CN114749669A - Hot die pressing mold preparation method based on nano material modification - Google Patents
Hot die pressing mold preparation method based on nano material modification Download PDFInfo
- Publication number
- CN114749669A CN114749669A CN202210313348.0A CN202210313348A CN114749669A CN 114749669 A CN114749669 A CN 114749669A CN 202210313348 A CN202210313348 A CN 202210313348A CN 114749669 A CN114749669 A CN 114749669A
- Authority
- CN
- China
- Prior art keywords
- hot
- parts
- coating
- molding die
- oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000004048 modification Effects 0.000 title claims abstract description 23
- 238000012986 modification Methods 0.000 title claims abstract description 23
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000007723 die pressing method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 141
- 239000011248 coating agent Substances 0.000 claims abstract description 118
- 238000000576 coating method Methods 0.000 claims abstract description 118
- 238000000465 moulding Methods 0.000 claims abstract description 75
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 56
- 239000011265 semifinished product Substances 0.000 claims abstract description 42
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 37
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000007731 hot pressing Methods 0.000 claims abstract description 36
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 28
- 229910003443 lutetium oxide Inorganic materials 0.000 claims abstract description 27
- 230000007246 mechanism Effects 0.000 claims abstract description 27
- MPARYNQUYZOBJM-UHFFFAOYSA-N oxo(oxolutetiooxy)lutetium Chemical compound O=[Lu]O[Lu]=O MPARYNQUYZOBJM-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 claims abstract description 22
- 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 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 17
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 16
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 16
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims description 46
- 238000001354 calcination Methods 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000001035 drying Methods 0.000 claims description 40
- 238000000227 grinding Methods 0.000 claims description 40
- 238000000498 ball milling Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 22
- 239000002270 dispersing agent Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 16
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 15
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 15
- 238000004140 cleaning Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 238000005485 electric heating Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 6
- 230000001070 adhesive effect Effects 0.000 claims description 6
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229920006244 ethylene-ethyl acrylate Polymers 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229940057838 polyethylene glycol 4000 Drugs 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 8
- 230000003014 reinforcing effect Effects 0.000 abstract description 8
- 230000002035 prolonged effect Effects 0.000 abstract description 6
- 239000012744 reinforcing agent Substances 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 3
- 239000003381 stabilizer Substances 0.000 abstract description 2
- 239000000428 dust Substances 0.000 description 12
- 238000009434 installation Methods 0.000 description 10
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical class C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 230000003139 buffering effect Effects 0.000 description 3
- 230000010405 clearance mechanism Effects 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000001291 vacuum drying Methods 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 2
- -1 polydimethylsiloxane Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 229910001339 C alloy Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004049 embossing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- 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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/007—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of moulds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/22—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to internal surfaces, e.g. of tubes
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- B22F3/24—After-treatment of workpieces or articles
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
-
- 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
-
- 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
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
-
- 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
- C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
-
- 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
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/241—Chemical after-treatment on the surface
- B22F2003/242—Coating
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00482—Coating or impregnation materials
- C04B2111/00525—Coating or impregnation materials for metallic surfaces
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/2038—Resistance against physical degradation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Metallurgy (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Structural Engineering (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a hot-pressing die preparation method based on nano material modification, and relates to the technical field of hot-pressing die preparation. The method takes zirconia as a matrix, silicon nitride, silicon carbide and alumina as reinforcing agents, scandium oxide and lutetium oxide as stabilizing agents, and chromium powder, nickel powder, cobalt powder and vanadium powder as sintering aids; the silicon nitride, the silicon carbide and the aluminum oxide modify the zirconia to form an intra-crystal/inter-crystal mixed structure, and the multiple toughening and reinforcing mechanisms act synergistically to improve the mechanical property of the die material, increase the mechanical strength and the wear resistance and reduce the thermal expansion coefficient; scandium oxide and lutetium oxide play roles in modifying and refining grains, and chromium powder, nickel powder, cobalt powder and vanadium powder are dispersed in the grains in the sintering process; the friction-reducing wear-resisting performance of the inner cavity of the hot-molding die is improved by coating the reinforced wear-resisting coating material on the inner surface of the semi-finished product of the hot-molding die, the service life of the hot-molding die is prolonged, and the demoulding after die pressing is convenient.
Description
Technical Field
The invention relates to the technical field of hot-pressing die preparation, in particular to a hot-pressing die preparation method based on nanometer material modification.
Background
The hot-pressing die is made of die steel which has the advantages of enough hardness, enough wear resistance, enough strength and toughness, good processing performance and good pattern erodibility, so that medium carbon alloy steel is generally selected. With the rapid development of the technology, the high-temperature strength and wear resistance of the alloy steel die and the hard alloy die have lagged behind the requirements of actual production.
The prior art (CN101554758B) discloses a method for manufacturing a hot-molding mold by utilizing nano-material modified PDMS, which comprises the steps of using nano-material modified polydimethylsiloxane, mixing nano-particles with a curing agent of the polydimethylsiloxane and a prepolymer, adding the mixture to a positive mold after uniformly mixing, forming a modified PDMS negative mold with an opposite structure after curing, and removing the modified PDMS negative mold from a master mold to obtain the hot-molding mold. The method not only keeps the characteristics of easy demoulding and complete pattern copying of PDMS, but also improves the Young modulus of PDMS and reduces the coefficient of thermal expansion, and is a method for manufacturing the micro-mechanical hot-pressing process mould with high speed, high efficiency and low cost. However, the following technical problems exist: the mechanical property and the wear resistance of the finished product of the die are further improved without modification of nano materials, and the service life of the finished product of the die needs to be prolonged.
A solution is now proposed to address the technical drawbacks in this respect.
Disclosure of Invention
The invention aims to provide a hot-molding die preparation method based on nano material modification, which is used for solving the technical problems that the mechanical property and the wear resistance of a die finished product are not further improved through nano material modification in the prior art, and the service life of the die finished product needs to be prolonged.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the hot-molding die based on the modification of the nano material comprises the following steps:
s1, pretreatment: weighing 76-92 parts of nanoscale zirconia, 8-15 parts of silicon nitride, 6-12 parts of silicon carbide, 10-18 parts of alumina, 3-8 parts of scandium oxide, 1.5-3.2 parts of lutetium oxide, 3.5-6.7 parts of chromium powder, 2.2-3.7 parts of nickel powder, 0.2-0.8 part of cobalt powder and 0.4-1.6 parts of vanadium powder according to parts by weight; respectively placing zirconium oxide, silicon nitride, silicon carbide, aluminum oxide, scandium oxide and lutetium oxide in a calcining furnace, heating to 430-480 ℃, calcining for 1-2 hours to obtain a zirconium oxide calcining material, a silicon nitride calcining material, a silicon carbide calcining material, an aluminum oxide calcining material, a scandium oxide calcining material and a lutetium oxide calcining material, and temporarily storing in a nitrogen atmosphere;
S2, preparing a mixed suspension: adding a zirconia calcined material, an alumina calcined material, a scandium calcined material and a lutetium oxide calcined material into a compound dispersing agent with the weight being 3-5 times that of the raw materials, fully stirring and mixing, and performing ultrasonic dispersion for 20-30 min to obtain a suspension a; adding a silicon nitride calcined material, a silicon carbide calcined material, chromium powder, nickel powder, cobalt powder and vanadium powder into a compound dispersing agent with the weight being 3-5 times that of the silicon nitride calcined material, fully stirring and mixing, and performing ultrasonic dispersion for 10-20 min to obtain a suspension b; after the suspension a and the suspension b are mixed, performing ultrasonic dispersion for 30-40 min to obtain a mixed suspension;
s3, ball-milling and drying: adding the mixed suspension into a ball milling tank, adding absolute ethyl alcohol and zirconia grinding balls with the diameter of 5-10 mm, carrying out ball milling for 25-37 hours under the protection of nitrogen, and filtering to obtain a grinding material; drying the ground material in vacuum at 95-110 ℃ to obtain a dried material;
s4, hot-pressing sintering: adding the dried material into a positive plate mold, sintering after hot pressing, and taking the positive plate mold off the female mold to obtain a semi-finished product of the hot molding mold;
s5, coating of the wear-resistant enhancement coating: cleaning the semi-finished product of the hot-molding die by ethanol and acetone in sequence, and drying by blowing; coating a reinforced wear-resistant coating material on the inner surface of the semi-finished product of the hot-molding die, carrying out temperature programming drying and natural cooling to obtain a reinforced wear-resistant coating, and carrying out secondary hot pressing to obtain a finished product of the hot-molding die; the pressure of the secondary hot pressing is 25-30 MPa.
The invention relates to a hot-molding die preparation method based on nano material modification, which comprises the steps of pretreatment, mixed suspension preparation, ball-milling drying, hot-pressing sintering and reinforced wear-resistant coating. Specifically, silicon nitride belongs to a high-temperature insoluble compound, has no melting point, strong high-temperature creep resistance, stable chemical properties of silicon carbide, high thermal conductivity, small thermal expansion coefficient, good wear resistance, uniform granularity of alumina, smooth surface and high mechanical strength, and silicon nitride, silicon carbide and alumina modify zirconia to form an intra-crystal/inter-crystal mixed structure, so that a fracture mode along a crystal/crystal-crossing mixed type is realized, a plurality of toughening and reinforcing mechanisms act synergistically, the mechanical properties of a die material are improved, the mechanical strength and the wear resistance are increased, and meanwhile, the thermal expansion coefficient is reduced; scandium oxide and lutetium oxide play roles in modifying and refining grains, and chromium powder, nickel powder, cobalt powder and vanadium powder are dispersed in the grains in the sintering process, so that the mechanical property and the wear resistance of the finished product of the hot-molding die are further improved.
In the pretreatment process, oxygen adsorbed by zirconia, silicon nitride, silicon carbide, alumina, scandium oxide and lutetium oxide is removed by calcination, so that the refinement of matrix grains is prevented from being influenced in the pressure sintering process. The reinforced wear-resistant coating is coated on the inner surface of the semi-finished product of the hot molding die, so that the antifriction and wear-resistant performance of the inner cavity of the hot molding die is further improved, the service life of the hot molding die is prolonged, and the demoulding after die pressing is convenient.
Further, the compound dispersing agent is prepared from polyethylene glycol 4000, tween-80 and an ethylene-ethyl acrylate copolymer according to the weight ratio of 5: 3: 1 by mixing.
Further, the amount of the absolute ethyl alcohol is 2-4 times of the weight of the mixed suspension liquid; the weight ratio of the mixed suspension to the zirconia grinding balls is 1: 6-8.
Further, the hot pressing pressure is 32-36 MPa, the sintering temperature is 1450-1560 ℃, and the sintering heat preservation time is 45-70 min.
Further, the preparation method of the reinforced wear-resistant coating material comprises the following steps: mixing 65-78 parts of alumina, 6-10 parts of zirconia, 3-8 parts of silicon nitride and 1-3 parts of graphene oxide according to parts by weight to obtain a mixture, adding the mixture into a ball milling tank, taking agate balls as a grinding medium, wherein the weight ratio of the mixture to the grinding medium is 1: 6-10, adding ethanol which is 3-5 times of the weight of the mixture, and performing ball milling for 10-16 hours to obtain a ball grinding material, wherein the weight ratio of the ball grinding material to the silica gel adhesive is 8-12: 1, mixing, stirring and grinding.
The reinforced wear-resistant coating material takes alumina as a substrate, zirconia and silicon nitride are added as reinforcing agents, graphene oxide is used as a dispersing agent, the substrate, the reinforcing agents and the dispersing agents are bonded by a silica gel adhesive, and then the substrate, the reinforcing agents and the dispersing agents are stirred, ground and dispersed, and after coating and heating setting are carried out in an inner cavity of a semi-finished product of a hot die-pressing die, a compact reinforced, antifriction and wear-resistant coating can be formed, so that the service life of the hot die-pressing die is prolonged.
Further, the programmed temperature rise specifically comprises: heating to 60-70 ℃ at the speed of 3-5 ℃/min, and keeping the temperature for 30-50 min; heating to 95-110 ℃ at the speed of 5-8 ℃/min, and keeping the temperature for 50-60 min; heating to 210-230 ℃ at the speed of 10-15 ℃/min, and preserving heat for 1-2 hours.
Further, the specific processing procedures of coating the reinforced wear-resistant coating material and programmed heating and drying are as follows: accommodating a plurality of semi-finished hot molding dies in a die fixing seat of the continuous coating and drying device, driving a detachable coating mechanism to extend into an inner cavity of the semi-finished hot molding dies after a coating cylinder extends, and spraying a reinforced wear-resistant coating material into the inner wall of the semi-finished hot molding dies from a coating hole through a feeding pipe and a pouring hole under the pressurization effect of a booster pump and adhering the coating material;
The driving motor drives the rotating platform to rotate, the rotating platform drives the mold fixing seat to rotate and move to the position below the electric heating pipe, the telescopic cylinder drives the electric heating pipe to move downwards to stretch into the inner cavity of the semi-finished product of the hot molding mold, and the temperature rise control of the program temperature rise controller is matched to heat and dry the reinforced wear-resistant coating material.
The invention has the following beneficial effects:
1. the method takes zirconia as a matrix, silicon nitride, silicon carbide and alumina as reinforcing agents, scandium oxide and lutetium oxide as stabilizing agents, and chromium powder, nickel powder, cobalt powder and vanadium powder as sintering aids; silicon nitride, silicon carbide and aluminum oxide modify zirconia to form an intra-crystal/inter-crystal mixed structure, so that the mechanical property of the die material is improved along a crystal/transcrystal mixed fracture mode under the synergistic action of multiple toughening and reinforcing mechanisms, the mechanical strength and the wear resistance are improved, and the thermal expansion coefficient is reduced; scandium oxide and lutetium oxide play roles in modifying and refining grains, and chromium powder, nickel powder, cobalt powder and vanadium powder are dispersed in the grains in the sintering process, so that the mechanical property and the wear resistance of the hot-molding die finished product are further improved.
2. The reinforced wear-resistant coating is coated by coating the reinforced wear-resistant coating material on the inner surface of the semi-finished product of the hot-molding die, so that the antifriction and wear-resistant performance of the inner cavity of the hot-molding die is further improved, the service life of the hot-molding die is prolonged, and the demoulding after die pressing is convenient.
3. Continuous coating drying device carries out the holding to a plurality of hot embossing mould semi-manufactured goods and fixes, and cooperation coating mechanism carries out the coating of reinforcing abrasion-resistant coating material, and the heating drying mechanism carries out the programming drying, and the fixed clearance mechanism of mould adsorbs and removes remaining coating material, accomplishes continuous high-efficient coating, dry environment that keeps the install bin clean simultaneously.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of a hot-molding die preparation method based on nanomaterial modification in the embodiment of the invention;
FIG. 2 is a schematic structural diagram of a continuous coating application and drying device in an embodiment of the invention;
FIG. 3 is a schematic structural diagram of a continuous coating application drying device with an installation case shell removed according to an embodiment of the invention;
FIG. 4 is an enlarged view of a portion of the invention at A in FIG. 3;
FIG. 5 is an enlarged view of a portion of the invention at B in FIG. 3;
FIG. 6 is an exploded view of a removable coating mechanism in an embodiment of the present invention;
FIG. 7 is a top view of a mold securing and cleaning mechanism in accordance with an embodiment of the present invention;
FIG. 8 is a top view of another mold chase cleaning mechanism in accordance with an embodiment of the present invention.
Reference numerals: 1. a support; 2. installing a box; 3. a mounting frame; 4. a die fixing and cleaning mechanism; 5. a coating mechanism; 6. a heating and drying mechanism; 7. hot-molding the semi-finished product of the mold; 31. a booster pump; 32. a feed pipe; 41. a rotating table; 42. a drive motor; 43. a mold fixing seat; 44. a groove; 45. a dust removal pump; 46. a dust collection pipe; 47. a material collecting pipe; 48. a dust exhaust pipe; 49. a collection hopper; 51. a first reduction motor; 52. a first ball screw; 53. coating the cylinder; 54. a first lead screw base; 55. a first clamping seat; 56. a removable coating mechanism; 57. buffering the mounting post; 58. a buffer spring; 61. a second reduction motor; 62. an L-shaped bracket; 63. a second ball screw; 64. a second lead screw base; 65. a second clamping seat; 66. a telescopic cylinder; 67. an insulating mounting head; 68. an electric heating tube; 471. a collection pipe; 561. mounting a plate; 562. fixing a column; 563. a wave spring; 564. coating a board; 565. mounting holes; 566. a pouring hole; 567. the pores are coated.
Detailed Description
The technical solutions of the present invention will be described below clearly and completely in conjunction with the embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in fig. 2-3 and 7, the embodiment provides a continuous coating and drying device for continuous coating and temperature programmed drying of reinforced wear-resistant coating materials in a hot-molding die preparation method based on nano-material modification, which comprises a support 1, an installation box 2 and installation frames 3, wherein the installation box 2 is arranged on the support 1, the two installation frames 3 are arranged on two sides of the top of the installation box 2, a die fixing and cleaning mechanism 4 for fixing a plurality of hot-molding die semi-finished products 7, driving the hot-molding die semi-finished products to rotate and cleaning residual coating materials is arranged on the installation box 2, and a coating and coating mechanism 5 for adjusting and coating the hot-molding die semi-finished products 7 and a heating and drying mechanism 6 for temperature programmed drying of the hot-molding die semi-finished products 7 are arranged on the installation frames 3. This serialization coating drying device carries out the holding through fixed clearance mechanism 4 of mould to a plurality of hot molding mould semi-manufactured goods 7 and fixes, and cooperation coating mechanism 5 carries out the coating of reinforcing wear-resisting coating material, and heating drying mechanism 6 carries out the programming drying, and the fixed clearance mechanism 4 of mould adsorbs the residual coating material of detaching, accomplishes the environment that serialization high efficiency coating was coated, was dry and keeps install bin 2 clean.
Specifically, as shown in fig. 2-5 and 7-8, the mold fixing and cleaning mechanism 4 includes a rotating table 41, a driving motor 42 and a mold fixing seat 43, the rotating table 41 is disposed on the upper surface of the installation box 2, the driving motor 42 extends from the bottom of the installation box 2, the plurality of mold fixing seats 43 are distributed on the upper surface of the rotating table 41 in an annular array, and a plurality of ring grooves 44 are distributed on the upper surface of the mold fixing seat 43. The mold holder 43 is cylindrical as shown in fig. 7, and a circular receiving cavity for fixing the hot-molding mold semi-finished product 7 is formed therein. Another embodiment of the mold holder 43 has a rectangular shape as shown in fig. 8 and has a rectangular receiving cavity therein for holding the hot-molding mold half-finished product 7. Two dust removing pumps 45 are symmetrically arranged at the bottom of the rotating platform 41, the dust suction ends of the dust removing pumps 45 are communicated with a material collecting pipe 47 arranged in the rotating platform 41 through a dust suction pipe 46, and the dust discharge ends of the dust removing pumps 45 are communicated with a material collecting hopper 49 through a dust discharge pipe 48. The upper part of the material collecting pipe 47 is communicated with the die fixing seat 43 and the groove 44 through a plurality of collecting pipes 471.
In the mold fixing and cleaning mechanism 4, the driving motor 42 drives the rotating table 41 to rotate, the rotating table 41 drives the mold fixing seat 43 to rotate, and the shape and the size of the mold fixing seat 43 are changed along with the shape and the size of the hot press molding mold semi-finished product 7. When the dried coating material falls into the inner cavity of the semi-finished product 7 of the hot-molding die or the rotary table 41, under the negative pressure action of the dust removal pump 45, the coating material enters the bottom of the inner cavity of the semi-finished product 7 of the hot-molding die and the groove 44, and enters the collecting hopper 49 through the collecting pipe 471, the collecting pipe 47 and the dust exhaust pipe 48, so that the centralized treatment is facilitated, and the re-cleaning of the finished product of the hot-molding die is avoided.
In the process that the first speed reducing motor 51 drives the first ball screw 52 to rotate, the first screw seat 54 horizontally moves along the direction of the first ball screw 52, so that the position of the coating cylinder 53 is convenient to adjust, and the coating cylinder 53 extends to drive the detachable coating mechanism 56 to extend into the inner cavity of the hot-molding die semi-finished product 7, so as to coat the inner surface of the hot-molding die semi-finished product with the enhanced wear-resistant coating material. The buffer spring 58 is wound around the periphery of the buffer mounting post 57 to alleviate vibration generated during the expansion and contraction of the coating cylinder 53.
As shown in fig. 2, 4 and 6, the detachable coating mechanism 56 includes a mounting plate 561, an inner cavity of the mounting plate 561 is provided with an inner thread assembled with the bottom of the buffer mounting post 57, fixing posts 562 are provided on two sides of the mounting plate 561, and a wave spring 563 is wound around the periphery of the fixing posts 562. Two coating plates 564 are symmetrically arranged on two sides of the mounting plate 561, and mounting holes 565 for the fixing columns 562 and the wave springs 563 to pass through are formed in the upper portions of the coating plates 564. The upper surface of coating plate 564 is provided with a pour hole 566, and the outer surface of coating plate 564 is provided with a plurality of coating holes 567 communicating with pour hole 566. The cross-sectional shape and size of the coated plates 564 are adapted to the inner surface of the hot-molding die blank 7, and the area surrounded by the two coated plates 564 is circular or rectangular. The outer side of one mounting block 3 is provided with a booster pump 31, and the booster pump 31 injects the reinforcing abradable coating material into the injection hole 566 via the feed pipe 32.
After the inner cavity of the mounting plate 561 is screwed with the bottom of the buffer mounting post 57, the fixing posts 562 and the wave spring 563 on both sides thereof extend into the mounting hole 565 and can move relatively, so that the coating plate 564 can move along the fixing posts 562 adaptively in the inner cavity of the hot-molding die semi-finished product 7. The wear-resistant reinforcing coating material is injected into the inner wall of the hot-molding die semi-finished product 7 from the coating hole 567 through the feed pipe 32 and the pouring hole 566 under the pressurizing action of the pressurizing pump 31 and is adhered.
As shown in fig. 2 to 3 and 5, the heating and drying mechanism 6 includes a second speed reduction motor 61, an L-shaped bracket 62, and a second ball screw 63, the L-shaped bracket 62 is disposed below the first ball screw 52, one end of the second ball screw 63 penetrates the L-shaped bracket 62, the other end penetrates the mounting bracket 3, and the second speed reduction motor 61 is disposed outside the mounting bracket 3 and connected to the second ball screw 63. The periphery of the second ball screw 63 is connected with a second screw seat 64 through a thread, a telescopic cylinder 66 is fixed at the bottom of the second screw seat 64 through a second clamping seat 65, an electric heating pipe 68 is installed at the bottom of the telescopic cylinder 66 through an insulating mounting head 67, and the electric heating pipe 68 is subjected to temperature rise control through a program temperature rise controller.
In the process that the second speed reducing motor 61 drives the second ball screw 63 to rotate, the second screw seat 64 moves along the direction of the second ball screw 63, the positions of the telescopic cylinder 66 and the electric heating pipe 68 move to be matched with the mold fixing seat 43, the telescopic cylinder 66 drives the electric heating pipe 68 to move downwards to stretch into the inner cavity of the hot molding mold semi-finished product 7, the temperature rise control of the temperature rise controller is matched, the reinforced wear-resistant coating material is heated and dried, and the drying rate and the molding quality of the reinforced wear-resistant coating are improved.
The working method of the continuous coating and drying device comprises the following steps:
step one, accommodating a plurality of hot molding die semi-finished products 7 into a die fixing seat 43, driving a detachable coating mechanism 56 to extend into an inner cavity of the hot molding die semi-finished product 7 after a coating cylinder 53 extends, and spraying a reinforced wear-resistant coating material into the inner wall of the hot molding die semi-finished product 7 from a coating hole 567 through a feeding pipe 32 and a pouring hole 566 under the pressurization effect of a booster pump 31 and adhering the coating material;
step two, the driving motor 42 drives the rotating table 41 to rotate, the rotating table 41 drives the die fixing seat 43 to rotate and move to the position below the electric heating pipe 68, the telescopic cylinder 66 drives the electric heating pipe 68 to move downwards and extend into the inner cavity of the hot-molding die semi-finished product 7, and the enhanced wear-resistant coating material is heated and dried by matching with the temperature rise control of the programmed temperature rise controller;
and step three, repeating the step one and the step two, and carrying out continuous coating, temperature programmed drying on the reinforced wear-resistant coating material.
Example 2
As shown in fig. 1, this embodiment provides a method for preparing a hot-molding mold based on nanomaterial modification, including the following steps:
s1, pretreatment: weighing 83 parts of nanoscale zirconia, 11 parts of silicon nitride, 8 parts of silicon carbide, 13 parts of alumina, 6 parts of scandium oxide, 2.3 parts of lutetium oxide, 4.7 parts of chromium powder, 2.8 parts of nickel powder, 0.5 part of cobalt powder and 0.9 part of vanadium powder according to parts by weight; respectively placing zirconium oxide, silicon nitride, silicon carbide, aluminum oxide, scandium oxide and lutetium oxide in a calcining furnace, heating to 455 ℃, calcining for 1.5 hours to obtain a zirconium oxide calcining material, a silicon nitride calcining material, a silicon carbide calcining material, an aluminum oxide calcining material, a scandium oxide calcining material and a lutetium oxide calcining material, and temporarily storing in a nitrogen atmosphere; wherein the grain sizes of the zirconium oxide, the silicon nitride, the silicon carbide, the aluminum oxide, the scandium oxide and the lutetium oxide are 10-100 nm, and the grain sizes of the chromium powder, the nickel powder, the cobalt powder and the vanadium powder are 1-10 nm.
S2, preparing a mixed suspension: adding a zirconia calcined material, an alumina calcined material, a scandium calcined material and a lutetium oxide calcined material into a compound dispersing agent with the weight being 3.6 times that of the raw materials, fully stirring and mixing, and performing ultrasonic dispersion for 25min to obtain a suspension a; adding the silicon nitride calcined material, the silicon carbide calcined material, the chromium powder, the nickel powder, the cobalt powder and the vanadium powder into a compound dispersing agent with the weight being 4.2 times that of the silicon nitride calcined material, fully stirring and mixing, and performing ultrasonic dispersion for 15min to obtain a suspension b; after the suspension a and the suspension b are mixed, performing ultrasonic dispersion for 36min to obtain a mixed suspension; wherein the compound dispersant is prepared from polyethylene glycol 4000, tween-80 and ethylene-ethyl acrylate copolymer according to the weight ratio of 5: 3: 1 by mixing.
S3, ball-milling and drying: adding the mixed suspension into a ball milling tank, adding absolute ethyl alcohol and zirconia grinding balls with the diameter of 6mm, carrying out ball milling for 32 hours under the protection of nitrogen, and filtering to obtain a grinding material; vacuum drying the ground material at 106 deg.C to obtain dried material; wherein the dosage of the absolute ethyl alcohol is 3.2 times of the weight of the mixed suspension; the weight ratio of the mixed suspension to the zirconia grinding balls is 1: 7.
s4, hot-pressing and sintering: adding the dried material into a positive mold, sintering after hot pressing, and taking the positive mold off the female mold to obtain a semi-finished product of the hot-molding mold; wherein the hot pressing pressure is 34MPa, the sintering temperature is 1520 ℃, and the sintering heat preservation time is 57 min.
S5, coating of the wear-resistant enhancement coating: cleaning the semi-finished product of the hot-molding die by ethanol and acetone in sequence, and drying by blowing; and coating a reinforced wear-resistant coating material on the inner surface of the semi-finished product of the hot-molding die, performing temperature programming drying and natural cooling to obtain a reinforced wear-resistant coating, and performing secondary hot-pressing to obtain a finished product of the hot-molding die. The pressure of the secondary hot pressing is 28 MPa. The specific process of applying the reinforcing abradable coating material to the inner surface of the hot-stamped mold half-product and performing temperature-programmed drying is described in example 1.
The preparation method of the reinforced wear-resistant coating material comprises the following steps: mixing 75 parts of aluminum oxide, 8 parts of zirconium oxide, 6 parts of silicon nitride and 1.5 parts of graphene oxide according to parts by weight to obtain a mixture, adding the mixture into a ball milling tank, taking agate balls as a grinding medium, wherein the weight ratio of the mixture to the grinding medium is 1: 9, adding ethanol with the weight 4.2 times of that of the mixture, and performing ball milling for 15 hours to obtain a ball grinding material, wherein the weight ratio of the ball grinding material to the silica gel adhesive is 11: 1, mixing, stirring and grinding.
The temperature programming specifically comprises the following steps: heating to 67 deg.C at a rate of 4 deg.C/min, and maintaining for 40 min; heating to 106 deg.C at a rate of 7 deg.C/min, and maintaining for 56 min; the temperature is raised to 218 ℃ at the speed of 12 ℃/min, and the temperature is kept for 1.6 hours.
Through detection, the hardness of the hot die pressing die finished product in the embodiment is 17.8GPa, the bending strength is 856MPa, the compression strength is 1062MPa, and the fracture toughness is 9.3 MPa.m1/2Coefficient of thermal expansion of 6.8X 10-6m/m·K。
Example 3
As shown in fig. 1, this embodiment provides a method for preparing a hot-molding mold based on nanomaterial modification, including the following steps:
s1, pretreatment: weighing 87 parts of nanoscale zirconia, 13 parts of silicon nitride, 10 parts of silicon carbide, 15 parts of alumina, 5 parts of scandium oxide, 2.1 parts of lutetium oxide, 5.2 parts of chromium powder, 3.2 parts of nickel powder, 0.4 part of cobalt powder and 1.2 parts of vanadium powder according to parts by weight; respectively placing zirconium oxide, silicon nitride, silicon carbide, aluminum oxide, scandium oxide and lutetium oxide in a calcining furnace, heating to 465 ℃, calcining for 1.5 hours to obtain a zirconium oxide calcining material, a silicon nitride calcining material, a silicon carbide calcining material, an aluminum oxide calcining material, a scandium oxide calcining material and a lutetium oxide calcining material, and temporarily storing in a nitrogen atmosphere.
S2, preparing a mixed suspension: adding a zirconia calcined material, an alumina calcined material, a scandium calcined material and a lutetium oxide calcined material into a compound dispersing agent with the weight being 3.8 times that of the raw materials, fully stirring and mixing, and performing ultrasonic dispersion for 27min to obtain a suspension a; adding the silicon nitride calcined material, the silicon carbide calcined material, the chromium powder, the nickel powder, the cobalt powder and the vanadium powder into a compound dispersing agent with the weight of 4.5 times, fully stirring and mixing, and performing ultrasonic dispersion for 14min to obtain a suspension b; after the suspension a and the suspension b are mixed, carrying out ultrasonic dispersion for 35min to obtain a mixed suspension; wherein the compound dispersant is prepared from polyethylene glycol 4000, tween-80 and ethylene-ethyl acrylate copolymer according to the weight ratio of 5: 3: 1 are mixed.
S3, ball-milling and drying: adding the mixed suspension into a ball milling tank, adding absolute ethyl alcohol and zirconia grinding balls with the diameter of 9mm, carrying out ball milling for 35 hours under the protection of nitrogen, and filtering to obtain a grinding material; vacuum drying the ground material at 103 deg.C to obtain dried material; wherein the dosage of the absolute ethyl alcohol is 3.2 times of the weight of the mixed suspension; the weight ratio of the mixed suspension to the zirconia grinding balls is 1: 6.7.
s4, hot-pressing and sintering: adding the dried material into a positive mold, sintering after hot pressing, and taking the positive mold off the female mold to obtain a semi-finished product of the hot-molding mold; wherein the hot-pressing pressure is 34MPa, the sintering temperature is 1490 ℃, and the sintering heat preservation time is 62 min.
S5, coating of the wear-resistant enhancement coating: cleaning the semi-finished product of the hot-molding die by ethanol and acetone in sequence, and drying by blowing; coating a reinforced wear-resistant coating material on the inner surface of the semi-finished product of the hot-molding die, carrying out temperature programming drying and natural cooling to obtain a reinforced wear-resistant coating, and carrying out secondary hot pressing to obtain a finished product of the hot-molding die. The pressure of the secondary hot pressing is 25-30 MPa.
The preparation method of the reinforced wear-resistant coating material comprises the following steps: mixing 74 parts of aluminum oxide, 8 parts of zirconium oxide, 6 parts of silicon nitride and 2.2 parts of graphene oxide according to parts by weight to obtain a mixture, adding the mixture into a ball milling tank, taking agate balls as a grinding medium, wherein the weight ratio of the mixture to the grinding medium is 1: and 8, adding ethanol with the weight 4.7 times that of the mixture, and performing ball milling for 15 hours to obtain a ball grinding material, wherein the weight ratio of the ball grinding material to the silica gel adhesive is 10: 1, mixing, stirring and grinding.
The temperature programming specifically comprises the following steps: heating to 62 deg.C at a rate of 4.5 deg.C/min, and maintaining for 46 min; heating to 106 deg.C at a rate of 7 deg.C/min, and maintaining for 58 min; the temperature is raised to 225 ℃ at the speed of 13 ℃/min, and the temperature is kept for 1.6 hours.
The test shows that the hardness of the hot-pressing die finished product in the embodiment is 17.6GPa, the bending strength is 850MPa, the compression strength is 1048MPa, and the fracture toughness is 9.1 MPa.m1/2Coefficient of thermal expansion of 6.7X 10-6m/m·K。
Example 4
As shown in fig. 1, the present embodiment provides a method for preparing a hot-molding mold based on nanomaterial modification, comprising the following steps:
s1, pretreatment: weighing 90 parts of nanoscale zirconia, 14 parts of silicon nitride, 12 parts of silicon carbide, 17 parts of alumina, 7 parts of scandium oxide, 3.1 parts of lutetium oxide, 6.6 parts of chromium powder, 3.5 parts of nickel powder, 0.7 part of cobalt powder and 0.8 part of vanadium powder according to parts by weight; respectively placing zirconium oxide, silicon nitride, silicon carbide, aluminum oxide, scandium oxide and lutetium oxide in a calcining furnace, heating to 473 ℃, calcining for 2 hours to obtain a zirconium oxide calcining material, a silicon nitride calcining material, a silicon carbide calcining material, an aluminum oxide calcining material, a scandium oxide calcining material and a lutetium oxide calcining material, and temporarily storing in a nitrogen atmosphere.
S2, mixed suspension preparation: adding a zirconia calcined material, an alumina calcined material, a scandium calcined material and a lutetium oxide calcined material into a compound dispersing agent with the weight 5 times that of the raw materials, fully stirring and mixing, and performing ultrasonic dispersion for 30min to obtain a suspension a; adding silicon nitride calcined material, silicon carbide calcined material, chromium powder, nickel powder, cobalt powder and vanadium powder into a compound dispersing agent with the weight 5 times that of the mixture, fully stirring and mixing, and performing ultrasonic dispersion for 18min to obtain a suspension b; after the suspension a and the suspension b are mixed, carrying out ultrasonic dispersion for 40min to obtain a mixed suspension; wherein the compound dispersant is prepared from polyethylene glycol 4000, tween-80 and ethylene-ethyl acrylate copolymer according to the weight ratio of 5: 3: 1 are mixed.
S3, ball-milling and drying: adding the mixed suspension into a ball milling tank, adding absolute ethyl alcohol and zirconia grinding balls with the diameter of 10mm, carrying out ball milling for 36 hours under the protection of nitrogen, and filtering to obtain a grinding material; vacuum drying the ground material at 108 deg.C to obtain dried material; wherein the dosage of the absolute ethyl alcohol is 4 times of the weight of the mixed suspension; the weight ratio of the mixed suspension to the zirconia grinding balls is 1: 7.6.
s4, hot-pressing sintering: adding the dried material into a positive mold, sintering after hot pressing, and taking the positive mold off the female mold to obtain a semi-finished product of the hot-molding mold; wherein the hot pressing pressure is 35MPa, the sintering temperature is 1530 ℃, and the sintering heat preservation time is 65 min.
S5, coating of the wear-resistant enhancement coating: cleaning the semi-finished product of the hot-molding die by ethanol and acetone in sequence, and drying by blowing; coating a reinforced wear-resistant coating material on the inner surface of the semi-finished product of the hot-molding die, carrying out temperature programming drying and natural cooling to obtain a reinforced wear-resistant coating, and carrying out secondary hot pressing to obtain a finished product of the hot-molding die. The pressure of the secondary hot pressing is 30 MPa.
The preparation method of the reinforced wear-resistant coating material comprises the following steps: mixing 76 parts of aluminum oxide, 10 parts of zirconium oxide, 8 parts of silicon nitride and 2.8 parts of graphene oxide according to parts by weight to obtain a mixture, adding the mixture into a ball milling tank, taking agate balls as a grinding medium, wherein the weight ratio of the mixture to the grinding medium is 1: 9, adding ethanol with the weight 5 times of that of the mixture, and ball-milling for 15 hours to obtain a ball grinding material, wherein the weight ratio of the ball grinding material to the silica gel adhesive is 9: 1, mixing, stirring and grinding.
The temperature programming specifically comprises the following steps: heating to 70 deg.C at a rate of 5 deg.C/min, and maintaining for 46 min; heating to 108 deg.C at a rate of 8 deg.C/min, and maintaining for 60 min; the temperature is raised to 226 ℃ at the speed of 14 ℃/min, and the temperature is kept for 2 hours.
The hardness of the hot-pressing die finished product of the embodiment is 17.5GPa, the bending strength is 843MPa, the compression strength is 1029MPa, and the fracture toughness is 8.9 MPa.m1/2Coefficient of thermal expansion of 6.8X 10-6m/m·K。
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the invention as defined in the following claims.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. The preparation method of the hot-molding die based on the modification of the nano material is characterized by comprising the following steps of:
s1, pretreatment: weighing 76-92 parts of nanoscale zirconium oxide, 8-15 parts of silicon nitride, 6-12 parts of silicon carbide, 10-18 parts of aluminum oxide, 3-8 parts of scandium oxide, 1.5-3.2 parts of lutetium oxide, 3.5-6.7 parts of chromium powder, 2.2-3.7 parts of nickel powder, 0.2-0.8 part of cobalt powder and 0.4-1.6 parts of vanadium powder according to parts by weight; respectively placing zirconium oxide, silicon nitride, silicon carbide, aluminum oxide, scandium oxide and lutetium oxide in a calcining furnace, heating to 430-480 ℃, calcining for 1-2 hours to obtain a zirconium oxide calcining material, a silicon nitride calcining material, a silicon carbide calcining material, an aluminum oxide calcining material, a scandium oxide calcining material and a lutetium oxide calcining material, and temporarily storing in a nitrogen atmosphere;
S2, preparing a mixed suspension: adding a zirconia calcined material, an alumina calcined material, a scandium calcined material and a lutetium oxide calcined material into a compound dispersing agent with the weight being 3-5 times that of the raw materials, fully stirring and mixing, and performing ultrasonic dispersion for 20-30 min to obtain a suspension a; adding a silicon nitride calcined material, a silicon carbide calcined material, chromium powder, nickel powder, cobalt powder and vanadium powder into a compound dispersing agent with the weight being 3-5 times that of the silicon nitride calcined material, fully stirring and mixing, and performing ultrasonic dispersion for 10-20 min to obtain a suspension b; after the suspension a and the suspension b are mixed, performing ultrasonic dispersion for 30-40 min to obtain a mixed suspension;
s3, ball-milling and drying: adding the mixed suspension into a ball milling tank, adding absolute ethyl alcohol and zirconia grinding balls with the diameter of 5-10 mm, carrying out ball milling for 25-37 hours under the protection of nitrogen, and filtering to obtain a grinding material; drying the ground material in vacuum at 95-110 ℃ to obtain a dried material;
s4, hot-pressing sintering: adding the dried material into a positive mold, sintering after hot pressing, and taking the positive mold off the female mold to obtain a semi-finished product of the hot-molding mold;
s5, coating of the wear-resistant enhancement coating: cleaning the semi-finished product of the hot-molding die by ethanol and acetone in sequence, and drying by blowing; coating a reinforced wear-resistant coating material on the inner surface of the semi-finished product of the hot-molding die, carrying out temperature programming drying and natural cooling to obtain a reinforced wear-resistant coating, and carrying out secondary hot pressing to obtain a finished product of the hot-molding die; the pressure of the secondary hot pressing is 25-30 MPa.
2. The method for preparing the hot molding die based on nanomaterial modification of claim 1, wherein the compound dispersant is prepared from polyethylene glycol 4000, tween-80, and ethylene-ethyl acrylate copolymer in a weight ratio of 5: 3: 1 by mixing.
3. The method for preparing the hot-pressing mold based on nanomaterial modification according to claim 1, wherein the amount of the absolute ethyl alcohol is 2-4 times of the weight of the mixed suspension; the weight ratio of the mixed suspension to the zirconia grinding balls is 1: 6-8.
4. The method for preparing the hot-pressing mold based on the nanomaterial modification, according to claim 1, is characterized in that the hot-pressing pressure is 32-36 MPa, the sintering temperature is 1450-1560 ℃, and the sintering heat preservation time is 45-70 min.
5. The method for preparing a hot-molding die based on nanomaterial modification according to claim 1, wherein the reinforced wear-resistant coating material is prepared by the following steps: mixing 65-78 parts of alumina, 6-10 parts of zirconia, 3-8 parts of silicon nitride and 1-3 parts of graphene oxide according to parts by weight to obtain a mixture, adding the mixture into a ball milling tank, taking agate balls as a grinding medium, wherein the weight ratio of the mixture to the grinding medium is 1: 6-10, adding ethanol which is 3-5 times of the weight of the mixture, and performing ball milling for 10-16 hours to obtain a ball grinding material, wherein the weight ratio of the ball grinding material to the silica gel adhesive is 8-12: 1, mixing, stirring and grinding.
6. The nanomaterial modification-based hot stamping die preparation method according to claim 1, wherein the temperature programming specifically comprises: heating to 60-70 ℃ at the speed of 3-5 ℃/min, and keeping the temperature for 30-50 min; heating to 95-110 ℃ at the speed of 5-8 ℃/min, and keeping the temperature for 50-60 min; heating to 210-230 ℃ at the speed of 10-15 ℃/min, and preserving heat for 1-2 hours.
7. The method for preparing the hot-molding die based on the nanomaterial modification as claimed in claim 1, wherein the specific processes of coating the reinforced wear-resistant coating material and heating and drying by program are as follows: accommodating a plurality of hot-molding die semi-finished products into a die fixing seat (43) of a continuous coating drying device, driving a detachable coating mechanism (56) to extend into an inner cavity of the hot-molding die semi-finished product (7) after a coating cylinder (53) extends, and spraying a reinforced wear-resistant coating material into the inner wall of the hot-molding die semi-finished product from a coating hole (567) through a feeding pipe (32) and a pouring hole (566) under the pressurization effect of a booster pump (31) and adhering the coating material;
the driving motor (42) drives the rotating table (41) to rotate, the rotating table (41) drives the die fixing seat (43) to rotate and move to the lower part of the electric heating pipe (68), the telescopic cylinder (66) drives the electric heating pipe (68) to move downwards and extend into the inner cavity of the hot die pressing die semi-finished product (7), and the enhanced wear-resistant coating material is heated and dried by matching with the temperature rise control of the programmed temperature rise controller.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210313348.0A CN114749669A (en) | 2022-03-28 | 2022-03-28 | Hot die pressing mold preparation method based on nano material modification |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210313348.0A CN114749669A (en) | 2022-03-28 | 2022-03-28 | Hot die pressing mold preparation method based on nano material modification |
Publications (1)
Publication Number | Publication Date |
---|---|
CN114749669A true CN114749669A (en) | 2022-07-15 |
Family
ID=82327510
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210313348.0A Pending CN114749669A (en) | 2022-03-28 | 2022-03-28 | Hot die pressing mold preparation method based on nano material modification |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114749669A (en) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101554758A (en) * | 2009-04-09 | 2009-10-14 | 上海交通大学 | Method for producing hot molding die with nano material modified PDMS |
CN104163625A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Scandium oxide and neodymium oxide composite stabilized titanium oxide-based multi-element nano-composite ceramic die |
CN104163626A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Zirconium oxide and zirconium carbide composite reinforced titanium oxide-based multi-element nano-composite ceramic die |
CN107602117A (en) * | 2017-09-07 | 2018-01-19 | 苏州浩焱精密模具有限公司 | A kind of zirconium oxide base nano composite ceramic mold materials and preparation method thereof |
CN208848680U (en) * | 2018-11-23 | 2019-05-10 | 湖南省新化县鑫星电子陶瓷有限责任公司 | A kind of ceramic insulator coats molybdenum manganese device automatically |
CN214351759U (en) * | 2020-12-21 | 2021-10-08 | 郑州立佳热喷涂机械有限公司 | Production line for wear-resistant coating of glass mold |
-
2022
- 2022-03-28 CN CN202210313348.0A patent/CN114749669A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101554758A (en) * | 2009-04-09 | 2009-10-14 | 上海交通大学 | Method for producing hot molding die with nano material modified PDMS |
CN104163625A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Scandium oxide and neodymium oxide composite stabilized titanium oxide-based multi-element nano-composite ceramic die |
CN104163626A (en) * | 2014-08-04 | 2014-11-26 | 余姚市巧迪电器厂 | Zirconium oxide and zirconium carbide composite reinforced titanium oxide-based multi-element nano-composite ceramic die |
CN107602117A (en) * | 2017-09-07 | 2018-01-19 | 苏州浩焱精密模具有限公司 | A kind of zirconium oxide base nano composite ceramic mold materials and preparation method thereof |
CN208848680U (en) * | 2018-11-23 | 2019-05-10 | 湖南省新化县鑫星电子陶瓷有限责任公司 | A kind of ceramic insulator coats molybdenum manganese device automatically |
CN214351759U (en) * | 2020-12-21 | 2021-10-08 | 郑州立佳热喷涂机械有限公司 | Production line for wear-resistant coating of glass mold |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109439940B (en) | Method for preparing particle reinforced aluminum matrix composite material by hot-pressing sintering under atmospheric atmosphere | |
CN113185302B (en) | Large-size silicon nitride ceramic ball for wind power generation and preparation method and application thereof | |
CN106512751A (en) | Preparation method of disc-type multi-channel plate ceramic membrane | |
CN111056858A (en) | Preparation method of flat ceramic membrane support and ceramic pug thereof | |
CN110668813A (en) | Preparation method of nano zirconia granulated powder | |
CN113277859A (en) | Nano-coated alumina particles and high-purity thermal shock resistant alumina ceramic material prepared from same | |
CN114749669A (en) | Hot die pressing mold preparation method based on nano material modification | |
CN113896528A (en) | Method for preparing high-performance zirconia ceramic material through DLP-3D printing | |
CN112174668A (en) | Preparation method and application of transparent ceramic with multilayer composite structure | |
CN115724681B (en) | Preparation method and application of porous silicon carbide ceramic with regular pore structure | |
CN118143260A (en) | Aluminum-based silicon carbide ingot casting preparation process based on isostatic pressing technology | |
CN112194491A (en) | Pressureless sintering boron carbide ceramic powder and preparation method and application thereof | |
CN113735601A (en) | Nano-zirconia composite material for injection molding and preparation method and application thereof | |
CN102581938B (en) | Mould for using two-dimensional fiber fabric to produce blanks of carbon-carbon composite barrel products | |
CN109053193A (en) | A kind of silicon nitride ceramics nozzle and preparation method thereof | |
CN107602117A (en) | A kind of zirconium oxide base nano composite ceramic mold materials and preparation method thereof | |
CN117105606A (en) | Heat storage foam concrete and preparation method thereof | |
CN113121209B (en) | Preparation method of 996 aluminum oxide ceramic substrate | |
CN109182931A (en) | A kind of preparation method of 6061 aluminum matrix composite | |
CN113979406A (en) | Method for sintering hydrogen storage material by using nano particles | |
CN109317662B (en) | Preparation process of artificial diamond sintered body | |
CN111646775A (en) | Method for preparing sheet molecular sieve membrane support by using natural attapulgite | |
CN221851232U (en) | Hydraulic mould thickness adjustable mould pressing cushion block assembly | |
CN219340474U (en) | Raw material storage tank for preparing nanoscale zirconia powder | |
CN109734454A (en) | A kind of method that injection forming prepares compact silicon nitride ceramic material |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220715 |
|
RJ01 | Rejection of invention patent application after publication |