CN106811661A - The preparation method of alloy hot-work die base steel steel bonded carbide in a kind of TiC - Google Patents
The preparation method of alloy hot-work die base steel steel bonded carbide in a kind of TiC Download PDFInfo
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- CN106811661A CN106811661A CN201710074661.2A CN201710074661A CN106811661A CN 106811661 A CN106811661 A CN 106811661A CN 201710074661 A CN201710074661 A CN 201710074661A CN 106811661 A CN106811661 A CN 106811661A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/10—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on titanium carbide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
- B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
- C22C33/0228—Using a mixture of prealloyed powders or a master alloy comprising other non-metallic compounds or more than 5% of graphite
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0292—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with more than 5% preformed carbides, nitrides or borides
Abstract
The present invention relates to a kind of preparation method of alloy hot-work die base steel steel bonded carbide in TiC, comprise the following steps：Proportionally weigh carbonized titanium powder and middle alloy hot die steel matrix powder, alloyed powder is put into ball mill and is mixed and is crushed, wherein addition absolute ethyl alcohol is process control agent, wet mixed powder is put into vacuum drying chamber after ball milling is dried, standby after drying.Organic monomer and initiator are added in solvent and prepare premixed liquid；Add the additive for improving slurry fluidity and dispersiveness；Add catalyst and pH adjusting agent and stir, obtain slurry；The slurry solidifying mould of injection note is vacuumized or shaken degasification, base substrate is put into vacuum drying chamber after slurry curing shaping is dried, dried base substrate is carried out into integrated degumming and sintering in vacuum sintering furnace, prepare steel bonded carbide.The present invention has the advantages that relatively low process is simple, cost, easily prepared large scale, Irregular Shaped Parts on the basis of it ensure that steel bonded carbide macro property.
Description
Technical field
The present invention relates to a kind of preparation method of alloy hot-work die base steel steel bonded carbide in TiC, belong to Metal Substrate
Field of composite material preparation.
Background technology
Steel bonded carbide is a kind of composite with ceramic phase and with steel as bonding matrix, and its performance is between common hard
Between matter alloy and steel, while having a series of other advantages, it is set to be widely used in many fields.Prepare at present
The method of this kind of material is mainly powder metallurgy process, including compressing, cold isostatic compaction, injection moulding etc., with laggard
Row vacuum-sintering is used as final shaping.Larger pressure needed for larger part is prepared using compressing and cold isostatic compaction and nothing
Can be power, the parts for preparing complicated shape are more difficult, simultaneously for preparing, ceramic crystalline grain size is smaller to answer with content is higher
When condensation material, shape more difficult and crystal grain and easily grow up；The small parts of this kind of material are produced using ejection forming method, but
This kind of method is not suitable for the preparation of the parts of large-size, while the colloid adulterated in this kind of technique is more, usually time
It is more long, while the consistency of blank of material is relatively low, it is unfavorable for quickly carrying out production and the raising of consistency；Also utilize self- propagating
Combustion synthesis reaction method prepares such material, but the material for preparing often has relatively low consistency.Some are with high temperature insostatic pressing (HIP)
Sintering etc. as final sintering process, but it is costly.
The content of the invention
Exist in terms of shaping and sintering the present invention be directed to existing steel bonded carbide and be difficult to quick, economic preparation
The difficulty of the aspects such as crystallite dimension is smaller and content is higher, large-size, complicated shape part, there is provided one kind prepare large scale,
The preparation method of alloy hot-work die base steel steel bonded carbide in complicated shape and simple production process, lower-cost TiC.
The present invention provides a kind of preparation method of alloy hot-work die base steel steel bonded carbide in TiC, including following mistake
Journey：
（1）Proportionally weigh alloy hot die steel matrix powder, 0.03~0.3% in 30~60% carbonized titanium powders and 33~60%
Ce, 0.05~0.3% Nb, 0.1~0.8% SiMgRe, 0.2~0.6% graphite powder, 5~10% carbonyl iron dusts, by the powder
Last being put into ball mill with rare earth, Nb powder is mixed and is crushed, wherein addition absolute ethyl alcohol is process control agent, will be mixed
Powder is dried in being put into vacuum drying chamber, standby after drying；
（2）Organic monomer and initiator are added in solvent and prepare premixed liquid；
（3）Dry mixed powder is added in premixed liquid and stirred, it is slurry that percentage by volume is added in whipping process
The oleic acid of the 1~3% of material, to improve slurry fluidity and dispersiveness；
（4）Add catalyst and pH adjusting agent and stir, obtain slurry；Slurry is injected into mould and with vacuumizing or shake
Method bubble removing, slurry curing shaping, the demoulding after the reaction regular hour obtains final product base substrate；
（5）Base substrate is put into vacuum drying chamber and is dried, dried base substrate is carried out into degumming and final sintering；
First, the middle alloy hot-work die steel matrix that described steel matrix includes include 4Cr5MoSiV, 4Cr5MoSiV1,
One of 4Cr5W2VSi, 4Cr3Mo3SiV1,3Cr3Mo3VNb are planted；
Second, described organic monomer is hydroxy-ethyl acrylate, solvent is toluene, initiator is benzoyl peroxide；Wherein have
The volume ratio of machine monomer and solvent is 1：2~2：1, the content of initiator is 0.6~1.5 g in every 100 ml premixed liquids；
3rd, mixed powder percentage by volume in the slurry is 40~60%；
4th, initiator used is dimethylaniline, and the percentage that addition accounts for slurry volume is 0.1~0.2%；
5th, pH adjusting agent used is ammoniacal liquor, and regulation pH value is 7~8；
6th, degumming and sintering carry out integral sintering using vacuum sintering furnace, and technique is：Base substrate is incubated 1 at 400~500 DEG C
~3 h carry out degumming, and being incubated 1~2h at 1400~1450 DEG C is finally sintered.
Beneficial effect
Beneficial effects of the present invention are：
1st, the invention allows to quick, economic preparation crystallite dimension is smaller, the part of large-size, complicated shape.
2nd, Gelcasting Technique be in low viscosity, the powder-solvent concentrate suspension of solid volume fraction high, plus
Enter organic monomer, organic monomer chemical crosslinking polymerization or physics in then making suspended substance in the presence of catalyst and initiator
Tridimensional network is cross-linked into, so that suspended substance in-situ solidifying is molded, is finally discharged colloid a small amount of in base substrate, then carry out
Sintering obtains compact components.Gel casting can reduce the quantity of gross blow hole in base substrate, and pore-size distribution is more uniform, improves
The uniformity of base substrate；Gel casting cycle is short, the structure and even density of product are not in the segregation of particle, material
It is stable and reliable for performance.Additionally, gel casting to mould without specific requirement, it is considered to be improve reliability of material, prepare
One of large scale, most effectual way of complicated form part.The reunion of particle can be efficiently controlled due to gel casting, is made
For the base substrate for going out structure and even density, so as to obtain high performance sintered body, the use reliability of material is improved.It is simultaneously solidifying
Limitation of the glue casting to ceramic crystalline grain size and content is smaller, makes it use scope wider.During gel casting
Can also by controlling the parameter of each additive, and then control solidification time and body crack defects etc., so that it is different to meet preparation
The demand of parts.Low pressure sintering process can promote the mobility of liquid phase in liquid sintering process, can shorten sintering time, have
Beneficial to the uniformity and compactness of tissue, moreover it is possible to ceramic phase and binder alloy boundary strength are improved, so as to improve the performance of material.
3rd, to prevent serious adhesive wear, more preferably self-lubricating effect is obtained, the present invention is by steel bonded carbide
The graphite of the middle certain content of addition, makes to contain the micro- graphite-phase of many self-lubricatings in materials microstructure, makes the friction of hard alloy
Coefficient is greatly improved, so that friction factor reduction.
4th, in order to adjust the granularmetric composition of compound, improve suppression performance, greatly improve shaping density, the present invention
A certain proportion of carbonyl iron dust is added in reduced iron powder.Substituting reduced iron powder with carbonyl iron dust can improve powder forming
Can, make green density higher, acceleration of sintering process reduces sintering temperature.Make steel knot of the invention by adding carbonyl iron dust
The mechanics of hard alloy is significantly improved, and hardness brings up to 81.8HRA by 77.5HRA, bending strength by 1123MPa or to
1447MPa。
5th, the present invention is by adding Ce, SiMgRe, and makes Ce, SiMgRe powder content between 0.2% and 0.5%, can rise
To rare earth reinforced effect.Because Ce, SiMgRe chemical property are active, in ball milling and sintering process, RE has to alloy powder
Obvious deoxidation and carbon effect is protected, contribute to improving for wetability between different constituent elements, so as to be conducive to densification process,
Reach the purpose for reducing porosity so that the porosity in steel bonded carbide is reduced, and the reduction of porosity will be helped
In the raising of plasticity and bending strength.At a sintering temperature, rare earth is gathered in TiC particle surfaces, its surface is reduced, and hinders
TiC crystallization of the dissolution and precipitation processes in the liquid phase, suppress growing up for TiC crystal grain；Ce, SiMgRe can be with metal dust interfaces simultaneously
On impurity and oxide-film effect, play a part of to purify interface, the segregation of S, P, Sb in crystal boundary can be suppressed, play deoxidation, de-
Sulphur, crystal grain thinning and improve Liquid phase flowability and wetability etc. and act on.So as to improve the performance of alloy material.
And because SiMgRe may also operate as inoculation(effect) in the alloy, the alloying pellet in matrix material is obtained ball
Shape, so as to improve the toughness of Steel-bonded Cemented Carbide.Therefore intensity, the toughness of steel bonded carbide of the invention
It is improved with consistency, bending strength can reach more than 1700MPa, consistency reaches more than 97.4%.
The present invention is by adding Ce, Nb, SiMgRe, it is suppressed that crystal grain is grown up, and plays a part of dispersion-strengtherning.
Specific embodiment
Embodiment 1：Weigh mass fraction be 50% TiC powder and 0.10% Ce, 0.05% Nb, 0.1% SiMgRe,
0.3% graphite powder, 6% carbonyl iron dust, alloy hot die steel matrix material powder in 4Cr5MoSiV1, by material powder and dilute
Soil, Nb powder are put into ball mill and are mixed and crushed, wherein addition absolute ethyl alcohol is process control agent, wet mixed powder are put
To enter be dried in vacuum drying chamber, it is standby after drying；According to volume ratio 1：1 measures organic monomer hydroxy-ethyl acrylate and solvent
Toluene prepares premixed liquid, to the benzoyl peroxide that 1.2 g/100 ml are added in premixed liquid and stirs；Will be dry mixed
Close powder to be added in premixed liquid, while 2% oleic acid being added dropwise and stirring, form slurry；To two of addition 0.15% in slurry
Methylaniline and add ammoniacal liquor regulation PH be 7；Base substrate is put into vacuum sintering furnace after removing bubble with vacuumizing method is taken off
Glue is sintered with final, and technique is：Being incubated 2 h at 500 DEG C carries out degumming, and being incubated 2h at 1450 DEG C is finally sintered；Finally
Furnace cooling obtains steel bonded carbide part.
Embodiment 2：Weigh mass fraction be 60% TiC powder and 0.2% Ce, 0.2% Nb, 0.25% SiMgRe,
0.4% graphite powder, 8% carbonyl iron dust, alloy hot die steel matrix material powder in 4Cr5W2VSi, by material powder and rare earth,
Nb powder is put into ball mill and is mixed and crushed, wherein addition absolute ethyl alcohol is process control agent, wet mixed powder is put into
It is dried in vacuum drying chamber, it is standby after drying；According to volume ratio 1：2 measure organic monomer hydroxy-ethyl acrylate and solvent first
Benzene prepares premixed liquid, to the benzoyl peroxide that 0.6 g/100 ml are added in premixed liquid and stirs；By dry mixing
Powder is added in premixed liquid, while 1% oleic acid being added dropwise and stirring, forms slurry；To the dimethyl of addition 0.1% in slurry
Aniline and add ammoniacal liquor regulation PH be 7.5；Base substrate is put into vacuum low-pressure sintering furnace after removing bubble with vacuumizing method carried out
Degumming is sintered with final, and technique is：Being incubated 1 h at 500 DEG C carries out degumming, and being incubated 2h at 1400 DEG C is finally sintered；Most
Furnace cooling afterwards obtains the part of steel bonded carbide.
Embodiment 3：Weigh mass fraction be 40% TiC powder and 0.25% Ce, 0.25% Nb, 0.3% SiMgRe,
0.5% graphite powder, 9% carbonyl iron dust, alloy hot die steel matrix material powder in 4Cr3Mo3SiV1, by material powder and dilute
Soil, Nb powder are put into ball mill and are mixed and crushed, wherein addition absolute ethyl alcohol is process control agent, wet mixed powder are put
To enter be dried in vacuum drying chamber, it is standby after drying；According to volume ratio 2：1 measures organic monomer hydroxy-ethyl acrylate and solvent
Toluene prepares premixed liquid, to the benzoyl peroxide that 1.5 g/100 ml are added in premixed liquid and stirs；Will be dry mixed
Close powder to be added in premixed liquid, while 3% oleic acid being added dropwise and stirring, form slurry；To the diformazan of addition 0.2% in slurry
Base aniline and add ammoniacal liquor regulation PH be 8；Base substrate is put into vacuum low-pressure sintering furnace after removing bubble with vacuumizing method carried out
Degumming is sintered with final, and technique is：Being incubated 3h at 400 DEG C carries out degumming, and being incubated 1h at 1450 DEG C is finally sintered；Finally
Furnace cooling obtains the part of steel bonded carbide.
Embodiment 4：Weigh TiC powder and 0.3% Ce that mass fraction is 30%, 0.3% Nb, 0.5% SiMgRe, 0.6%
Graphite powder, 10% carbonyl iron dust, alloy hot die steel matrix material powder in 3Cr3Mo3VNb, by material powder and rare earth, Nb
Powder is put into ball mill and is mixed and crushed, wherein addition absolute ethyl alcohol is process control agent, wet mixed powder is put into very
It is dried in empty drying box, it is standby after drying；According to volume ratio 2：1 measures organic monomer hydroxy-ethyl acrylate and solvent toluene
Premixed liquid is prepared, to the benzoyl peroxide that 1.5 g/100 ml are added in premixed liquid and is stirred；By dry mixed powder
It is added in premixed liquid, while 3% oleic acid being added dropwise and stirring, forms slurry；To the dimethyl benzene of addition 0.2% in slurry
Amine and add ammoniacal liquor regulation PH be 8；Base substrate is put into vacuum low-pressure sintering furnace after removing bubble with vacuumizing method carry out degumming
Sintered with final, technique is：Being incubated 3h at 400 DEG C carries out degumming, and being incubated 1h at 1450 DEG C is finally sintered；Finally with stove
Cooling obtains the part of steel bonded carbide.
Claims (7)
1. in a kind of TiC alloy hot-work die base steel steel bonded carbide preparation method, it is characterised in that comprise the following steps：
（1）Proportionally weigh alloy hot die steel matrix powder, 0.03~0.3% in 30~60% carbonized titanium powders and 33~60%
Ce, 0.05~0.3% Nb, 0.1~0.8% SiMgRe, 0.2~0.6% graphite powder, 5~10% carbonyl iron dusts, by the powder
Last being put into ball mill with rare earth, Nb powder is mixed and is crushed, wherein addition absolute ethyl alcohol is process control agent, will be mixed
Powder is dried in being put into vacuum drying chamber, standby after drying；
（2）Organic monomer and initiator are added in solvent and prepare premixed liquid；
（3）Dry mixed powder is added in premixed liquid and stirred, it is slurry that percentage by volume is added in whipping process
The oleic acid of the 1~3% of material, to improve slurry fluidity and dispersiveness；
（4）Add catalyst and pH adjusting agent and stir, obtain slurry；By the slurry solidifying mould of injection note and with vacuumizing or
Lash method bubble removing, slurry curing shaping, the demoulding after the reaction regular hour obtains final product base substrate；
（5）Base substrate is put into vacuum drying chamber and is dried, dried base substrate is carried out into degumming and final sintering.
2. preparation method according to claim 1, it is characterised in that described middle alloy hot-work die steel matrix includes
One of 4Cr5MoSiV, 4Cr5MoSiV1,4Cr5W2VSi, 4Cr3Mo3SiV1,3Cr3Mo3VNb are planted.
3. preparation method according to claim 1, it is characterised in that described organic monomer is hydroxy-ethyl acrylate, solvent
For toluene, initiator are benzoyl peroxide；Wherein the volume ratio of organic monomer and solvent is 1：2~2：1, every 100 ml premixs
The content of initiator is 0.6~1.5 g in liquid.
4. preparation method according to claim 1, it is characterised in that mixed powder percentage by volume in the slurry is 40~
60%。
5. preparation method according to claim 1, it is characterised in that initiator used is dimethylaniline, addition accounts for slurry
The percentage for expecting volume is 0.1~0.2%.
6. preparation method according to claim 1, it is characterised in that pH adjusting agent used is ammoniacal liquor, regulation pH value is 7~
8。
7. preparation method according to claim 1, it is characterised in that degumming and sintering carry out one using vacuum sintering furnace
Change sintering, technique is：Base substrate is incubated 1~3 h and carries out degumming at 500 DEG C, and being incubated 1~2h at 1400~1450 DEG C is carried out finally
Sintering.
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| CN115233068A (en) * | 2022-07-07 | 2022-10-25 | 广东正信硬质材料技术研发有限公司 | Light high-strength hard alloy material and preparation method thereof |
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