CN115710118A - Tape casting gradient functional material and preparation method thereof - Google Patents
Tape casting gradient functional material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a tape casting gradient functional material and a preparation method thereof, wherein the preparation method comprises the following steps: s1, preparing various slurries according to a system of gradient functional materials, and performing vacuum defoaming on the prepared slurries; s2, setting flow periodic functions of a plurality of slurries along with time change according to the component gradient and the casting speed of the prepared material, controlling the flow rate of the slurries to flow into a mixer through a flow controller for mixing, and then enabling the slurries to enter a casting machine material box through the mixer; s3, a casting machine works, in the casting process, a casting sheet produced in one flow change period corresponds to one sample, and the casting sheet is marked every period; and S4, stacking the prepared casting sheets in each period in sequence according to the marks, pressing and molding, and sintering to obtain the gradient functional material. The invention provides a brand-new preparation method of a gradient functional material, which can carry out continuous production on one tape casting production line by preparing various slurries and adjusting the flow of each slurry, thereby improving the production efficiency.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a tape casting gradient functional material and a preparation method thereof.
Background
The functional gradient material is a novel composite material, compared with the traditional composite material, the composition and the physical properties of the functional gradient material are continuously changed, the residual stress and the thermal stress caused by the macroscopic interface of the two materials can be avoided, the advantages of the composite material are fully exerted, and the functional gradient material has wide application prospects in the aspects of aerospace, material connection, functional devices and the like.
The preparation method of the functional gradient material mainly comprises a powder metallurgy method, a vapor deposition method, a self-propagating reaction synthesis method, plasma spraying, an electroforming method, an electroplating method, tape casting and the like. Compared with other processes, the casting method has the advantages of simple process, low cost, micron-order single-layer thickness and smooth transition layer change, but the functional gradient material prepared by the conventional casting method still has defects. For example, the method for preparing the W-Cu system gradient composite material by the tape casting method disclosed in patent CN103317140a needs to be realized by tape casting sheets with different components, and needs to prepare slurries with multiple components for tape casting. During production, each component needs to occupy one set of cast sheet production line, and equipment cost is greatly increased. And if the casting sheets with a plurality of components are prepared in sequence, continuous production cannot be realized, and the production efficiency is greatly reduced. Multi-component cast sheet lamination also presents a problem of continuity of gradient change. Although the tape casting method can realize one layer of one component theoretically, the method usually only adopts 3-5 components to prepare the gradient material after comprehensively considering the equipment and time cost, and the advantage that the components can be changed nearly continuously is difficult to exert.
In order to solve the problem, patent CN101503297a (tape casting preparation method of gradient material in rotating magnetic field) proposes to use the difference of magnetic properties between ferromagnetic substance and weak magnetic substance to form component gradient in the tape casting process. Patent CN105039830a (tape casting preparation method of metal/ceramic gradient material in alternating magnetic field) proposes that the metal/ceramic gradient material in alternating magnetic field is prepared by controlling the movement of metal particles with alternating magnetic field. However, the two methods have requirements on the physical properties of the material, and CN101503297a requires that one of the prepared composite materials has ferromagnetism and the other one is weak magnetism; CN105039830a requires one material to be metallic and the other non-metallic. This limits the range of applications of both methods.
Disclosure of Invention
In view of the defects of the prior art, the main object of the present invention is to provide a method for preparing a near-continuous variable functionally gradient material, which is not limited by material properties and is suitable for mass production.
The invention provides a preparation method of a tape casting gradient functional material on one hand, which comprises the following steps:
s1, preparing various slurries according to a system of gradient functional materials, and performing vacuum defoaming on the prepared slurries;
s2, setting flow periodic functions of a plurality of slurries along with time change according to the component gradient and the casting speed of the prepared material, controlling the flow rate of the slurries through a flow controller, enabling the slurries to flow into a mixer for mixing, and enabling the slurries to enter a material box of the casting machine through the mixer;
s3, a casting machine works, in the casting process, a casting sheet produced in one flow change period corresponds to one sample, and each period is marked on the casting sheet;
and S4, stacking the prepared casting sheets in each period in sequence according to the marks, and performing compression molding and sintering to obtain the gradient functional material.
Compared with the prior art, the invention provides a brand-new method for preparing the gradient functional complex phase material by adopting the tape casting process, continuous production can be carried out on one tape casting production line by preparing a plurality of slurries and adjusting the flow of each slurry, the machine does not need to be stopped for replacing materials, the requirements on the physical properties of a material system, such as electricity, magnetism and the like, are avoided, the production efficiency is greatly improved, the waste is reduced, and the method is particularly suitable for the production of medium and small-batch products.
In a preferred or alternative embodiment, in the step S2, the sum of the flow rate periodic functions of the slurries is a fixed value, so as to ensure that the casting speed and the thickness of the cast sheet are unchanged in a period, and the casting machine works normally.
In a preferred or alternative embodiment, in step S2, the flow rate periodic function of each slurry is a univariate function, and the independent variable is time t. Therefore, the periodic function has only one independent variable, the flow rate of the slurry is controllable, and the material components are controlled as required.
In a preferred or alternative embodiment, in the step S2, the flow rate periodic function of each slurry is one or more of a linear function, a quadratic function, a multiple function, an exponential function, a power function, a trigonometric function, or a logarithmic function. Therefore, the multiphase functional material with any gradient can be prepared according to the requirement, the component gradient of the material is approximately and continuously changed, and no obvious component step exists.
In a preferred or alternative embodiment, the time of one cycle is T = LH/vh, where L is the target product side length, H is the target product thickness, v is the casting speed, and H is the cast sheet thickness. Therefore, the cycle time is set according to the target product, and the stable work of the casting machine is ensured.
In a preferred or alternative embodiment, in step S1, only n +1 slurries need to be prepared for materials having n independent compositional variables, thereby greatly reducing the amount of slurry preparation work.
In a preferred or alternative embodiment, the multiple slurries are mutually soluble in step S1. Therefore, the mixed slurry is prevented from precipitation, solidification, layering and the like, and the failure of the slurry is avoided.
In a preferred or alternative embodiment, the solvents and excipients used in the plurality of slurries are the same. Therefore, the good intersolubility of the slurry is ensured.
In a preferred or alternative embodiment, in step S2, the mixer used is selected from one or a combination of several of the following: SV type static mixer, SK type static mixer, SX type static mixer, SH type static mixer, SL type static mixer, mixing pump, supercritical mixer, stirring mixer. Therefore, the proper mixer can be selected according to the characteristics of the slurry, and the uniform mixing is ensured.
The invention also provides a tape casting gradient functional material prepared by the preparation method. The component gradient of the gradient functional material of the invention is approximately continuously changed, no obvious component step exists, and the material performance is excellent.
Drawings
FIG. 1 is a flow chart of a method for preparing a gradient functional material by tape casting according to an embodiment of the present invention;
FIG. 2 is a schematic view showing the flow rate cycle change of each slurry in example 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. It should be noted that the following examples are only used to illustrate the implementation method and typical parameters of the present invention, and are not used to limit the scope of the parameters of the present invention, so that reasonable variations can be made and still fall within the protection scope of the claims of the present invention.
It is noted that the endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and that such ranges or values are understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The embodiment of the invention discloses a tape-casting gradient functional material and a preparation method thereof, and as shown in figure 1, the method comprises the following steps:
s1, preparing various slurries according to a system of gradient functional materials, and carrying out vacuum defoaming on the prepared slurries. For materials with n independent compositional variables, n +1 slurries are prepared, one containing no compositional variables and each of the remaining slurries containing a maximum of one compositional variable, e.g., a two-component material AB, with 1 independent compositional variable B, two slurries can be prepared 100 a, 100B, and if the B content is less, an AB mixed slurry can also be prepared instead of 100B, e.g., 80 a 20B, based on the B content satisfying the desired maximum content. The method needs a small amount of prepared slurry, and greatly reduces the workload of slurry preparation.
Furthermore, multiple slurries can be mutually soluble, so that the mixed slurries are prevented from precipitation, solidification, layering and the like, and the failure of the slurries is avoided. In the preferred scheme, the solvents and auxiliary materials used by the multiple slurries are the same, so that good intersolubility among the slurries is ensured.
S2, setting flow periodic functions of a plurality of slurries along with time change according to the component gradient and the casting speed of the prepared material, controlling the flow of the slurries through a flow controller, enabling the slurries to flow into a mixer for mixing, and enabling the slurries to enter a casting machine material box through the mixer.
Further, the flow rate periodic function of each slurry is a unitary function f 1 (t)、f 2 (t)…f n+1 And (t) the independent variable is time t, so that the slurry components are gradually changed according to the requirement. And the sum of all slurry flows is a fixed value, so that the casting speed and the thickness of the casting sheet are ensured to be unchanged in a period, and the casting machine works normally. The form of the flow rate periodic function can be adjusted according to the system of the gradient functional material, such as a primary function, a secondary function, a multiple function, an exponential function, a power function, a trigonometric function, a logarithmic function or a combination of the functions, and the gradient functional material prepared by using the flow rate periodic functions in different formsThe change rule of the components is changed correspondingly.
The mixer used in this step is not particularly limited, and an appropriate mixer may be selected according to the characteristics of the slurry, such as an SV type static mixer, an SK type static mixer, an SX type static mixer, an SH type static mixer, an SL type static mixer, a mixing pump, a supercritical mixer, an agitation mixer, or the like, or the above-mentioned mixers may be used in combination to ensure uniform mixing of the slurry.
And S3, the casting machine works, in the casting process, a casting sheet produced in one flow change period corresponds to one sample, and the casting sheet is marked every period, so that the casting sheet is conveniently stacked and pressed for forming. The time of one period is T = LH/vh, wherein L is the side length of the target product, H is the thickness of the target product, v is the casting speed, and H is the thickness of the casting sheet.
And S4, stacking the prepared casting sheets in each period in sequence according to the marks, performing compression molding, determining a sintering process according to the characteristics of the sample, and performing corresponding sintering to obtain the gradient functional material.
The functional gradient material prepared by the method has the following advantages:
a) The slurry components can be gradually changed as required by adjusting the flow rate of the slurry entering the stirrer, the component gradient of a finished product is approximately continuously changed, no obvious component step is formed, and the material performance is excellent;
b) For materials with n independent component variables, only n +1 kinds of slurry are needed to be prepared, so that the workload of slurry preparation is greatly reduced;
c) The continuous casting production can be realized by using one casting device without stopping and changing materials, the production efficiency is greatly improved, the waste is reduced, and the continuous casting device is particularly suitable for the production of medium and small-batch products.
The present invention will be described in detail below by way of specific examples.
Example 1
In this example, an alumina/zirconia gradient functional material is prepared, the thickness of the material is 10 … mm, the side length is 100mm, and the components are calculated by mass fraction, and the material is changed from 100% alumina on one side to 80% alumina 20% zirconia on the other side.
The preparation method comprises the following steps:
s1, preparing two slurries by using alumina powder and zirconia powder as raw material powder, wherein the slurry 1 contains 100 parts of alumina powder, and the slurry 2 contains 80 parts of alumina powder and 20 parts of zirconia powder; the other auxiliary agents of the two slurries are the same, and specifically comprise: 10 parts of polyvinyl butyral serving as a binder, 4 parts of polyethylene glycol serving as a plasticizer, 2 parts of herring oil serving as a dispersant, 100 parts of absolute ethyl alcohol serving as a solvent and 100 parts of butanone serving as a solvent. Mixing the raw materials, and performing ball milling for 48 hours to obtain slurry 1 and slurry 2; and placing the prepared slurry 1 and the prepared slurry 2 in respective defoaming barrels for vacuum defoaming.
S2, the discharging width of a casting machine is 200mm, the casting speed is 1m/min, the thickness of a casting sheet is 0.1mm, the total flow is 100mL/min, and the flow change period T is 10min. The slurry flows into the stirring mixer to be mixed by controlling the flow rate through the flow controller, and then enters the casting machine material box through the mixer. The flow rates of the two slurries in one period are linearly changed, and the flow rate periodic function of the slurry 1 is f 1 (t) =10t, t epsilon [0,10), and the flow rate periodic function of slurry 2 is f 2 (t) =100 to 10t, t ∈ [1,10), and the change in the ratio of the flow rates of slurry 1 and slurry 2 to the total flow rate in one cycle is shown in fig. 2.
And S3, setting the flow change period T to be 10min, working the casting machine, wherein in the casting process, the casting sheet in one period corresponds to one sample, and marking the casting sheet every other period.
S4, sequentially cutting the casting sheets in each period, laminating, and performing compression molding under the pressure of 30 MPa; heating to 1600 ℃ in air atmosphere, sintering, and preserving heat for 2 hours to obtain the alumina/zirconia gradient functional ceramic block.
Example 2
In the preparation of the tungsten-copper gradient functional material, the thickness of the material is 20mm, the side length is 50mm, and the composition is calculated by mass fraction, wherein 100% of tungsten on one surface is transited to 50% of tungsten and 50% of copper on the other surface.
The preparation method comprises the following steps:
s1, selecting tungsten powder and copper powder as raw material powder, and preparing two slurries, wherein the slurry 1 contains 100 parts of tungsten powder and the slurry 2 contains 100 parts of copper powder; the other auxiliary agents of the two slurries are the same, and specifically comprise: 10 parts of hydroxyethyl cellulose as a binder, 4 parts of dibutyl phthalate as a plasticizer, 2 parts of octylphenol polyoxyethylene ether as a dispersing agent, 100 parts of methyl ethyl ketone as a solvent and 100 parts of trichloroethylene as a solvent. Mixing the raw materials, and performing ball milling for 48 hours to obtain slurry 1 and slurry 2; and respectively placing the prepared slurry 1 and the prepared slurry 2 into respective defoaming barrels for vacuum defoaming.
S2, the discharging width of a casting machine is 100mm, the casting speed is 1m/min, the thickness of a casting sheet is 0.2mm, the total flow is 100mL/min, and the flow change period T is 5min. The slurry flows into the static mixer to be mixed by controlling the flow rate through the flow controller, and then enters the casting machine material box through the mixer. The flow rate of the two slurries in one period is constant, and the flow rate periodic function of the slurry 1 and the slurry 2 is a quadratic function.
And S3, setting the flow change period T to be 5min, working the casting machine, wherein in the casting process, the casting sheet in one period corresponds to one sample, and marking is carried out on the casting sheet every other period.
S4, sequentially cutting and laminating the casting sheets in each period, and performing compression molding under the pressure of 100 MPa; heating to 1200 ℃ in hydrogen atmosphere, sintering, and preserving heat for 3 hours to obtain the tungsten-copper gradient functional material.
Example 3
In the preparation of the aluminum/silicon carbide gradient functional material, the thickness of the material is 50mm, the side length is 50mm, and the composition is calculated by mass fraction, and the transition is from 100% of metal aluminum on one surface to 30% of aluminum of 70% of silicon carbide on the other surface.
The preparation method comprises the following steps:
s1, selecting aluminum powder and silicon carbide powder as raw material powder, and preparing two slurries, wherein the slurry 1 contains 100 parts of aluminum powder, and the slurry 2 contains 80 parts of silicon carbide powder and 20 parts of aluminum powder; the other auxiliary agents of the two slurries are the same, and specifically comprise the following components: 10 parts of polyvinyl alcohol serving as a binder, 4 parts of diethyl oxalate serving as a plasticizer, 2 parts of triolein serving as a dispersant, 100 parts of toluene serving as a solvent and 100 parts of xylene serving as a solvent. Mixing the raw materials, and performing ball milling for 48 hours to obtain slurry 1 and slurry 2; and placing the prepared slurry 1 and the prepared slurry 2 in respective defoaming barrels for vacuum defoaming.
S2, the discharging width of a casting machine is 100mm, the casting speed is 1m/min, the thickness of a casting sheet is 0.5mm, the total flow is 200mL/min, and the flow change period T is 5min. The slurry flows into the static mixer to be mixed by controlling the flow rate through the flow controller, and then enters the casting machine material box through the mixer. The flow rate of the two slurries is constant in one period, and the flow rate periodic functions of the slurry 1 and the slurry 2 are sine functions.
And S3, setting the flow change period T to be 5min, working the casting machine, wherein in the casting process, the casting sheet in one period corresponds to one sample, and marking is carried out on the casting sheet every other period.
S4, sequentially cutting the casting sheets in each period, laminating, and performing compression molding under the pressure of 250 MPa; and (3) carrying out hot-pressing sintering at the sintering temperature of 600 ℃ under the sintering pressure of 45MPa, and preserving heat for 1 hour to obtain the aluminum/silicon carbide gradient functional material.
Example 4
In this example, a silicon carbide/boron nitride gradient functional material is prepared, the thickness of the material is 10mm, the side length is 60mm, and the composition is calculated by mass fraction, and the transition from 100% silicon carbide on one surface to 40% boron nitride of 60% silicon carbide on the other surface is carried out.
The preparation method comprises the following steps:
s1, selecting silicon carbide powder and boron nitride powder as raw material powder, and preparing two slurries, wherein the slurry 1 contains 100 parts of silicon carbide powder, and the slurry 2 contains 60 parts of silicon carbide powder and 40 parts of boron nitride powder; the other auxiliary agents of the two slurries are the same, and specifically comprise: 4 parts of aluminum oxide and yttrium oxide respectively serving as sintering aids, 10 parts of polyvinyl alcohol serving as a binder, 4 parts of polyethylene glycol serving as a plasticizer, … A … serving as a dispersant and deionized water serving as a solvent. Mixing the raw materials, and performing ball milling for 48 hours to obtain slurry 1 and slurry 2; and placing the prepared slurry 1 and the prepared slurry 2 in respective defoaming barrels for vacuum defoaming.
S2, the discharging width of a casting machine is 100mm, the casting speed is 1m/min, the thickness of a casting sheet is 0.2mm, the total flow is 100mL/min, and the flow change period T is 3min. The slurry flows into the static mixer to be mixed by controlling the flow rate through the flow controller, and then enters the casting machine material box through the mixer. The flow rates of the two slurries are constant in one period, and the flow rate periodic functions of the slurry 1 and the slurry 2 are linear functions.
And S3, setting the flow variation period T to be 3min, working the casting machine, wherein in the casting process, the casting sheet in one period corresponds to one sample, and marking is carried out on the casting sheet every other period.
S4, sequentially cutting the casting sheets in each period, laminating, and performing compression molding under the pressure of 50 MPa; and (3) carrying out hot-pressing sintering at the sintering temperature of 1800 ℃, under the sintering pressure of 50MPa and in the sintering atmosphere of argon, and carrying out heat preservation for 2 hours to obtain the silicon carbide/boron nitride gradient functional material.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A preparation method of a tape casting gradient functional material is characterized by comprising the following steps:
s1, preparing various slurries according to a system of gradient functional materials, and performing vacuum defoaming on the prepared slurries;
s2, setting flow periodic functions of a plurality of slurries along with time change according to the component gradient and the casting speed of the prepared material, controlling the flow of the slurries through a flow controller, enabling the slurries to flow into a mixer for mixing, and enabling the slurries to enter a material box of the casting machine through the mixer;
s3, the casting machine works, in the casting process, a casting sheet produced in one flow change period corresponds to one sample, and the casting sheet is marked every period;
and S4, stacking the prepared casting sheets in each period in sequence according to the marks, and performing compression molding and sintering to obtain the gradient functional material.
2. The method according to claim 1, wherein in step S2, the sum of the flow rate periodic functions of each slurry is a constant value.
3. The method of claim 1, wherein in step S2, the flow rate periodic function of each slurry is a unitary function, and the independent variable is time t.
4. The method for preparing a gradient functional material by tape casting according to any one of claims 1 to 3, wherein in the step S2, the flow rate periodic function of each slurry is one or more of a linear function, a quadratic function, a multi-step function, an exponential function, a power function, a trigonometric function, or a logarithmic function.
5. The method of claim 1, wherein the period of time is T = LH/vh, where L is the target product side length, H is the target product thickness, v is the casting speed, and H is the casting sheet thickness.
6. The method for preparing a gradient functional material by tape casting according to claim 1, wherein in the step S1, n +1 kinds of slurries are prepared for a material having n independent compositional variables.
7. The method for preparing a gradient functional material by tape casting according to claim 1, wherein in step S1, a plurality of slurries are mutually soluble.
8. The method of claim 6, wherein the plurality of slurries are prepared using the same solvent and the same excipient.
9. The method for preparing a gradient functional material by tape casting according to claim 1, wherein in the step S2, the mixer is selected from one or more of the following combinations: SV type static mixer, SK type static mixer, SX type static mixer, SH type static mixer, SL type static mixer, mixing pump, supercritical mixer, and stirring mixer.
10. A tape-cast gradient functional material, characterized by being produced by the production method as recited in any one of claims 1 to 9.
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| CN112194484A (en) * | 2020-09-17 | 2021-01-08 | 深圳陶陶科技有限公司 | Preparation method of gradient-color ceramic material |
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| JP2002292611A (en) * | 2001-03-30 | 2002-10-09 | Gifu Prefecture | Method for manufacturing gradient function material |
| CN101962803A (en) * | 2010-10-30 | 2011-02-02 | 北京大学 | Heteroepitaxial growth method for high-quality monocrystalline thick-film material |
| CN103317140A (en) * | 2013-06-25 | 2013-09-25 | 武汉理工大学 | Method for manufacturing gradient composite of W-Cu system by aid of tape casting process |
| US20160291610A1 (en) * | 2015-04-06 | 2016-10-06 | Horiba Stec, Co., Ltd. | Flow rate ratio control apparatus and program for flow rate ratio control apparatus |
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