CN115138826A - Near-zero expansion Al-ZrW 2 O 8 Method for preparing composite material - Google Patents
Near-zero expansion Al-ZrW 2 O 8 Method for preparing composite material Download PDFInfo
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- CN115138826A CN115138826A CN202110339364.2A CN202110339364A CN115138826A CN 115138826 A CN115138826 A CN 115138826A CN 202110339364 A CN202110339364 A CN 202110339364A CN 115138826 A CN115138826 A CN 115138826A
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- B22D23/00—Casting processes not provided for in groups B22D1/00 - B22D21/00
- B22D23/04—Casting by dipping
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/001—Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material
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- 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
- B33Y10/00—Processes of additive manufacturing
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- 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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- 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
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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- 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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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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Abstract
Near-zero expansion Al-ZrW 2 O 8 The preparation method of the composite material comprises the steps of preparing ZrW by adopting a 3D ink-jet printing method 2 O 8 Micro-truss structure, zrW 2 O 8 The precursor of the micro-truss printing structure is ZrW with the granularity range of 10-500 mu m 2 O 8 The particles are prepared with water-based or organic-based solution to form stable rheological fluid; printed ZrW 2 O 8 Sintering the micro-truss in an air environment at 450-700 ℃ to obtain ZrW 2 O 8 The porosity of the framework structure is controlled to be 28-32%; then, zrW is infiltrated into the aluminum or aluminum alloy melt within the temperature range of 400-750 DEG C 2 O 8 Skeleton, obtaining ZrW 2 O 8 Al-ZrW of skeleton structure 2 O 8 The composite material has a thermal expansion coefficient of (-0.5) x 10 within the temperature range of-100 deg.C ‑6 K ‑1 。
Description
Technical Field
The invention relates to a preparation method of a low-expansion coefficient material in the field of precision instruments, in particular to Al-ZrW with a near-zero expansion coefficient in a wide temperature range 2 O 8 A method for preparing the material.
Background
The near-zero expansion material is an important requirement for supporting the structural dimensional stability, low environmental sensitivity and structural and functional stability under the conditions of cold and hot impact of a precision device, and is a key material in the fields of satellite communication, optical systems, electronic packaging, precision instruments, information safety and the like.
Invar is an Invar alloy having a temperature near room temperatureAlloys with very low coefficients of thermal expansion (about 1.5X 10) - 6 K -1 ) The method has mature and reliable manufacturing process, and is widely applied to scientific instruments such as length scales, geodetic baseline rulers, microwave technologies, liquid gas containers, resonant cavities, aerospace remote sensors, precise lasers, optical measurement systems, waveguide tube structural parts, astronomical telescope supporting systems, optical lenses and the like. However, invar exists in a dense state (density 8.1 g/cm) 3 ) The low expansion region has narrow temperature range (-20 ℃), low thermal conductivity (only 1/4-1/3 of the thermal conductivity coefficient of 45 steel), and is difficult to meet the development requirements of the fields of modern aerospace and optical communication.
ZrW 2 O 8 Zirconium tungstate is an isotropic negative expansion material, exhibits negative expansion effect within the temperature range of-270-770 ℃, and has negative expansion coefficient reaching-8.9 multiplied by 10 -6 K -1 The composite material matched with the aluminum alloy has the advantages of low density, high thermal conductivity and near-zero thermal expansion coefficient in a wider temperature range. However, al-ZrW has been prepared 2 O 8 The coefficient of thermal expansion of the material is often significantly larger than the theoretical calculation value obtained by matching two components, and the coefficient of thermal expansion close to zero cannot be obtained.
Al-ZrW prepared 2 O 8 The reason why the material cannot obtain a near-zero thermal expansion coefficient is that ZrW 2 O 8 Dispersed and granular distribution in the material, although the single particles can provide deformation space for the surrounding aluminum matrix and reduce the deformation of the whole material during the temperature change, the ZrW 2 O 8 The particles can not be coordinated with each other to play an integral constraint role, the aluminum alloy matrix can still deform to the surrounding 3D space without constraint, and the thermal expansion coefficient of the material is obviously greater than that of the material based on Al and ZrW 2 O 8 The thermal expansion coefficient of each of the two elements is calculated theoretically, and the thermal expansion coefficient value close to zero cannot be obtained.
If Al-ZrW can be changed 2 O 8 ZrW in material 2 O 8 Phase distribution of ZrW 2 O 8 The phase changes from a discrete distribution to a continuous skeletal distribution, thenCan make ZrW 2 O 8 Not only provides a reverse deformation space for the aluminum phase in the micro-scale, but also can play an integral constraint role in the macro-scale, so that the ZrW 2 O 8 The framework completely bears the internal stress of the aluminum alloy matrix due to temperature change and counteracts the deformation degree of the aluminum alloy matrix, and the reverse deformation of the Al alloy phase, the Al phase and the ZrW phase are restrained on the whole structure 2 O 8 The mutual cooperation of the two produces the thermal expansion coefficient equivalent to the theoretical calculated value, thereby accurately producing the Al-ZrW with the near-zero expansion coefficient by the component design 2 O 8 A composite material.
Disclosure of Invention
The invention aims to provide a ZrW-supported ceramic material 2 O 8 Al-ZrW with continuous framework structure 2 O 8 Method for preparing a composite material, thereby obtaining Al-ZrW 2 O 8 Realizes the integral structure that the aluminum alloy phase and the zirconium tungstate phase are mutually restricted in the microcosmic and macroscopical aspects in the material, and obtains Al-ZrW with the coefficient of thermal expansion close to zero in a wider temperature range 2 O 8 A composite material.
In order to achieve the above object, the technical principle of the present invention is as follows:
firstly, obtaining three-dimensional ZrW by adopting a 3D ink-jet printing method 2 O 8 A framework structure. ZrW for subsequent infiltration joining of aluminum alloys 2 O 8 Skeleton to obtain Al alloy phase and ZrW 2 O 8 Monolithic structures that are constrained to each other on both a macro and micro scale.
In order to achieve the purpose of the invention, the technical scheme of the invention is realized as follows:
a preparation method of a near-zero expansion Al-ZrW2O8 composite material comprises the following steps:
1. ZrW preparation by 3D ink-jet printing and sintering method 2 O 8 A framework structure.
(1) ZrW with the grain size range of 10-500 mu m is adopted 2 O 8 Particles, adding the particles into water-based and organic matter-based solutions to prepare ZrW 2 O 8 A particle suspension configured to form a stable rheology;
(2) Will contain ZrW 2 O 8 Loading the granules into 3D ink-jet printer cartridge as printing ink, setting computer program of structure to be printed, extruding the granules through needle under the control of program to form ZrW 2 O 8 A micro-truss 3D structure of particles and additives.
(3) Drying and sintering the micro-truss in an air environment at 450-700 ℃, removing additive components and obtaining ZrW 2 O 8 The porosity of the framework structure is controlled to be 28-32%.
2. Infiltrating ZrW into the aluminum or aluminum alloy melt at the temperature range of 400-750 DEG C 2 O 8 Skeleton, obtaining ZrW 2 O 8 Al-ZrW with skeleton structure 2 O 8 The composite material has a thermal expansion coefficient of (-0.5) x 10 within the temperature range of-100 deg.C -6 K -1 。
Detailed Description
The following examples are provided to explain embodiments of the present invention in detail.
Example one
The steps of this embodiment are:
1. ZrW preparation by 3D ink-jet printing and sintering method 2 O 8 A framework structure.
(1) Preparation of Water-based printing ink (ZrW) 2 O 8 Water-based suspension of particles), zrW 2 O 8 The particle size range of the particles is 100-150 μm: and (3) adding deionized water: polyethylene glycol (PEG-4000) solution =4, as a premix, a mixed solution of 1, 0.2% triethanolamine dispersant was added, and after mixing well, 20wt% ZrW was added 2 O 8 Granulating, stirring for 8 hours, adjusting the pH value of the solution to about 7 by using hydrochloric acid to obtain ZrW for ink-jet printing 2 O 8 A particulate ink.
(2) Printing ZrW 2 O 8 Micro-truss structure of particles: the resulting water-based liquid mixture (ink) was transferred to a syringe of a 3D ink-jet printer and extruded through a metal needle having an orifice diameter of 410 μm at a printing speed of 20mm · s under the control of a computer-programmed program -1 Printed as 30/60 degree alternately repeating microtrussThe macroscale of the structure, the micro-truss, is 200X 100mm, wherein the distance between the fibers in each layer is 1mm, and the distance between the two adjacent layers is 350 mu m. The apparent porosity of the micro-truss structure is about 60%.
(3) Preparation of ZrW 2 O 8 Framework: the printed precursor was dried in an air oven at 80 ℃ for 12 hours to remove residual solvent. Then sintering in air environment, wherein the sintering method comprises the steps of heating to 600 ℃ at a heating rate of 2 ℃/min, and keeping the temperature for 2 hours to prepare ZrW 2 O 8 The porosity of the framework is 28-30%.
2. Infiltration of aluminum alloy: sintering the ZrW 2 O 8 Placing the framework in a graphite die, placing 25% of magnesium and ZrW in a mass ratio above the framework 2 O 8 Al-Mg alloy with 10% more skeleton, and graphite paper surrounding graphite mould for adding ZrW 2 O 8 The framework and the aluminum magnesium alloy are isolated from the graphite die. Molding graphite and ZrW therein 2 O 8 Heating the skeleton and the aluminum-magnesium alloy to 580 ℃ in a vacuum environment in a vacuum heating furnace, preserving heat, then filling 0.5MPa of argon into the vacuum furnace, and infiltrating the aluminum-magnesium melt into ZrW under pressure 2 O 8 In the skeleton, al-ZrW with skeleton structure and near zero thermal expansion coefficient value is prepared 2 O 8 A composite material.
Example two
The steps of this embodiment are:
1. ZrW preparation by 3D ink-jet printing and sintering method 2 O 8 A framework structure.
(1) Preparation of printing ink (ZrW) 2 O 8 Organic mixture of particles): polystyrene (polymer binder): dichloromethane (solvent): dibutyl phthalate (plasticizer): ethylene glycol monobutyl ether (surfactant) was prepared as a 4:12:1:6 until the solid is completely dissolved, and then ZrW with the granularity range of 74-100 mu m is mixed and stood 2 O 8 The particles being added to a prepared organic liquid, zrW 2 O 8 The mass ratio of the particles to the organic liquid is 1:1.2, to ZrW 2 O 8 The mixture of powder and organic liquid was stirred for 3 hours to make a homogeneous mixture. Will be provided withThe resulting liquid mixture is heated in a water bath at 50 ℃ for 2-4 hours to continuously raise the viscosity of the liquid mixture until it is ready for printing.
(2) Printing ZrW 2 O 8 Micro-truss structure of particles: the resulting liquid mixture (ink) was transferred to a syringe of a 3D ink printer and extruded through a metal needle having a bore diameter of 300 μm at a printing speed of 15mm · s under the control of a computer-programmed program -1 And printing a 0/90-degree alternately repeated micro-truss structure, wherein the macro size of the micro-truss is 200 multiplied by 150mm, the distance between fibers in each layer is 0.8mm, and the distance between the upper layer and the lower layer is 200 mu m. The apparent porosity of the micro-truss structure is about 60%.
(3) Preparation of ZrW 2 O 8 Framework: and drying the printed precursor in an air furnace at 80 ℃ for 12 hours to remove residual solvent. Then sintering in air environment, wherein the sintering method comprises the steps of heating to 650 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 2 hours to prepare ZrW 2 O 8 The porosity of the framework is 29-31%.
2. Infiltration of aluminum alloy: zrW after sintering 2 O 8 The skeleton is put into a steel die, the steel die and ZrW therein 2 O 8 Heating the skeleton to 570-580 deg.C, keeping the temperature, casting aluminum-silicon melt containing 10wt% silicon at 590-610 deg.C into steel die, applying 50MPa mechanical pressure, and infiltrating ZrW into the aluminum-silicon melt under pressure 2 O 8 In the framework, al-ZrW with a framework structure and a near zero coefficient of thermal expansion in the temperature range of-100 ℃ is prepared 2 O 8 A composite material.
EXAMPLE III
1. ZrW preparation by 3D ink-jet printing and sintering method 2 O 8 A framework structure.
(1) Preparation of Water-based printing ink (ZrW) 2 O 8 Water-based suspension of particles), zrW 2 O 8 The particle size range of the particles is 150-200 μm: deionized water is adopted: polyethylene glycol (PEG-1000) solution =1 mixed solution as a premix, and after mixing uniformly, 15wt% ZrW was added 2 O 8 Granules, stirred for 8 hours, used for ink-jet printingContaining ZrW 2 O 8 A particulate ink.
(2) Printing ZrW 2 O 8 Micro-truss structure of particles: the resulting water-based liquid mixture (ink) was transferred to a syringe of a 3D ink-jet printer and extruded through a metal needle having an orifice diameter of 450 μm under the control of a computer-programmed program at a printing speed of 25mm · s -1 And printing into a micro-truss structure with alternately repeated spirals, wherein the macro size of the micro-truss is 300 multiplied by 200mm, the distance between fibers in each layer is 1mm, and the distance between two adjacent layers is 300 mu m. The apparent porosity of the micro-truss structure is about 60%.
(3) Preparation of ZrW 2 O 8 Framework: drying the printed precursor in an air furnace at 100 ℃ for 12 hours, and then sintering in an air environment, wherein the sintering method comprises the steps of heating to 620 ℃ at the heating rate of 2 ℃/min, and preserving heat for 3 hours to prepare ZrW 2 O 8 The porosity of the framework is 28-30%.
2. Infiltration of aluminum alloy: zrW after sintering 2 O 8 The skeleton is put into a steel die, the steel die and ZrW therein 2 O 8 Heating the framework to 550-560 ℃ for heat preservation, then casting pure aluminum melt with the temperature of 690-700 ℃ into a steel die, applying mechanical pressure of 60MPa, and infiltrating ZrW into the pure aluminum melt under pressure 2 O 8 In the skeleton, the prepared thermal expansion coefficient is (-0.5) x 10 within the temperature range of-100 DEG C -6 K -1 Al-ZrW of 2 O 8 A composite material with a skeleton structure.
Claims (5)
1. Near-zero expansion Al-ZrW 2 O 8 The preparation method of the composite material is characterized by comprising the following steps:
firstly, zrW is prepared by adopting a 3D ink-jet printing method 2 O 8 A micro-truss structure, sintering the micro-truss in air to obtain ZrW 2 O 8 A skeleton structure, wherein the porosity of the skeleton structure is controlled to be 28-32%; then infiltrating ZrW into the molten aluminum or aluminum alloy 2 O 8 Skeleton, obtaining ZrW 2 O 8 Al-ZrW with skeleton structure 2 O 8 Composite materialThe range of the thermal expansion coefficient of the composite material is (-0.5) multiplied by 10 -6 K -1 。
2. A near zero expansion Al-ZrW in accordance with claim 1 2 O 8 The preparation method of the composite material is characterized in that the preparation method of the 3D ink-jet printing ink is as follows: zrW with the grain size range of 10-500 mu m is adopted 2 O 8 Particles of ZrW 2 O 8 Adding the particles into a water-based or organic matter-based solution to prepare Al-ZrW 2 O 8 A suspension of particles configured to form a stable rheology.
3. A near zero expansion Al-ZrW in accordance with claim 1 2 O 8 The preparation method of the composite material is characterized in that the 3D ink-jet printing mode is as follows: will contain ZrW 2 O 8 Loading the granules into 3D ink-jet printer cartridge as printing ink, setting computer program of structure to be printed, extruding the granules through needle under the control of program to form ZrW 2 O 8 A 3D micro-truss structure of particles and additives.
4. A near zero expansion Al-ZrW in accordance with claim 1 2 O 8 The preparation method of the composite material is characterized in that the sintering mode is as follows: drying and sintering the micro-truss in an air environment at 450-700 ℃, removing additive components and obtaining ZrW 2 O 8 The porosity of the framework structure is controlled to be 28-32%.
5. A near zero expansion Al-ZrW in accordance with claim 1 2 O 8 The preparation method of the composite material is characterized in that the infiltration mode is as follows: infiltrating ZrW into pure aluminum or aluminum alloy melt at the temperature range of 400-750 DEG C 2 O 8 Skeleton, obtaining ZrW 2 O 8 Al-ZrW with skeleton structure 2 O 8 The composite material has a thermal expansion coefficient of (-0.5) x 10 in the temperature range of-100 deg.C -6 K -1 。
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2021
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Non-Patent Citations (1)
| Title |
|---|
| 黄兰萍;陈康华;: "近零膨胀ZrW_2O_8/A l6013复合材料的制备与性能", 金属热处理, no. 01, pages 20 - 22 * |
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