CN106316385A - Preparation method of super alloy 3D printing composite - Google Patents

Preparation method of super alloy 3D printing composite Download PDF

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Publication number
CN106316385A
CN106316385A CN201610701879.1A CN201610701879A CN106316385A CN 106316385 A CN106316385 A CN 106316385A CN 201610701879 A CN201610701879 A CN 201610701879A CN 106316385 A CN106316385 A CN 106316385A
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powder
parts
printing
hydrogen
sintering
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CN201610701879.1A
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Chinese (zh)
Inventor
毛国栋
毛梅娟
高强
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Suzhou Ju Guan Matrix Material Co Ltd
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Suzhou Ju Guan Matrix Material Co Ltd
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Priority to CN201610701879.1A priority Critical patent/CN106316385A/en
Publication of CN106316385A publication Critical patent/CN106316385A/en
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    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B33—ADDITIVE MANUFACTURING TECHNOLOGY
    • B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y70/00—Materials specially adapted for additive manufacturing
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3817—Carbides
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602—Making the green bodies or pre-forms by moulding
    • C04B2235/6026—Computer aided shaping, e.g. rapid prototyping

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a super alloy 3D printing composite which comprises 40-48 parts of titanium tetrachloride, 12-14 parts of acetonitrile, 24-29 parts of tertiary amine, 4-9 parts of unsymmetrical dimethylhydrazine, 1-5 parts of hydrogen cyanide, 1-3 parts of hydrogen, 30-36 parts of nitrogen, 30-40 parts of TiO2 powder, 10-15 parts of TiC powder and 20-24 parts of dextrin powder and is prepared by the following steps of: mixing the TiO2 powder, the TiC powder, the dextrin powder and a prepared Ti(C.N) material with distilled water by a medium-temperature chemical vapor deposition method; performing ball milling for 10-24h and mixing uniformly; removing moisture by a vacuum freeze dryer; sieving to obtain mixed powder; and performing three-dimensional printing moulding (3DP) of the mixed powder to obtain a preform. The super alloy 3D printing composite has the advantages of low density, high hardness, corrosion resistance, wear resistance and good high-temperature oxidation resistance; and the technology solves the problem of relatively low strength of the 3DP component caused by relatively high porosity of a 3DP ligand.

Description

A kind of superalloy 3D printing composite material preparation method
Technical field
The present invention relates to 3D printed material technical field, be specifically related to a kind of superalloy 3D printing composite material preparation side Method.
Background technology
3D prints the one that (3DP) is rapid shaping technique, and it is a kind of based on mathematical model file, uses powder Shape metal or plastics etc. can jointing material, by the way of successively printing, carry out the technology of constructed object.
3D prints and is typically with what digital technology file printing machine realized.Often lead in Making mold, industrial design etc. Territory is used for modeling, after be gradually available for the direct manufacture of some products, had use this technology to print zero Parts.This technology is in jewelry, footwear, industrial design, building, engineering and construction (AEC), automobile, Aero-Space, dentistry and medical treatment Industry, education, GIS-Geographic Information System, civil engineering, gun and other field have been applied.
3DP has been demonstrated to manufacture the various complicated form part being made up of metal, pottery and polymeric material.With poly- Compound sill is different, uses 3 D-printing technique to manufacture metal and ceramic component is still within development, need to find material Material and new method overcome the deficiency of existing technique, and the process characteristic of 3DP is powder granule stacking and is bonded together by binding agent, The hole of 3DP base substrate is more, and this causes the intensity of 3DP parts relatively low.In order to improve the intensity of 3DP material, locate after needing to use Science and engineering skill, wherein conventional aftertreatment technology is sintering process, and its sintering temperature needs a marginal value, has both ensured to improve material close Degree does not the most change materials microstructure and member profile structure, but, the line of material shrinkage factor after sintering is the biggest.
Summary of the invention
For problem above, the invention provides a kind of superalloy 3D printing composite material, the Ti of preparation3AlC2Toughness reinforcing Ti2O3-Al2O3Composite has the high-temperature oxidation resistance that density is low, hardness is high, anticorrosive, wear-resistant and good, should Technique solves the problem that the more intensity causing 3DP parts of 3DP part porosity is relatively low, not only can guarantee that raising density of material but also Not changing materials microstructure and member profile structure, the line of material shrinkage factor after sintering has declined, and can effectively solve the back of the body Problem in scape technology.
To achieve these goals, the technical solution used in the present invention is as follows: a kind of superalloy 3D printing composite material Preparation method, uses following formula and technique:
Formula:
Titanium tetrachloride 40-48 part, acetonitrile 12-14 part, tertiary amine 24-29 part, uns-dimethylhydrazine 4-9 part, Blausure (German) 1-5 part, Hydrogen 1-3 part, nitrogen 30-36 part, TiO2Powder 30-40 part, TiC powder 10-15 part, dextrine powder 20-24 part.
Processing technique:
(1) use middle temperature chemical gaseous phase depositing process, with organic compound acetonitrile, tertiary amine, uns-dimethylhydrazine, Blausure (German) be Dominant response gas produces decomposition, combination reaction with titanium tetrachloride, hydrogen and nitrogen at a temperature of 700-900 DEG C, generates Ti (C.N) material；
(2) by TiO2Ti (C.N) material that powder, TiC powder, dextrine powder and above-mentioned steps (1) obtain mixes with distilled water, Ball milling 10-24h mix homogeneously, uses vacuum freeze drier to remove moisture removal, sieves and obtain mixed powder；
(3) gained mixed powder makes precast body through 3 D-printing molding, in an inert atmosphere 1400-1500 DEG C of sintering 30-50min；
(4) quantitative aluminium ingot is placed on the precast body surface of sintering, and puts in corundum crucible, at 1300-1500 DEG C Insulation 70-100min, obtains Ti3AlC2Toughness reinforcing Ti2O3-Al2O3Composite.
Beneficial effects of the present invention:
Ti prepared by the present invention3AlC2Toughness reinforcing Ti2O3-Al2O3Composite has that density is low, hardness is high, anticorrosive, wear-resistant Damaging and good high-temperature oxidation resistance, it is relatively low that this technique solves the more intensity causing 3DP parts of 3DP part porosity Problem, not only can guarantee that raising density of material but also do not changed materials microstructure and member profile structure, the line of material after sintering Shrinkage factor has declined.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, to the present invention It is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to Limit the present invention.
Embodiment 1:
The invention provides a kind of superalloy 3D printing composite material, its formula is:
Titanium tetrachloride 40 parts, acetonitrile 12 parts, tertiary amine 24 parts, uns-dimethylhydrazine 4 parts, Blausure (German) 1 part, hydrogen 1 part, nitrogen 30 Part, TiO230 parts of powder, 10 parts of TiC powder, dextrine powder 20 parts.
Its preparation technology comprises the steps:
(1) use middle temperature chemical gaseous phase depositing process, with organic compound acetonitrile, tertiary amine, uns-dimethylhydrazine, Blausure (German) be Dominant response gas produces decomposition, combination reaction with titanium tetrachloride, hydrogen and nitrogen at a temperature of 700 DEG C, generates Ti (C.N) material Material；
(2) by TiO2Ti (C.N) material that powder, TiC powder, dextrine powder and above-mentioned steps (1) obtain mixes with distilled water, Ball milling 10h mix homogeneously, uses vacuum freeze drier to remove moisture removal, sieves and obtain mixed powder；
(3) gained mixed powder makes precast body through 3 D-printing molding, in an inert atmosphere 1400 DEG C of sintering 30min；
(4) quantitative aluminium ingot is placed on the precast body surface of sintering, and puts in corundum crucible, 1300 DEG C of insulations 70min, obtains Ti3AlC2Toughness reinforcing Ti2O3-Al2O3Composite.
Embodiment 2:
The invention provides a kind of superalloy 3D printing composite material, its formula is:
Titanium tetrachloride 46 parts, acetonitrile 13 parts, tertiary amine 26 parts, uns-dimethylhydrazine 6 parts, Blausure (German) 4 parts, hydrogen 2 parts, nitrogen 35 Part, TiO235 parts of powder, 13 parts of TiC powder, dextrine powder 22 parts.
Its preparation technology comprises the steps:
(1) use middle temperature chemical gaseous phase depositing process, with organic compound acetonitrile, tertiary amine, uns-dimethylhydrazine, Blausure (German) be Dominant response gas produces decomposition, combination reaction with titanium tetrachloride, hydrogen and nitrogen at a temperature of 700-900 DEG C, generates Ti (C.N) material；
(2) by TiO2Ti (C.N) material that powder, TiC powder, dextrine powder and above-mentioned steps (1) obtain mixes with distilled water, Ball milling 18h mix homogeneously, uses vacuum freeze drier to remove moisture removal, sieves and obtain mixed powder；
(3) gained mixed powder makes precast body through 3 D-printing molding, in an inert atmosphere 1450 DEG C of sintering 40min.
(4) quantitative aluminium ingot is placed on the precast body surface of sintering, and puts in corundum crucible, 1400 DEG C of insulations 85min, obtains Ti3AlC2Toughness reinforcing Ti2O3-Al2O3Composite.
Embodiment 3:
The invention provides a kind of superalloy 3D printing composite material, its formula is:
Titanium tetrachloride 48 parts, acetonitrile 14 parts, tertiary amine 29 parts, uns-dimethylhydrazine 9 parts, Blausure (German) 5 parts, hydrogen 3 parts, nitrogen 36 Part, TiO240 parts of powder, 15 parts of TiC powder, dextrine powder 24 parts.
Its preparation technology comprises the steps:
(1) use middle temperature chemical gaseous phase depositing process, with organic compound acetonitrile, tertiary amine, uns-dimethylhydrazine, Blausure (German) be Dominant response gas produces decomposition, combination reaction with titanium tetrachloride, hydrogen and nitrogen at a temperature of 900 DEG C, generates Ti (C.N) material Material；
(2) by TiO2Ti (C.N) material that powder, TiC powder, dextrine powder and above-mentioned steps (1) obtain mixes with distilled water, Ball milling 24h mix homogeneously, uses vacuum freeze drier to remove moisture removal, sieves and obtain mixed powder；
(3) gained mixed powder makes precast body through 3 D-printing molding, in an inert atmosphere 1500 DEG C of sintering 50min.
(4) quantitative aluminium ingot is placed on the precast body surface of sintering, and puts in corundum crucible, 1500 DEG C of insulations 100min, obtains Ti3AlC2Toughness reinforcing Ti2O3-Al2O3Composite.
In the above process, the precast body porosity of 3 D-printing molding is 55%, the precast body porosity after presintering Being 63%, the increase of porosity is that dextrin decomposition causes.In pyrolytic process, the dextrin in precast body resolves at 800 DEG C Carbon, and carbon in sintering process in 1400 DEG C TiO2It is reduced into Ti2O3。
Using process above closely size can prepare the parts of complicated shape, 3 D-printing precast body obtains after oozing Al Ti3AlC2Toughness reinforcing TiAl3—Al2O3Composite material component, cad model compares, and the face inner volume of 3 D-printing composite expands It is only 1.5%, is perpendicular to the volume contraction in direction in face and is only 3.2%.
Use Ti3AlC2Toughness reinforcing TiAl3—Al2O3The monolateral notched specimen of composite has carried out cracks can spread behavioral study, Result shows, this composite material exhibits goes out significant R-curve behavior.Ti3AlC2Nanometer laminated structure reduce crack tip Stress, adds crack surfaces, serves crackle bridge joint and the effect of pinning, and this causes crack growth resistance along with the expansion of crackle Open up and increase.
3 D-printing technique has the advantage such as low cost, cycle short, easy operation.Use 3 D-printing molding and reaction melt Osmosis process combines, and not only can realize the nearly size manufacture of complicated form part, and can realize new ceramics base composite wood The component of material and microstructure design, thus can the ceramic matric composite of synchronization gain excellent performance and complicated form part thereof.
Based on above-mentioned, it is an advantage of the current invention that Ti prepared by the present invention3AlC2Toughness reinforcing Ti2O3-Al2O3Composite has Having the high-temperature oxidation resistance that density is low, hardness is high, anticorrosive, wear-resistant and good, this technique solves 3DP part hole Rate is more causes the relatively low problem of the intensity of 3DP parts, not only can guarantee that raising density of material but also do not change materials microstructure and Member profile structure, the line of material shrinkage factor after sintering has declined.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.

Claims (2)

1. a superalloy 3D printing composite material preparation method, it is characterised in that use following formula:
Titanium tetrachloride 40-48 part, acetonitrile 12-14 part, tertiary amine 24-29 part, uns-dimethylhydrazine 4-9 part, Blausure (German) 1-5 part, hydrogen 1-3 part, nitrogen 30-36 part, TiO2Powder 30-40 part, TiC powder 10-15 part, dextrine powder 20-24 part.
A kind of superalloy 3D printing composite material preparation method the most according to claim 1, it is characterised in that use such as Lower technique:
(1) use middle temperature chemical gaseous phase depositing process, be main with organic compound acetonitrile, tertiary amine, uns-dimethylhydrazine, Blausure (German) Reacting gas produces decomposition, combination reaction with titanium tetrachloride, hydrogen and nitrogen at a temperature of 700-900 DEG C, generates Ti (C.N) material Material；
(2) by TiO2Ti (C.N) material that powder, TiC powder, dextrine powder and above-mentioned steps (1) obtain mixes with distilled water, ball milling 10-24h mix homogeneously, uses vacuum freeze drier to remove moisture removal, sieves and obtain mixed powder；
(3) gained mixed powder makes precast body through 3 D-printing molding, in an inert atmosphere 1400-1500 DEG C of sintering 30- 50min；
(4) quantitative aluminium ingot is placed on the precast body surface of sintering, and puts in corundum crucible, 1300-1500 DEG C of insulation 70-100min, obtains Ti3AlC2Toughness reinforcing Ti2O3-Al2O3Composite.
CN201610701879.1A 2016-08-22 2016-08-22 Preparation method of super alloy 3D printing composite Pending CN106316385A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019140972A1 (en) * 2018-01-17 2019-07-25 华南理工大学 Gas-liquid chemical reaction deposition-based 3d printer and operating method thereof
CN112126772A (en) * 2020-02-17 2020-12-25 中冶长天国际工程有限责任公司 Iron-containing mixture for 3D printing sintering and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101037730A (en) * 2007-01-12 2007-09-19 西北工业大学 Preparation method of Titanium Trialuminum radical composite material
CN102965639A (en) * 2011-08-29 2013-03-13 钴碳化钨硬质合金公司 Cutting insert with a titanium oxycarbonitride coating and method for making the same

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101037730A (en) * 2007-01-12 2007-09-19 西北工业大学 Preparation method of Titanium Trialuminum radical composite material
CN102965639A (en) * 2011-08-29 2013-03-13 钴碳化钨硬质合金公司 Cutting insert with a titanium oxycarbonitride coating and method for making the same

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
TOSHIFUMI SUGAMA ET AL.: "CVD-titanium carbonitride coatings as corrosion-preventing barriers for steel in acid-brine steam at 200℃", 《MATERIALS LETTERS》 *
XIAOWEI YIN ET AL.: "Three-Dimensional Printing of Nanolaminated Ti3AlC2 Toughened TiAl3–Al2O3 Composites", 《J. AM. CERAM. SOC.》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019140972A1 (en) * 2018-01-17 2019-07-25 华南理工大学 Gas-liquid chemical reaction deposition-based 3d printer and operating method thereof
CN112126772A (en) * 2020-02-17 2020-12-25 中冶长天国际工程有限责任公司 Iron-containing mixture for 3D printing sintering and preparation method and application thereof

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Application publication date: 20170111