 | 北京科技大学 | Method for uniformly dispersing additional nanoparticles in steel |
| CN105925918A (en) * | 2016-06-27 | 2016-09-07 | 山东建筑大学 | Making method for aluminum oxide-silicon carbide crystal whisker reinforced cold work die steel material |
| CN107848034A (en) * | 2015-07-23 | 2018-03-27 | 俄罗斯国立科技大学莫斯科钢铁合金研究所 | The method that electrode is prepared by the alloy based on nickel aluminide |
| CN111893395A (en) * | 2020-06-09 | 2020-11-06 | 黄石市鑫楚精密模具股份有限公司 | High-strength die steel and heat treatment method thereof |
| CN115386786A (en) * | 2022-08-26 | 2022-11-25 | 昆明理工大学 | Method for enhancing bonding strength of ceramic particles and matrix |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103212718A (en) * | 2013-04-18 | 2013-07-24 | 辽宁科技大学 | Preparation method of over-spreading pre-dispersion molten iron attached nanometer oxide powder |
| CN103212718B (en) * | 2013-04-18 | 2015-02-18 | 辽宁科技大学 | Preparation method of over-spreading pre-dispersion molten iron attached nanometer oxide powder |
| CN103243194A (en) * | 2013-05-31 | 2013-08-14 | 安徽工业大学 | Method for optimizing steel structure by adding nano particles into steel liquid |
| CN103243194B (en) * | 2013-05-31 | 2015-01-21 | 安徽工业大学 | Method for optimizing steel structure by adding nano particles into steel liquid |
| CN104726639A (en) * | 2015-03-13 | 2015-06-24 | 北京科技大学 | Method for uniformly dispersing additional nanoparticles in steel |
| CN107848034A (en) * | 2015-07-23 | 2018-03-27 | 俄罗斯国立科技大学莫斯科钢铁合金研究所 | The method that electrode is prepared by the alloy based on nickel aluminide |
| CN107848034B (en) * | 2015-07-23 | 2019-11-15 | 俄罗斯国立科技大学莫斯科钢铁合金研究所 | The method that electrode is prepared by the alloy based on nickel aluminide |
| CN105925918A (en) * | 2016-06-27 | 2016-09-07 | 山东建筑大学 | Making method for aluminum oxide-silicon carbide crystal whisker reinforced cold work die steel material |
| CN111893395A (en) * | 2020-06-09 | 2020-11-06 | 黄石市鑫楚精密模具股份有限公司 | High-strength die steel and heat treatment method thereof |
| CN115386786A (en) * | 2022-08-26 | 2022-11-25 | 昆明理工大学 | Method for enhancing bonding strength of ceramic particles and matrix |
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